Aa 6200 [PDF]

Zitiervorschau

206-94788A

ATOMIC ABSORPTION SPECTROPHOTOMETER

AA-6200 (P/N 206-50000-36)

INSTRUCTION MANUAL

Read this instruction manual thoroughly before you use the product. Keep this instruction manual handy so that you can refer to it when necessary.

COPYRIGHT : •Copyright c Shimadzu Corporation 2000. All rights reserved. This publication may not be reproduced in whole or in part without written permission from Shimadzu Corporation. •Since Shimadzu products are frequently upgraded and improved, information in this publication is subject to change without notice. •The contents of this manual have been thoroughly inspected. Even if errors and omissions are found, however, we might not correct them immediately. •MS-DOS, Windows, Windows95, Windows98, and Windows NT are trademarks and trade names of Microsoft. Other product names described in this manual are each manufacturer's trademarks or registered trademarks.

Precautions for safe operation

The atomic absorption spectrophotometer is used as an analytical equipment for quantitative analysis. To operate this equipment safely, strictly observe the following precautions. If not observed, the safety may be compromised. (1) Do not use the equipment for any purpose other than the above-mentioned types of analysis. (2) Follow the procedures described in the instruction manual. (3) Observe all warnings and cautions. (4) Do not disassemble or modify the equipment without the express approval of an authorized Shimadzu Representative. (5) For internal repair of the equipment, contact your Shimadzu Representative. (6) The meshed descriptions about installation in this instruction manual are intended for Shimadzu service personnel. Don't use them and install the parts by yourself because it is dangerous.

Meaning of caution signs

WARNING

Warning indicates a potentially hazardous situation which, if not avoided, could result in death, serious injury or moderate injury.

CAUTION

Caution indicates a potentially hazardous situation which, if not avoided, may result in minor injury, or may result in machine damage.

NOTE

A Note is used to emphasize essential information.

AA-6200

General cautions

For safe operation of the AA-6200, strictly observe the following cautions. If not observed, the safety of the instrument may be compromised. (1) When pressing the ignition button (during ignition), never put your face or hands in the burner compartment (combustion chamber). Do not look down into the combustion chamber or hold your hands over the combustion chamber. When a N2O-C2H2 flame is ignited, the flame rises approximately 40cm from the top of the AA-6200. Proceed carefully around this flame. Before igniting, close the flame shield of the burner compartment. (2) Do not ignite unless the burner is mounted to the chamber. (3) Do not ignite unless the nebulizer is mounted to the chamber. (4) Do not ignite a flame unless the drain tank is filled with water. (5) Do not ignite when the U-tube is removed from the chamber. (6) Do not remove the nebulizer from the chamber during combustion. (7) Do not remove the U-tube from the chamber during combustion. (8) Do not remove the burner during combustion. (9) Never touch the burner while it is hot. (10) Never touch the deuterium lamp while it is hot. (11) Do not put any foreign objects into the hole of burner select sensor. (12) Do not use the standard burner (10cm slot burner) when the burner recognizing pin is still left in the hole of the burner select sensor. (13) Do not put fingers or hands in the hole of lamp turret, igniter, or flame monitor. (14) Do not put any foreign objects in the lamp socket. (15) Do not touch the end of the cleaning wire for the nebulizer capillary directly with your hand. The wire may prick your finger. (16) Do not remove the thermal shield plate while using the AA-6200. The flame heats the inside and the measurement may be unreliable if the shield is removed. (17) Check the gas flow rate setting before igniting the burner. (18) Do not touch the flame shield during ignition. It is very hot. (19) Do not touch the flame shield and burner directly by your hand for about one hour after extinguishment of the flame. It is very hot by the heat of the flame. (20) Do not hold any substance over the flame. (21) Do not use the flame for other purpose than analysis. (22) Do not connect the power cable to an ungrounded outlet.

AA-6200

Precautions on handling high pressure gas

(1) High pressure gas must be handled carefully. Observe all laws regarding the handling of high pressure gas. For example in Japan, you must obtain permission to store over 300m3 of gas. (2) Adhere to regulations and laws regarding the handling of high pressure gas as well as these precautions. Cautionary items in this manual should be read carefully. 1. Installation of gas cylinder (1) Install the gas cylinders outdoors away from direct sunlight. (2) Ensure that the gas cylinders become no hotter than 40˚C. Do not allow any flame within 2 meters of the gas cylinders. (3) Secure gas cylinders so they cannot drop or fall over. Always keep cylinders containing liquefied gas (acetylene, propane, nitrogen monoxide, etc.) in a vertical position and do not allow them to fall to a horizontal position. (4) Ensure that the connector used at the outlet side of the gas pressure regulator conforms to local regulations. 2. Acetylene gas (1) When using acetylene gas, use a pressure reduction valve especially for use with acetylene gas. Do not allow acetylene to flow through tubes, and do not use equipment made from copper, silver, mercury, or their alloys to prevent the formation of metal-acetylides. Decomposition of such compounds could result in a "decomposition explosion" resulting from a shock. (2) The acetylene gas cylinder contains solvents such as acetone. If the primary pressure drops below 0.5MPa, replace the cylinder with a new one in order to prevent the solvents from leaking. 3. Oxygen gas Do not use Oxygen gas. 4. Air Supply dry air. If air contains water vapor, the moisture may adhere to the inside of the gas regulator and prevent normal operation. Remove moisuture from the air with a trap between the air supplying source and the instrument.

AA-6200

Precautions on handling high pressure gas

5. After using gas After gas is used, be sure to close the main valve as well as the stop valve. 6. Pressure gauge Periodically inspect the pressure gauge to ensure that it is operating normally. 7. Pressure regulator (1) Use approved pressure regulators and connectors. For details, contact your Shimadzu Representative. (2) When installing a pressure regulator on a cylinder, be sure to remove any dust from the cylinder outlet. (3) Damaged or cracked screws for installing the pressure regulator may cause gas leakage. Do not install the pressure regulator forcibly, but replace with a new gas cylinder. (4) Use the pressure regulator that has the function to prevent freezing for nitrous oxide cylinder. If the regulator has no freezing-proof function, Evaporation of liquid nitrous oxide in the cylinder may freeze the regulator and the make the flow rate of nitrous oxide unstable. This situation may cause a flashback. 8. Cylinder opening/closing (1) Before opening the cylinder, ensure that the stop valve is closed. Turn the secondary pressure adjusting valve fully to the left, and open the cylinder using a special handle. Even if the main valve is too tight to open, do not hit the handle or main valve with a hammer or other object. (2) After the main valve is opened, apply soapy water to the pressure regulator connection to ensure no gas is leaking. Also check the connection at the main valve. (3) Completely open the main valve of the nitrous oxide gas cylinder. If it is not completely opened, the flow rate of the gas may fluctuate. (4) Be sure to rotate the main valve of the acetylene gas cylinder by 1 rotation or 1.5 rotations short of completely being closed. To prevent acetone from leaking from the cylinder, do not open the valve more than 1.5 rotations short of being completely closed. If the main valve is not sufficiently opened, a nitrous oxide acetylene flame (high temperature burner) may flashback due to insufficient acetylene when the flame switches from air - acetylene flame to nitrous oxide acetylene flame.

AA-6200

Precautions on Handling Hollow Cathode Lamp

Electrodes of some hollow cathode lamps contain harmful metal elements (As, Be, Hg, Se, etc.). Some electrode metals may ignite when touched with air or water (K, Li and Na). Read the precautions attached to the hollow cathode lamp thoroughly and handle the lamp very carefully for safety. 1. When disposing of the lamp If the hollow cathode lamp should be broken or its life is finished, dispose of the lamp separately from general garbage. When disposing of the hollow cathode lamp supplied from Shimadzu Co., select a method which will not influence the environmental pollution or human body, or ask a special disposal dealer. The material of hollow cathode lamp are as follows. • Metals(including electrode element) • Quartz glass • Plastic Some electrode contains harmful metal(Hg, As, etc.). 2. Specifications change The specifications of the hollow cathode lamp are subject to change for improvement without notice. In this case, set the lighting current referring to the precautions attached to the hollow cathode lamp.

AA-6200

Precautions on Handling Deuterium(D2) Lamp

When disposing of the lamp If the deuterium(D2) lamp should be broken or its life is finished, dispose of the lamp separately from general garbage. When disposing of the deuterium(D2) lamp supplied from Shimadzu Co., select a method which will not influence the environmental pollution or human body, or ask a special disposal dealer. The material of deuterium(D2) lamp are as follows. • Metals(Tungsten) • Quartz glass • Ceramic • Plastic

AA-6200

Handling Waste Liquid

Waste liquid discharged during measurement or pretreatment should be handled in different ways in accordance with the solute and solvent contained in that waste liquid. The way of handling waste liquid is different depending upon the country or region. Be sure to dispose of waste liquid according to the location of use.

Supply Period of Replacement Parts

Replacement parts are supplied by the Shimadzu Parts Center. The supply period of these parts is determined as below. As a general rule, ten (10) years after the discontinuation of the product. Note, however, that the availability of units or parts not manufactured by Shimadzu shall be determined by the relevant manufacturers. If Shimadzu should receive a notice of the discontinuation of the units or parts, the necessary quantity for the above period is immediately calculated and secured. However, such parts may cease to be available within ten years after the discontinuation of the product, depending on the situation of the relevant manufacturers or change of the necessary quantity.

AA-6200

Installation and operation

The atomic absorption spectrophotometer generally uses high pressure gas. Therefore, pay full attention to the installation site and handling. Read the following precautions and cautionary items throughout this manual carefully. 1. Ventilation Combustible high pressure gas used in the atomic absorption spectrophotometer is flammable. Be sure to ventilate the room. 2. Using fire When measuring flammable samples, special care must be taken to handling fire. A fire extinguisher should be placed in case of accident. 3. Exhaust duct Provide combustion gas exhaust ducts over the atomic absorption spectrophotometer burner. 4. Condensation Avoid using the unit where condensation may form. 5. Waste Disposal The user assumes responsibility for the proper collection and disposal of waste in accordance with local and federal regulations. 6. Power supply - AA-6200 main unit Voltage

220V, 230V AC

Allowable voltage range

±10%

Power capacity

300VA

Source frequency

50/60Hz

Connections

Grounded outlet

Fuse capacity

3.15A (250V) Type T (time lag)

7. High temperature burner When using a nitrous oxide - acetylene flame, be sure to use the high temperature burner head supplied as an optional accessory.

AA-6200

Installation and operation

8. Standard measurement conditions Standard measurement conditions provided in the unit are typical conditions. They vary depending on the temperature and humidity in the environment, the viscosity of the sample and the unit itself. Before measuring, change the gas flow rate and obtain optimum measurement conditions for the elements to be measured. 9. Internal repair and maintenance of the unit Since the ordinary maintenance can be performed without removing the main unit cover, do not remove the unit cover. Also, don't exchange the fuses. If the repair which requires to remove the cover is necessary, ask it for Shimadzu Representative. Before using any cleaning or decontamination methods not specifically recommended by the manufacturer, verify with the manufacturer that the equipment will not be damaged. 10. Gas supply hose Each time the unit is operated, the rubber hose should be checked for cracking or deterioration from chemicals adhering to the hose. If the hose is cracked or deteriorated, replace it with a new one. 11. Drain tube The U-tube connected to the chamber is not durable with petroleum (kerosene, naphtha, gasoline, etc). When measuring these samples, ask Shimadzu for information. Every time when using the instrument, check the U-tube and confirm there is no liquid leak from the U-tube. 12. Lightening surge from the power source line When a momentary large voltage change is given to the instrument from the power source during using the instrument, the communication with PC is disconnected because some function is stopped to protect the instrument. In this case, once turn off the power of the main unit then turn on the power again and connect it to the PC again. Then the preparation for restarting the measurement is ready. If the instrument does not work properly when powered on, contact your Shimadzu representative. 13. Cleaning the instrument When cleaning your instrument, wipe off the outer cover and other portions with a dry soft cloth. For details of cleaning method for component parts, refer to Chapter 6 “Maintenance”.

AA-6200

Warning labels indicated on the unit

Symbol

Meaning Alternating Current Protective conductor terminal Power on Power off

Table 1: Symbols on the Equipment

WARNING! EXTREMELY HOT/OPEN FLAME

Figure 1 : Hot Surface (1) Avoid Burns (2) Check for open flame through the flame shield window. (3) Allow the burner head and walls to cool before handling.

AA-6200

Warning labels indicated on the unit

WARNING! HAZARDOUS VOLTAGE

Figure 2 : Hazardous Voltage DO NOT touch the electrodes while the instrument is active.

WARNING! HOT SURFACE

Figure 3 : Hot Surface Allow the lamp to cool to room temperature before replacement.

AA-6200

Warning labels indicated on the unit

WARNING! EXPLOSION POTENTIAL

Figure 4 : Explosion Potential ! DO NOT use oxygen gas mixture.

WARNING! FLAMMABLE GAS BE SURE TO READ the part "Igniting and Extinguish the flame" in the instruction manual before ignition.

Warning label

Figure 5 : FLAMMABLE GAS

AA-6200

Emergency stop operation

If the unit is not operating properly, take the following emergency actions. Bofore operating the unit again, inspect it and contact Shimadzu service personnel if necessary. (1) Switch the power switch of the unit off. Even during measurement, the flame can be extinguished by turning the power switch off. (2) Switch all accessory unit power switches off. (3) Close the main valve of the piping that supplies acetylene gas, air, nitrous oxide gas. (4) Shut off power supply. If the power cable is screwed onto the distributor panel, switch the switch on the distributor panel off. If the power cable is connected to the plug, disconnect the power cable.

Figure 5 : Power switch and power cable

AA-6200

Inspection Procedure in Case of Flashback

Since the AA-6200 is equipped with the several safety systems that prevent a flashback, there is little possibility a flashback occurs. In case a flashback should occur, however, a service engineer from Shimadzu will perform fhe following inspection procedure. Never ignite the flame before the safety is confirmed as the result of the inspection. ③ Chamber cover

① Burner head

⑫ Gas tube

⑬ Quick-connect joint

⑮ O-rings

⑭ Burner head  fixing port

⑨ Ceramic ball ⑥ Retaining plate

⑤ O-ring ④ Safety bung

⑦ Fixing screw

⑧ Nebulizer ② Chamber fixing screw ⑪ O-ring

⑩ Mixer

⑯ U-tube

Figure 6 : Burnet Unit (1) Remove the burner head q. Note that the burner head is still hot just after the flame is extinguished. (2) Loosen the chamber fixing screw w and remove the chamber cover e. (3) If the safety bung r is released, check that the O-ring t of the safety bung is not cracked or deteriorated, then push the safety bung surely into the rear of the AA-6200

Inspection Procedure in Case of Flashback

chamber unit. Even if the safety bung is not released, push the safety bung and check that it is properly mounted to the chamber. After that, mount the chamber and chamber cover back to the original position then fix them with the screws. (4) Loosen the lock screw u on the nebulizer retaining plate y and then take out the nebulizer i. Check that the ceramic ball o in the spray assembly is not damaged. (5) Check that the mixer !0 in the chamber is not damaged. (6) Check that the O-ring !1 in the nebulizer is not cracked or deteriorated then mount the nebulizer back to the chamber. At this time, check that the nebulizer O-ring is not pressed out from the socket. (7) Fix the nebulizer firmly with the retaining plate. (8) Check that the gas tube !2 connected with the chamber is not damaged. (9) Insert the gas tube connected with the quick-connect joint !3 and check that it is not disconnected by pulling it. (10) Check that burner head slot is not clogged. If clogged, clean the burner head. (11) Check that the O-rings !5 of the burner head fixing port !4 are not cracked or deteriorated. Then mount the burner head to the port. (12) Check that the U-tube !6 is not damaged. Finally, pour water from the drain tank opening until the water overflows the outlet of the drain tank.

Moving or Transporting the AA-6200

To move or transport the installed AA-6200, contact our sales office or representative. If the AA-6200 is move or transported without the above contact, the warranty will not be applied to any failure.

Warning on Sample to Be Measure

Do not measure any explosive sample. Such measurement not only could cause a failure in or damage to the AA-6200, but also might endanger the user's safety. AA-6200

Table of Contents

1 Introduction 1.1 Overview of AA-6200 …………………………………………………………………1-1 1.2 Hardware Specifications ……………………………………………………………1-2 1.3 Software Specifiaions ………………………………………………………………1-3 1.3.1 Signal process ……………………………………………………………………1-4 1.4 Notes for when upgrading from the AA-6200 16 bit software ……………………1-5 2 Installation 2.1 Parts inspection ………………………………………………………………………2-1 2.2 Instrument placement and site requirements ………………………………………2-2 2.2.1 Power requirments ………………………………………………………………2-4 2.2.2 Gas requrements …………………………………………………………………2-4 2.2.3 Ventilation system …………………………………………………………………2-7 2.2.4 Use of an air compressor …………………………………………………………2-8 2.2.5 General precautions for handling gas cylinders ………………………………2-9 2.2.6 Installing pressure regulators (optional) and checking for leaks ……………2-10 2.2.7 Software operation requirements (provided by user) ………………………2-12 2.2.7.1 PC Specifications ……………………………………………………………2-12 2.2.7.2 Operating System ……………………………………………………………2-12 2.2.7.3 Connection cable ……………………………………………………………2-12 2.2.8 Connecting the Drain Tube ……………………………………………………2-13 2.2.9 Assembling the burner unit ……………………………………………………2-14 2.2.10 Cable connections ………………………………………………………………2-15 2.2.11 Hose connections ………………………………………………………………2-17 2.3 Installing the PC software …………………………………………………………2-18 3 Instrument configuration 3.1 AA-6200 configuration ………………………………………………………………3-1 3.1.1 Spectrophotometer main unit ……………………………………………………3-1 3.1.2 Hollow cathode lamp turret………………………………………………………3-3 3.1.3 Deuterium lamp……………………………………………………………………3-4 3.1.4 Burner and burner module ………………………………………………………3-5 3.1.5 Optical system ……………………………………………………………………3-8 3.1.6 Photometric System ………………………………………………………………3-9

AA-6200

Table of Contents

4 Basic Operation 4.1 Switching On the Power and Starting the Software ………………………………4-1 4.1.1 Switching the instrument power supply on and off ……………………………4-1 4.1.2 Starting Up the Software …………………………………………………………4-2 4.2 Software Basic Operation ……………………………………………………………4-3 4.2.1 Software Basic Operation ………………………………………………………4-3 4.2.1.1 Operation Flowchart …………………………………………………………4-3 4.2.1.2 Wizard Selection ………………………………………………………………4-4 4.2.1.3 Element Selection ……………………………………………………………4-4 4.2.1.4 Preparation Parameters ………………………………………………………4-6 4.2.1.5 Sample ID ……………………………………………………………………4-10 4.2.1.6 Sample Selection ……………………………………………………………4-11 4.2.1.7 Connect to Instrument/Send Parameters …………………………………4-12 4.2.1.8 Optics Parameters for Lamp Position Adjustment ………………………4-13 4.2.1.9 Lamp Position Adjustment …………………………………………………4-16 4.2.1.10 Optics Parameters……………………………………………………………4-17 4.2.1.11 Gas Flow Rate Setup…………………………………………………………4-19 4.2.2 Saving the Template ……………………………………………………………4-20 4.3 Measurement Procedures …………………………………………………………4-22 4.3.1 Measurement Operation…………………………………………………………4-22 4.4 Saving/Printing/Deleting the Data …………………………………………………4-26 4.4.1 Saving the Data …………………………………………………………………4-26 4.4.2 Printing the Data …………………………………………………………………4-26 4.4.3 Deleting the Data…………………………………………………………………4-26 4.5 Completing the Measurement ………………………………………………………4-27 4.6 Explanation of Main Window ………………………………………………………4-28 4.6.1 Menu bar …………………………………………………………………………4-29 4.6.2 Standard tool bar…………………………………………………………………4-29 4.6.3 Measurement element tool bar …………………………………………………4-29 4.6.4 Absorbance digital display………………………………………………………4-29 4.6.5 Real time graph …………………………………………………………………4-29 4.6.6 Peak Profile (Latest four measurements and overlay display) ………………4-31 4.6.7 Calibration Curve Display ………………………………………………………4-33 4.6.8 MRT work sheet …………………………………………………………………4-36 4.6.9 Function buttons …………………………………………………………………4-37 4.6.10 Status bar …………………………………………………………………………4-38

AA-6200

Table of Contents

4.7 Operating the MRT work sheet ……………………………………………………4-39 4.7.1 Fields of MRT work sheet ………………………………………………………4-39 4.7.2 Right Mouse Button Menu ………………………………………………………4-45 4.7.3 Right Mouse Button on Summary Table ………………………………………4-48 4.7.4 Inserting and Deleting the Measurement Row ………………………………4-48 4.7.5 Active Cell Movement by Shortcut Key and Cell Selection …………………4-49 4.7.5.1 Moving an Active Cell ………………………………………………………4-49 4.7.5.2 Selecting Cells ………………………………………………………………4-50 4.7.6 Copy and Paste …………………………………………………………………4-50 4.7.6.1 Copy …………………………………………………………………………4-50 4.7.6.2 Paste …………………………………………………………………………4-51 4.7.7 Changing Column Width and Column Header Height of MRT Worksheet …4-51 4.8 Igniting and extinguishing the flame ………………………………………………4-53 4.8.1 Control locations…………………………………………………………………4-53 4.8.2 Safety Precautions Prior to Ignition ……………………………………………4-53 4.8.3 Igniting and extinguishing an Air-C2H2 flame …………………………………4-54 4.8.4 Igniting and extinguishing N2O-C2H2 flame ……………………………………4-56 4.8.5 Flame conditions when analyzing organic solvent samples …………………4-59 4.8.6 Changing the chamber position…………………………………………………4-60 4.9 Standard Addition Method and Simple Standard Addition Method ……………4-61 4.9.1 Overview …………………………………………………………………………4-61 4.9.2 Setting the measurement procedure for simple standard addition method …4-62 4.9.3 Setting the measurement procedure for standard addition method ………4-64 4.10 Conditions and Operation for Flame Emission Analysis …………………………4-67 4.10.1 "Optics Parameters" Page ………………………………………………………4-67 4.10.2 "Gas Flow Rate Setup" Page ……………………………………………………4-68 4.10.3 Line Search and Beam Balance …………………………………………………4-70 5 Menu Commands 5.1 Wizard Selection dialog box …………………………………………………………5-1 5.1.1 "Wizard" page ………………………………………………………………………5-1 5.1.2 "Recent Files" page ………………………………………………………………5-2 5.1.3 "Recent Templates" page …………………………………………………………5-2 5.2 [File] ……………………………………………………………………………………5-3 5.2.1 [New] ………………………………………………………………………………5-4 5.2.2 [Open] ………………………………………………………………………………5-4

AA-6200

Table of Contents

5.2.3 [Save] ………………………………………………………………………………5-4 5.2.4 [Save As...] …………………………………………………………………………5-5 5.2.5 [Additional Load] …………………………………………………………………5-6 5.2.6 [File Export...] ……………………………………………………………………5-7 5.2.7 [Export Items] ……………………………………………………………………5-8 5.2.8 [Auto Save]…………………………………………………………………………5-9 5.2.8.1 Saving the backup file automatically ………………………………………5-9 5.2.8.2 Exporting the MRT work sheet data automatically in text file …………5-10 5.2.8.3 Executing a program by command line ……………………………………5-12 5.2.9 [Print Data/Parameters...] ………………………………………………………5-14 5.2.10 [Print Table Data...] ………………………………………………………………5-14 5.2.11 [Print Style] ………………………………………………………………………5-15 5.2.11.1 "Print Style Setup" page ……………………………………………………5-15 5.2.11.2 "Table Show/Hide" page ……………………………………………………5-16 5.2.11.3 "Font" page ……………………………………………………………………5-16 5.2.12 [Print Setup]………………………………………………………………………5-17 5.2.13 Recent Files ………………………………………………………………………5-17 5.2.14 [Exit] ………………………………………………………………………………5-17 5.3 [Edit] ……………………………………………………………………………………5-18 5.3.1 [Insert Row] ………………………………………………………………………5-18 5.3.2 [Delete Rows] ……………………………………………………………………5-18 5.3.3 [Import Other Schedule] ………………………………………………………5-18 5.3.4 [Collective Edit] …………………………………………………………………5-19 5.3.5 [Remeasure Selected Range] ……………………………………………………5-20 5.3.6 [Clear Measurement Result] ……………………………………………………5-20 5.3.7 [Copy] ……………………………………………………………………………5-20 5.3.8 [Paste] ……………………………………………………………………………5-20 5.4 [Refer to Parameters] ………………………………………………………………5-21 5.5 [Parameters] …………………………………………………………………………5-22 5.5.1 "Element Selection" Page ………………………………………………………5-24 5.5.1.1 "Cookbook" page ……………………………………………………………5-25 5.5.1.2 "Template" page ………………………………………………………………5-26 5.5.2 "Preparation Parameters" Page …………………………………………………5-27 5.5.2.1 Weight Correction Factors …………………………………………………5-28 5.5.2.2 [Preparation Parameters]-[STD Samples] …………………………………5-29 5.5.2.3 [Preparation Parameters]-[Blank Samples] ………………………………5-30

AA-6200

Table of Contents

5.5.3 "Sample ID" Page…………………………………………………………………5-30 5.5.4 "Sample Selection" Page…………………………………………………………5-31 5.5.5 "Connect to Instrument/Send Parameters" Page………………………………5-32 5.5.6 "Optics Parameters" Page ………………………………………………………5-33 5.5.6.1 Button ……………………………………………………5-36 5.5.6.2 Button ………………………………………………………5-37 5.5.6.3 Button ……………………………………………5-38 5.5.7 "Lamp Position Adjustment" Page………………………………………………5-40 5.5.8 "Gas Flow Rate Setup" Page ……………………………………………………5-41 5.6 [Edit Parameters] ……………………………………………………………………5-43 5.6.1 "Measurement Parameters" Page ………………………………………………5-44 5.6.2 "Repeat Measurement Conditions" Page ………………………………………5-47 5.6.3 "Weight Correction Factors" Page………………………………………………5-49 5.6.4 "Y-axis Print Range" Page ………………………………………………………5-50 5.6.5 "Analyst" Page ……………………………………………………………………5-50 5.6.6 "Comment" Page …………………………………………………………………5-50 5.6.7 "Sequence" Page …………………………………………………………………5-51 5.6.8 "QA/QC Setup" Page ……………………………………………………………5-52 5.6.9 "Calibration Curve Parameters" Page …………………………………………5-54 5.6.10 "Optics Parameters" Page ………………………………………………………5-55 5.6.11 "Gas Flow Rate Setup" Page ……………………………………………………5-55 5.7 [Default Parameters]…………………………………………………………………5-56 5.7.1 [Flame] ……………………………………………………………………………5-56 5.7.2 [Furnace] …………………………………………………………………………5-56 5.7.3 [Graph] ……………………………………………………………………………5-56 5.7.4 [Analyst] …………………………………………………………………………5-56 5.8 [Instrument] …………………………………………………………………………5-57 5.8.1 [Connect] …………………………………………………………………………5-58 5.8.2 [Option Connect]…………………………………………………………………5-60 5.8.3 [Configuration] …………………………………………………………………5-60 5.8.4 [Lamp Position Setup] …………………………………………………………5-64 5.8.4.1 When not using the lamp position setup function ………………………5-66 5.8.4.2 When using the lamp position setup function ……………………………5-66 5.8.5 [Lamp History]……………………………………………………………………5-68 5.8.5.1 When is a use of "Lamp History" dialog box necessary? …………………5-68 5.8.5.2 How to use the "Lamp History" dialog box ………………………………5-69

AA-6200

Table of Contents

5.8.5.3 Displaying a message when the lamp used time exceeds the lamp life …5-72 5.8.6 [Maintenance] ……………………………………………………………………5-73 5.8.6.1 [D2 Lamp Position] ……………………………………………………………5-73 5.8.6.2 [Wavelength Adjustment] ……………………………………………………5-74 5.8.6.3 [Burner Origin Position Adjustment] ………………………………………5-74 5.8.6.4 [Furnace Origin Position Adjustment] ………………………………………5-74 5.8.6.5 [ASC Maintenance] ……………………………………………………………5-74 5.8.6.5.1 [Set Syringe Volume] ……………………………………………………5-74 5.8.6.5.2 [Change Syringe] …………………………………………………………5-74 5.8.6.6 [Maintenance only for service engineer] ……………………………………5-74 5.8.7 [Lamp Status] ……………………………………………………………………5-74 5.8.8 [Change Graphite Tube] …………………………………………………………5-76 5.8.9 [Gas Controller Status] …………………………………………………………5-76 5.8.10 [Gas Leak Check] ………………………………………………………………5-77 5.8.11 [Remaining Gas Combustion] …………………………………………………5-77 5.8.12 [Execute Line Search] …………………………………………………………5-79 5.8.13 [Cleaning] …………………………………………………………………………5-79 5.8.14 [Rinse Nozzle] ……………………………………………………………………5-79 5.8.15 [Flame Nozzle Position] …………………………………………………………5-80 5.8.16 [Furnace Nozzle Position] ………………………………………………………5-80 5.9 [Help] …………………………………………………………………………………5-81 5.9.1 [Search for Help on...] ……………………………………………………………5-81 5.9.2 [About WizAArd...] ………………………………………………………………5-81 5.10 Rounding the absorbance and setting the decimal places for correction factors and actual concentration ………………………………………5-82 5.10.1 Rounding the absorbance value ………………………………………………5-82 5.10.2 Setting the decimal places for correction factors and actual concentration value………………………………………………………5-84 6 Maintenance 6.1 Burner maintenance …………………………………………………………………6-1 6.1.1 Cleaning the burner head …………………………………………………………6-1 6.1.2 Nebulizer maintenance……………………………………………………………6-2 6.1.2.1 Cleaning the Nebulizer ………………………………………………………6-2 6.1.2.2 Replacing the polyethylene tube ……………………………………………6-4 6.1.3 Washing the chamber ……………………………………………………………6-4

AA-6200

Table of Contents

6.2 Checking for gas leaks in tubing ……………………………………………………6-6 6.2.1 Checking for gas leaks in the gas hoses and gas piping ………………………6-6 6.2.2 Checking for gas leaks in the instrument ………………………………………6-6 6.3 Replacing the deuterium lamp ………………………………………………………6-8 6.4 Rinsing ………………………………………………………………………………6-10 6.4.1 Rinsing the exterior ……………………………………………………………6-10 6.4.2 Rinsing the quartz window plate ………………………………………………6-10 6.5 List of maintenance parts……………………………………………………………6-11 6.6 Optional accessories list ……………………………………………………………6-12 6.6.1 For Flame Analysis ………………………………………………………………6-12 6.6.2 Hollow cathode lamps …………………………………………………………6-12 6.6.2.1 Single element lamp …………………………………………………………6-12 6.6.2.2 Multi-element lamps …………………………………………………………6-14 6.6.3 Other accessories ………………………………………………………………6-14 7 Troubleshooting 7.1 Troubleshooting ………………………………………………………………………7-1 7.1.1 Power supply indicator lamp does not light when the power switch of the spectrophotometer is switche on ……………………7-1 7.1.2 Communications between the PC and the AA-6200 do not initialize properly …7-1 7.1.3 Wavelength origin error occurs at initialization ………………………………7-1 7.1.4 Cannot recognize the autosampler at initialization ……………………………7-1 7.1.5 Photometric value is abnormal …………………………………………………7-1 7.1.6 Noisy beseline (S/N is poor) ……………………………………………………7-2 7.1.7 Error occurs in line search/beam balance ………………………………………7-2 7.1.8 Flame does not ignite ……………………………………………………………7-3 7.1.9 Air-C2H2 does not change over to N2O-C2H2 ……………………………………7-3 7.1.10 Flame is not stable ………………………………………………………………7-3 7.2 Error Messages ………………………………………………………………………7-4 8 Appendix 8.1 Measurement conditions for Flame Atomic Absorption analysis…………………8-1 8.2 Analysis line wavelengths for Flame Emission analysis …………………………8-4

AA-6200

1

Introduction

1 Introduction

Contents 1.1 Overview of AA-6200 ………………………………………………………………1-1 1.2 Hardware Specifications……………………………………………………………1-2 1.3 Software Specifiaions ………………………………………………………………1-3 1.3.1 Signal process ………………………………………………………………1-4 1.4 Notes for when upgrading from the AA-6200 16 bit software …………………1-5

AA-6200

1

Introduction

AA-6200

1.1

Overview of AA-6200 1

The Shimadzu Atomic Absorption Spectrophotometer AA-6200 is used for Flame Atomic Absorption Analysis and Flame Emission Analysis. Features include a double beam optical system and D2 (deuterium lamp) background correction method.

Introduction

The WindowsTM-based AA-6200 software is easy to use. Using the Measurement Wizard, even a first time operator can easily set measurement conditions. You can automatically analyze any element when the AA-6200 is combined with the autosampler, ASC-6100F. This feature is a great time saver. The following optional accessories are available : a) Hydride vapor generator, HVG-1 b) Mercury vaporizer unit, MVU-1A For the terms and practice used in WindowsTM, refer to the WindowsTM instruction manuals.

1-1 AA-6200

1.2

1

Hardware Specifications

Optics Monochromator

Introduction

Wavelength range Slit Background Correction Lamp Turret Lamp Mode Frequency Nebulizer Chamber Burner

Gas Control Safety

Ignition Software Dimension and weight Power requirements Ambient temp. and humidity range

1-2 AA-6200

Double Beam (chopper mirror) Aberration corrected Czerny-Turner monochromator Holographic grating (1,600 lines/mm) 190-900nm Automated wavelength selection 0.2nm - 0.7nm, manual setting D2-Lamp method 2-lamps simultaneously lit (manual turret) Emission, Non-BGC, BGC-D2 100Hz Nebulizer, ceramic impact bead and jacket tip Pt/Ir capillary Polypropylene Fixed back/forward position and burner height (Switchs between Air/C2H2 and N2O/C2H2 burner) Titanium 10cm slot burner (Optional high temperature burner) Manual setting of flow rate Automatic Air/N2O switching system Gas pressure monitoring to prevent flashback Automatic flame monitoring Safety interlock prevents burner misuse Automatic flame extinguisher for power failure Push Ignite button MS-Windows TM based W690 × D425 × H370mm, 38kg AC220V, 230V ±10%, 50/60Hz, 300VA (Certification of CE marking) Temperature : 10 – 35˚C Humidity : 45 ~ 80% (but less than 70% if temperature is over 30˚C)

1.3

Software Specifiaions

Concentration conversion Measurement type

Calibration curve

Repetitive analysis Accuracy enhancement Sensitivity enhancement Actual concentration calculation

Introduction

Data processing

1

Calibration method, standard addition method, simple standard addition method Autozero, blank, standard, unknown method of standard addition, simple method of standard addition, wait, pause Determines measurement type by designating the above actions Linear regression analysis by least square method, Abs = f (Conc.) Dimension : first order, second order, third order, ON/OFF of zero intercept Select calibration curve by Curve ID Maximum 20 analyses per sample Usage of average value, cancellation of abnormal data by limitation of RSD or SD values. Automatic calculation by sensitivity correction Automatic calculation of actual concentration by sample volume, constant volume, and dilution factor upon data acquisition

1-3 AA-6200

1.3 Software Specifiaions

1

1.3.1 Signal process Measurment time

Introduction

Response Measurement procedure setting Data display MRT Worksheet

Signal display

Retrieval and storage of data

Import/Export of data Report

1-4 AA-6200

Pre-spray : 99 seconds, Accumulation time : 99 seconds 4 response time options Easy setting by Wizard function Measurement procedure, analysis results, actual concentration, calculation factor of actual concentration, combined display of data and time Displays several element measurements on the same worksheet Signal profile display area : 4 Current signal profile display area : 1 Overlay display of signal profiles by designating the line color Automatic loading of template parameter file upon software activation Automatic data storage on File/Save command Raw profile data can be stored Import sample name from clipboard Export data file to ASCII file Summary report : display and output sample results Output after analysis : Parameter, raw data, signal, sequence Format and output items options

1.4

Notes for when upgrading from the AA-6200 16 bit software 1

Introduction

The main limitations and changes when upgrading to the WizAArd from the AA-6200 16bit software are as follows. • Measurement and conditions files of AA-6200 16 bit software cannot be opened with the WizAArd. • Take note that the standard conditions have been altered in parts. • The “AA 6200 16 bit” software and the WizAArd cannot be used simultaneously. When starting the WizAArd is started up while the “AA-6200 16 bit software” has been started up, an application error occurs. Furthermore, note that there are also the following limitations and changes in addition to the above. [Edit] • The function to create a sample schedule of standard addition method (MSA) automatically in the MRT worksheet is not supported. • The function to insert “Periodic Sensitivity Correction” automatically in the MRT worksheet is not supported. • To import “Sample ID” from a text file, open the text file by the notepad and copy & paste it to the “Sample ID” page of the WizAArd or “Sample ID “ field of the MRT worksheet. [Measurement] • The measurement will not stop immediately when it is interrupted by user. The measurement will stop once the present measurement is completed. • To set the warm up lamp, it is necessary to register the schedule of that element in the MRT worksheet. • The “Measure” lamp is turned off even if the measurement file for the same element as the “Measure” lamp is opened. • The “Measure” lamp and “Warm up” lamp cannot be switched unless either lamp is once turned off. • With the AA-6200 16 bit software, in cases where the repeat measurement type was set to "SM-SM..." in flame measurement (flame continuous mode) when using the ASC, the ASC raises up its nozzle and stops sucking the sample in the intervals between the repeat measurements. This has been eliminated in the WizAArd, and the same operation is carried out as when the repeat measurement type is "SM-M-M-...". • [Rinse at Starting Measurement] check box in Configuration dialog box has been abolished. When executing a rinse at the start of measurement, set [RINSE] or 1-5 AA-6200

1.4 Notes for when upgrading from the AA-6200 16 bit software

1

Introduction

[AUTO ZERO] in the first row on the MRT worksheet. • When the autosampler is being used and the AUTO ZERO button of the main window is clicked, the auto-zeroing is performed while the rinsing liquid is sucked with the R0 (rinse bottle position). • When operating with the intention of switching multiple ASC trays within a series of measurements, insert the PAUSE row that displays the message prompting the exchange of the ASC tray into the appropriate position in the MRT worksheet. [Data Processing] • The drift correction method has been changed from the time proportionality coefficient method to the calibration curve re-slope method. • The specification of the text file output content of the MRT worksheet is different. Take note of this when carrying out data processing etc. using the outputted results.

1-6 AA-6200

2

Installation

2 Installation

Contents 2.1 Parts inspection ……………………………………………………………………2-1 2.2 Instrument placement and site requirements ……………………………………2-2 2.2.1 Power requirments …………………………………………………………2-4 2.2.2 Gas requrements……………………………………………………………2-4 2.2.3 Ventilation system …………………………………………………………2-7 2.2.4 Use of an air compressor …………………………………………………2-8 2.2.5 General precautions for handling gas cylinders …………………………2-9 2.2.6 Installing pressure regulators (optional) and checking for leaks ……2-10 2.2.7 Software operation requirements (provided by user) …………………2-12 2.2.7.1 PC Specifications ………………………………………………………2-12 2.2.7.2 Operating System ………………………………………………………2-12 2.2.7.3 Connection cable ………………………………………………………2-12 2.2.8 Connecting the Drain Tube ………………………………………………2-13 2.2.9 Assembling the burner unit ………………………………………………2-14 2.2.10 Cable connections…………………………………………………………2-15 2.2.11 Hose connections …………………………………………………………2-17 2.3 Installing the PC software ………………………………………………………2-18

AA-6200

2

Installation

AA-6200

2.1

Parts inspection

After unpacking, verify that the following parts are included in your shipment. If any parts are missing or damaged, please contact your Shimadzu Representative. Item # 1

Part Name Qty Atomic absorption spectrophotometer 1

2

Part No. 206-50373-91

Table 2-1 : AA-6200 Main Unit Installation

Standard accessories 13

15

14

Figure 2-1 : Standard Accessories Item # 2-1 2-2 2-3 2-4 2-5 2-6 2-7 2-8 2-9 2-10 2-11 2-12 2-13 2-14 2-15 2-16

Part Name Grease in cup PE tube, 8 × 1(drain tube) Sampling tube Polyethylene tube, #3 Cleaning wire Hex-wrench, 3MM Hose assembly (Air) Hose assembly (C2H2) Wire band for 16mm (hose band) Cable, RS-232C 9P Cord, KP-4819+KS31A Disk, AA-6200 Screw, M3 × 6 Drain bottle assembly Seal joint assembly Instruction manual

Qty 1 1(1m) 5 1(0.5m) 1 1 1 1 2 1 1 1 2 1 1 1

Part No. 206-50442-91 016-43201-02 206-50438-91 200-31328-01 201-79229-01 086-03804 206-50389-91 206-50389-92 037-61019 206-50325-91 071-60814-05 206-51659-91 020-46534 206-50748-92 206-52039-91 206-94788

Table 2-2 : Standard Accessories NOTE 1. The instruction manual is not shown in Figure 2-1. 2. The hollow cathode lamps, high temperature burner head, pressure regulator and compressor are not included among the standard accessories. 2-1 AA-6200

2.2

Instrument placement and site requirements

The insrument components are positioned as shown in Figure 2-2. (Personal Computer System is not shown in the figure.)

2

Installation

(1) The installation site should be : (a) Away from devices that generate strong magnetic and electrical fields or high frequencies (b) Well ventilated (c) Free from vibration (d) Free from excessive dust and moisture and not exposed to corrosive gases (e) Away from direct exposure to daylight

CAUTION The AA-6200 is equipped with various safety systems which utilize an optical sensor. When installing the instument near a window, ensure that the instrument is not exposed to strong daylight. Exposure to strong daylight may interfere with normal operation of the extinguished flame safety system which monitors flame combustion (Flame Monitor). (f) Ambient temperature range : 10 to 35˚C (g) Humidity : 45 to 80% (but less than 70% if temperature is over 30˚C) (2) The installation platform (table or counter top) must be capable of supporting the combined weights of the components listed below and a personal computer system. AA-6200 : 38kg ASC-6100 : 8kg PC : 25 to 30kg (3) Since gas pipes and cables are connected to the back of the instrument, leave 15 to 20cm between the back of the instrument and a wall.

2-2 AA-6200

2.2 Instrument placement and site requirements

Top view

2

Installation

Front view

(Unit: mm) Figure 2-2 : Instrument Placement

2-3 AA-6200

2.2 Instrument placement and site requirements

2.2.1 Power requirments The following table gives the power requirements for each component. (The power requirement for a personal computer system is not shown in the table.)

2

Installation

Voltage Allowable voltage range Power capacity Source frequency Connections

AA-6200 220, 230V Within ±10% 300VA 50/60Hz Grounded outlet

Table 2-3 : Power Requirements

NOTE 1. When using power supply voltages other than those shown above, use a step-up transformer. 2. If voltage fluctuation exceeds ±10%, use an appropriate stabilizer.

2.2.2 Gas requrements (1) Gas specifications Gas

Supply pressure

Max. Consumption

Purity

Air

0.35±0.03MPa

24L/min

Free from oil, moisture, and dust

Nitrous oxide

0.35±0.03MPa

15L/min

Purity ≥ 98%, moisture ≤ 1%

4.9 L/min(Air-C2H2 flame) 9.9 L/min(N2O-C2H2 flame)

Purity ≥ 98%

Acetylene 0.09±0.01 MPa

Table 2-4 : Gas Specification WARNING! Use only gases in Table 2-4 for flame analyses Do not use oxygen gas.

Be sure that gases are supplied according to the specifications in Table 2-4.

2-4 AA-6200

2.2 Instrument placement and site requirements

NOTE If the gas supply pressure changes during the analysis, the resulting fluctuations in the flame will adversely affect measurement reproducibility. Ensure that gas pressure does not fluctuate.

2

Installation

(2) Placement of gas cylinders To ensure safety, we recommend placing the cylinders outdoors. Select a location for the cylinders that is : (a) Not exposed to heat sources such as direct sunlight, furnaces, and heaters. Always keep the cylinders at a temperature below 40˚C. (b) Away from spark sources such as switchboards, ground wires, and high voltage power sources. (c) Away from flammable materials such as oil, gasoline, and organic solvents. (d) Sufficiently ventilated. (e) If outdoors, not exposed to wind and rain. (3) Gas piping If the cylinders are placed outdoors, additional piping must be supplied within 5 m of the instrument by the user. In this case, be sure to follow the precautionary measures listed below. (a) Use stainless steel pipes for the piping. Do not use pipes that contain over 62% copper for acetylene piping. (b) Ensure that the pipe diameters are not too small to supply gas at the pressures indicated in Table 2-4. A pipe diameter of at least 7mm will be sufficient. (c) Place a trap in the air piping system at the location indicated in Figure 2-3. If dry air is supplied, a trap is unnecessary. (d) Figure 2-3 displays examples of recommended piping configurations. (e) Use a hose fitting with an outside diameter of 8.4 to 8.9mm so that the provided gas supply hose (inside diameter 7.9mm) can be connected to the end or the gas piping.

2-5 AA-6200

2.2 Instrument placement and site requirements

2

Installation Figure 2-3 : Recommended Piping Configuration

2-6 AA-6200

2.2 Instrument placement and site requirements

2.2.3 Ventilation system Place a ventilation duct with a hood above the atomizer. (1) The hood, duct and ventilation fans used should all be made of metal. Plastic is inappropriate as it is softened by heat. (2) A Cooling- fan air capacity of about 600 to 1200 m3/h is appropriate. Too much suction force will cause the flame to flicker and create excessive noise. Placing a damper in the duct system will help create the optimum air flow.

2

Installation

(Unit: mm) Figure 2-4 : Typical Ventilation System

2-7 AA-6200

2.2 Instrument placement and site requirements

2.2.4 Use of an air compressor The air compressor described in this section may not be available in all countries. Use of another brand of air compressor is acceptable providing that it supplies air which is free of oil, water, and dust at the pressures indicated below. in addition, the air compressor should be equipped with the necessary safety devices and meet the standards required by the local regulations. The following procedure is used for confirming the operation status of the air compressor shown in Figure 2-5.

2

Installation

(1) Confirm that the oil level falls between the red lines on the oil gauge t. (2) Shut the stop cock !0 and drain cocks y & u, turn the secondary pressure control handle q counter-clockwise, and then connect the compressor to a power source. (3) When the primary pressure reaches 0.5MPa, the motor will stop. Remove the safety valve by hand e and confirm that it is working properly. (You will hear a loud hissing sound, but there is no danger.) (4) When the primary pressure reaches 0.4MPa, the motor will start. (5) After the primary pressure reaches 0.5MPa again, turn the secondary pressure control handle q clockwise and set the secondary pressure to 0.35MPa. The compressor is normally used in this state. (6) Apply soapy water or another leak detector to the connecting parts of the pressure gauges, air transformer, etc., to check for leaks.

NOTE 1. If the compressor does not work using the above procedure, refer to the compressor instruction manual. 2. In order to set the secondary pressure correctly, the secondary pressure must always be lowered to nearly 0MPa before turning the control handle q. 3. During use, make sure that the oil level always stays between the red lines on the oil gauge. 4. After use, always open the drain cocks and discharge the water and oil inside the tank and the transformer. 5. If a hand compressor or compressed air pipe is to be used to supply air, verify the following : (a) That air is supplied at a pressure of 0.35 to 0.4MPa. (b) That the pressure does not fluctuate. (c) That the air supplied does not contain water, oil, or dust. 2-8 AA-6200

2.2 Instrument placement and site requirements

q Secondary pressure control handle w Primary pressure gauge e Safety valve (not visible in figure) r Lubrication hole t Oil gauge y Drain cock

u Drain cock i Air transformer o Air output port !0 Stop cock !1 Secondary pressure gauge

2

Installation

Figure 2-5 : Air Compressor Accessory

2.2.5 General precautions for handling gas cylinders Handle the cylinders carefully, observing the following precautions : (1) Before installing a pressure regulator on a cylinder, always remove any dust from the cylinder outlet. (2) When opening the cylinder main valve, turn the secondary pressure control handle counter-clockwise and, after checking that there is no one standing on the outlet side, gently open the valve. (3) When using nitrous oxide, open the cylinder main valve sufficiently. With acetylene, do not turn the cylinder main valve more than one and a half turns in order to prevent the acetone of DMF (dimethylformamide) inside from flowing out. (4) When using a nitrous oxide-acetylene flame, always open the valve of the acetylene cylinder 1 to 1.5 turns. If the valve is opened less than this, the acetylene flow rate may be insufficient and cause flashback when switching from an air-acetylene flame to a nitrous oxide-acetylene flame. (5) When using nitrous oxide, the flow rate may become unstable if the main valve is not opened enough. Ensure that the main valve is sufficiently opened. 2-9 AA-6200

2.2 Instrument placement and site requirements

(6) Place all the cylinders upright. (7) Always leave the cylinder handle attached to the main valve even during use. (8) After use, not only close the stop cock but also always shut the cylinder main valve. (9) When the source pressure of the acetylene cylinder decreases to 0.5MPa, replace the cylinder. For acetylene gas, a porous mass inside the high-pressure container is soaked with acetone or DMF (dimethylformamide), and the acetylene gas is dissolved in the mass by compression. If the internal pressure of the cylinder decrease to less than 0.5MPa, vapor of acetone or DMF becomes mixed in the acetylene gas, and the gas flow rate becomes unstable. If the internal pressure decreases to less than 0.3MPa, the acetone or DMF flows out, and it is not possible to control the gas flow rate.

2

Installation

2.2.6 Installing pressure regulators (optional) and checking for leaks (1) Remove any dust adhering to the outlet of the cylinder. (2) Refer to Figures 2-7 and 2-6 to install the pressure regulators on the cylinders. If the screw for mounting the regulators on the cylinder appears ready to break, replace the cylinder without attempting to mount the regulator. (3) Open the cylinder main valve gently after closing the stop cock and turning the secondary pressure control handle sufficiently counter-clockwise. (4) Turn the secondary pressure control handle clockwise and set the secondary pressure to the following values : Acetylene : 0.09MPa Nitrous oxide : 0.35MPa (5) Apply soapy water or other leak detector to each of the connecting joints to check for leaks. Due care should be taken to detect and eliminate any leaking at the cylinder cock.

WARNING! 1. Exercise caution ; mistake in piping may cause flashback during ignition. 2. Always set the gas supply pressures at the values indicated above. 3. Never use a broken regulator. This may result in an accident. 4. Use the pressure regulator that has the function to prevent freezing for nitrous oxide cylinder. If the regulator has no freezing-proof function, Evaporation of liquid nitrous oxide in the cylinder may freeze the regulator and the make the flow rate of nitrous oxide unstable. This situation may cause a flashback.

2-10 AA-6200

2.2 Instrument placement and site requirements

(

Secondary pressure control handle When turned clockwise, the secondary pressure rises ; when turned counter-clockwise, it decreases. The secondary pressure is normally set to 0.35MPa.

Secondary pressure gauge

Cylinder main valve Open by turning counter-clockwise ; close by turning clockwise. Use almost wide open.

2

)

Installation

(

)

Stop cock

Connecting nut

Figure 2-6 : Pressure Regulator for Nitrous Oxide

Secondary pressure gauge

(

Primary pressure gauge

Cylinder main valve

(

Open by turning counter-clockwise; close by turning clockwise. Use turned counter-clockwise 1.5 turns.

Secondary pressure control handle When turned clockwise, the secondary pressure rises ; when turned counter-clockwise, it decreases. The secondary pressure is normally set to 0.09MPa.

)

)

Figure 2-7 : Pressure Regulator for Acetylene

2-11 AA-6200

2.2 Instrument placement and site requirements

2.2.7 Software operation requirements (provided by user) In order to run the AA-6200 software and control the instrument, the following software and hardware must be provided. 1) Personal computer (PC) and peripheral accessories 2) Operating system 3) Connection cable

2

Installation

2.2.7.1 PC Specifications Table 2-5 PC Specifications CPU RAM

Recording device Screen resolution I/O port Peripherals

Specifications Pentium 75 or faster (Pentium 200 or faster CPU recommended) 32MB or larger (64MB or larger recommended) 1 floppy disk drive (3.5inch size) (for installing the program) Hard disk drive (with at least 10MB free disk space for AA software) SVGA (800 × 600 or higher) (1024 × 768 or higher resolution recommended) 1 serial port for AA Monitor Keyboard Mouse or other pointing device Printer

2.2.7.2 Operating System The computer must contain one of the following software in order to run the AA6200 software. Windows95 Windows98 WindowsNT4.0 (Windows95, Windows98, and WindowsNT4.0 are registered trademarks of Microsoft Co.) 2.2.7.3 Connection cable In order to connect the PC and AA-6200, an RS-232C reverse cable is provided as standard accessory. This cable has a female 9-pin DSUB connector for connecting to the RS-232C connector (PC) at the rear of the AA-6200 main unit, and a female 9-pin DSUB connector for connecting to serial port connector on the typical IBM PC/AT and compatible computers. Figure 2-8 shows the wiring diagram of the standard accessory cable. 2-12 AA-6200

2.2 Instrument placement and site requirements

2

Installation

Figure 2-8 : Cable Pin Assignment

2.2.8 Connecting the Drain Tube To prevent gas from leaking through the drain tube, the liquid in the drain tank placed in the drain line must be maintained at a constant level so that the water pressure may provide proper sealing. (1) Fasten the drain bottle assy on right side front panel of the instrument using the two M3 × 6 screws. (2) Connect the U-tube from the chamber to the joint at the bottom of the drain tank to the joint on the spray chamber and then lock it firmly with the band. (3) Connect the provided PE tube (e) to the discharge port (w) on the drain tank as shown in Figure 2.9. (4) Provide an appropriate container (t) to receive the drain liquid. (5) Pour water from the drain tank opening (q) until the water overflows the outlet of the drain tank. q Drain tank opening

w Discharge port

e Drain tube t U-tube r Drain container

Figure 2-9 : Drain Tube Configuration 2-13 AA-6200

2.2 Instrument placement and site requirements

CAUTION Before igniting, be sure to check that water is filled in the drain tank. Do not ignite a flame unless the drain tank is filled with water. If the drain tank is not filled with water, combustion gas flows out from the chamber and cause flashback

2

Installation

(6) To ensure that drainage is performed smoothly: (a) The drain tube should hang downward so that there is no crimping of the tube. (b) Leave the end of the drain tube free in the air. If drainage is not performed smoothly, excessive noise will be produced and reproducibility may be adversely affected. CAUTION 1. U-tube cannot be used for petroleum solvents. 2. Especially for organic solvent waste, prepare a suitably sized drain container (approx. 10L) of appropriately resistant material. 3. Dispose frequently the drain generating hazardous gases. 4. Do not use a glass-made container since it may be broken. 5. Dispose of waste liquid according to the applicable regulation in your country or region.

2.2.9 Assembling the burner unit Refer to Figure 2.10 for the burner unit configuration.

q Burner head t Nebulizer retaining plate

e O-rings

r Nebulizer fixing screw

w Burner head fixing port

y Nebulizer i Capillary tube

u Sampling tube Enlarge the opening! o Chamber

!0 O-ring

Figure 2-10 : Assembling the Burner Unit 2-14 AA-6200

2.2 Instrument placement and site requirements

(1) Pull out the burner head (q) to confirm that O-rings (e) are set in the burner head fixing port (w). Then insert the burner head into the burner head fixing port, and push it down firmly. (2) Loosen the nebulizer fixing screw (r), shift the nebulizer retaining plate (t) to right, and pull out the nebulizer (y) from the chamber (o) disconnecting the SPRAY joint attached to the nebulizer. Confirm that the O-ring (!0) is properly fitted to the nebulizer. (3) Insert the nebulizer to the chamber certainly, and set the nebulizer retaining plate with the screw. (4) Insert a pen into the end of the sampling tube (u) to enlarge the opening to more than 1mm in diameter. (5) Exercising maximum care so as not to damage the capillary tube (i), insert the enlarged end of the sampling tube onto the opening containing the capillary tube of the nebulizer. Make sure that the sampling tube fits securely over the capillary tube. (6) Finally connect the SPRAY joint as before.

2

Installation

CAUTION O-rings are placed at the mounting surfaces of the burner head and the nebulizer to prevent gas leakage. When assembling, always verify that the O-rings (e,!0) are in place. NOTE 1. If it is difficult to fit the sampling tube onto the capillary, warm up the end of the tube to enlarge the opening. Since the capillary is very thin and fragile, be careful that it does not break. 2. A polyethylene tube covers the capillary to ensure a snug fit between the smpling tube and the capillary. 3. Insert the nebulizer fully. If not, combustion gas can leak from the chamber or the sensitivity may deteriorate.

2.2.10 Cable connections Referring to Figure 2-11, connect the AC cable included in the standard accessories and connect the RS-232C cable to the PC. (For details on connecting PC to monitor, keyboard, mouse and printer, refer to the computer's documentation.) Connect the RS-232C reverse cable to the connector labeled (PC) at the rear of the AA-6200 main unit, and to the serial port connector on the PC. The PC serial interface may be called an RS-232C or COM port, depending on the computer. Refer tohe documentation provided with the PC. Be sure to verify that the AA-6200 2-15 AA-6200

2.2 Instrument placement and site requirements

main unit power switch is OFF before connecting the AC cable. The connector labeled (ASC) at the rear of the AA-6200 main unit is connected to the RS-232C cable of the autosampler ASC-6100 (optional accessory). The pin assignment of this connector is shown in Table 2-6.

2

Installation

CAUTION In the case of 2-wire socket, be sure to ground the earth terminal of AC cable.

Connector Pin # Case 2 3 4

Signal Type FG TxD RxD SG

Funcion Frame ground Output data line Input data line Signal ground

Table 2-6 : Connections

Figure 2-11 : Cable Connections

2-16 AA-6200

2.2 Instrument placement and site requirements

2.2.11 Hose connections Refer to Figure 2-12 when connecting hoses.

2

WARNING DO NOT use oxygen gas mixture.

Installation

Connect the compressor, gas cylinders, and the hose couplings at rear of the main unit as follows : (1) The hose joints are connected to the rubber hoses as follows : Black rubber hose with 8mm diam. hose nozzle - for air. Green rubber hose with 6mm diam. hose nozzle - for nitrous oxide. Red rubber hose with 8mm diam. hose nozzle - for acetylene. (2) Connect one end of the rubber hoses to the compressor and gas cylinder without using a hose connector. Secure them with the hose bands provided as standard accesories. (3) Connect the other end of the rubber hose with the hose connector to the specified gas inlet port at the left back of the main unit. The gas inlet port is provided with cap nut and sleeve. First, pass the cap nut and sleeve through the hose nozzle. Next, insert the hose connector deeply into the gas inlet port and tighten the cap nut by hand. Finally, tighten the screw firmly using spanners. (4) Check gas leak according to 6.2 Checking for Gas Leaks in Tubing.

Figure 2-12 : Hose Connections

2-17 AA-6200

2.3

Installing the PC software

This procedure assumes that MS-Windows is already installed on the PC. For its installation, refer to the appropriate documentation. 1) Start up MS-Windows. 2) Insert the AA software setup disk #1 in the floppy disk drive of the PC. 3) Select [Run...] from in the task bar. 4) Input "A:¥setup" to the [Open] in the [Run] dialog box and click on (A: refers to the floppy disk drive name. Enter this or "B", "C", "D", etc., according to the PC configuration). 5) First, a note for installation is displayed. Read it and click on to go ahead. 6) AA-6200 is already selected as main unit type. Click on to go ahead. 7) Check the installation destination folder. You may change the folder here, if desired. Click on to go ahead. 9) Select the program folder. Click on to start setup. 10) When the message appears to prompt inserting the next disk, insert the disk #2 into the floppy disk drive and click on . 11) Finally, when the message shows that the setup is completed, click on . When the [Yes, I want to read README.TXT] check box is check-marked, the README.TXT is displayed by the Notepad. Be sure to read this, since the important information about AA software operation is described in the README.TXT. Exit the Notepad, then installation procedure is finished.

2

Installation

NOTE 1. Set all the electric power-saving functions to OFF both in the BIOS setup of PC and in the control panel of Windows. Otherwise, the electric power-saving function may cause a trouble in communication between the AA main unit and the PC. How to display the BIOS setup screen is different depending on the PC model. Refer to the instruction manual provided with the PC. 2. When installing WizAArd to the Windows NT4.0, login with the authorization of Administrator.

2-18 AA-6200

3

Contents 3.1 AA-6200 configuration ……………………………………………………………3-1 3.1.1 Spectrophotometer main unit ……………………………………………3-1 3.1.2 Hollow cathode lamp turret ………………………………………………3-3 3.1.3 Deuterium lamp ……………………………………………………………3-4 3.1.4 Burner and burner module…………………………………………………3-5 3.1.5 Optical system ………………………………………………………………3-8 3.1.6 Photometric System ………………………………………………………3-9

AA-6200

Instrument configuration

3 Instrument configuration

3

Instrument configuration

AA-6200

3.1

AA-6200 configuration

3.1.1 Spectrophotometer main unit Front

3

Instrument configuration

Right side

Left side 12

Rear

Figure 3-1 : Spectrophotometer Main Unit

3-1 AA-6200

3.1 AA-6200 configuration

No. Name 1 Power Switch 2 Extinguish button 3

Function Switches ON the instrument Extinguishes the flame. Pressing this button and Purge button simultaneously ignites the burner with the pilot flame.

Ignite button

3

Open the cylinder or the compressor and press this button to supply the gas to the burner.

Instrument configuration

4

Press this button and Ignite button simultaneously to ignite the burner.

Purge button

Purges gas from the inside tubing when no gas is flowing from the gas cylinder or compressor. 5 6 7 8 9 10

Fuel gas flow adjusting knob Oxidant gas flow adjusting knob Fuel gas flow meter Oxidant gas flow meter Deuterium lamp house cover Power supply connector

11

Hollow cathode lamp turret

12

Hollow cathode lamp socket

13 14 15 16 17 18 19 20 21

Increase flow by turning to the left. Increase flow by turning to the left. Displays fuel gas flow. Displays oxidant gas flow. Remove to replace the deuterium lamp. Connects AC cable. Rotates to switch between the two mounted hollow cathode lamps. Insert into the pin of the hollow cathode lamp to supply power.

Deuterium lamp position adjusting Adjusts the position of the deuterium lamp. screw. Slit changing knob Changes the monochromator slit width. Should be operated only by qualified service Pilot flame flow adjusting knob personnel. Fuel gas bypass flow adjusting Should be operated only by qualified service knob personnel. Connects RS-232C cable for communication RS-232C (PC) connector with PC. Connects RS-232C cable for communication RS-232C (ASC) connector with ASC. N2O gas hose connecting port Connects the nitrous oxide gas hose. Air gas hose connecting port Connects the air gas hose. C2H2 gas hose connecting port Connects the acetylene gas hose. Table 3-1 : Spectrophotometer parts

*Items in gray should be operated only by qualified service personnel. 3-2 AA-6200

3.1 AA-6200 configuration

3.1.2 Hollow cathode lamp turret The hollow cathode lamp turret can hold and power two hollow cathode lamps simultaneously. To mount the lamp, insert the lamp socket onto the pin of the hollow cathode lamp. Use the lamp socket labeled HCL-1 when placing the hollow cathode lamp into turret opening 1, and HCL-2 when placing the hollow cathode lamp into turret opening 2. Then, insert the lamp into the appropriate turret opening. The lamp position adjusting knob is used to adjust the lamp optical path to the optical axis. When changing the lamp, hold the lamp turret rotation knob, and rotate the turret until the latch catches.

3

Instrument configuration

CAUTION 1. Before connecting/disconnecting the lamp socket, be sure to lower the lamp current to 0mA. 2. When installing a lamp, make sure that the socket is fully seated. If it is not, there is a danger from exposed pins carrying high voltage loads. NOTE Even if the lamp current is set to 0mA, the lamp may still glow weakly, depending on the element. It is not a defect of the instrument and does not affect the lamp service life.

Figure 3-2 : Hollow Cathode Lamp Turret

3-3 AA-6200

3.1 AA-6200 configuration

3.1.3 Deuterium lamp To access the deuterium lamp, remove the cover of the deutrium lamp house, shown in Figure 3-3. The deuterium lamp is used for background correction in the wavelength range of 190nm to 430nm. The deuterium lamp is inserted into the lamp socket mounted on the lamp base. Adjusting the deuterium lamp adjusting screw moves the lamp base. Lamp specifications are shown in the table below.

3

Instrument configuration

Part number Model Guaranteed life Characteristics

062-65055-05 L6380 500 hours Discharge voltage 80V Typ Discharge current 300mA Discharge starting voltage 350V Max Table 3-2 : Deuterium Lamp Specificiations

CAUTION Since the deuterium lamp radiates ultraviolet light, which is harmful to the eyes, keep the lamp cover closed while the lamp is on.

Figure 3-3 : Deuterium Lamp House

3-4 AA-6200

3.1 AA-6200 configuration

3.1.4 Burner and burner module The standard equipped burner head can be used only with the air - acetylene flame. You should install a high temperature burner head (optional) when using nitrous oxide - acetylene flame. To remove the burner head, turn the burner right and left while pulling the burner head upward. The burner can be removed. When using a burner accessory, adjust the burner position so the accessory is optically aligned. e Flame monitor

Instrument configuration

r Pilot flame

3

q Burner head w Burner angle adjusting lever

y Drain tank

t U-tube

Figure 3-4 : Burner Module

No.

Name

1

Burner head

2

Burner angle adjusting lever

3

Flame Monitor

4

Pilot flame

5

U-tube

6

Drain tank

Function The burner head provided as standard is used for air-acetylene flame. It cannot be used for nitrous oxide-acetylene flame. Used to adjust the burner angle to the optical path. The flame monitor has a built-in optical sensor that detects emission strength of the flame. If the flame goes out, a signal from this sensor closes the gassupplying valve of the unit to stop the gas outflow. Pressing the IGNITE and the PURGE button simultaneously ignites the pilot flame. Connected to the drain tank. Fill this portion with water. Water pressure seals the chamber to prevent a gas leak.

Table 3-3 : Burner Module Parts 3-5 AA-6200

3.1 AA-6200 configuration

No.

3

Name

7

Burner head fixing port

8

Nebulizer

9

Disperser

10 Instrument configuration

11 12

13

14 15 16

Function Insert the burner head into this port. The burner head is fixed using internal O-rings. This uses air pressure to suction the sample solution and sprays it from the tip of the capillary. This sprays the sample solution into an even finer mist and separates out the largest particles.

Nebulizer retaining plate and Holds the nebulizer. fixing screw The particles of sprayed sample solution are Chamber mixed with the combustion gas in this chamber. Mixing of the particles and combustion gas is Mixer promoted. In case of flashback, this valve is open to prevent the burner unit from being damaged. A flashback means a combustion or explosion which occurs in Safety valve the burner when the flame combustion rate is fast and the mixed gas flow rate is slow. In case a flashback should occur and the safety valve operates, set the safety valve back in the place. Larger particles of the sample solution spray are Drain discharge port discharged from this port. Chamber fixing screw Burner height is changed by loosening this screw. When optional hydride vapor generator or mercury Chamber positioning hole vaporizer unit is used, burner height is changed and fixed at the respective holes. Table 3-4 : Burner Module Parts

NOTE When measuring samples containing high-concentration coexistant like salts or when measuring samples with a nitrous-oxide flame, the mixer reduces the signal noises. Therefore, the mixer is usually mounted in the chamber. When measuring samples with low-concentration coexistant with air-acetylene flame, however, removing the mixer may improve the sensitivity. If a high sensitivity is required for such samples, you can remove the mixer if necessary. Remove the mixer referring to the section 6.1.3.

3-6 AA-6200

3.1 AA-6200 configuration

u Burner head fixing port

3

!0 Retaining plate !3 Safety bung

!2 Mixer

o Disperser

!0 Fixing screw

!1 Chamber

Instrument configuration

i Nebulizer

!4 Drain discharge port

Figure 3-5 : Burner

!6 Chamber positioning hole

!5 Chamber fixing screw

Figure 3-6 : Chamber Positioning Hole

3-7 AA-6200

3.1 AA-6200 configuration

3.1.5 Optical system Figure 3-7 shows the optical system. P.M.T Monochromator

3

Chopper mirror

Deuterium lamp

Instrument configuration

Reference beam

Sample beam

Burner

Hollow cathode lamp

Figure 3-7 : Optical System The light emitted from the hollow cathode lamp and the deuterium lamp is divided into the sample side beam and reference side beam by the half mirror. The light from the hollow cathode lamp and the deuterium lamp joint together as the sample side beam passed the atomizer unit. The combined light is absorbed by the sample. Then, the light enters the detector (photomultiplier tube) through the monochromator. The reference side beam passed through the space that is not absorbed by the sample and enters the detector (photomultiplier tube) through the monochromator. Respective beams are selected by the chopper mirror before entering the monochromator, which detects the sample beam and the reference beam alternately. By taking the balance of respective samples alternately received, the base line drift can be deducted. Since the chopper mirror is used, there is no light intensity loss in the sample beam and the reference beam. A quartz window plate and protective cover shield the optical elements from the outside air, dust, and corrosive gases.

3-8 AA-6200

3.1 AA-6200 configuration

3.1.6 Photometric System Figure 3-8 shows the photometric system.

Lamp power supply Deuterium lamp

3 SAMPLE

Monochrometer

Instrument configuration

Hollow cathode lamp

Analog signal processor

Detector Burner

Beam separator

REFERENCE

Beam combiner

CPU

PC Gas control unit

Figure 3-8 : Photometric System The personal computer sends the lamp currents, lamp mode, wavelength, and flame type parameters to the AA-6200 main unit through the RS-232C interface and sets the AA-6200 automatically. When measurement is started, the AA-6200 main unit sends data to the personal computer where it is displayed or processed. The personal computer maintains optimum sensitivity of the detector (photomultiplier tube) by monitoring the emission intensity from the lamp, or during flame emission analysis, from the flame. Three lamp modes are available for selection in this unit. Emission mode This mode measures concentrations by measuring the light emission energy of the substance. Use the mode to adjust the position of the hollow cathode lamp as well. Non-BGC mode This mode is used for atomic absorption analysis that does not require background correction. It is also used for atomic absorption analysis in the long wavelength 3-9 AA-6200

range (430~900nm) in which the deuterium lamp cannot be used. BGC-D2 mode Background correction is performed in this mode by the D2 method.

3

Instrument configuration 3-10 AA-6200

4 Basic Operation

4

Basic Operation

Contents 4.1 Switching On the Power and Starting the Software ……………………………4-1 4.1.1 Switching the instrument power supply on and off ……………………4-1 4.1.2 Starting Up the Software …………………………………………………4-2 4.2 Software Basic Operation ………………………………………………………4-3 4.2.1 Software Basic Operation ………………………………………………4-3 4.2.1.1 Operation Flowchart …………………………………………………4-3 4.2.1.2 Wizard Selection………………………………………………………4-4 4.2.1.3 Element Selection ……………………………………………………4-4 4.2.1.4 Preparation Parameters ……………………………………………4-6 4.2.1.5 Sample ID ……………………………………………………………4-10 4.2.1.6 Sample Selection ……………………………………………………4-11 4.2.1.7 Connect to Instrument/Send Parameters …………………………4-12 4.2.1.8 Optics Parameters for Lamp Position Adjustment ………………4-13 4.2.1.9 Lamp Position Adjustment …………………………………………4-16 4.2.1.10 Optics Parameters …………………………………………………4-17 4.2.1.11 Gas Flow Rate Setup ………………………………………………4-19 4.2.2 Saving the Template ……………………………………………………4-20 4.3 Measurement Procedures ………………………………………………………4-22 4.3.1 Measurement Operation ………………………………………………4-22 4.4 Saving/Printing/Deleting the Data………………………………………………4-26 4.4.1 Saving the Data …………………………………………………………4-26

AA-6200

4

Basic Operation

4.4.2 Printing the Data …………………………………………………………4-26 4.4.3 Deleting the Data ………………………………………………………4-26 4.5 Completing the Measurement …………………………………………………4-27 4.6 Explanation of Main Window ……………………………………………………4-28 4.6.1 Menu bar …………………………………………………………………4-29 4.6.2 Standard tool bar ………………………………………………………4-29 4.6.3 Measurement element tool bar …………………………………………4-29 4.6.4 Absorbance digital display………………………………………………4-29 4.6.5 Real time graph …………………………………………………………4-29 4.6.6 Peak Profile (Latest four measurements and overlay display)………4-31 4.6.7 Calibration Curve Display ………………………………………………4-33 4.6.8 MRT work sheet …………………………………………………………4-36 4.6.9 Function buttons …………………………………………………………4-37 4.6.10 Status bar ………………………………………………………………4-38 4.7 Operating the MRT work sheet …………………………………………………4-39 4.7.1 Fields of MRT work sheet ………………………………………………4-39 4.7.2 Right Mouse Button Menu ………………………………………………4-45 4.7.3 Right Mouse Button on Summary Table ………………………………4-48 4.7.4 Inserting and Deleting the Measurement Row ………………………4-48 4.7.5 Active Cell Movement by Shortcut Key and Cell Selection …………4-49 4.7.5.1 Moving an Active Cell ………………………………………………4-49 4.7.5.2 Selecting Cells ………………………………………………………4-50 4.7.6 Copy and Paste ……………………………………………………………4-50 4.7.6.1 Copy ……………………………………………………………………4-50 4.7.6.2 Paste……………………………………………………………………4-51 4.7.7 Changing Column Width and Column Header Height of MRT Worksheet…4-51 4.8 Igniting and extinguishing the flame……………………………………………4-53 4.8.1 Control locations …………………………………………………………4-53 4.8.2 Safety Precautions Prior to Ignition ……………………………………4-53 4.8.3 Igniting and extinguishing an Air-C2H2 flame …………………………4-54 4.8.4 Igniting and extinguishing N2O-C2H2 flame……………………………4-56 4.8.5 Flame conditions when analyzing organic solvent samples ………4-59 4.8.6 Changing the chamber position ………………………………………4-60 4.9 Standard Addition Method and Simple Standard Addition Method…………4-61 4.9.1 Overview …………………………………………………………………4-61 4.9.2 Setting the measurement procedure for simple standard addition method…4-62 4.9.3 Setting the measurement procedure for standard addition method…4-64

AA-6200

4.10 Conditions and Operation for Flame Emission Analysis ……………………4-67 4.10.1 "Optics Parameters" Page ……………………………………………4-67 4.10.2 "Gas Flow Rate Setup" Page …………………………………………4-68 4.10.3 Line Search and Beam Balance………………………………………4-70

4

Basic Operation

AA-6200

4

Basic Operation

AA-6200

4.1

Switching On the Power and Starting the Software

4.1.1 Switching the instrument power supply on and off (1) First, ensure that the instrument is set up correctly. (2) When connecting peripheral equipment such as an autosampler (ASC-6100), set the power switch on the peripheral to the "  " position (Figure 4-1). (3) Set the power switch at the front lower right of the AA-6200 main unit to the "  " position (Figure4-2). The green lamp illuminates. (4) When you are finished using the device, set the power switch of each device to the " O " position. Power is disconnected.

4

Basic Operation

NOTE To switch OFF the power of the AA-6200 main unit, first extinguish the flame. Then set the power switch located at the front lower right of main unit to the " O " position.

q Power switch Figure 4-1 : Power Switch of ASC-6100

4-1 AA-6200

4.1 Switching On the Power and Starting the Software

4

Basic Operation

Figure 4-2 : Power Switch of AA-6200

4.1.2 Starting Up the Software Switch ON the personal computer to start up the MS-Windows. Double click on the icon of AA Software. The "Wizard Selection" dialog box (Fig 4-3) will appear at the center of the screen.

4-2 AA-6200

4.2

Software Basic Operation

With the AA software, after starting up the software, you can set the necessary settings for the measurement just by following the instructions sequentially displayed on the screen (Wizard function). In this section, the easy operation using this Wizard function is described for flame method in regular sequence. Refer to Chapter 5 for details of each items.

4.2.1 Software Basic Operation 4.2.1.1 Operation Flowchart This Wizard has a sequence for setting as shown below. You can proceed to the next step or return to the preceding step by using the or button, respectively.

4

Basic Operation

(Starting up the AA Software) ↓ qWizard Selection wElement Selection ePreparation Parameters rSample ID tSample Selection yConnect to Instrument/Send Parameters uOptics Parameters for Lamp Position Adjustment iLamp Position Adjustment oOptics Parameters !0Gas Flow Rate Setup (Finish) ↓ (Start Measurement)

NOTE When measuring plural elements, you cannot set parameters for the elements other than the current measurement one on the "Optics Parameters for Lamp Position Adjustment", "Lamp Position Adjustment", "Optics Parameters" and "Gas Flow Rate Setup" pages. If you use the ASC to measure plural elements automatically and you need to modify the parameters for other elements than the current measurement one, you can change these parameters by using the button in the "Element Selection" page.

4-3 AA-6200

4.2 Software Basic Operation

4.2.1.2 Wizard Selection

4

Basic Operation

Figure 4-3 : "Wizard Selection" Dialog Box When the "Wizard Selection" dialog box appears, if you make a new parameter set, select the Element Selection icon on the Wizard sheet and click on the . Then the "Element Selection" page will appear. 4.2.1.3 Element Selection

Figure 4-4 : "Element Selection" Page 4-4 AA-6200

4.2 Software Basic Operation

(1) First, click on the . Then the "Load Parameters" will appear.

4

Basic Operation

Figure 4-5 : "Cookbook" Page in "Load Parameters" (2) In this page, select the element first. You can use one of the methods below to select the element. (a) Enter the element symbol directly in the element field from the keyboard. (b) Click on the ▼ button at the right of the element field, and select the element from the element symbol list shown in alphabetical order. (c) Click on button and select the element from the periodic table. (3) [Flame] radio button is already selected for the measurement method. (4) [Normal Lamp] radio button is already selected (AA-6200 doesn’t support SR method as the background correction method). (5) When using the autosampler, click on [Using ASC] check box. (6) After completing the settings, click on . Then the "Element Selection" page is displayed again and the selected element is shown in the table. (7) When plural elements are to be analyzed, return to this "Element Selection" page once and then click on button again to select the next element. Repeat the procedure below as required. Click on button → Select an element → Click on button (8) When returning to the Element Selection page after selecting an element, the selected element is added to the list one by one. If you need to delete any of them, click on the row to highlight it and then click on . The [Meas. 4-5 AA-6200

4.2 Software Basic Operation

Element] at the right lower of the page indicates the element to be analyzed first. (9) For details on button, refer to the section 5.5.1 in Chapter 5. Here, you can go ahead without using it. (10) Click on button. Although another message appears, go ahead by clicking on button. Then "Preparation Parameters" page will appear. NOTE When analyzing plural elements sequentially, the order on the "Element Selection" page becomes the measurement order. If you need to change the order, click on the element to highlight it and then click on or to move the row. If the [Meas. element] at the right lower of the page is different from the first row element, the measurement is started from the [Meas. Element] and the elements upper than it are not to be measured.

4

Basic Operation

4.2.1.4 Preparation Parameters

Figure 4-6 : "Preparation Parameters" Page First, select the row of the element to be set by clicking on its row to highlight it, then click on button. The "Preparation Parameters" page will appear. Set the parameters as below.

4-6 AA-6200

4.2 Software Basic Operation

4

Basic Operation

Figure 4-7 : "Edit Preparation Parameters" Page (1) Select "Calibration Curve" for [Measurement Type]. If you need to select "SMSA"(Simple Standard Addition Method) or use Standard Addition Method, refer to the section 4.9. (2) Select "1st" for [Order] of equation if the calibration curve is straight. You may also select "2nd" or "3rd" if it is curved. Anyway, you can change the order after measurement. So, select "1st" here. [Zero Intercept] is used to make a calibration curve equation that forcibly intercepts the origin. This setting can also be changed later.

NOTE After the data evaluation based on the QA/QC setup is executed, the calibration curve order, zero intercept and signal processing mode settings cannot be changed after the measurement. For details on QA/QC setup, refer to the section 5.6.8. (3) Pressing button displays the "Repeat Measurement Conditions" page. The number of measurements for the same one sample is set here. The default value of the number of measurement repetitions is "1" in the case of flame measurement. (4) Select [Conc. Unit] of the prepared standard samples. Click on ▼ button to 4-7 AA-6200

4.2 Software Basic Operation

select it from the list. (5) Input the [Weight Correction Factors]. These factors are necessary for calculating the actual concentration. The [Weight Factor], [Volume Factor], [Dilution Factor] and [Correction Factor] are used in the following equation. Actual concentration =(Conc.) × [Volume Factor] × [Dilution Factor] × [Correction Factor]/[Weight Factor]

4

Basic Operation

The actual concentration is calculated with the above equation. Note that the unit is not converted automatically. Convert the unit using [Correction Factor] if necessary (Refer to the example below). If the above calculation for actual concentration is not necessary, leave all the factors as "1" . Each factor is expressed in MRT work sheet and data print as follows. [Volume Factor] [VF] [Dilution Factor] [DF] [Correction Factor] [CF] [Weight Factor] [WF] (Example) 2g of sample was weighted, filled with water to 50ml, diluted to 5 times and measured. In this case, the actual concentration is calculated with the following equation using the factors; [Weight Factor]: 2(g), [Volume Factor]: 50(mL), [Dilution Factor]: 5(times) and [Correction Factor]: 1. Actual conc. = (Conc.) × (50 mL) × (5 times) × 1/ (2g) Also, if calculating the actual conc.(%) from the conc.(ppm) by converting the unit, use 0.0001 for [Correction Factor] since 1ppm is 0.0001%. Actual conc.(%) = (Conc.(ppm)) × (50 mL) × (5 times) × 0.0001/ (2g) (Note) Generally, "ppm" is the concentration unit of 10–6. In the atomic absorption analysis, "ppm" indicates both "µg/g" for solid samples and "µg/mL (mg/L)" for liquid samples.

4-8 AA-6200

4.2 Software Basic Operation

(6) Enter the [Number of STD]. Then a table composed of as many rows as the sample number is created in the [STD samples] preparation parameters. (7) Input the actual concentrations of the prepared standards into the table, although the default values from the cookbook are indicated on the table. When using the ASC, also input the turntable positions (1 to 60, R1 to R8). (8) [Blank Samples] Set up the periodic blank measurement here. Periodic Blank Measurement is a function to create a measurement procedure on the MRT to remove the influence of baseline drift by inserting a blank measurement in a fixed interval. Use it when the sample number is large or the baseline drift occurs. • When the [Periodic Blank] is not used Leave the [Periodic Blank] field "Off" . • When the [Periodic Blank] is used qClick on the [Periodic Blank] field and click on the ▼ button at the right of "Off" . Then the list for "On" / "Off" is displayed. Select "On" . wClick on the [Meas. Interval] field and enter the numerical value to insert the blank measurement in every some samples. e[Pos.] indicates the blank position on the ASC turn table. When using the ASC, click on the ▼ button at the right of [Pos.] and select the position from the list.

4

Basic Operation

(9) After setting the parameters, click on to return to the "Preparation Parameters" page. In the case of multi-element analysis, click on the next row to highlight it, then click on and set the parameters in the same way. (10) When completing all the settings, click on . Then the "Sample ID" page will appear.

4-9 AA-6200

4.2 Software Basic Operation

4.2.1.5 Sample ID

4

Basic Operation Figure 4-8 : "Sample ID" Page (1) In this "Sample ID" page, enter the number of samples first. Then enter the sample ID (sample name) into the cell of [Sample ID] from the keyboard one by one. (2) When using the same name with successive No. for all the samples, click on . Then the "Sample ID Collective Setup" dialog box will appear.

Figure 4-9 : "Sample ID Collective Setup" Dialog Box

4-10 AA-6200

4.2 Software Basic Operation

Put a check mark in the "Create Sample ID" check box, and enter a common sample name to [Name]. Then names with successive number are automatically created and shown in the table (e.g. Sample001, Sample002,...). Entering the first sample position in [ASC Start Pos.] sets the sample positions of the second and after in the table automatically. Click on to return to the "Sample ID" page. (3) You can input and change the name individually after the collective setup. (4) The [Pos.] in the table shows the sample position on ASC turntable. When not using the ASC, this is not required. (5) After completing the settings, click on . Then the "Sample Selection" page will appear.

4

Basic Operation

4.2.1.6 Sample Selection

Figure 4-10 : "Sample Selection" Page In this Sample Selection page, the samples to be measured for each element are selected. • [When all the samples are to be measured for all elements] Confirm that each field has a check mark and click on to proceed to the "Connect to Instrument/Send Parameters" page. 4-11 AA-6200

4.2 Software Basic Operation

• [When some of the samples are not to be measured for all elements] (1) Click the check box of the sample not to be measured to clear it. To clear some check boxes together, drag the mouse cursor to select the range, and press the DEL key on the keyboard or select "Not Measure" by clicking the right mouse button. (2) After completing the settings, click on to proceed to the "Connect to Instrument/Send Parameters" page.

4 4.2.1.7 Connect to Instrument/Send Parameters

Basic Operation Figure 4-11 : "Connect to Instrument/Send Parameters" Page Check that the power of the AA is already ON and click on . The "Initialize" dialog box is opened and AA main unit is initialized. At the step of [Wavelength Origin Search], the following message appears. "Please set slit width to 0.2nm." Set slit width to 0.2nm by the slit changing knob on the left side of the instrument and click on to close the message. After completing the initialization, click on to close the "Initialize" dialog box. After closing the "Initialize" dialog box, "Instrument Check List for Flame Analysis" is displayed.

4-12 AA-6200

4.2 Software Basic Operation

4

Basic Operation

Figure 4-11-2 : "Instrument Check List for Flame Analysis" To use the instrument safely, check the items indicated on this dialog box before igniting a flame. Put a check mark to the item after checking it. When all the items are marked, you can select . After completing the inspection, click on to close the dialog box. Then, click on in the "Connect to Instrument/Send Parameters" page to proceed to the "Optics Parameters for Lamp Position Adjustment" page.

4.2.1.8 Optics Parameters for Lamp Position Adjustment On the "Optics Parameters for Lamp Position Adjustment" dialog box (Figure 412), the PC automatically sets the wavelength and lamp current on the hollow cathode lamp using standard data for the element being analyzed. Note that this setting is applied to only the element to be firstly measured (element specified in [Meas. Element] at the right lower part in "Element Selection" dialog box and "Connect to Instrument/Send Parameters" dialog box).

4-13 AA-6200

4.2 Software Basic Operation

4

Basic Operation

Figure 4-12 : Optics Parameters for Lamp Position Adjustment Dialog Box (1) This dialog box displays default settings for Wavelength, Lamp Current, and Slit Width for the element specified in the [Meas. Element] field on the "Element Selection" dialog box. You can accept these default settings or change them as necessary. (2) Next, set the slit width of the main unit to the band width displayed in the [Slit Width] field. The slit selection knob is located on the left side of the AA-6200 main unit toward the back of the unit. (3) Since this dialog box is used for lamp adjustment, the lamp mode is fixed to Emission mode. On a later dialog box you will select the actual mode you will use for your analysis. (4) In [Socket #] , select the number (1 or 2) of the lamp socket connected to the hollow cathode lamp of the element. Rotate the hollow cathode lamp turret of the AA-6200 main unit and set the hollow cathode lamp of the specified element on the optical axis. (5) In the [Lamp ID], the currently used lamp ID (set at the time of lamp history data registration) is displayed. (6) In the [Lamp Status], a necessary message, for example, "Line Search is necessary" is indicated. NOTE In some elements, the lamp may be feebly bright even when it is off. This is not a defective of the equipment and does not affect the life of lamp. (7) When all settings are complete, select the [Lamp On] check box. The hollow cathode lamp illuminates. 4-14 AA-6200

4.2 Software Basic Operation

Perform coarse adjustment of the hollow cathode lamp position. (8) First, to check the beam, cut a square of white paper 4cm × 4cm and, using a straight edge as a guide, draw a straight line down the center of the paper. (9) Stand the square of paper on the center of the burner head so that the straight line is perpendicular to the burner slit. Use the line as a guide to ensure that the orange beam of the hollow cathode lamp is shining directly above the burner slit. (10) If the beam is not properly aligned, adjust the instrument so that the spot of light from the lamp is positioned directly above the burner slot. You can adjust the beam by rotating the hollow cathode lamp in the turret or using the position adjusting knob.

4

Basic Operation

Figure 4-13 : Line Search/Beam Balance Dialog Box (11) Next, click on the Line Search button. The "Line Search/Beam Balance" dialog box (Figure 4-13) opens and Line Search/Beam Balance is automatically executed if it is necessary. The monochromator is set to the wavelength of the analytical line for the specified element (Line Search), and the sensitivity adjustment of the detector automatically executes (Beam Balance). (12) When the [Line Search] and [Beam Balance] fields display "OK", click on the button to return to the previous dialog box ("Optics Parameters for 4-15 AA-6200

4.2 Software Basic Operation

Lamp Position Adjustment"). An error message may appear stating that the lamp energy is too low. If the energy is too low, raise the lamp Current value of the "Optics Parameters for Lamp Position Adjustment" dialog box. (13) button This is used to warm up the lamp of the next element to be analyzed after the current element. For details, refer to the section 5.5.6.1. (14) After all the settings are completed, click on to proceed to the "Lamp Position Adjustment" page.

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Basic Operation

NOTE When measuring plural elements, you cannot set parameters for the elements other than the current measurement one on the "Optics Parameters for Lamp Position Adjustment", "Lamp Position Adjustment", "Optics Parameters" and "Gas Flow Rate Setup" pages. If you use the ASC to measure plural elements automatically and you need to modify the parameters for other elements than the current measurement one, you can change these parameters by using the button in the "Element Selection" page.

4.2.1.9 Lamp Position Adjustment Figure 4-14 : Shows the "Lamp Position Adjustment" dialog Box. (1) The maximum value from the data observed so far displays in the [Max.] field and the minimum value in the [Min.] field. Current energy value displays in the [Current] field. To reset the current [Max.] and [Min.] values, click on the button. (2) Rotate the hollow cathode lamp in the turret around the optical axis or use the position adjusting knob to adjust the position of the hollow cathode lamp so that the current energy value get largest. (3) If the energy value exceeds 1.00, click on the button to return to the previous dialog box ("Optics Parameters for Lamp Position Adjustment"). Then, execute the Line Search again.

4-16 AA-6200

4.2 Software Basic Operation

4

Basic Operation

Figure 4-14 : Lamp Position Adjustment Dialog Box (4) When fine adjustment of the lamp position is complete, click on the button to proceed to the "Optics Parameters" dialog box.

4.2.1.10 Optics Parameters The "Optics Parameters" dialog box in shown in Figure 4-15.

Figure 4-15 : Optics Parameters Dialog Box On the "Optics Parameters" dialog box, the lamp mode is set for the element to be analyzed. This dialog box is similar to the "Optics Parameters for Lamp Position 4-17 AA-6200

4.2 Software Basic Operation

Adjustment" dialog box ; however, on that dialog box the lamp mode is fixed and on this dialog box it is modifiable. (1) From the [Lamp Mode] pull down list, select Emission, Non-BGC, or BGC-D2. These modes are used as follows.

4

Emission mode This mode measures concentrations by measuring the light emission energy of the substance. Use this mode to adjust the position of the hollow cathode lamp as well.

Basic Operation

Non-BGC mode This mode is used for atomic absorption analysis that does not require background correction. It is also used for atomic absorption analysis in the long wavelength range (430~900nm) in which the deuterium lamp cannot be used. BGC-D2 mode Background correction is performed in this mode by the D2 method. (2) Then click on the button, the "Line Search/Beam Balance" dialog box appears. When the Line Search/Beam Balance is necessary, it is automatically executed. If the Line Search/Beam Balance has already finished, the result is displayed. (3) When all results display "OK", click on the button. (4) Click the button in the "Optics Parameters" dialog box to proceed to the "Gas Flow Rate Setup" dialog box. For function of [Wavelength Memory], refer to the section 5.5.6.3.

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4.2 Software Basic Operation

4.2.1.11 Gas Flow Rate Setup Lastly, set the gas conditions. The default conditions are appropriate for most types of analysis.

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Basic Operation

Figure 4-16 : Gas Flow Rate Setup Dialog Box (1) On the "Gas Flow Rate Setup" dialog box, select the type of flame to be used from the [Flame Type] list box. You must use the 10cm slot burner supplied as a standard accessory with an Air-C2H2 flame. NOTE To use a N2O-C2H2 flame, use the high temperature burner head optional accessory. When the [Flame Type] is set to "N2O-C2H2", insert the pin attached with the high temperature burner head into the burner select sensor. The Air-C2H2 flame is automatically used for the ignition then the flame is automatically switched to N2O-C2H2 after that. (2) Adjust the gas flow rate of the main unit to match the values displayed in the [Fuel Gas Flow Rate] and [Support Gas Flow Rate] fields on the "Gas Flow Rate Setup" dialog box. Open the main valve of the gas cylinder and the air compressor and supply the gas. Then, press the Purge button located under the oxidant flow meter on the left of the main unit. Set the gas flow rate with the flow rate adjusting knob. The [Fuel Gas Flow Rate] and [Support Gas Flow Rate] fields are information fields only. Entering new information does not affect the actual gas flow. 4-19 AA-6200

4.2 Software Basic Operation

CAUTION 1. Fuel gas flows from the burner slot when the Purge button is pressed. Never allow fire near the burner head while the Purge button is pressed. 2. Ensure that the room is well ventilated. 3. Do not press the Purge button for more than five seconds. Wait at least ten seconds before pressing the Purge button again.

(3) After all the settings are completed, click on button. The Wizard ends and the main window appears. If you want to save these conditions as a template file, proceed to the section 4.2.2. If you want to start the measurement, proceed to the section 4.3.1.

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Basic Operation

CAUTION Before igniting the flame, carefully read 4.8 Igniting and Extinguishing the Flame and check safety precautions.

4.2.2 Saving the Template If you want to use the parameters set with the above procedures from the next time, you can save them as a template. Then you can load it in the "Wizard Selection" dialog box. (1) Click on [File] in the menu bar and select [Save As].

Figure 4-17 : "Save As" Dialog Box 4-20 AA-6200

4.2 Software Basic Operation

(2) Select "template (*.taa)" for [Save as type]. The extension of the file name displayed in [File name] is changed to ".taa". (e.g.) If "notitle.aa" is displayed in [File name] when the "Save As" dialog box is opened, selecting "template (*.taa)" changes the file name to "notitle.taa". (3) Input the file name. Leave the extension as ".taa". (e.g.) Change the part "notitle" in the "notitle.taa" to a name you like. (4) Press button. "Save As" dialog box is closed and the template file is saved.

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Basic Operation 4-21 AA-6200

4.3

Measurement Procedures

After completing all the settings, prepare the samples. Perform the measurement following the procedure indicated on the MRT work sheet. The current row is highlighted and its [Action] field shows the type of measurement. When using the ASC, set the samples in proper positions. If no setting is made on the MRT work sheet, a message appears to indicate that no schedule exists. In this case, select [Parameters]-[Schedule Creation Wizard] from the menu and set the measurement procedures.

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Basic Operation

NOTE If a menu or dialog box is kept opened during the measurement operation, the measurement operation may be interrupted. Be careful about it when checking the setup parameters during the operation.

4.3.1 Measurement Operation In the case of flame method, read the section "4.8 Igniting and Extinguishing the Flame" thoroughly before starting the measurement. Confirm that the gases are supplied at correct pressures and the burner head is mounted properly. If the lamp warmup time (unit: minute) is set, start the measurement after the time passes since the lamp is turned on. [Manual Measurement] (1) Igniting the Flame CAUTION Before igniting a flame, be sure to check that the U-tube is filled with water. If an ignition should be done without filling it with water, a flashback may be caused. Simultaneously press the IGNITE(white) button and PURGE(black) button on the front of the AA main unit to ignite the flame. (2) Auto Zero At the [AUTO ZERO] row on the MRT work sheet, put the suction nozzle into vaporized water (or solvent) and spray it. When the signal of real time graph is stabilized, click on at the bottom of the Main window (or press the F5/F6 key). Also, the Auto Zero can be executed by pressing (or F3 key), although the operation result of Auto Zero execution is 4-22 AA-6200

4.3 Measurement Procedures

not indicated on the MRT work sheet in this case. (3) Blank Measurement (if necessary) Spray the blank sample and click on at the bottom of the Main window (or press the F4 key). The "BLANK" row is inserted on the MRT work sheet and the measurement result is displayed. When the "BLANK" row is prepared on the MRT work sheet beforehand, press (or F5/F6 key). If the standard or unknown samples are measured after executing the blank measurement, their measured values (absorbance or energy) are indicated after the measured blank value is subtracted from their actual measured values. The difference between this measured blank value and the actual measured standard or unknown sample value is displayed in [Abs] ( or [Energy]) on the MRT until the next blank measurement is executed. (4) Standard Measurement Spray the standard sample. When the signal of real time graph is stabilized, click on at the bottom of the Main window (or press the F5 or F6 key) according to the set order. Measure the standard sample while checking that it accords with the current row on the window. If the repeat measurement is selected, clicking on inserts a new row for repeat measurement according to the set repeat parameters. Repeat the measurement following the row indication. (5) Checking the Calibration Curve After measuring the standard samples, check the calibration curve displayed on the right upper of the window. If the calibration curve graph display is too small, set the mouse cursor onto the border of the calibration curve graph to indicate an arrow with two directions. Drag it to specify the range ("drag" means moving the mouse while holding down the left mouse button).

4

Basic Operation

If the calibration curve is correctly made, proceed to the measurement of unknown samples. If you want to change the order or other parameters for calibration curve, click on above the calibration curve graph then make a change on the "Change Calibration Curve Condition" dialog box. (6) Unknown Sample Measurement Spray the unknown sample. When the signal of real time graph is stabilized, click on at the bottom of the Main window (or press the F5 or F6 key). If the repeat measurement is selected, clicking on inserts a new row for repeat measurement according to the set repeat parameters. Repeat the measurement following the row indication. Then continue to measure the 4-23 AA-6200

4.3 Measurement Procedures

unknown samples according to the specified order. Measure an unknown sample while checking that it accords with the current row on the window. If key is pressed when all the rows on the MRT work sheet have been executed, a new "UNK" row (unknown sample row) is added and its measurement result is displayed. When the "Periodic Blank" is ON in the "Edit Preparation Parameters" dialog box, "BLK" rows (blank measurement rows) are already inserted in the specified interval. Spray the blank at the rows and measure it.

4

Basic Operation

If you want to make the size of MRT (Measurement Result Table) work sheet larger, set the mouse cursor onto the upper border of the table to indicate an arrow with two directions. Press down the mouse left button and drag it to specify the range. More number of rows can be displayed. For details on changing sizes or using a scroll bar, refer to the Windows documentation. (7) Finishing the Measurement After finishing the measurement, put the suction nozzle in vaporized water and spray it for a while. Then press the EXTINGUISH(red) button on the front of the AA main unit to extinguish the flame. [Using the ASC] NOTE When using the ASC, put a check mark in the check box of [Using ASC] in "Sequence" page of "Edit Parameters" dialog box.

When using the ASC, verify that the position of each actual sample on the ASC turn table accords with the setting on the MRT work sheet. (1) Igniting the Flame Simultaneously press the IGNITE(white) button and PURGE(black) button on the front of the AA main unit to ignite the flame. (2) Starting the ASC (Auto Sample Changer) Click on at the bottom of the Main window (or press the F5 or F6 key) according to the set order. The automatic measurement is started with the ASC. (3) Extinguishing the Flame After finishing the measurement, press the EXTINGUISH(red) button on the 4-24 AA-6200

4.3 Measurement Procedures

front of the AA main unit to extinguish the flame (A flame is automatically extinguished if the automatic flame extinction is selected). (4) Checking the MRT work sheet Check the measured results on the MRT work sheet. If a remeasurement is necessary, refer to the section 4.7.2. When printing or saving the data, proceed to the section 4.4.

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Basic Operation 4-25 AA-6200

4.4

Saving/Printing/Deleting the Data

4.4.1 Saving the Data When all measurements are completed, save the data. Select [File]-[Save As] from the menu bar, and enter the file name in the "Save As" dialog box. File extension is limited to ".aa". NOTE A measurement data whose repeat measurement has not finished is not saved in the file. If the data is necessary although the repeat measurement cannot be completed, print it out before ending the AA software.

4

4.4.2 Printing the Data Basic Operation

Select [File]-[Print Data/Parameters] or [Print Table Data] from the menu bar. Then "Select Schedule" dialog box will appear. Click on the elements ( "Summary Report" is also available for [Print Table Data]) to highlight it. Then click on . Printing will be executed. [Print Data/Parameters] The measurement parameters and measured data are printed. You can select the items to be printed in the [File]-[Print Style]-[Print Style Setup] page. [Print Table Data] The current MRT work sheet is printed. You can select or change the items to be printed by selecting [File]-[Print Style...]-[Table Show/Hide] page from Menu. In the case of [Summary Report], the columns shown in the MRT work sheet on the window are printed. For details on printing, refer to the sections 5.2.9 to 5.2.12.

4.4.3 Deleting the Data If you want to use the same measurement conditions again, you can delete only the data with leaving the measurement sequence. Execute [Edit]-[Clear Measurement Result] from the menu bar. When deleting all of the measurement parameters, measured data and measurement sequence, select [File]-[New] from the menu bar to open a new file.

4-26 AA-6200

4.5

Completing the Measurement

(1)When the measurement is completed, verify that the flame is extinguished and tighten the main valve of the gas cylinder and compressor in the case of flame method. (2) Quit the software. For example, select [File]-[Exit] from the menu bar. The communication with the instrument is shut off first, then the main window is closed. It takes approximately 30 seconds. (3) Turn off the power switch of AA main unit. (4) Turn off the power switches for peripheral equipments such as the ASC.

4

Basic Operation 4-27 AA-6200

4.6

Explanation of Main Window

When the Wizard is completed, the following main window appears. q Menu bar w Standard tool bar e Measurement element tool bar (Display and switch the current measurement element) r Absorbance digital display t Real time graph y Peak profile (latest four measurements and overlay display) u Calibration curve tool bar (Selection of calibration curve and type) i Calibration curve display o MRT work sheet !0 Function buttons !1 Status bar

4

Basic Operation

e

ru

y

i

q w

t

o

!0 !1 Figure 4-18 : Main Window NOTE While the [Properties] is opened from the right mouse button menu on the graph or MRT work sheet, the measurement is stopped. In this case, the measurement can be continued again when the [Properties] is closed. 4-28 AA-6200

4.6 Explanation of Main Window

4.6.1 Menu bar Place the mouse cursor onto the menu ([File],[Edit],[Parameters],etc.) and click on it. Then a drop-down menu appears. Select an item from the menu and click on it. For details on each item, refer to Chapter 5.

4.6.2 Standard tool bar The items frequently used are displayed in the tool bar. Quick selection is possible if you use this instead of selecting from the menu bar. Each tool function is described below.

4

New

Basic Operation

: All the data and parameters are cancelled and parameters are set newly. (Same as [File]-[New] in the menu bar) Open : A file already created is opened. (Same as [File]-[Open] in the menu bar) Save As : Current data and parameters are saved in the file. (Same as [File]-[Save As] in the menu bar) Print : Data and parameters are printed. (Same as [File]-[Print Data/Parameters] in the menu bar)

4.6.3 Measurement element tool bar The element currently measured (or to be measured) is indicated. If you want to change the element, click on the ▼ and select one from the drop-down list. Then the Measurement Preparation Wizard starts. Set the parameters if necessary and click on (or to close the sheet without changes). The MRT work sheet is also changed to that for selected element.

4.6.4 Absorbance digital display The current absorbance value (or emission intensity in emission mode) is displayed. When the instrument is BUSY, it is highlighted.

4.6.5 Real time graph The changing absorbance value (or emission intensity in the case of emission mode) under measurement is displayed in analog. You can check the peak shape and baseline conditions with this graph.

4-29 AA-6200

4.6 Explanation of Main Window

[Right mouse button menu] If you want to change the scale or print the graph, place the cursor in the graph area and click on the right button of the mouse. Then the pop-up menu shown in Figure 4-19 appears. Select an item and make settings.

4

Basic Operation Figure 4-19 : Right Mouse Button Menu (Real Time Graph) (1) [Properties...] [Real Time Graph Scale] (Flame) You can change the graph ordinate and abscissa scale. Enter the maximum value and minimum value in [Ordinate Max] and [Ordinate Min], respectively. Enter a numeric value in [Time Interval] (unit: second) for abscissa. Clicking on sets them to the values specified in [Parameters]-[Default Parameters]-[Graph]. [Colors] You can select colors of [Data Line], [BG Line], [Background] and [Grid]. Click on the ▼ and select the color from the list. [Grid] You can select grids to be displayed from [Major & Minor Grids], [Major Grid] or [None]. You can also select the line type of [Major Grid Line] and [Minor Grid Line]. (2) [Copy] Executing [Copy] copies the currently displayed graph to the clipboard. Then start up the word processor or other application and move the cursor to the location where you want to paste the graph. Select [Paste] command in the word processor, etc., and the graph will be displayed at the cursor position. 4-30 AA-6200

4.6 Explanation of Main Window

(3) [Radar] The display range is automatically set so as to display the entire graph. (4) [Print...] Selecting this opens the "Print" dialog box. Check the printer name, copies, etc. and click on . The real time waveform currently displayed will be printed.

4.6.6 Peak Profile (Latest four measurements and overlay display) The latest four measurement signal profiles are displayed. Both standard samples and unknown samples are displayed here. The abscissa shows time and the ordinate shows absorbance value (emission intensity in EMISSION mode). The signal profile is displayed during the integral time. In the rightmost area, plural number of signal profiles can be overlapped and displayed. Specify their colors in the [Graph] on the MRT work sheet.

4

Basic Operation

[Right mouse button menu] If you want to change the scale or print the graph, place the cursor in the graph area and click on the right button of the mouse. Then the pop-up menu shown in Figure 4-20 appears. Select an item and make settings.

Figure 4-20 : Right Mouse Button Menu (Peak Profile) (1) [Properties...] [Scale] You can set the maximum value [Max] and minimum value [Min] of the graph ordinate and abscissa scales. The scale setting is used commonly for 4-31 AA-6200

4.6 Explanation of Main Window

the five graph. Clicking on sets the Y-axis to the value specified in [Parameters]-[Default Parameters]-[Graph]. [Colors] You can select colors of [Data Line], [BG Line], [Background] and [Grid]. Click on the ▼ and select the color form the list. [Grid] You can select grids to be displayed from [Major & Minor Grids], [Major Grid] or [None]. You can also select the line type of [Major Grid Line] and [Minor Grid Line].

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Basic Operation

(2) [Draw BG Line] Selecting this displays a profile of background signal. The display is deleted by selecting this menu again (The check mark of [Draw BG Line] is deleted). (3) [Copy] Executing [Copy] copies the currently displayed graph to the clipboard. Then start up the word processor or other application and move the cursor to the location where you want to paste the graph. Select [Paste] command in the word processor, etc., and the graph will be displayed at the cursor position. (4) [Cross Hair] This is used to read coordinate values in the graph. Move the mouse cursor in the graph area first, then select [Cross Hair]-[Display] from the right button menu. When the mouse cursor is in the graph area, the coordinate values at the cross hair intersection position are displayed. The graph area is divided into five areas, and the coordinate values can be read only in each area. If you want to read an coordinate value in another graph, erase the cross hair cursor once by clicking the right mouse button and selecting [Cross Hair]-[Display] (then the check mark of [Display] will be deleted), then set the mouse cursor to another area and select [Cursor][Display] again. While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-[Lock] will fix the cross hair at that position. To free the cross hair, click on the right mouse button again and select [Cross Hair]-[Lock] (then the check mark of [Lock] will be deleted). While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-[Display] (then the check mark of [Display] will 4-32 AA-6200

4.6 Explanation of Main Window

be deleted) will erase the cross hair regardless of the [Lock] condition. (5) [Radar] This automatically sets the display range so that the selected graph by the mouse cursor is displayed in an appropriate size. At the same time, other four data scales are also changed to the same scale. (6) [Print...] Move the mouse cursor to the graph area to be printed. Then the "Print" dialog box appears. Check the printer name, copies, etc. and click on . Only the selected peak profile will be printed.

4

4.6.7 Calibration Curve Display Basic Operation

After the standard samples are measured, the calibration curve is created and displayed. (1) Calibration Curve Display If you want to check a calibration curve other than the currently displayed one, set the button to OFF (the button is embossed) and enter the element name and calibration curve number (C#). The settings here are limited to display and recalculation is not executed. (2) Changing the Calibration Curve Conditions If you want to change the calibration curve parameters after viewing the created calibration curve, use the button. Clicking on opens the "Change Calibration Curve Condition" dialog box where you can change order of calibration curve and permission of zero intercept.

Figure 4-21 : "Change Calibration Curve Condition" Dialog Box

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4.6 Explanation of Main Window

Changing the condition and clicking on immediately recalculates the concentration of unknown samples based on the new calibration curve and renews the quantitation result on the MRT work sheet. The recalculation is only applied to the unknown sample using the same C# as changed calibration curve. The result is invalid when the element is different, or when the C# is different even if the element is same.

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Basic Operation

NOTE After the data evaluation based on the QA/QC setup is executed, the calibration curve order, zero intercept and signal processing mode settings cannot be changed after the measurement. For details on QA/QC setup, refer to the section 5.6.8.

[Symbols in Calibration Curve Equation] When a calibration curve is created, calibration curve equation is displayed above the graph. Symbols in a calibration curve equation mean as follows; Symbol Abs E Conc r e ^

Meaning Absorbance Energy (Only for EMISSION mode) Concentration Correlation Coefficient When a coefficient is very small, this symbol is used to express it by using index. "AeB" means "A × 10B" This symbol means power. "Conc^2" means the second power of concentration.

(Example) Calibration curve equation q means equation w Abs = -9.5e-005Conc^2 + 0.011636Conc + 0···············q Abs = -9.5 × 10-5 × Conc2 + 0.011636 × Conc + 0········w

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4.6 Explanation of Main Window

[Right mouse button menu] If you want to change the scale or print the graph, place the cursor in the graph area and click on the right button of the mouse. Then the pop-up menu shown in Figure 4-22 appears. Select an item and make settings.

4

Basic Operation

Figure 4-22 : Right Mouse Button Menu (Calibration Curve Display) (1) [Properties] [Scale] You can set the maximum value [Max] and minimum value [Min] of the graph ordinate and abscissa scales. Enter the values. [Options] You can set the graph color and data point shape. Clicking on each ▼ of [Data Point], [Calibration Curve], [Background] and [Grid] displays the list from which you can select the color. The shape of [Data Point] can be selected from the list displayed by clicking on the ▼ . [Grid] You can select grids to be displayed from [Major & Miner Grids], [Major Grid] or [None]. You can also select the line type of [Major Grid Line] and [Minor Grid Line]. (2) [Copy] Executing [Copy] copies the currently displayed graph to the clipboard. Then start up the word processor or other application and move the cursor to the location where you want to paste the graph. Select [Paste] command in the word processor, etc., and the graph will be displayed at the cursor position. 4-35 AA-6200

4.6 Explanation of Main Window

(3) [Cross Hair] This is used to read coordinate values in the graph. Move the mouse cursor in the graph area first, then select [Cross Hair]-[Display] from the right button menu. When the mouse cursor is in the graph area, the coordinate values at the cross hair intersection position are displayed. To erase the cross hair, select [Cross Hair]-[Display] (then the check mark of [Display] will be deleted). While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-[Lock] will fix the cross hair at that position. To free the cross hair, click on the right mouse button again and select [Cross Hair]-[Lock] (then the check mark of [Lock] will be deleted). While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-[Display] (then the check mark of [Display] will be deleted) will erase the cross hair regardless of the [Lock] condition. (4) [Radar] This automatically sets the display range so that the entire graph can be displayed. (5) [Print] Selecting this menu item opens the "Print" dialog box. Check the printer name, copies, etc. and click on . Then the calibration curve currently displayed is printed out. This menu is not displayed when no calibration curve exists.

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Basic Operation

4.6.8 MRT work sheet It is possible to create measurement sequence, execute measurement, display the result, and calculate the actual concentration in the MRT work sheet. If measurement of plural elements is required, the work sheet is prepared for each element and the work sheets can be changed over with the tab. In [Summary], the measurement result for sample can be displayed at one time. The tab title consists of the element name and comment. As the comment, only the first line is displayed when a line feed is included in the comment, and the first ten characters are displayed when the number of characters exceeds ten. The comment is inputted by selecting [Parameters]-[Edit Parameters]-[Comment] page from the Menu bar. For details on each item in MRT work sheet, refer to the section 4.7. NOTE The currently measured element (or the element about to be measured) can be changed not by the tab at the left lower of the main window but by the measurement element tool bar. 4-36 AA-6200

4.6 Explanation of Main Window

4.6.9 Function buttons Functions of Wizard selection, auto zero execution, blank measurement, starting sample measurement, test measurement, ASC rinse are assigned to the buttons at the left below the MRT work sheet. These correspond to function keys on the keyboard as follows. button : {F3} key button : {F4} key button : {F5, F6} keys This switches to button during measurement. button : {F9} key button : {F10} key

4

Basic Operation

The relations between the current measurement mode and the available buttons are shown below. "Auto (using ASC)" means the status where the ASC is connected and the [Using ASC] check box is checkmarked in [Parameters]-[Edit Parameters]-[Sequence] page from the Menu bar. Flame Manual

Flame Auto(using ASC)

O

O

O

×

O

O

×

×



O = Available

× = Not available

Clicking on button executes the Auto Zero while rinsing the nozzle in the case of flame auto-measurement (using ASC). In other cases, only the Auto Zero is executed. When clicking on button, nozzle rinse is executed. The nozzle rinse time in flame measurement is set in "Configuration" dialog box opened by selecting [Instrument]-[Configuration] from Menu. If the setting is "0" , 10 seconds rinse is executed regardless the setting. Clicking on stops the measurement. However, while acquiring the data, the measurement is stopped after the data acquisition is finished. is not available for AA-6200.

4-37 AA-6200

4.6 Explanation of Main Window

4.6.10 Status bar

q

w

e

r

t

y

Figure 4-23 : Status Bar

4

Basic Operation

The current measurement mode, operating mode, operating status of instrument, and connecting status of peripheral equipments (ASC) are indicated here. qDisplays current operating status of the instrument and error messages. wDisplays the hollow cathode lamp which is currently lit and its socket number. While the lamp is lit, the pane pops up. eDisplays the hollow cathode lamp which is under warming-up and its socket number. While the lamp is lit, the pane pops up. rDisplays whether the deuterium lamp is lit or not. When the lamp is lit on, the pane pops up. The "Lamp Status" dialog box can be displayed from the [Lamp Status] menu displayed by clicking the right mouse button in the regions of w to r. tDisplays whether the ASC is connected. When it is connected, "ASC" is displayed. yDisplays the current connecting status of the instrument. OFF The communication between the instrument and the PC is off. READY The instrument is ready to execute commands or conduct measurement. BUSY The instrument is executing a command. While this is displayed, another command cannot be executed.

4-38 AA-6200

4.7

Operating the MRT work sheet

In the MRT (Measurement Result Table) work sheet, the functions of setting of measurement sequence, execution of measurement, result display, actual concentration calculation, and setting of ASC sample position are integrated. For example, if you create a calibration curve by measuring three standard samples and measure eight unknown samples, the measurement is proceeded in the following procedure. Row 1 to 3 : Executes measurement of standard samples. Row 4 to 11 : Executes measurement of unknown samples (SAMPLE001 to SAMPLE008)

4

Basic Operation

As the measurement procedure, prepare the sample shown in the [Action] column and click on . You can proceed the measurement in the order from top row to down. When a repeat measurement is set, rows for repetition are inserted at the time of measurement.

4.7.1 Fields of MRT work sheet This section explains about the fields of MRT work sheet.

Figure 4-24 : MRT work sheet (1) [Action] Clicking on the cell in this field opens the drop-down list, showing the following indications. This [Action] field contains the measurement operations, operation using the ASC, QA/QC operation, etc.. For details on QA/QC, refer to the section 5.6.8. 4-39 AA-6200

4.7 Operating the MRT work sheet

NOTE 1. Executing "FILESAVE" overwrites and saves the file even if the file of the same name exists. 2. When the path name is not set at all in [FILESAVE] or [FILEEXPORT], a path name is created based on the setting in [File]-[Auto Save]. When only the file name is set, the file is saved in the folder that was used in the last time for "Open" or "Save as" screen. 3. To enable the QA/QC actions, it is necessary to put a check mark in the check box of each QC type in "QA/QC Setup" page.

4

Basic Operation Figure 4-25 : Drop-down List of [Action] BLK

STD UNK CAL-CHK

4-40 AA-6200

: Specifies the blank sample measurement. The measured value of blank sample is subtracted from the subsequent measured values of standard and unknown samples until a new blank measurement is done. : Specifies the standard sample measurement by calibration curve method. : Specifies the unknown sample measurement by calibration curve method. : Specifies the evaluation of calibration curve after the standard sample measurement (The correlation coefficient is checked). This is usually inserted to the row just after the last "STD" . This setting is not necessary in the case of standard addition

4.7 Operating the MRT work sheet

method or simple standard addition method because the evaluation is done at "MSA-RES" row. QC : Specifies the measurement and evaluation by LCS (Laboratory Control Sample/Standard substance). SPIKE : Specifies the measurement and evaluation by SPK (Pre-Digestion Spike/ addition and recovery check without pretreatment). This is usually inserted to the row just after the objective "UNK" . RESLOPE : Specifies the measurement for sensitivity correction (Usually, the standard sample of highest concentration is used). After this, "A,B,C..." is added to C# on the MRT and a new calibration curve number (C#) is created. MSA : Specifies the measurement by standard addition method. SMSA : Specifies the unknown sample measurement by simple standard addition method. MSA-RES : Specified as the result of standard addition method. When the measurement of a set of standard addition samples is finished, the calibration curve is created and the result is indicated in this row at the same time. AUTOZERO : Shifts the current displayed value to zero. In the case of flame measurement using the ASC, the Auto Zero can be executed while aspirating the sample. The aspirating time (0 to 600 seconds) in second unit can be specified in [Sample ID] field. RINSE : When the ASC is used, the nozzle is rinsed. The rinse time (0 to 600 seconds) in second unit can be specified in [Sample ID] field. CLEANING : Specifies cleaning of the graphite tube This is not available to AA6200. PAUSE : Specifies temporary stop until the is selected. Input a message to be displayed on the message box in the [Sample ID] field. WAIT : Specifies a stop in a fixed time. Input waiting time (0 to 7200 seconds) in the unit of second in the [Sample ID] field. COMMAND : Specifies execution of command line. Specify the command to be executed in the [Sample ID] field. FILESAVE : Specifies the file saving of the data collected so far. Specify the file name in the [Sample ID] field. FILE EXPORT : Specifies the text file saving of the data collected so far on the MRT work sheet. Specify the file name in the [Sample ID] field.

4

Basic Operation 4-41

AA-6200

4.7 Operating the MRT work sheet

(2) [Sample ID] In normal operation, sample ID is entered in this field. Sample name can be entered only when [Action] field indicates measurement of standard sample or unknown sample (STD, UNK, BLK, QC, SPIKE, RESLOPE, MSA, SMSA and MSA-RES). When the [Action] is CAL-CHK, the sample name cannot be entered. When the Element Selection Wizard or Schedule Creation Wizard was executed, the sample name set in the "Sample ID" page is entered when [Action] is unknown sample. When the [Action] is standard sample, the name automatically given in the "Edit Preparation Parameters" dialog box (STD1, STD2,...) is entered. In the following cases, the [Sample ID] has a special meaning. a) When "RINSE" is set in flame auto-measurement (using ASC), enter the aspiration time in second unit (0 to 600 seconds) in this [Sample ID] . b) When "PAUSE" is set, enter the message to be displayed on the message box in this [Sample ID]. c) When "WAIT" is set, enter the wait time of second unit in this [Sample ID] (0 to 7200 seconds). d) When "COMMAND" is set, describe the command line in this [Sample ID]. e) When "FILESAVE" is set, enter the file name together with path to save the data measured so far (e.g. C:¥AA¥WATER CU.aa). Use ".aa" for extension. f) When "FILEEXPORT" is set, enter the file name together with path. Then the data on the MRT work sheet data of the currently measured element is saved in a text file (e.g. C:¥AA¥WATER_CU.txt). Use ".txt" for extension. (3) [Graph] When overlaying the peak profiles, click on the right part of the cell and select the color of data lines from the list. The overlaid profiles are displayed on the rightmost of peak profile area. On the other hand, the BG lines are overlaid by the same one color. (4) [X] (Exclusion) Double clicking this excludes the data in the row. Double clicking again enables the data to be recovered. (5) [M] (Modified) Rewriting the absorbance data after measurement displays M mark (Modified). Once rewritten, this check mark is always displayed and the original data cannot be recovered. Only absorbance can be written. (6) [Q] When the control standard which is set by selecting [Parameters] - [Edit

4

Basic Operation 4-42

AA-6200

4.7 Operating the MRT work sheet

Parameters] - [QA/QC Setup] page from the menu bar is applied to the row, a check mark is indicated. Marked data cannot be excluded or modified. For details on "QA/QC setup" page, refer to the section 5.6.8 (7) [True Value (and unit)] The set concentration (and unit) of standard samples is indicated. This can be entered only when the [Action] is STD, SPIKE, RESLOPE, QC or MSA. In the case of "SPIKE" , enter the added concentration. (8) [Conc. (and Unit)] Displays the result of concentration obtained with measurement. As the [True Value] column heading, the unit specified in the "Preparation Parameters" page is automatically displayed. (9) [Abs.] Displays the measured absorbance. Energy intensity is displayed instead in the case of EMISSION mode. If a blank measurement is executed prior to this, the value is indicated after the measured blank value is subtracted from the actual measured value. (10) [BG] For measurement in BGC-D2 mode, absorbance of background signal is

4

Basic Operation

displayed. This is not displayed in the lamp modes in which the background signal is not acquired. (11) [Pos.] Indicates the sample position in the turn table of the autosampler (ASC). For details, refer to the instruction manual provided with the ASC. (12) [WF] [VF] [DF] [CF] Each acronym means as follows. [WF] [Weight Factor] [VF] [Volume Factor] [DF] [Dilution Factor] [CF] [Correction Factor] These are factors necessary for actual concentration calculation. The factors set in [Weight Correction Factors] in the "Edit Preparation Parameters" dialog box are displayed. For details on the equation of actual concentration calculation, refer to the section 5.5.2.1. (13) [Actual Conc.] Indicates the result of actual concentration calculation. For the calculation, the factors of WF, VF, DF and CF are used. 4-43 AA-6200

4.7 Operating the MRT work sheet

(14) [Actual Conc. Unit] Enter the unit used for actual concentration of the sample. Clicking on the right part of the cell opens the drop-down list from which the unit can be selected. Note that changing this unit does not recalculate the actual concentration. It is necessary to change the factors used for calculation. (15) [%RSD] [SD] [%R] The [%RSD] and [SD] are calculated in repeat measurement. The [%R] is calculated when "QC" or "SPIKE" is measured. For details on these calculation equations, refer to the section 5.6.2 and 5.6.8. (16) [C#] Indicates calibration curve number. When plural calibration curves are created on the same sheet, number is put in the order of creation and indicated. If entering a changed number, in the case of standard sample, a calibration curve is created by the standard samples of the same curve number and in the case of unknown sample, the concentration is calculated using the calibration curve of the entered number. This can be entered when the [Action] is STD, UNK, CAL-CHK, QC, SPIKE, RESLOPE, MSA or SMSA. This number is also used when selecting the calibration curve to be displayed (refer to 4.6.7). (17) [Out of Control Remark] A Note is displayed when QA/QC function judges that the acquired data is out of standard range. (18) [Date] Displays the date when the data was obtained by measurement. (19) [Time] Displays the time when the data was obtained by measurement. In the case of repeat measurement, the time displayed in the average row is the time of the first measurement.

4

Basic Operation 4-44

AA-6200

4.7 Operating the MRT work sheet

4.7.2 Right Mouse Button Menu Clicking on the right mouse button on the MRT work sheet opens the pop-up menu as below.

4

Basic Operation

Figure 4-26 : Right Mouse Button Menu (MRT work sheet) (1) [Properties] [Table Show/Hide] You can select to show or hide each column on the MRT work sheet. Only checkmarked items are displayed. Click on the item you don't want to show, and erase the check mark. The show/hide selection for each column has no relation to the print items in the [File]-[Print Table Data]. To select the items to be printed in Table Print, select [File]-[Print Style] from the menu and select the items in "Table Show/Hide" page. When the ASC is set not to be used in the [Parameters]-[Edit Parameters][Sequence], the [Pos.] is not shown or printed, even if it is set to be shown or printed in the "Table Show/Hide" page.

4-45 AA-6200

4.7 Operating the MRT work sheet

4

Basic Operation

Figure 4-27 : Table Show/Hide (MRT work sheet) [Row Style] Font (style, size, etc.), color and ruled line type can be set for each row group (row and column header, basic style, current row, measurement result row and excluded row).

Figure 4-28 : Row Style (MRT work sheet) 4-46 AA-6200

4.7 Operating the MRT work sheet

(2) [Hide Repetition] When this is selected in the case of repeat measurement, only the row of average value is shown and the rows of repeating process are not shown. The repetition rows are not printed in the "Print Table Data", either. While this is selected, a check mark is indicated in the drop-down menu. (3) [Hide Excluded Row] When this is selected, a row with a check mark in its [X](excluded) field is not shown. The excluded rows are not printed in the "Print Table Data", either. (4) [Hide Blank] When this is selected, a row of blank measurement is not shown. The blank rows are not printed in the "Print Table Data", either. (5) [Hide Command Row] When this is selected, a row whose [Action] field is "Command" is not shown. The command rows are not printed in the "Print Table Data", either. (6) [Keep Meas. Row Visible] When this is selected, the MRT work sheet is automatically scrolled as the measurement proceeds so that the row under measurement may be always displayed. (7) [Add Successive No. to Meas.] Selecting this puts successive numbers to "UNK" and "SMSA" of [Action]. This setting also has an effect on "Print Table Data". (8) [Remeasure Selected Range] When excluding measured rows and remeasuring the sample, the operation is as follows. qFirst, select rows to be remeasured by using the mouse (Click the first row and drag to the last row while pressing the button). In the case of repeat measurement, the selected range must include the average row. A row (or sample) that is already excluded cannot be remeasured. If remeasuring the excluded row is necessary, double click the [X] field to recover it once. wClick the right mouse button and select [Remeasure Selected Range] from the displayed menu. eThe remeasurement rows are added below the last measured row on the MRT work sheet. The rows in the selected range are marked in the [X] fields and excluded. (9) [Collective Edit] To change the factors and unit for actual concentration calculation together which are already set on the MRT work sheet, follow the procedure described below.

4

Basic Operation 4-47

AA-6200

4.7 Operating the MRT work sheet

qSelect the cell range to be changed by using the mouse (Click the first row to be changed and drag to the last row with pressing the button). wClick the right mouse button and select the [Collective Edit...] from the displayed menu. Then the "Collective Edit" dialog box appears. Put a check mark to the check box of each item to be changed. Enter a new setup value to the item with the check mark.

4

Basic Operation Figure 4-29 : "Collective Edit" Dialog Box eWhen completed, click on to close the "Collective Edit" dialog box. Settings are changed and the actual concentration is recalculated simultaneously and the work sheet is renewed.

4.7.3 Right Mouse Button on Summary Table Clicking on the right mouse button on the Summary table displays the pop-up menu where you can select Show/Hide of Absorbance, Concentration, Actual Concentration and Concentration Unit. This Show/Hide selection is also used for the "Print Table Data".

4.7.4 Inserting and Deleting the Measurement Row Only the row that has not been measured can be inserted or deleted for measurement.

4-48 AA-6200

4.7 Operating the MRT work sheet

To insert the row: (1) Click on the number of row position to be inserted (a new row is added above the row). (2) Select [Edit]-[Insert Row] from the menu bar. To delete the row: (1) Select the number of row (or the range of plural rows) to be deleted. (2) Select [Edit]-[Delete Rows] from the menu bar.

4

Basic Operation

NOTE Insertion and deletion of a row next to current measuring row can't be done during measurement.

4.7.5 Active Cell Movement by Shortcut Key and Cell Selection 4.7.5.1 Moving an Active Cell Clicking a cell with the mouse pointer displays a bold frame around the cell. The cell in this status is called an active cell. However, all the cells cannot be activated. Some cells can be activated but some cannot be. The active cell can be moved through the following key input. Home This key moves the active cell to the leftmost cell that can be active in the current row. End This key moves the active cell to the rightmost cell that can be active in the current row. Ctrl+Home These key move the active cell to the leftmost cell that can be active in the first row unexecuted. Ctrl+End These key move the active cell to the rightmost cell that can be active in the last measurement row. Tab This key moves the active cell to the right. After moving to the rightmost cell, it moves to the leftmost cell in the next row below. It skips a cell that cannot be activated and moves to the next cell. 4-49 AA-6200

4.7 Operating the MRT work sheet

Shift+Tab These keys move the active cell to the left. After moving to the leftmost cell, it moves to the rightmost cell in the upper row. It skips a cell that cannot be activated and moves to the next cell. 4.7.5.2 Selecting Cells Using the mouse can select contiguous plural cells as described below.

4

Basic Operation

Cell range Click the cell in the upper left corner of the region to be selected and drag to the cell in the lower right corner. Column When selecting a column, click the column header of the column to be selected. When selecting contiguous plural columns, drag along the column header. Row When selecting a row, click the row header of the row to be selected. When selecting contiguous plural rows, drag along the row header. Whole table Click the upper left cell of the header. Then all of the rows entered on the table are selected.

4.7.6 Copy and Paste Numeric values and characters on the MRT worksheet and summary table can be copied to the clipboard. Also, text data can be pasted from the clipboard only to the sample ID column in the MRT work sheet. 4.7.6.1 Copy Select an area on the table to be copied using the mouse and select [Edit]-[Copy] menu or press "Ctrl+C" key. Then the values in the selected area are copied to the clipboard. These copied values can be pasted as text data to the word processor or spreadsheet software. NOTE 1. The contents of column header and row header are not copied. 2. Graph column is never copied. 3. Hidden column is not copied. 4. Hidden row included in the selected area is always copied.

4-50 AA-6200

4.7 Operating the MRT work sheet

4.7.6.2 Paste Text data can be pasted from the clipboard to the sample ID column. [Copy & Paste of Sample ID between MRT work sheets] 1. Select a cell area of sample ID as the copy source and copy it to the clipboard by [Edit]-[Copy] menu or "Ctrl+C" key. If hidden rows are included in the selected area, the contents of the sample ID cells in the hidden rows are also copied. Therefore, set all the rows displayed and check the contents to be copied before executing the copy. 2. Click the top cell of the sample ID cell area in the paste destination. Note that paste is not applied to the rows already measured or rows under repeat measurement. 3. Select [Edit]-[Paste] menu or press "Ctrl+V" key in this status. Then the sample ID is overwritten on the cells from the top cell to down. 4. When the number of sample ID in the copy source is over the number of rows in the paste destination, the excess are added as new rows.

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Basic Operation

NOTE 1. If a value other than numeric value is pasted to the items for which time should be set in the sample ID field (WAIT, AUTO ZERO or RINSE at the use of ASC), it is reset to "0". Numeric values out of the acceptable entry range are also ignored. 2. If the paste is applied to the items for which nothing can be entered in sample ID field (CAL-CHK, etc.), it is ignored. 3. Also, sample IDs created using a word processor or spreadsheet software can be pasted to the MRT worksheet. When creating sample IDs using a word processor, insert a line feed between the sample IDs. Also, the sample ID must not contain the tab code.

4.7.7 Changing Column Width and Column Header Height of MRT Worksheet The column width for an arbitrary column and the column header height can be changed in the MRT work sheet. [Procedure for setting the column width] (1) Position the mouse cursor on the column border line in the column header. The mouse shape changes to a two-direction arrow. (2) While the mouse cursor is in the two-direction arrow status, press the left mouse button down and drag to the right or left. The cell width of the column header is changed. 4-51 AA-6200

4.7 Operating the MRT work sheet

(3) Release the left mouse button at the appropriate position. The column width is set at the position. [Procedure for setting the column header height] (1) Position the mouse cursor on the bottom line of the leftmost cell in the column header. The mouse shape changes to a two-direction arrow. (2) While the mouse cursor is in the two-direction arrow status, press the left mouse button down and drag upward or downward. The height of the leftmost cell is changed. (3) Release the left mouse button at the appropriate position. The column header height is set at the position.

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Basic Operation 4-52 AA-6200

4.8

4.8 Igniting and extinguishing the flame

4.8.1 Control locations This section identifies the locations of controls used to ignite and extinguish the flame. The IGNITE button, EXTINGUISH button, fuel gas flow meter, and oxidant gas flow meter are located at the front left of the main unit (Figure 4-30). fuel gas flowmeter oxidant gas flowmeter high temperature burner head

4 PURGE

Basic Operation

EXTINGUISH

IGNITE

burner select sensor burner-recognizing pin

Figure 4-30 : Panel of Gas Controller

The burner select sensor for the high temperature burner head for N2O-C2H2 flame is located at the lower left of the chamber.

4.8.2 Safety Precautions Prior to Ignition (1) Switch the room exhaust duct fan on. (2) Check that gas is available and gas pressure is set correctly. Gas type Supply pressure

Air, N2O 0.35+/-0.03MPa

C2H2 0.09+/-0.01MPa

(3) Confirm that the drain tank is filled with water. CAUTION If an ignition should be done with the drain tank not filled with water, the combustion gas flows out from the chamber and may cause flashback

(4) Verify that there are no leaks in any of the gas lines. Refer to the section 6.2. (5) Check that the flame and burner head to be used are appropriately matched. Refer to the following table. 4-53 AA-6200

4.8 Igniting and extinguishing the flame

High temperature burner head (option)

Standard burner head Slot length

10cm

5cm

Usable flame

Air - acetylene flame

Air - acetylene flame Nitrous oxide - acetylene flame

CAUTION Before igniting a flame, check that the ignition buttons work properly.

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Basic Operation

1. Referring to section 4.1, turn on the power of the instrument. 2. Referring to section 4.2.1.7, initialize the instrument and wait until the 10minute gas leak check step after the initialization has finished. 3. Perform Element Selection Wizard of AA software or open a flame measurement file so that the AA main unit is ready for the ignition. 4. Press only the lower button (white). When the ignition is not executed, it is normal. 5. If the above step 4 ignite a flame, the switch system is broken. Stop using the instrument immediately.

CAUTION 1. If the fuel gas is not supplied at the specified supply pressure, the flame cannot be ignited. 2. When the fuel gas is supplied at the specified pressure, the fuel gas in the piping flows from the burner slot when the PURGE button is pressed. Do not press the PURGE button for more than five seconds.

4.8.3 Igniting and extinguishing an Air-C2H2 flame (1) Turn ON the communication between the AA software and the AA main unit. Open the measurement file or execute the Element Selection Wizard so that the AA main unit is ready for the ignition. (2) While pressing the PURGE button, set the respective gas flow rates using the flow adjusting knob at the lower portion of the Fuel and Oxidant flow meters. Read the flow at the center of the float (ball). Gas Type Acetylene (C2H2) gas Air

4-54 AA-6200

Flow meter reading 2.0 to 3.0 (L/min) 8.0 (L/min)

4.8 Igniting and extinguishing the flame

(3) Simultaneously press the IGNITE and PURGE buttons. The pilot flame ignites first, then the burner head. Continue pressing the two buttons until the flame is completely ignited. If the flame is not ignited after the buttons have been pressed for three seconds or more, immediately stop the igniting operation. Wait at least ten seconds before trying to ignite the flame again.

CAUTION Pressing the PURGE button discharges fuel gas. Igniting a flame immediately after pressing the PURGE button is liable to cause a flash. Wait at least for 10 seconds before the ignition.

4

Basic Operation

When the ignition has failed, the AA software may display an error message like "Flame has been extinguished". When such a message is displayed, the AA main unit is locked so that the ignition cannot be done. To release this lock, close all the error messages displayed on the software. (4) Set the flow rate of fuel gas and oxidant gas, if necessary. Referring to the Gas Condition dialog box or 8.1 Measurement Conditions for Flame Atomic Absorption Analysis, confirm the flow rate of the standard fuel gas of each element. (5) Press the EXTINGUISH button to extinguish the flame.

NOTE 1. The flame automatically extinguishes if the gas pressure drops while the flame is burning. If this occurs, check the supply pressure before re-igniting the flame. 2. If you attempt to ignite the flame when no oxidant gas is supplied or the oxidant gas pressure is low, the safety mechanism prevents fuel gas from being supplied to the burner slot. The instrument generates an ignition spark but the flame does not ignite. In this condition, the monitor does not display a low pressure error message. If no error message displays and the flame will not ignite, check the supply pressure of the oxidant gas. 3. If the flame will not extinguish when you press the EXTINGUISH button, follow these steps. qSwitch the Power switch at the lower right of the instrument's front panel OFF. This operation mechanically closes the solenoid valve of the gas controller, shutting off the gas supply safely. wClose the gas main valve. eDo not operate the instrument again until the unit is repaired. You may schedule repairs at the Shimadzu sales office nearest you. 4. When the following error messages are displayed on the AA software, the AA 4-55 AA-6200

4.8 Igniting and extinguishing the flame

main unit is locked so that the ignition cannot be done. To release this lock, solve the problems in the instrument settings then close all the error messages displayed on the software. While the error messages are displayed, the ignition cannot be done. - Fuel gas pressure is too low. - Support gas pressure is too low. - Flame has been extinguished.

4

4.8.4 Igniting and extinguishing N2O-C2H2 flame

Basic Operation

(1) Remove the standard burner head (10cm slot length) and mount the high temperature burner head (5cm slot length) supplied as an optional accessory. (For optional accessories, refer to 6.6 Optional Accessories List.) (2) Insert the burner-recognizing pin (connected by wire to the high temperature burner head) into the hole of the burner select sensor. (3) Turn on the communication between AA software and AA main unit. Open measurement file or perform Element Selection Wizard and open the "Gas Flow Rate Setup" page, and select "N2O-C2H2" from [Flame Type] list. (4) While pressing the PURGE button, set the respective gas flow rates using the flow adjusting knobs located beneathe the Fuel and Oxidant flow meters. Read the flow at the center of the float (ball). Flow meter FUEL OXIDANT

Flow meter reading 3.0 8.0

NOTE 1. Selecting "N2O-C2H2" for [Flame Type] on the "Gas Flow Rate Setup" dialog box displays the [Meter] field. The [Meter] field displays a value by subtracting 4.0(L/min), which is to be automatically increased by the system, from the flow rate set in [Fuel Gas Flow Rate] field. After igniting a flame, to set the fuel gas flow rate to the same condition saved in the file, set the flow rate to the value displayed in this [Meter] field instead. The fuel gas flow meter indication doesn’t include the 4.0 (L/min) to be automatically increased by the system. 2. The oxidant gas flow meter is scaled so as to display the actual flow rate of Air. Therefore, when the oxidant gas is N2O, note that the scale in the flow meter differs from the actual flow rate. For example, the actual flow rate of N2O gas is set to 6.5 L/min when adjusting the oxidant gas flow meter to "8.0" shown in the scale.

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4.8 Igniting and extinguishing the flame

(5) Simultaneously press the IGNITE button and the PURGE button. The pilot flame ignites first, then the burner ignites. Continue pressing the two buttons until the flame is completely ignited. If the flame is not ignited even if the buttons are pressed for three seconds or more, stop igniting operation once, and retry after ten seconds or more. When the ignition has failed, the AA software may display an error message like "Flame has been extinguished". When such a message is displayed, the AA main unit is locked so that the ignition cannot be done. To release this lock, close all the error messages displayed on the software. Six or seven seconds after the Air-C2H2 flame ignites. the C2H2 flow rate

4

Basic Operation

automatically increases by 4.0L/min and the flame intensity increases. Then, the burner gas automatically changes from Air to N2O, and the Air-C2H2 flame changes to a N2O-C2H2 flame. CAUTION Pressing the PURGE button discharges fuel gas. Igniting a flame immediately after pressing the PURGE button is liable to cause a flash. Wait at least for 10 seconds before the ignition.

NOTE Even if N2O-C2H2 is selected in the [Flame Type] list box on the "Gas Flow Rate Setup" page, the flame will not switch if the burner-recognizing pin attached to the high temperature burner head is not inserted at the burner select sensor. In this case, when the burner-recognizing pin is inserted in the hole of the burner select sensor, the oxidant gas is automatically changed from Air to N2O then the flame is switched from AIR-C2H2 to N2O-C2H2.

(6) To extinguish the flame, press the EXTINGUISH button. The instrument automatically changes the oxidant gas from N2O to Air, then the N2O-C2H2 flame changes to an Air-C2H2 flame. Finally, the flame is extinguished.

CAUTION 1. Always use the high temperature burner head when using a nitrous oxideacetylene flame. Using the standard burner head with this gas poses a danger of flashback. 2. When the acetylene flow rate is high, carbon is deposited around the burner slot. When this occurs, use the provided large screwdriver to scrap off the carbon 4-57 AA-6200

4.8 Igniting and extinguishing the flame

deposit while taking care about the following points. • Insert the screwdriver at the center on the burner slot while keeping the top portion of the screwdriver lengthwise. Don't close a large part of the burner slot by keeping the top portion of screwdriver horizontally. • While keeping the top portion of screwdriver lengthwise, slide it from the center to the outside (right or left side) and scrap off the carbon deposit gently. To prevent the flame from going out, don't slide the screwdriver from the outside to the center. Insert it at the center again and scrap off to the outside. • Be careful not to scratch the burner head and slot. • Remove the carbon deposit inside the burner slot using a piece of hard paper, after the flame is extinguished and the burner is completely cooled.

4

Basic Operation

Carbon deposit

High temperature burner head

Figure 4-31 : Removing Carbon Deposit in N2O-C2H2 Flame 3. When using a nitrous oxide-acetylene flame, decreasing the acetylene or increasing the nitrous oxide will cause the pink portion of the flame (red feather) to gradually decrease. If the red feather decreases to less than 2mm, the flame will split and if the acetylene flow is reduced further, flashback may occur. Blue

Pink (Red Feather) Dark blue

Figure 4-32 : Nitrous Oxide-Acetylene Flame 4-58 AA-6200

4.8 Igniting and extinguishing the flame

In case of flashback, set the safety bung at the back of the chamber as it was if it is out of place. Also, remove the spray unit to check it. And confirm that the disperser is not damaged and the U-tube connected to the drain port of the chamber is firmly connected.

4.8.5 Flame conditions when analyzing organic solvent samples Since an organic solvent itself will burn in the flame, the flame will not be completely combusted using the normal flame conditions, as the result, the measurement accuracy will be decreased. To perform an accurate measurement, it is necessary to decrease the sample spray amount as well as decrease the acetylene gas flow rate, compared with the aqueous solution. The procedure for setting the flame conditions when using organic solvent is as follows. (1) Replace the sampling tube with the provided polyethylene capillary tube. (2) While solvent is being sprayed into the flame, decrease the acetylene gas flow rate so that the color of the flame changes from blue to light red (air-acetylene flame). Next, while the organic sample is being sprayed, adjust the acetylene flow rate until the maximum S/N ratio (signal to noise ratio) is achieved. (3) Overly decreasing the acetylene flow may cause the flame to go out when the organic sample spray ceases. In this situation, increase the acetylene gas flow rate in 0.1L/min increments until the flame no longer extinguishes at the end of spraying the organic solvent sample. Then adjust the flame condition by increasing the oxidant gas flow rate. When using a nitrous oxide-acetylene flame, be sure that the red feather (red portion of the flame) is more than 2-3mm.

4

Basic Operation 4-59

AA-6200

4.8 Igniting and extinguishing the flame

4.8.6 Changing the chamber position When executing analysis using a hydride generator HVG-1 and mercury vaporizing unit MVU-1A (optional), quartz cells must be set on the burner. Changes the height of the burner according to the procedure shown below. (1) Loosen the chamber fixing screws with the hexagonal wrench so that the pins for the chamber position come out. (2) When using HVG-1, move the chamber to the position w, and insert the pins for the chamber position into the positioning holes. When MVU-1A is used, move to position e. (3) Firmly tighten the chamber fixing screw with the hexagonal wrench.

4

Basic Operation Chamber positioning hole

Position

Chamber fixing screw

Figure 4-33 : Changing the Chamber Position

4-60 AA-6200

4.9

Standard Addition Method and Simple Standard Addition Method

4.9.1 Overview The standard addition method is used when there is interference by coexistent material (matrix) in the sample and its influence is given to the measured value. For the standard addition method, equal volumes of unknown sample solution are prepared, and a standard solution of different but known concentration is added to each of the unknown sample solutions. The absorbance is measured for each of these samples, and a calibration curve is created. The unknown sample concentration is obtained from the point at which the extended calibration curve intersects with the horizontal axis.

Basic Operation

Absorbance

4

Standard addition concentration Concentration of unknown sample

Figure 4-34 : Standard Addition Method

Absorbance

When the coexistent material or matrix of plural unknown samples are similar, measure one of them by standard addition method, and you can use the slope of the same calibration curve to determine the concentrations of other unknown samples. This is called simple standard addition method.

Sample concentration by simple standard addition method

Figure 4-35 : Simple Standard Addition Method 4-61 AA-6200

4.9 Standard Addition Method and Simple Standard Addition Method

When using these methods, the absorbance of standard addition samples must be within the range that has linearity of calibration curve. To check whether the result is valid or not, refer to the coefficient of correlation.

4.9.2 Setting the measurement procedure for simple standard addition method The measurement procedure for simple standard addition method can be created by using the Element Selection Wizard or Schedule Creation Wizard.

4

In this explanation, the setting procedure is explained along the following analysis example.

Basic Operation

(Analysis example) Three types of unknown samples A, B and C whose matrixes are relatively similar are measured quantitatively in the simple standard addition method. The unknown sample A is measured in the standard addition method and other unknown samples B and C are measured using the calibration curve obtained from the quantitative analysis of unknown sample A. Add the standard sample to the unknown sample to prepare four samples whose known concentrations are 0, 10, 20 and 30 ppm. To prepare each sample, take 50 mL of unknown sample A and add the standard and diluent up to the final volume 200mL. Also, take 50 mL of unknown samples B and C respectively and dilute them up to the final volume 200mL while keeping the matrix similarity as far as possible. (Setting procedure) (1) Execute the Element Selection Wizard or Schedule Creation Wizard and forward the page until the Preparation Parameters page is displayed. (2) When the Preparation Parameters page is displayed, first, click on the element row for setup to highlight it and click on . Then "Edit Preparation Parameters" dialog box opens. (3) Select "SMSA" for the [Measurement Type]. (4) Setup of [Order] and [Zero Intercept] is not possible. The order is automatically set to the 1st (linear) and zero is not intercepted. (5) Select [Conc. Unit]. Click on the ▼ and select the unit from the list. (Example) Select "ppm". (6) Enter the [Weight Factor], [Volume Factor], [Dilution Factor] and [Correction Factor] in the field of [Weight Correction Factors]. (Example) 4-62 AA-6200

4.9 Standard Addition Method and Simple Standard Addition Method

Since the 50 mL of unknown sample is prepared to the final volume 200mL, enter "50" in [Weight Factor] and "200" in [Volume Factor]. (7) Set the preparation parameters of the unknown sample to be measured in the standard addition method in [STD Samples] table in [Preparation Parameters]. Enter the number of samples created from the unknown sample to be measured in the standard addition method in [Number of STD], then a table is displayed in the [STD Samples] field. Enter the added concentrations of the standard samples. (Example) The four samples are prepared by adding the standard sample so that the known concentrations are 0, 10, 20 and 30. Therefore, enter "4" in [Number of STD] and "0", "10", "20" and "30" in [Conc] fields in the STD samples table. (8) When completing the setup, click on . Then "Preparation Parameters" page is displayed again. When measuring plural elements, make setup for other elements in the same procedure. (9) Click in "Preparation Parameters" page and proceed to "Sample ID". (10) In [Number of Samples] of "Sample ID", enter the number of unknown samples including the unknown sample to be measured in the standard addition method. (Example) Since three unknown samples A, B and C are to be quantitatively measured, enter "3" in [Number of Samples]. (11) Forward the Wizard pages until all the settings are completed, and click button to end the Wizard. The measurement procedure as shown in Table 4.3 is set on the MRT worksheet.

4

Basic Operation

The indication of [Action] on the MRT work sheet related to "SMSA (Simple Method of Standard Addition)" and "MSA (Method of Standard Addition)" is described below. Action MSA MSA-RES SMSA

Description Indicates standard addition method. Indicates the concentration of unknown sample calculated from the result of measuring a set of standard addition samples. Indicates simple standard addition method. Unknown sample is measured using a calibration curve created by another sample for standard addition method.

(12) Following this procedure, execute the measurement. The concentration of each unknown sample before the dilution is displayed in [Actual Conc.] field. 4-63 AA-6200

4.9 Standard Addition Method and Simple Standard Addition Method

Table 4.3 Measurement Procedure for Simple Standard Addition Method Action

4

True Value (ppm)

WF

VF

C#

Basic Operation

1

AUTOZERO

2

MSA

0.00

01

3

MSA

10.00

01

4

MSA

20.00

01

5

MSA

30.00

01

6

MSA-RES1

50.00

200.00

01

7

SMSA2

50.00

200.00

01

8

SMSA3

50.00

200.00

01

Description Perform auto zero Measures Sample A with standard 0ppm addition Measures Sample A with standard 10ppm addition Measures Sample A with standard 20ppm addition Measures Sample A with standard 30ppm addition Indicates concentration result of Sample A Measures Sample B by Simple Standard Addition Method Measures Sample C by Simple Standard Addition Method

4.9.3 Setting the measurement procedure for standard addition method The measurement procedure to measure plural samples in standard addition method cannot be created by using the Wizard. Therefore, set the element schedule and measurement procedure firstly in the simple standard addition method, then edit the MRT worksheet directly to create the measurement procedure. In this explanation, the setting procedure is explained along the following analysis example. (Analysis example) All the three unknown samples A, B and C are measured quantitatively in the standard addition method. Add the standard sample to each unknown sample to prepare each four samples whose known concentrations are 0, 10, 20 and 30 ppm. To prepare each sample, take 50 mL of unknown sample and add the standard and diluent up to the final volume 200mL. (Setting procedure) (1) Create a measurement procedure firstly in the simple standard addition method, referring to the section 4.9.2. 4-64 AA-6200

4.9 Standard Addition Method and Simple Standard Addition Method

(Example) The measurement procedure as shown in Table 4.3 is obtained on the MRT worksheet. (2) Edit this measurement procedure. Delete the measurement procedure of simple standard addition method (SMSA rows) and enter the measurement procedure of standard addition method (MSA rows and MSA-RES rows) for each unknown sample instead. The MSA-RES row is required to display the quantitative result of each unknown sample in the standard addition method. (Example) Delete SMSA rows of unknown samples B and C (Row No.7 and 8) in Table 4.3 by using [Edit]-[Delete Rows] from the menu. Next, create the MSA rows and MSA-RES rows in Table 4.4 (Row No.7 to 16) on the MRT worksheet. Set the MSA-RES row at the last measurement row of each sample series of unknown samples B and C. (3) In [True Value] field, enter the known concentrations of standard addition. (Example) The sample series are prepared by adding the standard sample so that the known concentrations are 0, 10, 20 and 30 ppm. Therefore, enter "0", "10", "20" and "30" in [True Value] fields. (4) Enter the weight correction factors. (Example) Since the 50 mL of unknown sample is prepared to the final volume 200mL, enter "50" in [WF](Weight Factor) and "200" in [VF]( Volume Factor) of the MSA-RES rows (Row No.11 and No.16 in Table 4.4). (5) In the standard addition method, a calibration curve needs to be created for each unknown sample. Specify a different calibration curve number for each sample in [C#] field. Adding an MSA row on the MRT worksheet automatically allocates a calibration curve number. Check that the calibration curve numbers are allocated correctly to the series of standard addition samples. (Example) In the case of this analysis example, three calibration curves are created. Enter "2" in [C#] field of unknown sample B series (Row No.7 to 11 in Table 4.4) and enter "3" in [C#] field of unknown sample C series (Row No.12 to 16 in Table 4.4). (6) After finishing the measurement procedure setup, start the measurement according to this procedure. The concentration of each unknown sample before diluted is displayed in [Actual Conc.] field.

4

Basic Operation 4-65

AA-6200

4.9 Standard Addition Method and Simple Standard Addition Method

Table 4.4 Measurement Procedure for Standard Addition Method Action

4

True Value (ppm)

WF

VF

C#

Basic Operation

1

AUTOZERO

2

MSA

0.00

01

3

MSA

10.00

01

4

MSA

20.00

01

5

MSA

30.00

01

6

MSA-RES1

7

MSA

0.00

02

8

MSA

10.00

02

9

MSA

20.00

02

10 MSA

30.00

02

50.00

11 MSA-RES2

50.00

200.00

200.00

01

02

12 MSA

0.00

03

13 MSA

10.00

03

14 MSA

20.00

03

15 MSA

30.00

03

16 MSA-RES3

4-66 AA-6200

50.00

200.00

03

Description Perform auto zero Measures Sample A with standard 0ppm addition Measures Sample A with standard 10ppm addition Measures Sample A with standard 20ppm addition Measures Sample A with standard 30ppm addition Indicates concentration result of Sample A Measures Sample B with standard 0ppm addition Measures Sample B with standard 10ppm addition Measures Sample B with standard 20ppm addition Measures Sample B with standard 30ppm addition Indicates concentration result of Sample B Measures Sample C with standard 0ppm addition Measures Sample C with standard 10ppm addition Measures Sample C with standard 20ppm addition Measures Sample C with standard 30ppm addition Indicates concentration result of Sample C

4.10

Conditions and Operation for Flame Emission Analysis

Flame emission quantitative analysis is described here. As the case of atomic absorption analysis, the Wizard can be used for setup. However, the setup procedures in the "Optics Parameters" and "Gas Flow Rate Setup" pages are different in some points. Other operations are the same as those of the flame method of atomic absorption analysis.

4.10.1 "Optics Parameters"Page

4

Basic Operation

Figure 4-36 : "Optics Parameters" Page (1) [Wavelength] For wavelength used for flame emission analysis, refer to the section 8.2. Enter the numeric value if the wavelength is different from that for atomic absorption analysis. (2) [Slit Width] It is recommended to set the slit width to "0.7nm". (3) [Socket #] Any socket number is OK because lamp is not used. Although if Lamp Position Setup dialog box is used (refer to the section 5.8.4) and button is shown on "Optics Parameters" page, it is necessary to set an arbitrary socket number as a dummy. (Procedure for dummy setup) 1. Press the button to display the "Lamp Position Setup" dialog box. 2. For an arbitrary [Socket #], select "*" in the [Element] and "Normal" in the [Lamp Type]. 4-67 AA-6200

4.10 Conditions and Operation for Flame Emission Analysis

3. Select "Emission" in [Lamp ID]. This lamp ID is a special ID of dummy lamp for flame emission analysis. 4. Press to close the "Lamp Position Setup" dialog box and return to the "Optics Parameters" page. Then select the socket # in which the dummy lamp for flame emission analysis was set. When performing the line search using a lamp, set a proper lamp in "Lamp Position Setup" dialog box. (4) [Lamp Mode] Set the [Lamp Mode] to "EMISSION". (5) [Lamp Current] Set the [Low] to "0" (zero). (6) In the case of flame emission analysis, a line search is performed when the flame has been ignited and the standard sample is being sprayed. So, the line search is not performed in this page. Proceeds to the next " Gas Flow Rate Setup" page first and set the parameters so that ignition may be possible. After that, return to this page perform the line search. It is also possible to perform a line search using the hollow cathode lamp. In this case, light on the hollow cathode lamp to perform the line search. If the lamp is lit on in the EMISSION mode, the lamp is automatically turned off when the key is pressed to start the measurement. Don't forget to turn off the lamp, however, when observing a signal in the "Gas Flow Rate Setup" page while aspirating the sample. (7) Click on button to proceed to the "Gas Flow Rate Setup" page first.

4

Basic Operation

4.10.2 "Gas Flow Rate Setup" Page (1) Confirm the flame type, fuel gas flow rate and support gas flow rate indicated on this page.

4-68 AA-6200

4.10 Conditions and Operation for Flame Emission Analysis

4

Basic Operation

Figure 4-37 : "Gas Flow Rate Setup" Page [Flame Type] Since the flame used for atomic absorption analysis is indicated, click on the ▼ and select the flame type used for flame emission analysis. As a flame type used for flame emission analysis, generally, the high temperature N2OC2H2 flame is good. However, in the cases of alkaline metals (Na, K, etc.), other flame (Air-C2H2) is also available for measurement of sufficiently minute quantities. [Fuel Gas Flow Rate] Since the flow rate for atomic absorption analysis is indicated by default, enter the flow rate value for flame emission analysis. It is necessary to check the optimum value for each element beforehand. In general, a low acetylene flow rate is best. When using the N2O-C2H2 flame, adjust the flow rate so that the red feather (pink portion of flame) is approx. 2 to 3 mm in height. (2) Set the angle of burner head according to the purpose. Generally, the S/N ratio is better when the angle is set at 0 degree for optical axis (parallel) than at 90 degrees, but its linearity may become worse. When the concentration of analysis element is relatively high, the burner head is used at 90 degrees.

4-69 AA-6200

4.10 Conditions and Operation for Flame Emission Analysis

4.10.3 Line Search and Beam Balance After completing the condition setup in the "Gas Flow Rate Setup" page, click on to return to the "Optics Parameters" page. Read the section 4.8 thoroughly and set the conditions so that a flame can be ignited. (1) Ignite the flame. (2) Start spraying the standard sample of the highest concentration. If the sample position of the highest concentration standard sample on ASC turn table is set to the [ASC Sample Pos. for EMISSION Line Search], the automatic spray using the ASC is possible. (3) While spraying the sample, click on button. Then the line search/beam balance is executed. Continue spraying the sample until the line search/beam balance operation is completely finished. When the ASC is used, the spray of the sample in the specified position on the ASC turn table is started before starting the line search/beam balance. The line search/beam balance is started when the pre-spray time set in the [Parameters]-[Edit Parameters]-[Measurement Parameters] is finished after starting the spray. (4) If the line search fails and the message stating insufficient energy is displayed, prepare and spray a standard sample of even higher concentration and try it again. (5) When the line search is completed, click on to return to the "Optics Parameters" page. Then click on button to proceed to the "Gas Flow Rate Setup" page again. While monitoring the real time graph on the "Gas Flow Rate Setup" page, spray vaporized water and check that the signal becomes almost zero. (6) If the signal does not become small, it is possible that the analysis line was not correctly detected. In that case, go back to the "Optics Parameters" page and perform the line search once again following the procedures (1) to (5).

4

Basic Operation 4-70

AA-6200

5 Menu Commands 5

Contents 5.1 Wizard Selection dialog box ……………………………………………………5-1 5.1.1 "Wizard" page ……………………………………………………………5-1 5.1.2 "Recent Files" page ………………………………………………………5-2 5.1.3 "Recent Templates" page…………………………………………………5-2 5.2 [File] …………………………………………………………………………………5-3 5.2.1 [New] ………………………………………………………………………5-4 5.2.2 [Open] ………………………………………………………………………5-4 5.2.3 [Save] ………………………………………………………………………5-4 5.2.4 [Save As...] …………………………………………………………………5-5 5.2.5 [Additional Load] …………………………………………………………5-6 5.2.6 [File Export...]………………………………………………………………5-7 5.2.7 [Export Items]………………………………………………………………5-8 5.2.8 [Auto Save] …………………………………………………………………5-9 5.2.8.1 Saving the backup file automatically ………………………………5-9 5.2.8.2 Exporting the MRT work sheet data automatically in text file …5-10 5.2.8.3 Executing a program by command line …………………………5-12 5.2.9 [Print Data/Parameters...] ………………………………………………5-14 5.2.10 [Print Table Data...] ………………………………………………………5-14 5.2.11 [Print Style] ………………………………………………………………5-15 5.2.11.1 "Print Style Setup" page ……………………………………………5-15 AA-6200

Menu Commands

This chapter explains items and functions displayed on the screen of PC software that controls the AA instruments.

5

Menu Commands

5.2.11.2 "Table Show/Hide" page ……………………………………………5-16 5.2.11.3 "Font" page …………………………………………………………5-16 5.2.12 [Print Setup] ………………………………………………………………5-17 5.2.13 Recent Files ………………………………………………………………5-17 5.2.14 [Exit] ………………………………………………………………………5-17 5.3 [Edit] ………………………………………………………………………………5-18 5.3.1 [Insert Row] ………………………………………………………………5-18 5.3.2 [Delete Rows] ……………………………………………………………5-18 5.3.3 [Import Other Schedule]…………………………………………………5-18 5.3.4 [Collective Edit] …………………………………………………………5-19 5.3.5 [Remeasure Selected Range] …………………………………………5-20 5.3.6 [Clear Measurement Result] ……………………………………………5-20 5.3.7 [Copy] ……………………………………………………………………5-20 5.3.8 [Paste] ……………………………………………………………………5-20 5.4 [Refer to Parameters] ……………………………………………………………5-21 5.5 [Parameters]………………………………………………………………………5-22 5.5.1 "Element Selection" Page ………………………………………………5-24 5.5.1.1 "Cookbook" page ……………………………………………………5-25 5.5.1.2 "Template" page ……………………………………………………5-26 5.5.2 "Preparation Parameters" Page ………………………………………5-27 5.5.2.1 Weight Correction Factors …………………………………………5-28 5.5.2.2 [Preparation Parameters]-[STD Samples] ………………………5-29 5.5.2.3 [Preparation Parameters]-[Blank Samples] ………………………5-30 5.5.3 "Sample ID" Page ………………………………………………………5-30 5.5.4 "Sample Selection" Page ………………………………………………5-31 5.5.5 "Connect to Instrument/Send Parameters" Page ……………………5-32 5.5.6 "Optics Parameters" Page ………………………………………………5-33 5.5.6.1 Button ……………………………………………5-36 5.5.6.2 Button ………………………………………………5-37 5.5.6.3 Button ……………………………………5-38 5.5.7 "Lamp Position Adjustment" Page ……………………………………5-40 5.5.8 "Gas Flow Rate Setup" Page …………………………………………5-41 5.6 [Edit Parameters]…………………………………………………………………5-43 5.6.1 "Measurement Parameters" Page ……………………………………5-44 5.6.2 "Repeat Measurement Conditions" Page ……………………………5-47 5.6.3 "Weight Correction Factors" Page ……………………………………5-49 5.6.4 "Y-axis Print Range" Page ………………………………………………5-50 5.6.5 "Analyst" Page……………………………………………………………5-50 AA-6200

5.8.6 [Maintenance] ……………………………………………………………5-73 5.8.6.1 [D2 Lamp Position] …………………………………………………5-73 5.8.6.2 [Wavelength Adjustment] …………………………………………5-74 5.8.6.3 [Burner Origin Position Adjustment] ………………………………5-74 5.8.6.4 [Furnace Origin Position Adjustment] ……………………………5-74 5.8.6.5 [ASC Maintenance] …………………………………………………5-74 5.8.6.5.1 [Set Syringe Volume] ……………………………………………5-74 5.8.6.5.2 [Change Syringe] …………………………………………………5-74 5.8.6.6 [Maintenance only for service engineer] …………………………5-74 5.8.7 [Lamp Status] ……………………………………………………………5-74 5.8.8 [Change Graphite Tube]…………………………………………………5-76 5.8.9 [Gas Controller Status] …………………………………………………5-76 5.8.10 [Gas Leak Check] ………………………………………………………5-77 5.8.11 [Remaining Gas Combustion] …………………………………………5-77 5.8.12 [Execute Line Search] …………………………………………………5-79 5.8.13 [Cleaning] …………………………………………………………………5-79 AA-6200

5

Menu Commands

5.6.6 "Comment" Page…………………………………………………………5-50 5.6.7 "Sequence" Page ………………………………………………………5-51 5.6.8 "QA/QC Setup" Page ……………………………………………………5-52 5.6.9 "Calibration Curve Parameters" Page …………………………………5-54 5.6.10 "Optics Parameters" Page ………………………………………………5-55 5.6.11 "Gas Flow Rate Setup" Page …………………………………………5-55 5.7 [Default Parameters] ……………………………………………………………5-56 5.7.1 [Flame] ……………………………………………………………………5-56 5.7.2 [Furnace] …………………………………………………………………5-56 5.7.3 [Graph] ……………………………………………………………………5-56 5.7.4 [Analyst] …………………………………………………………………5-56 5.8 [Instrument] ………………………………………………………………………5-57 5.8.1 [Connect] …………………………………………………………………5-58 5.8.2 [Option Connect] …………………………………………………………5-60 5.8.3 [Configuration] ……………………………………………………………5-60 5.8.4 [Lamp Position Setup] …………………………………………………5-64 5.8.4.1 When not using the lamp position setup function ………………5-66 5.8.4.2 When using the lamp position setup function ……………………5-66 5.8.5 [Lamp History] ……………………………………………………………5-68 5.8.5.1 When is a use of "Lamp History" dialog box necessary? ………5-68 5.8.5.2 How to use the "Lamp History" dialog box ………………………5-69 5.8.5.3 Displaying a message when the lamp used time exceeds the lamp life …5-72

5.8.14 [Rinse Nozzle] ……………………………………………………………5-79 5.8.15 [Flame Nozzle Position] …………………………………………………5-80 5.8.16 [Furnace Nozzle Position] ………………………………………………5-80 5.9 [Help] ………………………………………………………………………………5-81 5.9.1 [Search for Help on...] …………………………………………………5-81 5.9.2 [About WizAArd...] ………………………………………………………5-81 5.10 Rounding the absorbance and setting the decimal places for correction factors and actual concentration ………………………………5-82 5.10.1 Rounding the absorbance value ………………………………………5-82 5.10.2 Setting the decimal places for correction factors and actual concentration value …5-84

5

Menu Commands AA-6200

5.1

Wizard Selection dialog box

After the software is started, the "Wizard Selection" dialog box shown in Figure 5.1 is displayed. Clicking on closes this dialog box, and clicking on at left lower of the main window displays this dialog box again.

5

Menu Commands

Figure 5.1 : "Wizard Selection" dialog box

5.1.1 "Wizard" page The following three icons are indicated on the "Wizard" page in the "Wizard Selection" dialog box. Each Wizard can be started by selecting one of the icons and clicking on . However, when you start newly, or when no element has been selected, the [Schedule Creation] and [Measurement Preparation] are not displayed. [Element Selection] The element selection Wizard is started. Selection of measurement elements and setup of measurement element order are performed here. You may close the Wizard in the element selection page only. Or you may also proceed to the pages of schedule creation and measurement preparation to set the parameters until the measurement can be performed in that conditions. This is equivalent to selecting [Parameters]-[Element Selection Wizard] from the menu. [Schedule Creation] Setup of calibration curve parameters, setup of sample preparation parameters, setup of the sample information, and input of factors for actual concentration 5-1 AA-6200

5.1 Wizard Selection dialog box

calculation are performed here and the measurement sequence is created on the MRT work sheet. This is equivalent to selecting [Parameters]-[Schedule Creation Wizard] from the menu. [Measurement Preparation] This is applied for one element when the measurement sequence is already created. Lighting of hollow cathode lamp, line search/beam balance, and setup of the burner position and gas flow rate or setup of furnace temperature program are performed. This is equivalent to selecting [Parameters]-[Measurement Preparation Wizard] from the menu.

5

5.1.2 "Recent Files" page Menu Commands

A data file lately used can be selected from the list and opened.

5.1.3 "Recent Templates" page A template lately used can be selected from the list and opened.

5-2 AA-6200

5.2

[File]

This menu summarizes functions associated with WizAArd's file and print. In the WizAArd, two file types of "*.aa" and "*.taa" are handled. The "*.aa" refers to a data file and contains the measurement parameters, calibration curve, sample information, measurement procedure and measured data. The information for plural elements can be saved in one file. The "*.taa" refers to a template and is different from a data file in the following points. (1) Measured data is not included. The contents are the same as those of "*.aa" file before measurement. If a file is saved as a template file in [File]-[Save As] after measurement, the measured data is cleared and other contents are saved. (2) When a template file is loaded, it has no name. When a template file is loaded, the title bar displays "notitle - WizAArd". If selecting the [File]-[Save], the [Save As] dialog box always appear instead. (3) It can be utilized as a cookbook (standard parameters for each element). When using the parameters, such as wavelength, lamp current and gas flow rate, which are different from the standard parameters built in the software, save them as a template file so that you can use it easily instead of the built-in standard parameters (refer to the section 5.5.1.2.["Template" page]).

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Menu Commands

Figure 5.2 : Drop-down Menu of [File]

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5.2 [File]

5.2.1 [New] This command is used to create measurement parameters and measurement procedures. Execution of this command resets the data and parameters already existing on MRT work sheet. When the data exists on MRT work sheet, save the data with [Save] or [Save As...] command before executing [New].

5.2.2 [Open] This command is used to read the files already saved in the disk. Execution of this command opens the "Open" dialog box (Figure 5.3). Specify the [Look in], [Files of type] and [File name], and click on .

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Menu Commands Figure 5.3 : "Open" Dialog Box

If a comment has been written with the file to be opened, the comment can be read. Enter [File name] and click on , then the comment is displayed.

5.2.3 [Save] This command is used to save the parameters and data currently loading on the software, without changing the file name. When the file name does not exist (not named), same as [Save As...] is executed. NOTE A measurement data whose repeat measurement has not finished is not saved in the file. If the data is necessary when the repeat measurement cannot be completed, print it out before closing the AA software. 5-4 AA-6200

5.2 [File]

5.2.4 [Save As...] This command is used to save the parameters and data currently loading on the software with a new file name. When this command is executed, the "Save As" dialog box (Figure 5.4) opens. Specify the [Save in], [Save as type] and [File Name], and click on . If the "*.taa" is selected for file type, data is not saved. NOTE A measurement data whose repeat measurement has not finished is not saved in the file. If the data is necessary when the repeat measurement cannot be completed, print it out before closing the AA software.

5

Menu Commands

Figure 5.4 : "Save As" Dialog Box If a file is saved as "template.aa" in the same folder (default: C:¥Program Files¥WizAArd¥") of the execution file ("Wizaa.exe"), the "template.aa" file is automatically loaded when starting AA software at next time or when newly creating file with [New] command. It is convenient to save a frequently used measurement parameter file in your routine as "template.aa".

This button is used to record your comment. Click on button, then "File Comment" dialog box opens. Write your comment and click on . The comment is saved with the file.

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5.2 [File]

5.2.5 [Additional Load] Schedules of measurement element in a file saved in the disk are added to the end of the current schedule of measurement element. This function can be used for the following purposes. (1) A file for continuous measurement of plural elements can be created using several measurement files (or measurement template files) created for single element. (2) One summary report can be created from several files. [Operation] (1) Select [File]-[Additional Load] menu. "Merge File" dialog box is displayed.

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Menu Commands Figure 5.5 : "Merge File" Dialog Box (2) In this dialog box, select a measurement file (extension is "aa") or template file (extension is "taa") you want to additionally read in, and click . (3) The measurement element schedule of the selected file is added to the end of the measurement element schedule series at present. NOTE When a schedule of the same element is added, it is not combined in one schedule but added as another schedule. When the total number of schedules exceeds 20, the schedules over it are not read in.

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5.2 [File]

5.2.6 [File Export...] This command is used to create a text file from data on the MRT work sheet of currently opened file. The text file can be read in word processor software or spreadsheet software. Executing this command opens the dialog box (Figure 5.6) to indicate the selection items. From this list, select items to be converted to text data and click on . Then the "Save As" dialog box as shown in Figure 5.4 opens. Specify the [Save in], [Save as type] and [File name], and click on . NOTE Only the data on the MRT work sheet can be output to text file. Measurement parameters and waveform data cannot be output.

5

Menu Commands

Figure 5.6 : "Select Schedule" Dialog Box

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5.2 [File]

5.2.7 [Export Items] This specifies output items to output the data on the MRT work sheet to the text file. This setting is valid to the following text file output functions. (1) Output from [File]-[File Export...] menu. (2) Output by setting the automatic output of text file in [File]-[Auto Save] menu (3) Output by setting "FILEEXPORT" in [Action] field in the MRT work sheet [Operation] (1) Select [File]-[Export Items] menu. "Export Items" dialog box is displayed.

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Menu Commands Figure 5.7 : "Export Items" Dialog Box (2) Select the item you want to output and click the button.

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5.2 [File]

5.2.8 [Auto Save] 5.2.8.1 Saving the backup file automatically Automatic saving of the backup of measurement file can be set up in the style of "every X samples are measured". This setting is valid both for automatic measurement using the auto-sampler and for manual measurement. [Operation] (1) Select [File]-[Auto Save] menu. "File Auto Saving and Exporting" dialog box is displayed.

5 w

Menu Commands

q

r e

Figure 5.8 : "File Auto Saving and Exporting" Dialog Box (2) Set the following items. q [Auto Save] When saving a backup file automatically, select this check box. The saving interval and file name can be entered. w [every X samples] Enter the interval for saving a backup file. The input range is 1 to 300. The 5-9 AA-6200

5.2 [File]

number of measurement items (BLK, STD, UNK, MSA, SMSA, RESLOPE, QC and SPIKE) on the MRT is counted as the sample number. e [File Name] Set a path name (drive name + folder name + file name) of backup file. A path name can be entered easily by using < Brows...> (r). If a backup name is not entered, the default file name "autosave.aa" is automatically set. (3) Click the button to fix the settings.

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NOTE When the automatic saving is executed, the preceding backup file of auto-saving is renamed and backed up by adding ".sav." to the end of the file name.

Menu Commands

Example: When the auto saving is set with a file of the name "autosave.aa", executing another auto saving creates "autosave.aa.sav." as a backup of the preceding file.

5.2.8.2 Exporting the MRT work sheet data automatically in text file When performing an automatic measurement using the auto-sampler, the measurement result of the schedule and summary report can be exported in text style at the end of schedule of each element (or when the execution of the last row of each element on the MRT is finished). This setup is invalid for manual measurement. Also, only the data in the MRT work sheet can be exported in text file, but the measurement parameters and waveform data cannot be exported. NOTE To perform the text file auto export in manual measurement, set a "FILEEXPORT" row in the MRT work sheet.

[Operation] (1) Select [File]-[Auto Save] menu. "File Auto Saving and Exporting" dialog box is displayed.

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5.2 [File]

q w r e

5 t y

Menu Commands

o

u i

Figure 5.9 : "File Auto Saving and Exporting" Dialog Box (2) Set the following items. q [One element text file at the end of schedule] Select this check box to export the measurement result of each element in text style. w [Summary text file at the end of schedule] Select this check box to export the summary report in text style. e [Folder Name] This sets a destination folder of the text file automatically exported. Selecting the checkbox q or w makes this entry possible. A destination folder name can be entered easily by using < Brows...> (r). (3) Click the button to fix the settings. [Details] The AA software automatically gives a file name of the automatically exported text file. The measurement result of each element schedule is given a file name as "element name + measurement type (Flame:1, Furnace:2, HVG/MVU:3).txt". 5-11 AA-6200

5.2 [File]

For example, when Pb is measured in flame method, the text file name is "Pb1.txt". The file name of summary report is fixed to "summary.txt". These files are saved over the preceding one without any warning message. Therefore, "summary.txt" is overwritten whenever a measurement of each element is finished. Also, when the same element is measured in the same measurement method, note that firstly exported measurement result is overwritten. This automatic export function can be used for the automatic data collection by the host computer on the network, in a combination with the following "Executing a program by command line".

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Menu Commands

5.2.8.3 Executing a program by command line In the automatic measurement using the auto-sampler, a command line can execute a program when the schedule of each element is finished (when the execution of the last row on the MRT work sheet of each element is finished, or immediately after the auto-export of text file is finished). A command line means a method to specify an execution file name and start/execute the program, as MS-DOS prompt or "Start"-"Run..." in Windows. When executing a program from the command line, specify a combination of the execution file name or batch file name and its argument. In this dialog box, a name of text file to be exported automatically can be set up as argument. NOTE When executing a program by command line in manual measurement, set up "COMMAND" row in the MRT work sheet. [Operation] (1) Set the following items. t [Execute command after exporting text file] Select this check box to execute a program by command line. Then the command file name can be entered. y [Command File Name] Enter the execution file name. A file name can be entered easily by using < Brows...> (o). u [Add the element file name to the command] When this check box is selected, the single element text file name is set up as argument of command. This check box is selectable when the check boxes q and t are selected. 5-12 AA-6200

5.2 [File]

i [Add the summary file name to the command] When this check box is selected, the summary text file name is set up as argument of command. This check box is selectable when the check boxes w and t are selected. (2) Click the button to fix the settings. [Details] A file name of text file automatically exported is enclosed by " " (double quotation marks) and added to the end of a specified command line with an intervening space between them. When the both file names of schedule measurement result and summary report are added in the setting, the file name of summary report is added to the end of the file name of measurement result with an intervening space between them.

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Menu Commands

For example, when the command line is "C:¥something.bat" and when the Pb flame measurement result and summary report are to be automatically exported to the "C:¥My Documents¥AA Export" folder, and the both file names are to be added to the command line, the actual command line to be executed is as follows. C:¥something.bat "C:¥My Documents¥AA Export¥Pb1.txt" "C:¥My Documents¥AA Export¥summary.txt" If a special program is additionally prepared, this function can be utilized to give a notice of the measurement end to another room through a computer network or to collect or handle the measurement results outputted in text style.

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5.2 [File]

5.2.9 [Print Data/Parameters...] This command is used to print the measurement parameters and data of the currently opened file. When this command is selected, the element symbols available for printing the data and parameters are displayed in the dialog box that is same as Figure 5.6. From this list, select items to be printed and click on . Then the dialog box shown in Figure 5.10 opens. Set the [Copies] and click on . In the Print dialog box invoked from [Print Data/Parameters] menu, only [All] can be selected at [Print range].

NOTE When the parameters are changed in the middle of the measurement in one schedule, only the final parameters are printed out. To print the measured data and its parameters correctly on the report, create another schedule when measuring one element with different parameters.

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Menu Commands

Figure 5.10 : "Print" Dialog Box

5.2.10 [Print Table Data...] This command is used to print out the contents of MRT work sheet of currently opened file (For selecting items to be printed, refer to 5.2.11.2). When this command is executed, items which can be printed out are displayed in the dialog box as Figure 5.6. From this list box, select "Summary" or elements you want to print and click on . Clicking on button opens the "Print" dialog box (Figure 5.10). Operate in the same way as section 5.2.9. The data is printed out according to the format displayed on each MRT work sheet. 5-14 AA-6200

5.2 [File]

5.2.11 [Print Style] This command is used to make settings related to printing data and parameters from [Print Data/Parameters] menu. You can set the print mode, items and font here. When printing a peak profile data (waveform), set the graph scale in the "Y-axis Print Range" page by selecting [Parameters]-[Edit Parameters] from the menu bar. 5.2.11.1 "Print Style Setup" page

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Menu Commands

Figure 5.11 : "Print Style Setup" page Put check marks to the items or contents you want to print. Clicking on displays more detail items. In the [Data Print Mode], you can select it from the following three. All : All the data of repeat measurement with peak profile Without Profile : All the data of repeat measurement without peak profile Only Average : Only the average value calculated from repeat measurement data

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5.2 [File]

5.2.11.2 "Table Show/Hide" page When printing the data of MRT work sheet by selecting [File]-[Print Table Data] menu item, select items to be printed in this page. Put checkmarks in the items to be printed. 5.2.11.3 "Font" page

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Menu Commands Figure 5.12 : "Font" page Set the font type, size, style and other items. A sample of the characters based on the settings are displayed in [Preview]. These settings are valid only for "Print Data/Parameters".

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5.2 [File]

5.2.12 [Print Setup] Set the items related to the printer. Executing this command opens the "Print Setup" dialog box shown in Figure 5.13.

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Menu Commands

Figure 5.13 : "Print Setup" Dialog Box [Printer] Select the printer to be used from the drop-down list of [Name]. [Paper] Select [Size] and [Source]. [Orientation] Select [Portrait] or [Landscape] by clicking on radio button.

5.2.13 Recent Files Maximum four measurement file names recently opened are displayed. Click on the file name to be opened.

5.2.14 [Exit] When this command is executed, the communication with the instrument is shut off first and then the software is closed. Therefore, it takes approx. 30 seconds to exit the program. If the data has not been saved, a warning message to ask you whether you want to save the data before exiting the program or not.

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5.3

[Edit]

Functions to be used in editing the data row on MRT work sheet are summarized.

5 Figure 5.14 : Drop-down Menu of [Edit] Menu Commands

5.3.1 [Insert Row] This command is used to insert one row just before the row selected in the table. However, a row cannot be inserted to the row already measured.

5.3.2 [Delete Rows] This command is used to delete the selected rows in the table. However, the row already measured cannot be deleted. NOTE Insertion and deletion of a row next to current measuring row can't be done during measurement.

5.3.3 [Import Other Schedule] A measurement procedure created in other element's schedule is copied to the currently displayed (active) MRT work sheet. [Operation] (1) Click the element sheet tab of the MRT worksheet of the copy destination to make it active (displayed at the front). (2) Select [Edit]-[Import Other Schedule] menu. Then "Select Schedule" dialog box is displayed.

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5.3 [Edit]

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Figure 5.15 : "Select Schedule" Dialog Box

Menu Commands

In this dialog box, select the element schedule of copy source and click the button. All the measurement procedures in the element schedule of copy source are copied to the currently active element sheet.

NOTE If a measurement procedure already exists in the element schedule of the copy destination, a new measurement procedure is added to the end of the current measurement procedure continuously.

5.3.4 [Collective Edit] The values of a specified item can be changed collectively in selected rows on the MRT work sheet. The available items are C# (Calibration Number), Actual Conc. Unit, Weight Factor, Volume Factor, Dilution Factor and Correction Factor. [Operation] (1) Specify the region of the cells you want to change using the mouse (Click the first cell you want to change and drag it to the last cell while keeping the button pressed). (2) Select [Edit]-[Collective Edit] menu. "Collective Edit" dialog box is displayed. Each item has a check box. Put a check mark to the item you want to change. Enter a new set value in the checked items. (3) When completing them, click the to close the [Collective Edit] dialog box. The change is executed and the actual concentration is recalculated to renew the worksheet. 5-19 AA-6200

5.3 [Edit]

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Menu Commands

Figure 5.16 : "Collective Edit" Dialog Box

5.3.5 [Remeasure Selected Range] This is a function to perform a remeasurement on the data already measured. After selecting rows to be remeasured on the MRT work sheet, execute this. The rows already measured are excluded from the measurement result and new rows for the same measurement items are added on the MRT work sheet. In the case of repeat measurement, select a range including average rows to perform a remeasurement. A remeasuremnt cannot be executed for rows already excluded or rows with no data (RINSE, AUTOZERO, etc).

5.3.6 [Clear Measurement Result] All the measurement data on the MRT work sheet currently displayed are cleared and the status before measurement is recovered. The setting of measurement procedure remains without a change.

5.3.7 [Copy] Numeric values and characters on the MRT worksheet and summary table can be copied to the clipboard. Refer to the section 4.7.6 for details.

5.3.8 [Paste] Text data can be pasted from the clipboard only to the sample ID row in the MRT work sheet. Refer to the section 4.7.6 for details. 5-20 AA-6200

5.4

[Refer to Parameters]

Clicking on [Parameters] in Menu Bar during the measurement opens a drop-down menu.

Figure 5.17 : [Parameters] Drop-Down Menu

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Menu Commands

Selecting [Refer to Parameters] from this drop-down menu opens the property sheet, which is a dialog box to show the parameters for the element under measurement. The parameters can be shown but cannot be changed. To change the parameters, stop the measurement once and select [Parameters]-[Edit Parameters] from Menu Bar (Refer to section 5.6).

NOTE If a dialog box ("Line Search/Beam Balance", etc.) is opened in the sheet for referring to the parameters, the measurement operation is stopped temporarily. Therefore, close the dialog box immediately after referring to the necessary parameters.

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5.5

[Parameters]

Functions on parameter setup are summarized here.

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Figure 5.18 : Drop-down Menu of [Parameters]

Menu Commands

The following three Wizards are available. [Element Selection Wizard] Selection of measurement elements and setup of measurement element order are performed here. You may close the Wizard in the element selection page only. Or you may also proceed to the pages of schedule creation and measurement preparation to set the parameters until the measurement can be performed in that conditions. You can proceed to the next page only after selecting an element newly. Use the [Schedule Creation Wizard] or [Measurement Preparation Wizard] for elements already selected. [Schedule Creation Wizard] Setup of calibration curve parameters, setup of periodic blank measurement, setup of the sample information, and input of factors for actual concentration calculation are performed here and the measurement sequence is created on the MRT work sheet. This menu is valid when the element has been selected on the MRT work sheet. [Measurement Preparation Wizard] This is used for an element currently selected. Lighting of hollow cathode lamp, line search/beam balance, and setup of gas flow rate are performed. This menu is valid when an element exists on the MRT work sheet.

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5.5 [Parameters]

Each Wizard is composed of the pages shown below. Clicking on in each page opens the next page. You can close the Wizard by clicking on when the settings are completed on each page. [Element Selection Wizard] [Schedule Creation Wizard] Element Selection Element Selection Preparation Parameters Preparation Parameters Sample ID Sample ID Sample Selection Sample Selection Connect to Instrument/Send Parameters Optics Parameters for Lamp Position Adjustment Lamp Position Adjustment Optics Parameters Gas Flow Rate Setup

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Menu Commands

[Measurement Preparation Wizard] Connect to Instrument/Send Parameters Optics Parameters for Lamp Position Adjustment Lamp Position Adjustment Optics Parameters Gas Flow Rate Setup In the [Element Selection Wizard], the button is valid only when a newly selected element exists. In the [Measurement Preparation Wizard], the "Optics Parameters" is displayed first when the connection with instrument is already completed. The followings are description of each page in the Wizard.

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5.5 [Parameters]

5.5.1 "Element Selection" Page Measurement elements are selected and their parameters are edited here.

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Menu Commands

Figure 5.19 : "Element Selection" Page

When adding an element to be measured, click on this button. Then "Load Parameters" dialog box opens. For details, refer to 5.5.1.1 and 5.5.1.2.

Select an element row and click on this button. Then the "Edit Parameters" dialog box opens. For details, refer to section 5.6. NOTE After selecting an element row, click on the right mouse button. Then a selection of Stop/Continue at the end of measurement can be set up.

Select an element row and click on this button. Then the row moves up one row upper.

Select an element row and click on this button. Then the row moves down one row lower. 5-24 AA-6200

5.5 [Parameters]

If you want to delete a row, click on the row to make its color reversed and then click on . When the lamp of selected element is lit on, you can't delete it. Please turn off the lamp in "Optics Parameters" page for current measurement element or [Instrument]-[Lamp Status] menu and delete the element.

Communication between the personal computer and AA main unit is built. For details, refer to 5.8.1. [Meas. Element] Select the element to be measured first from the drop-down list. The measurement is started from this element and performed to the last row in order.

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Menu Commands

5.5.1.1 "Cookbook" page In the "Cookbook" page, select the target element from the drop-down list. Also, select the hollow cathode lamp socket number in this page. At this time, description of each parameter to be set is displayed on the screen. Since the contents of this cookbook has been written in the program beforehand, you cannot make a change.

Figure 5.20 : "Cookbook" page

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5.5 [Parameters]

Click on this button, then you can select the target element from the periodic table or element list. [Using ASC] When using the autosampler, put a check mark in the check box. [HVG] and [MVU] Putting a check mark in the check box calls the parameters for using the hydride vaporizer unit (HVG) or the mercury vaporizer unit (MVU). This check box gets active when the element measured by the cold vapor mercury technique or the hydride vapor technique is specified.

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5.5.1.2 "Template" page

Menu Commands Figure 5.21 : "Template" page In the "Template" page, a template (*.taa) already created can be read. Click on to open the "Open" dialog box. Then specify the [Look in] and [File name] and click on . When the template is opened, Figure 5.21 is displayed. Click on the element in [Element Selection] to highlight it, then the description of parameters for the element are displayed in the right side of the element. When the template contains plural elements, you can specify the element to read the parameters. Put a check mark in the check box next to the element name only for 5-26 AA-6200

5.5 [Parameters]

the element you need. Clicking on returns to the "Element Selection" page. You can check that the selected element name is added in the measurement order field. When using a wavelength or flame type which is different from that in the "Cookbook", it is convenient to create a template (*.taa) with the parameters beforehand. In WizAArd, "Cookbook.taa" (flames for Ca, Pb and Sn) and "HyperLamp.taa" (hyperlamps for As, Se, Sb and Pb) are already prepared.

5.5.2 "Preparation Parameters" Page You can set the calibration curve parameters and the preparation parameters for standard / unknown / periodic blank samples.

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Menu Commands

Figure 5.22 : "Preparation Parameters" Page Double-click on the element to be edited, or select the element row and click on to open the "Edit Preparation Parameters" dialog box.

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5.5 [Parameters]

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Menu Commands

Figure 5.23 : "Edit Preparation Parameters" Dialog Box [Measurement Type] Select either of "Calibration Curve" (calibration curve method) or "SMSA (Simple Method of Standard Addition)". In this case, the "MSA (Method of Standard Addition)" cannot be selected. To set the calibration curve parameters for MSA (Method of Standard Addition), refer to 4.9. [Order] and [Zero Intercept] Select the order of calibration curve polynomial. You can select 1st, 2nd or 3rd. Putting a check mark to [Zero Intercept] will force the calibration curve to pass through the origin. When the simple standard addition method is selected, 1st order without Zero Intercept are automatically set, and these items are not displayed on the screen.

Number of repeat measurement, Maximum number of repeat measurement, RSD limit and SD limit are set here. For details on the setting items, refer to 5.6.2. [Conc. Unit] Set the concentration unit used for [True Value] and [Conc.] in MRT work sheet. 5.5.2.1 Weight Correction Factors The factors used for calculating the actual concentration are set here. 5-28 AA-6200

5.5 [Parameters]

NOTE Actual concentration is calculated with the following equation. Actual Conc. = (Measured Conc.) × [Volume Factor] × [Dilution Factor] × [Correction Factor] / [Weight Factor] However, there is no particular function to set units for [Weight Factor] and [Volume Factor]. Note that the entered values are only calculated using the above equation. Use [Correction Factor] to convert the unit. [Weight Factor] Enter the sampling weight or sampling volume. [Volume Factor] Enter the weight or volume after the sample is dissolved or processed and brought up to a specific volume. [Dilution Factor] Enter the dilution factor when the sample solution is diluted after brought up to the above specific volume. [Correction Factor] Arbitrary factor necessary for unit conversion can be set.

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Menu Commands

5.5.2.2 [Preparation Parameters]-[STD Samples] The standard sample preparation parameters are set here. (when the ASC is not used, only the [Conc.] field of the table is available). [Number of STD] Enter the number of standard samples to be measured. Maximum 8 can be entered. The row number of the [Preparation Parameters]-[STD Samples] table displayed on the screen is set by this number. [Conc.] Enter the concentrations of standard samples in the order of measurement. [Pos.] In the case of calibration curve method, enter the position (1 to 60, R1 to R8) of standard sample. In the case of simple standard addition method ("SMSA"), enter the position (1 to 60, R1 to R8) of unknown sample to which the standard sample is added. NOTE When using the ASC, put a check mark in the check box of [Using ASC] in "Sequence" page of "Edit Parameters" dialog box. 5-29 AA-6200

5.5 [Parameters]

5.5.2.3 [Preparation Parameters]-[Blank Samples] Set how many every samples the periodic blank is inserted at the time of automatic creation of measurement schedule. [Periodic Blank] Selecting "On" will insert a blank measurement periodically at the time of automatic creation of measurement schedule. [Meas. Interval] For example, entering "5" will insert the blank measurement row after every five unknown sample rows. [Pos.] Set the position (1 to 60, R1 to R8) of blank sample when using the ASC.

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5.5.3 "Sample ID" Page Menu Commands

Number of unknown samples to be measured, sample names and sample positions for connected autosampler are set in the screen.

Figure 5.24 : "Sample ID" Page [Number of Samples] Enter number of unknown samples here. Then the rows as much as the sample number are created in the table. For each sample, the following setup are available. [Sample ID] Enter the name to identify the sample. In the "Summary" of MRT work sheet, concentration result of each element is listed based on this sample ID, then the summary report of plural elements are created for each sample. 5-30 AA-6200

5.5 [Parameters]

NOTE In the case of simple standard addition method, the position setting for the 1st sample is ignored because the 1st unknown sample is measured by the method of standard addition. The 1st sample position is set as the item of [STD Samples] preparation parameters in "Edit Preparation Parameters" dialog box.

[Pos.] When using the autosampler, set the sample position on the sampler turn table.

Clicking on this button opens "Sample ID Collective Setup" dialog box. In this dialog box, the sample ID described above can be easily entered.

5

Menu Commands

Figure 5.25 : "Sample ID Collective Setup" Dialog Box This dialog box is used to set sample ID with successive No. automatically and ASC start position for the autosampler. When completing the settings, click on . [Number of Samples] Enter the number of unknown samples. [Create Sample ID] Marking a check in this box allows to enter sample ID automatically. [Name] Enter a common sample name here. [Start No.] Enter the first number of successive number. [ASC Start No.] Enter the measurement start position on the autosampler turn table when using the ASC. Successive numbers are set as much as the number of samples.

5.5.4 "Sample Selection" Page Specify the elements to be measured for each sample. 5-31 AA-6200

5.5 [Parameters]

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Menu Commands

Figure 5.26 : "Sample Selection" Page Place a mark in the cell of element to be measured and delete a mark from the cell of element not to be measured. When selecting plural cells, drag them and click on the right mouse button to select "Measure/Not Measure".

5.5.5 "Connect to Instrument/Send Parameters" Page

Figure 5.27 : "Connect to Instrument/Send Parameters" Page 5-32 AA-6200

5.5 [Parameters]

Communication between the personal computer and AA main unit is connected. If the communication connection has been already completed, this button is invalid. For details, refer to the section 5.8.1.

If the power of ASC is not ON when connected to the instrument, ASC is not recognized. At that time, turn on the power of ASC then click on this button. [Meas. Element] Select an element whose parameters are to be set in the following "Optics Parameters" page, "Optics Parameters for Lamp Position Setup" page, "Lamp Position Setup" page and "Gas Flow Rate Setup" page.

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5.5.6 "Optics Parameters" Page Menu Commands

Wavelength, slit width, socket number, lamp current, lamp mode, lamp ON/OFF are set for the selected element. Since the default values in the "Element Selection" page of Wizard are automatically set, you don't have to change wavelength, slit width or lamp current. Select lamp mode according to the sample to be analyzed. "Optics Parameters for Lamp Position Adjustment" page is displayed prior to "Lamp Position Adjustment" described later (5.5.7). Set the optical parameters for adjusting the lamp position here. The lamp mode is fixed to Emission. If the lamp position adjustment has been already finished, cancel the execution of Line search/beam balance and go ahead. Optics parameters for measurement are set in "Optics Parameters" page displayed after the "Lamp Position Adjustment" page.

Figure 5.28 : "Optics Parameters" Page 5-33 AA-6200

5.5 [Parameters]

[Wavelength] The analysis wavelength is selected. As the default value, the wavelength of first resonance line (analysis line of the highest absorption sensitivity) is displayed. To use another wavelength, enter the value in the range of 190.0 to 900.0 (nm). When Line Search is executed, the wavelength is automatically set to this value. [Slit Width] The slit width of monochromator is set. A slit width used ordinarily is displayed. Turn the slit knob located on the left panel of the instrument to the selected slit width. If the light intensity of hollow cathode lamp is weak and if there is too much baseline noise, widen the slit width. Note that in the BGC-D2 mode, it is necessary to consider the balance between the light intensities of the deuterium lamp and the hollow cathode lamp. If the light intensity of the deuterium lamp is too great, narrow the slit width. Conversely, if the light intensity of the hollow cathode lamp is too great, widen the slit width.

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Menu Commands

NOTE When a neighboring line exists, note that the neighboring line may not be separated if the slit width is widened.

If the “Lamp Position Setup” dialog box is used and button is shown on "Optics Parameters" page, it is necessary to set the hollow cathode lamp to be used and its socket No. beforehand in "Lamp Position Setup" dialog box. Refer to the section 5.8.4 for details. [Socket #] Enter the socket number to which the hollow cathode lamp of the selected element is mounted. [Lamp Current] The lamp current is entered here. A recommended current has been entered already. If you want to change the lamp current, enter the current value not exceeding the maximum lamp current value according to the instruction manual of the hollow cathode lamp. Lamp is automatically lit with the specified current value when executing . When the lamp current is changed, it is actually reflected on the instrument in the following cases. • When the line search/beam balance is executed. 5-34 AA-6200

5.5 [Parameters]

• When the Parameters sheet or Wizard is closed with / (except when a necessary line search is cancelled). • The lamp current of warmup lamp is changed only when is clicked in the “Select Warmup Lamp” dialog box after is clicked in the [Optics Parameters] page of the main element lamp. [Lamp Mode] The following five modes are available (Also refer to the section 3.1.6). EMISSION mode This mode is used in flame emission analysis or when performing lamp or burner positioning adjustment. A value proportional to the intensity of light incident upon the detector is displayed. In flame emission analysis, energy intensity of emission spectrum of the target element generated in flame is measured without using the hollow cathode lamp. NON-BGC mode This mode is used for atomic absorption analysis that does not require background correction, or atomic absorption analysis in the long wavelength range (430 to 900 nm) where background correction by deuterium lamp cannot be used. The deuterium lamp does not light, so only the light of hollow cathode lamp is used. Transmission amount of lamp energy that passed the atomizer unit is detected and then is converted into absorbance. If molecular absorption other than the atomic absorption exists on the same wavelength of the target element, such absorption is simultaneously observed. In such case, use BGC-D2 mode. BGC-D2 mode This mode is used for atomic absorption with background correction by deuterium lamp. If molecular absorption other than the atomic absorption exists on the same wavelength of the target element, true absorbance cannot be obtained in NON-BGC mode. In such case, make the light of deuterium lamp together with the light of hollow cathode lamp pass through the atomizer unit. Though the light of deuterium lamp cannot detect atomic absorption of narrow band, it can detect absorption of wide band such as the molecular absorption. Accordingly, it is possible to get true absorbance by taking difference of absorbance at the both lamps. [Lamp Status] When the Line Search is not finished or when wavelength or slit width is changed after execution of Line Search, "Line Search is necessary" is indicated. When lamp current or lamp mode is changed after execution of Beam Balance, "Beam Balance is necessary" is indicated. If the button is pressed

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Menu Commands 5-35

AA-6200

5.5 [Parameters]

while these are indicated, the Line Search/Beam Balance is appropriately executed. When closing the "Optics Parameters" page with or button, a message appears to ask whether to execute the Line Search/Beam Balance or not. Execute it, if necessary. [Lamp ON] Click on the check box to put a mark in it. Then the hollow cathode lamp of specified socket number is lit on. When a check mark is already indicated, clicking on the check box will delete the check mark and the lamp is turned off. The lamp will be automatically lit on when the is executed even if the Lamp is OFF. [ASC Sample Pos. for EMISSION Line Search] In flame emission analysis, can be performed while spraying a sample automatically using the ASC. Set the position of the sample (ordinarily, the standard sample of the highest concentration) on the ASC turntable. This setting is valid only when the lamp mode is EMISSION and [Lamp Current] is "0".

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Menu Commands

5.5.6.1 Button Set the items to warm up the hollow cathode lamp of the element to be measured next. Clicking on this button opens the "Select Warmup Lamp" dialog box.

Figure 5.29 : "Select Warmup Lamp" Dialog Box

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5.5 [Parameters]

First, select an element in [Schedule]. Next, click on , then the parameters, [Socket #] and [Lamp Current], loaded in the element selection are automatically set and the lamp is lit ON. If you don't want to light on the lamp here, select [Schedule] then click on . When plural elements are selected in "Element Selection" page and autosampler is used, the instrument automatically judge and light on the warm-up lamp if no setting is made in this "Select Warmup Lamp" dialog box. In addition, according to the setting [Lamp Warmup Time] in "Sequence" page, the ending time is estimated and warming up of the hollow cathode lamp of the next measurement element is started. Therefore, when starting a measurement, the lamp of the next measurement element may not be lit on.

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Menu Commands

5.5.6.2 Button Clicking on this button opens the "Line Search/Beam Balance" dialog box. When the button is pressed in the "Optics Parameters" page of the currently measured element, the Line Search/Beam Balance is automatically executed, if necessary. If the Line Search/Beam Balance is already finished, only the result is displayed. When the element is not the currently measured element, only the result of the Line Search/Beam Balance execution is displayed.

Figure 5.30 : "Line Search/Beam Balance" Dialog Box 5-37 AA-6200

5.5 [Parameters]

When this button is clicked on, this dialog box is closed to return to previous screen.

If this button is clicked on during execution of line search, beam balance execution stops.

Clicking on this button lights the lamp, scans wavelength near the set wavelength, and detects the highest peak in the emission profile according to the parameters set on [Optics Parameters] page. Scanning wavelength is performed within the range of the set wavelength ±1.2 nm. When the correct peak is detected, "Line Search: OK" is indicated. Successively setup of lamp mode and optimization of detector sensitivity (beam balance) are performed. When the sensitivity setup is finished, "Beam Balance: OK" is indicated.

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Menu Commands

NOTE When the Beam Balance is performed, in some cases, an error message indicating that hollow cathode lamp emission is too high or too low compared with D2 lamp emission. Change [Lamp Current] to a smaller value when it is too high, and change [Lamp Current] to a larger value when it is too low.

The result of Line Search is printed out. 5.5.6.3 Button The line search detects the highest peak near the selected wavelength. However, in some cases, the neon gas sealed in the hollow cathode lamp radiates at a higher peak than the light of the measured element. You must select the appropriate peak from a list of detected peaks.

Figure 5-31 : Wavelength Memory Setup 5-38 AA-6200

5.5 [Parameters]

Select the element's highest peak from the Detected Peak list box and click on the arrow button. The selected wavelength is placed in the [Memory Wavelength] field. The wavelength is stored, and the wavelength will be used as an analysis line after the next line search is performed. Therefore, even if other higher peaks near the set wavelength are detected, the correct analysis line will be used. [Actual Wavelength] Displays the wavelength set in the Wavelength field on the "Optics Parameters" page. [Memory Wavelength] Select a wavelength used as the analysis line from the [Detected Peaks] list box. The wavelength set here is stored in the AA software.

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Menu Commands

[Detected Peak] The Detected Peak list box displays the wavelength peaks detected during the Line Search. Select the wavelength of the proper analysis line, and click on the Arrow button. The selected wavelength is entered into the [Memory Wavelength] field. [Clear] Click this button to clear the data from the [Memory Wavelength] field.

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5.5 [Parameters]

5.5.7 "Lamp Position Adjustment" Page The fields on this page (figure 5-32) adjust the position of the hollow cathode lamp to the optimum position. The bar graph monitors the lamp energy. The maximum value is recorded in the [Max.] field ; the minimum value is recorded in the [Min.] field.

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Menu Commands Figure 5-32 : Lamp Position Adjustment Dialog Box Manually rotate the hollow cathode lamp turret, searching for the position where the [Current] value equals the [Max.] value. Perform line search/beam balance in the previous "Optics Parameters for Lamp Position Adjustment" page to adjust lamp position correctly in this page. [Max.] (Maximum), [Min.] (Minimum), and [Current] The [Max.] and [Min.] fields display the maximum and minimum lamp energy recorded as you rotate the hollow cathode lamp turret. The [Current] field displays the current energy value.

Use the button to reset all fields on this tab. 5-40 AA-6200

5.5 [Parameters]

5.5.8 "Gas Flow Rate Setup" Page Parameters related to flame type and gas flow rate are set in this screen. In the graph displaying real time data, the right mouse button menu can be used as in the real time graph of the main window (refer to section 4.6.5). (Only the [Properties], [Copy] and [Radar] are available.)

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Menu Commands

Figure 5-33 : "Gas Flow Rate Setup" Page [Flame Type] Select a type of flame used for analysis from the drop-down list. When using a N2O-C2H2 flame, the optional high temperature burner head must be installed. [Fuel Gas Flow Rate] This field displays the flow rate of acetylene gas which should be used for analysis. The default flow rate is entered. If the gas flow rate should be changed, enter the flow rate into this field (which is an information field only) and on the instrument adjust the gas flow to the new setting. When N2O-C2H2 is selected, a [Meter] indication appears. Adjust the flow meter on the instrument so that it equals the rate displayed in the [Meter] field.

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5.5 [Parameters]

[Support Gas Flow Rate] The [Support Gas Flow Rate] displays the flow rate of the oxidant gas (Air or N2O) used for analysis. A default rate is entered. To change the gas flow rate, enter the new flow rate, then adjust the oxidant flow meter on the instrument accordingly.

NOTE The oxidant gas flow meter is scaled so as to display the actual flow rate of Air. Therefore, when the oxidant gas is N2O, note that the scale in the flow meter differs from the actual flow rate. For example, the actual flow rate of N2O gas is set to 6.5 L/min when adjusting the oxidant gas flow meter to "8.0" shown in the scale.

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Menu Commands

[Measured Data] The current measurement data is displayed. In the background correction modes, the indicated value as this [Measured Data] is the result calculated by subtracting the background data from the original measured data. [Background Data] In the background correction mode, the background data is displayed.

The current indicated value is shifted to zero.

5-42 AA-6200

5.6

[Edit Parameters]

Executing this opens the "Edit Parameters" dialog box. This is used to set each parameter individually without using Wizard. In this case, you can change the settings for the element of the MRT work sheet which you can select by clicking on the tab in the left lower of the main window.

NOTE In the "Edit Parameters" dialog box, you can make a change or reference only for the element selected on the MRT work sheet.

When completing the setup for all the pages, click on . To cancel the setting halfway, click on . Then the settings return to the previous conditions before changed.

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Menu Commands 5-43 AA-6200

5.6 [Edit Parameters]

5.6.1 "Measurement Parameters" Page

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Menu Commands

Figure 5.34 : "Measurement Parameters" Page At the start of sample aspiration, the signal is not stable. The time required for introducing sample to the flame until the signal becomes stable is referred to as pre-spray time.

Pre-Spray (Time)

Integration Time

Figure 5.35 : Pre-Spray and Integration Time.

5-44 AA-6200

5.6 [Edit Parameters]

[Repetition Sequence] This will set whether pre-spray is conducted during repeat measurement. There are 2 types of settings. (S:Spray, M:Measure) SM-SM-..

In repetition sequence, pre-spray is conducted prior to each repetition of sample measurement.

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Menu Commands

Figure 5.36 : Repetition Sequence (SM-SM-...) SM-M-M-... In repeat measurement, pre-spray is conducted only prior to the first repetition of sample measurement. Select this type when it is appropriate to continue spraying sample throughout the repeat measurements.

Figure 5.37 : Repetition Sequence (SM-M-M-...)

NOTE In the case of automatic measurement with the ASC, the instrument always operates as "SM-M-M-..." even if "SM-SM..." is selected as the repetition sequence.

5-45 AA-6200

5.6 [Edit Parameters]

[Pre-Spray Time] and [Integration Time] Enter the time interval to be used for pre-spraying and for signal integration (measurement time). The integration time (measurement time) will start directly after elapse of the pre-spray time. There is no integration of the signal during the pre-spray. [Response Time] This selects the time constant of signal response. The time constant of signal response corresponds to time constant in the Real Time Graph Monitor. That is to say, the signal profile displayed on the graph is affected by the response. In the case of #1, the profile is close to the actual signal profile. As the value increases from #1 to #4, the profile becomes more and more processed, as if a filter is applied. When excessive noise is a problem, settings in the direction of #4 will provide better repeatability.

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Menu Commands

NOTE [Pre-Spray Time] must be changed depending on the property of the sample. For example, take long [Pre-Spray Time] for sample with viscosity. If the absorbance of the sample is low, and liable to be affected by noise, take long [Response time]. In this case also, since it takes long time to become stable after spray of the sample, set the following time as [Pre-Spray Time] in standard operation. Time until stabilization Response Time 1 : 3 sec. Response Time 2 : 5 sec. Response Time 3 : 10 sec. Response Time 4 : 20 sec.

5-46 AA-6200

5.6 [Edit Parameters]

5.6.2 "Repeat Measurement Conditions" Page Number of repeat measurements is set here.

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Menu Commands

Figure 5.38 : "Repeat Measurement Conditions" Page

5-47 AA-6200

5.6 [Edit Parameters]

[Blank] This row is for setting the repeat conditions for blank measurement. [Standard] This row is for setting the repeat conditions for standard measurement and standard addition measurement. [Sample] This row is for setting the repeat conditions for unknown sample measurement and simple standard addition measurement. [Reslope] This row is for setting the repeat conditions for sensitivity correction measurement. [Num. of Reps.] and [Max. Num. of Reps] The number of repetition refers to the minimum number of measurement repetitions to be used in acquiring data. After completing this set number of measurement repetitions, the average value, relative standard deviation and standard deviation are calculated. Then, the measurement repetitions will continue until (1) the RSD value limit is satisfied, (2) the standard deviation limit is satisfied, or (3) the maximum number of repetition is reached. Setup is possible up to 20 for each item. [RSD Limit] and [SD Limit] Both the RSD (Relative Standard Deviation) limit and the SD (Standard Deviation) limit are indicators of data scattering. If these values are small enough, the data is considered to be stable and the measurement results reliable. Normally, set the SD limit value to 0 and use only the RSD limit. However, since the average value is used as the denominator for the RSD limit, as shown in the following equations, a small value is difficult to attain when samples of low concentration are measured. In such cases, use the SD limit in addition to the RSD limit. After the set repetition number (Num. of Reps) is over, the average value, RSD and SD are calculated using the combination of set number of measured data which provides the smallest amount of data scattering. n : Number of measurement data Xi : Measured data (i=1 to n)

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Menu Commands

Σ(Xi)

Average value :

µ=

SD

:

σ=

RSD

:

RSD = σ µ ×100(%)

5-48 AA-6200

n

nΣ(Xi2)-[ΣXi]2 n(n-1)

5.6 [Edit Parameters]

5.6.3 "Weight Correction Factors" page The following are set here. • Factors used in actual concentration calculation. • Actual concentration unit • Decimal place of the factors and actual concentration to display and print

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Menu Commands

Figure 5.39 : "Weight Correction Factors" Page

NOTE Actual concentration is calculated with the following equation. Actual Conc. = (Measured Conc.) × [Volume Factor] × [Dilution Factor] × [Correction Factor] / [Weight Factor] However, there is no particular function to set units for [Weight Factor] and [Volume Factor]. Note that the entered values are only calculated using the above equation. Use [Correction Factor] to convert the unit.

5-49 AA-6200

5.6 [Edit Parameters]

[Weight Factor] Enter the sampling weight or sampling volume. [Volume Factor] Enter the weight or volume after the sample is dissolved or processed and brought up to a specific volume. [Dilution Factor] Enter the dilution factor when the sample solution is diluted after brought up to the above specific volume. [Correction Factor] Arbitrary factor necessary for unit conversion can be set. [Actual Conc. Unit] Enter a unit for actual concentration. [Decimal Place] Set a decimal place for displaying and rounding the Weight Factor, Volume Factor, Dilution Factor, Correction Factor and Actual Conc. This decimal place is used for actual concentration calculation, the display on the screen and data print.

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Menu Commands

5.6.4 "Y-axis Print Range" Page Enter the graph scale to print the peak profile with [File]-[Print Data/Parameters...].

5.6.5 "Analyst" Page Enter the analyst name and file comment. They are output when printing the parameter, and saved together with the file.

5.6.6 "Comment" Page Comment is added to the element name. When the same element is measured with different parameters, you can identify them with this comment. This comment is displayed in the element combo box on the main window and on the MRT work sheet tab together with the element name. Characters up to 10 can be displayed on the tab. If a line feed is included, however, only the characters before the line feed are displayed.

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5.6 [Edit Parameters]

5.6.7 "Sequence" Page

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Menu Commands

Figure 5.40 : "Sequence" Page [Using ASC] Put a check mark in the check box when using the ASC. [At the End of Measurement] When measuring plural elements successively, you can select to stop the measurement once at the end of each element or to continue the measurement. [Lamp Warmup Time] Set the hollow cathode lamp warmup time, which is a waiting time after lighting on the lamp and before starting the measurement, in the unit of minute. To select the lamp warmup time, check the time from lighting the lamp to stabilizing the signal while observing the real time graph in the flame measurement. Usually it is set to 5 to 30 minutes depending on the element and the lamp condition such as deterioration degree.

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5.6 [Edit Parameters]

5.6.8 "QA/QC Setup" Page In this page, select the ON/OFF of checking with each QC type, set the standard value, and select the action when the result is out of standard range.

NOTE After the data evaluation based on the QA/QC setup is executed, the calibration curve order, zero intercept and signal processing mode settings cannot be changed after the measurement. When these settings are expected to be changed after the measurement, set all the check boxes to OFF before starting the measurement.

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Menu Commands Figure 5.41 : "QA/QC Setup" Page (1) The followings are the QC types. • Correlation coefficient (= r) This factor indicates the degree of agreement of the measured point (data) with the calibration curve obtained by the least squares method. A value closer to "1" is desirable. The "r" is calculated using the following equation. r=

N Σxiyi−ΣxiΣ yi [NΣxi2−(Σ xi)2]   [NΣyi2−( Σyi)2]   1 2

1 2

Put a check mark in this check box, and set "CAL-CHK" in [Action] field after a series of STD measurements on the MRT work sheet to execute the evaluation by correlation coefficient. 5-52 AA-6200

5.6 [Edit Parameters]

NOTE "CAL-CHK" setting is necessary only in the calibration curve method. In standard addition method and simple standard addition method, this setting is not necessary because the evaluation is done at "MSA-RES". • LCS (QC Standard) (Laboratory Control Sample: Evaluation by standard sample) This is the evaluation using a standard sample with known concentration. The ratio between certified value and obtained value is calculated for evaluation. %R= Concentration ×100 True Value

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In this case, "True Value" means a certified value. Set this value in [True Value] field on the MRT work sheet. Put a check mark in this check box, and set "QC" in [Action] field on the MRT work sheet to execute the evaluation by LCS.

Menu Commands

• SPK (Spike) (Pre-Digestion Spike: Addition and recovery without pretreatment) This evaluates the recovery degree of the amount added to the sample. It is calculated by the following equation. %R=

SSR – SR SA

×100

SR : Measured result of sample without addition ([Conc.] value of UNK on the MRT work sheet) SSR : Measured result of sample with addition ([Conc.] value of SPIKE on the MRT work sheet) SA : Amount of addition (Calculated value) (Enter this value in [True Value] field of SPIKE on the MRT work sheet) Mark a check in this check box, and set "SPIKE" in [Action] field after "UNK" whose recovery degree you wish to get on the MRT work sheet. It executes the evaluation by SPK. • Sample Upper Limit Put a check mark in the "Sample Upper Limit" check box, the software evaluates whether the concentration of each sample is within the standard value. • %RSD (Relative Standard Deviation) Put a check mark in the "%RSD" check box, the software evaluates whether the deviation of repeat measurement results of each sample is within the standard value. 5-53 AA-6200

5.6 [Edit Parameters]

NOTE RSD Limit and SD Limit on the Repeat Measurement Conditions page are used as the standard value of %RSD.

(2) The default (initial) standard values displayed on the screen are the values recommended by EPA (United States Environmental Protection Agency) method. However, the values can be changed. (3) Also, in the [Out of Control Remark], you can set "Stop Measurement" or "Mark and Continue" when each QC type value exceeds the range of standard value.

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5.6.9 "Calibration Curve Parameters" Page

Menu Commands Figure 5.42 : "Calibration Curve Parameters" Page [Order] Select an order of calibration curve equation. You can select 1st, 2nd or 3rd. [Zero Intercept] Putting a check mark in the check box will create the calibration curve equation that forcibly intercepts the origin. When the standard addition method or simple standard addition method is selected, setup is made automatically to "1st" and "no zero intercept", and these items are not displayed. 5-54 AA-6200

5.6 [Edit Parameters]

NOTE [Correlation Coefficient calculation of calibration curve when Zero Intercept is selected] When the order of the calibration curve is 1st, the correlation coefficient of the calibration curve is not changed by changing the selection of zero intercept. This may seem unnatural, but can be understood as follows. The correlation coefficient shows the relation of "increasing way" of two quantities. When the order of the calibration curve is 1st, the increase is linear whether the zero is intercepted or not. Therefore, the relation of increasing way is also not changed (the slope of linear line has no relation with "Correlation").

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[Conc. Unit] Unit of concentration used in MRT work sheet is set here.

Menu Commands

5.6.10 "Optics Parameters" Page The contents are the same as the "Optics Parameters" page in Wizard (Refer to 5.5.6).

5.6.11 "Gas Flow Rate Setup" Page The contents are the same as the "Gas Flow Rate Setup" page in Wizard (Refer to 5.5.8).

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5.7

[Default Parameters]

This sets the parameters which are read in as initial values when creating a new file. The parameters for QA/QC setup, calibration curve parameters, repeat measurement conditions, measurement parameters and sequence can be set here. Contents and operation of each page are completely the same as those of the "Edit Parameters" dialog box. Refer to the section 5.6.

5.7.1 [Flame] The "Default Parameters for Flame" dialog box is opened.

5.7.2 [Furnace] This menu item is not available for AA-6200.

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5.7.3 [Graph] Menu Commands

"Graph Default Scale" dialog box is opened. The ordinate scale and the time width for real time graph can be set here.

Figure 5.43 : "Graph Default Scale" Dialog Box

5.7.4 [Analyst] "Default Analyst" dialog box opens. Enter [Analyst] and [File Comment] newly, then the entered contents are used when creating a new file next time.

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5.8

[Instrument]

The functions related to instrument hardware are summarized in this menu.

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Menu Commands

Figure 5.44 : "Instrument" Drop-Down Menu

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5.8 [Instrument]

5.8.1 [Connect] If this menu is selected, communication between the instrument and personal computer will be performed. After starting communication, first "Initialize" screen is displayed, where the instrument information (model, ROM version, serial No.) of AA/ASC and the progress of hardware initialization is sequentially displayed. Item under check is indicated in yellow, items successfully completed are indicated in green, items with failure are indicated in red. In takes several minutes to finish the initialization. If all items are indicated in green, the initialization is correctly completed. Click on button to close the screen. The items of [ASC Check] is indicated in red even if it is not connected with the AA main unit. When the ASC is not used from the first, it doesn't mean an abnormal status. When the communication is performed again while the power of instrument is ON, "Wavelength Origin Search" is not performed.

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Menu Commands Figure 5.45 : "Initialize" Dialog Box After closing the "Initialize" dialog box, "Instrument Check List for Flame Analysis" is displayed.

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5.8 [Instrument]

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Menu Commands

Figure 5.46 : "Instrument Check List for Flame Analysis" Dialog Box To use the instrument safely, check the items indicated on this screen before igniting a flame. Put a check mark to the item after checking it. When all the items are marked, you can select . After completing the inspection, click on to close the dialog box.

NOTE "Instrument Check List for Flame Analysis" dialog box is displayed at every initialization time. This dialog box can also be displayed by a user's selection when an error related to gas controller occurs. When checking or setting the oxidant gas flow rate before ignition in the case of N2O-C2H2 flame analysis, the kind of oxidant gas flowing from the burner head by pressing the PURGE button is different depending on the timing of displaying this dialog box (see the table below). Timing of display At the time of initialization

Oxidant gas type flowing with PURGE button Always Air

When a gas controller error has occurred

N2O when the instrument is ready for N2O-C2H2 flame combustion. Air in other cases.

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5.8 [Instrument]

5.8.2 [Option Connect] This indicates the connection status between the AA main unit and the peripheral attachments (ASC).

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Figure 5.47 : "Option Connect" Dialog Box

Menu Commands

Click on this button when turning on the power of peripheral attachment (ASC) after the communication between the personal computer and AA main unit are completed.

5.8.3 [Configuration] The PC communication port and the type of AA main unit are set here. Selecting this menu opens "Configuration" dialog box.

Figure 5.48 : "Configuration" Dialog Box 5-60 AA-6200

5.8 [Instrument]

[COM Port] The communication port on the PC is set here. Set the number of port to which the communication cable with the AA main unit is connected. [Instrument Type] This indicates the AA main unit model with which this software can be connected. [Instrument type is checked when connected] Putting a check mark in the check box will give an alarm if the connected instrument is different from [Instrument Type]. [Flame ASC Rinse Time] Enter a numeric value from 0 to 600 (seconds). When a numeric value except "0" is entered, the ASC executes the rinse for every sample. [Flame ASC Autozero in Rinsing] This function is used to set the baseline to zero frequently in the flame measurement with ASC. When this check box is set to ON, the auto zero is executed every after the rinse for each sample while keeping the rinse liquid aspirated. For example, when [Flame ASC rinse time] is set to "10 seconds", the auto zero is executed (for 10 seconds) after executing the rinse for 10 seconds. So the rinse liquid is aspirated for approx. 20 seconds in total.

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Menu Commands

NOTE If the auto zero is executed with an insufficient rinse, the zero set is executed before the signal has not go back to the base, as the result, the measurement cannot be performed properly after that. Before using this function, check that the signal in the real time graph goes down to the base within the time set in [Flame ASC rinse time].

[Action setup when measurement is finished] This sets the Automatic Flame Extinction Yes/No and Automatic Lamp Extinction Yes/No when the measurement is finished. This action is also applied when "Stop" is selected for switching the element in measuring plural elements. This is valid only when using ASC. [Action setup when measurement is stopped] The measurement is stopped by QA/QC judging process. In this case, you can set "Automatic Flame Extinction YES/NO" and "Automatic Lamp Extinction YES/NO". These are valid only when using ASC. [Automatic Flame Extinction] Put a check mark in the check box to extinguish the flame automatically. 5-61 AA-6200

5.8 [Instrument]

[Wait Time] Enter a numeric value (minute) to wait before extinguishing the flame. In the automatic continuous measurement using the ASC and HVG, the hydrides are generated for a while after the measurement. If these hydrides are left in the absorption cell, the life of the absorption cell will be shortened. In order to purge the hydrides remaining in the cell, it is necessary to heat the absorption cell for a while after the measurement. Usually, 3 minutes is sufficient. [Automatic Lamp Extinction] Put a check mark in the check box to turn off the lamp automatically. [Show lamp used time over operating life message] Put a check mark in the check box to check whether the lamp used time is over the specified lamp life or not. [Show slit setting message] Put a check mark in the check box to display a message prompting you to set the slit before the line search. [Show turret setting message] Put a check mark in the check box to display a message prompting you to set the lamp turret before the line search or when changing a measurement element. [Use Lamp Position Setup Dialog Box] Putting a check mark in the check box allows you to select [Instrument]-[Lamp Position Setup] menu to set the lamp position. For details, refer to the section 5.8.4 [Lamp Position Setup]. [Use Rounded Abs. for calculation] The absorbance data is displayed or printed down to the fourth decimal place. The absorbance data kept in the internal memory is a little more precise. When this "Use Rounded Abs. for calculation" is checkmarked, the displayed rounded value is used for the calculations such as "Average", "%RSD value", "Standard deviation", "Calibration curve polynomial expression" and "Quantitation of unknown sample". When the check mark is deleted, the value kept in the internal memory is used for these calculations. Although the calculation is performed more precisely when the check mark is deleted, the value kept in the internal memory cannot be known instead. As the result, the WizAArd software processing is like a black box, and the calculation process cannot be verified from the outside. If the "Use Rounded Abs. for calculation" is checkmarked, the processing contents in the WizAArd software can be verified by a manual calculation with a calculator.

5

Menu Commands 5-62

AA-6200

5.8 [Instrument]

CAUTION If this setting is changed, the calibration curve and quantitation result of the measured data are also changed. Take note of this when changing the setting. When [Rounded absorbance is used for calculation] and [Decimal place] are changed, the calibration curve and quantitation results of the data measured before will be changed. Also, if the QA/QC judgment is already executed at the time of data acquisition, the file of the data cannot be read in. Note this when changing these settings. In both cases, to recover the data at the time of the measurement, read in the file after changing the rounding settings back to the original ones used at the time of measurement.

5

[Decimal place] This sets a decimal place to which the absorbance is rounded.

Menu Commands

The rounding method is as follows. When the figure below the specified place is just 5, it is rounded down if the specified figure is even and rounded up if the specified figure is odd. In other cases, it is rounded off normally. Example : When the specified decimal place is 4 Average between 0.1234 and 0.1235 is calculated as follows. (0.1234 + 0.1235) ÷ 2 = 0.12345000.... → 0.1234 Average between 0.1233 and 0.1234 is calculated as follows. (0.1233 + 0.1234) ÷ 2 = 0.12335000.... → 0.1234 [Show meas. file created by older version WizAArd message] When an old measurement file created in old version WizAArd (ver.1.x) is opened, the values such as absorbance and concentration on the MRT worksheet are not completely compatible and may have some differences in decimal fraction. To keep a complete compatibility, it is necessary to open the measurement file from the old version WizAArd in which the file was created. To check whether the measurement file was created in old version WizAArd or not, set the [Show meas. file created by older version WizAArd message] check box to ON. Then a message appears when an old measurement file is opened.

5-63 AA-6200

5.8 [Instrument]

5.8.4 [Lamp Position Setup] [General Description] The lamp used time can be used as a reference for lamp life management. The lamp used time is the product of lamp current and lamp lighting time in the default setting. For example, the used time is calculated as below when the lamp is lit at 10 mA for 10 hours. 10 (mA) × 10 (hrs) = 100 (mA*hrs) The lamp used time is saved in "lamphist.ref", which is a lamp database. The contents of this file can be displayed and edited in "Lamp History" dialog box opened by selecting [Instrument]-[Lamp History] menu. In order to manage the lamp used time properly, it is necessary to select whether to use the lamp position setup function or not depending on the hollow cathode lamp type to be used. When using a single element normal lamp supplied by Shimadzu for each element, it is recommended not to use the lamp position setup function (refer to the section 5.8.4.1). At the time of AA software installation, the default setting is not to use the lamp position setup function. In the following cases, a setting to use the lamp position setup function is recommended (refer to the section 5.8.4.2). (1) When using a multi-element lamp (2) When using a hyper lamp (3) When using a single element lamp whose specification is different from that of lamp supplied by Shimadzu. (4) When using plural lamps of the same element. If the lamp position setup has not been done in these cases, the lamp used time is automatically accumulated in the lamp data of the default lamp and, as the result, the lamp used time for each lamp cannot be managed separately when using a different lamp. Whether to use the lamp position setup function or not changes the accumulation method of the used time and the selection method of measurement lamp. To manage the lamp used time properly, it is also necessary to register and edit the lamp data in the "Lamp History" dialog box in the above cases of (3) and (4) or when changing a hollow cathode lamp for a new one (refer to the section 5.8.5).

5

Menu Commands 5-64

AA-6200

5.8 [Instrument]

[Operation] [Setting the Use or Not Use of Lamp Position Setup] (1) If an element schedule exists on the MRT worksheet, use [File]-[New] menu so that no element schedule exists on it. (2) Select [Instrument]-[Configuration]. Then "Configuration" dialog box is displayed.

5

Menu Commands

q

Figure 5.49 : "Configuration" Dialog Box (3) Select [Use Lamp Position Setup Dialog Box] check box (q) when using the lamp position setup function. If not using, clear it. Click the button and close "Configuration" dialog box to fix the setting.

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5.8 [Instrument]

5.8.4.1 When not using the lamp position setup function Default lamp data selection (1) Lamp History (lamphist.ref)

Accumulation of lamp used time

Optics Parameters

(2)

Lamp ON/OFF

Figure 5.50 : Management of Lamp Used time when the Lamp Position Setup function is not used

5

Menu Commands

(1) Selecting the measurement lamp Select the measurement element in the Element Selection dialog box. At this time, the socket # can be set in "Load Parameters" dialog box. The socket # also can be set in Optics Parameters page. When selecting an element and socket #, the default lamp data for the element is selected from the lamp data base (lamphist.ref). The lamp ID of the selected default lamp is displayed in [Lamp ID] in Optics Parameters page. (2) Accumulating the lamp used time The lamp used time is accumulated to the default lamp data selected in (1). The default lamp is a lamp with a check mark in "Default" field in "Lamp History" dialog box. Be sure to set one default lamp for each element when accumulating the lamp used time without using the lamp position setup function (a default lamp is already set at the time of installation). Specify the measurement element and socket # and light the lamp, then the used time is automatically accumulated to the lamp data of the default lamp of the element. 5.8.4.2 When using the lamp position setup function The lamp position setup function is a function to select a lamp to be used from the lamp database (lamphist.ref) set in "Lamp History" dialog box. If the intended lamp cannot be selected in "Lamp Position Setup" dialog box, it is necessary to register the lamp data in "Lamp History" dialog box (refer to the section 5.8.5).

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5.8 [Instrument]

Lamp data selection

(1)-(b)

Lamp History (lamphist.ref)

Lamp data selection

(1)-(c)

Lamp Position Setup (lampplace.ref)

Accumulation of lamp used time

(2)

Optics Parameters

Lamp ON/OFF

Figure 5.51 : Management of Lamp Used time when the Lamp Position Setup function is used

5

q

w

e

Menu Commands

(1) Selecting the measurement lamp Before selecting a measurement element, it is necessary to set the lamps to be used in "Lamp Position Setup" dialog box. (a) The lamp that is lit cannot be edited in "Lamp Position Setup" dialog box. After turning off the lamp, select [Instrument]-[Lamp Position Setup]. "Lamp Position Setup" dialog box is displayed. r

Figure 5.52 : "Lamp Position Setup" Dialog Box (b) Set the following items. q [Element] When a cell in [Element] fields is clicked, a drop-down list is displayed. From the list, select an element symbol of the lamp to be mounted to each socket. " * " is used as a wild card. When using a multi-element lamp, enter " * " instead of the element symbol. To clear the lamp already set, select "None" at the top of the drop-down list. 5-67 AA-6200

5.8 [Instrument]

w [Lamp Type] Set the correct type of hollow cathode lamp to be used. Usually, set "Normal". Both hyper lamp and multi-element lamp are also used as normal lamps (SR lamp is not used in the case of AA-6200). e [Lamp ID] When the element and lamp type have been set, the lamp ID can be selected in [Lamp ID] field from the registered lamps. Select the Lamp ID of the lamp to be used. The lamp ID of the lamp data registered at the installation of AA software is in the form of "Element symbol (,element symbol...)-1". Also, at the end of the element symbol, the letters "(HP)" and "(SR)" are attached in the cases of hyper lamp and SR lamp, respectively. Selecting the lamp ID displays [Judge], [Life Time], [Used Time] and [Unit] (shown inr) ( for items in r, refer to the section 5.8.5). After finishing the settings, click on the to fix the settings. The lamp position setup information is saved in "lampplace.ref" file.

5

Menu Commands

(c) Socket # of lamp cannot be set in "Load Parameters" dialog box. Set it in Optics Parameters page. In [Socket #] drop-down list in Optics Parameters page, the socket #s that accord with the measurement element among the lamps set in "Lamp Position Setup" dialog box are displayed. When " * " has been set instead of element symbol in "Lamp Position Setup" dialog box, the socket # can be selected for any measurement elements. Select an appropriate Socket #. In [Lamp ID] in Optics Parameters page, the lamp ID of the selected lamp is displayed. (2) Accumulation of lamp used time Specify the measurement element and socket # and light on the lamp. Then the lamp used time is accumulated to the lamp data of the selected lamp.

5.8.5 [Lamp History] Selecting this menu opens the "Lamp History" to register/delete/edit the lamp information for the lamp life management in the data base. 5.8.5.1 When is a use of "Lamp History" dialog box necessary? (1) When purchasing and replacing a hollow cathode lamp or D2 lamp, clear the accumulation of used time. (2) When using two or more lamps of the same element and of the same type in the 5-68 AA-6200

5.8 [Instrument]

same term, register the lamps to the lamp history newly. (3) When using a lamp whose specification is not in the lamp data at the time of AA software installation, register the lamp to the lamp history newly. 5.8.5.2 How to use the "Lamp History" dialog box In "Lamp History" dialog box, the lamp data of hollow cathode lamp in the following conditions cannot be registered, cleared, edited or deleted. • Lamp data selected in "Lamp Position Setup" • All lamp data when lamp position setup function is not used and a element schedule are registered on the MRT worksheet Therefore, when editing the lamp data in "Lamp History" dialog box, set the conditions so that the MRT worksheet has no element schedule and that no lamp is selected in "Lamp Position Setup" dialog box (These conditions are the same when not using the lamp position setup function).

5

Menu Commands

Selecting [Instrument]-[Lamp History] menu opens the "Lamp History" dialog box to register/delete/edit the lamp data in the database. The lamp used time is accumulated to the database set here. q

w

e r

t

y

u i o

!0

!1

!2 !3 !4

Figure 5.53 : "Lamp History" Dialog Box The first row in the table is fixed to the row for D2 lamp. The rows from the second and on can be freely used for the database of hollow cathode lamps. 5-69 AA-6200

5.8 [Instrument]

Description of Table Item No. in Figure

5

Item

Menu Commands

2

Lamp ID

3

Element

4

Lamp Type

5

Life Time

6

Used Time

7

Unit

8

Judge

9

Default

10

Comment

11

Lock

Description This indicates ID for identifying each hollow cathode lamp. Any name that doesn't duplicate can be used as ID (up to 20 characters). Enter the element of hollow cathode lamp. In the case of multi-element lamp, " * (asterisk)" is used. Select normal lamp or SR lamp. Hyper lamp is handled as a normal type. Enter the used time as a standard for lamp exchange. The time number that shows how long the lamp has been actually used is counted. Select the unit of used time. "mA*hrs" or "hrs" can be selected. (This is fixed to "hrs" in the cases of D2 lamp and SR lamp.) OK" is indicated when the "Used Time" is less than the "Life Time", and "over" is indicated when it is over. Select the default lamp data to accumulate the lamp used time for each element when the lamp position setup function is not used. Comment can be freely entered (up to 25 characters). This is used to lock or release the lamp data edit. When the used time accumulation is started, this is automatically selected.

[Registering a new lamp data] (1) Scroll the table to display the last row. (2) Enter a new lamp ID in [Lamp ID] field (w) in the blank row next to the last row. (3) Set the lamp element in [Element] field (e). "*" is used as a wildcard. When using a multi-element lamp, enter "*" instead of element name. (4) Set the type of hollow cathode lamp to be used in [Lamp Type] fields (r) correctly. (5) Next, set [Life Time] (t) and [Unit] (u) referring to the instruction manual for the lamp being used. The unit can be selected from "mA*hrs" or "hrs". In the case of normal lamp, usually select "mA*hrs". In the cases of SR lamp and D2 lamp, it is fixed to "hrs" (SR lamp is not used in AA-6200). (6) Use [Comment] (!0) field freely, for entering date for example. The registered lamp can be selected in the Lamp Position Setup dialog box. The used time (y) is accumulated as for the lamp set in the Lamp Position Setup dialog box. When the unit of used time is "mA*hrs", the used time is the product of lamp current and lamp lighting time. For example, the used time is calculated as below when the lamp is lit at 10 mA for 10 hours. 10 (mA) × 10 (hrs) = 100 (mA*hrs) 5-70 AA-6200

5.8 [Instrument]

When the unit of used time is "hrs", the lighting time is directly used, and the used time in this example becomes 10 (hrs). [Clearing the Lamp Used Time] The accumulation value of the lamp used time is cleared and the lamp information can be edited. Note that this operation resets the used time to "0.0". [Clearing only a row] (1) Clear [Lock] check box (!1).

5

Menu Commands

[Clearing plural rows collectively] (1) Click the row number (q) at the left end and select the rows to be cleared. Drag to select the successive several rows. (2) Click (!2). [Editing the Lamp Data] When the accumulation of used time has been started in the lamp data, the [Lock] check box is set to ON, and editing the items except [Default], [Comment] and [Lock] is prohibited. To edit them, use the button and once clear the accumulation. The lamp data except [Comment] field cannot be edited when the lamp is the default lamp of the element selected on the MRT worksheet or it is selected in "Lamp Position Setup". Only the fields [Life Time], [Used Time], [Comment] and [Lock] can be entered in the first row for D2 lamp. [Deleting the Lamp Data] If the lamp data is deleted carelessly, the lamp data cannot be selected in "Lamp Position Setup" dialog box or the socket # cannot be set in the Optics Parameters page. Care must be taken when deleting the lamp data. The first row for D2 lamp cannot be deleted. (1) Click the row number (q) at the left end and select the rows to be deleted. Drag to select the successive several rows. (2) Press (!3). [Printing the Lamp Data] (1) Click (!4). The lamp data table is printed out. 5-71 AA-6200

5.8 [Instrument]

5.8.5.3 Displaying a message when the lamp used time exceeds the lamp life When the lamp used time is over the lamp life, it can be detected and a message can be displayed at the start time of measurement. The lamp life already set in the "Lamp History" dialog box is a value guaranteed by the manufacturer. Although the used time is one of the signs to exchange the lamp, the lamp can be used if the line search/beam balance is performed without problem and if the noise level required for the analysis is satisfied. [Operation] (1) Select [Instrument]-[Configuration] menu. "Configuration" dialog box is displayed.

5

Menu Commands q

Figure 5.54 : "Configuration" Dialog Box (2) To display the message, select [Show lamp used time over operating life message] check box (q) and click . If you don't want to display the message, clear this check box and click . The setting is fixed and "Configuration" dialog box is closed.

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5.8 [Instrument]

5.8.6 [Maintenance] Selecting this menu allows you to use the functions for maintenance of the instrument. 5.8.6.1 [D2 Lamp Position] This is used to adjust the position of deuterium lamp when replaced. For the replacing procedures, refer to the section 6.3. [Operation] (1) Selecting this menu displays the message "D2 lamp position adjustment is going to start. Please adjust D2 lamp position roughly first.". Set the D2 lamp approximately to the center position using the adjusting screw and click on . (2) Next, the message "Set Slit Width to 0.2 nm." is displayed. Set the slit to 0.2 nm using the slit change knob and click . The D2 lamp is lit on and the beam balance is executed. When the beam balance has succeeded, "D2 lamp Adjustment" dialog box is displayed. If the error message "D2 lamp energy is too low. Please adjust D2 lamp

5

Menu Commands

position roughly." is displayed and the beam balance has failed to succeed, set the slit width to 0.7 nm once and adjust the D2 lamp position then set the slit width to 0.2 nm again and adjust the D2 lamp position.

Figure 5.55 : "D2 Lamp Adjustment" Dialog Box (4) The bar graph and [Current] indicate the current absorbance value of D2 lamp. Adjust the D2 lamp position so that the absorbance value may become minimum.

Clicking on this button resets the values of [Max] and [Min]. 5-73 AA-6200

5.8 [Instrument]

5.8.6.2 [Wavelength Adjustment] This field automatically adjusts the wavelength of the monochromator. A Mercury (Hg) hollow cathode lamp (refer to 6.6 Special Accessories List) is required to perform this operation. The adjustment takes about 20-30minites to execute. Before executing, confirm that there is nothing to cut the beam in the atomizer unit. Follow the on-screen directions to complete the operation. 5.8.6.3 [Burner Origin Position Adjustment] This menu item is not available for AA-6200. 5.8.6.4 [Furnace Origin Position Adjustment] This menu item is not available for AA-6200.

5

Menu Commands

5.8.6.5 [ASC Maintenance] 5.8.6.5.1 [Set Syringe Volume] This menu item is not available for AA-6200. 5.8.6.5.2 [Change Syringe] This menu item is not available for AA-6200. 5.8.6.6 [Maintenance only for service engineer] Only the service engineers can use this menu.

5.8.7 [Lamp Status] Selecting this menu opens "Lamp Status" dialog box and the status of the lamp currently used is displayed. This dialog box indicates how long the lamp has been lit on.

Figure 5.56 : "Lamp Status" Dialog Box 5-74 AA-6200

5.8 [Instrument]

[Lamp Status] The lighting ON/OFF of the lamp is displayed. If the checkmark is deleted, the hollow cathode lamp can be turned off but cannot be lit on. D2 lamp can be lit on or turned off. [Lighting Time] Elapsed time of the lamp lighting is displayed. Once the lamp is turned off, it resets to 0. [Wait Time] When the warmup time is set, the rest of warmup time is displayed. If the measurement is started before the wait time becomes "0", the "Hollow Cathode Lamp Warmup Waiting" dialog box is opened to indicates the wait time. Clicking on in this dialog box ignores the waiting time and starts measurement.

5

Menu Commands

Figure 5.57 : "Warmup Waiting" Dialog Box [Warmup Lamp Status] When the rest waiting time becomes "0", "Completed" is displayed to indicate that warmup of the lamp is completed. When the lamp is not lit or when the specified warmup has not been completed, "Not Completed" is displayed. [D2 Lamp Warmup Time (min)] Enter the time necessary for warming up the D2 lamp in the unit of minute. Since the D2 lamp is once turned off when the line search is executed, the wait time set here is started after the line search/beam balance at the measurement start time is finished. During the wait time, the "Hollow Cathode Lamp Warmup Waiting" (or "D2 Lamp Warmup Waiting") dialog box is displayed. 5-75 AA-6200

5.8 [Instrument]

The sequence of the lamp warmup and line search/beam balance at the measurement start time is as follows. Hollow cathode lamp and D2 lamp are lit on. ↓ Hollow cathode lamp is warmed up. ↓ Line search/beam balance is executed. ↓ D2 lamp is warmed up. ↓ Measurement is started.

5

Menu Commands

NOTE The warmup time of the hollow cathode lamp is set by selecting [Parameters]-[Edit Parameters]- "Sequence" page from the menu.

[Operation] [Operation for setting the D2 lamp warm-up time ] (1) Select [Instrument]-[Lamp Status] menu to open "Lamp Status" dialog box. (2) Set the warm-up time in the unit of minutes in [D2 Lamp Warmup Time (min)] of "Lamp Status" dialog box and click . [Operation for setting the warm-up time for hollow cathode lamp ] (1) Select [Parameters]-[Edit Parameters] menu to open "Sequence" page. (2) Set the warm-up time in the unit of minutes in [Lamp Warmup Time] of "Sequence" page. (3) Click and close the "Sequence" page.

5.8.8 [Change Graphite Tube] This menu item is not available for AA-6200.

5.8.9 [Gas Controller Status] This displays the state of the fuel gas pressure.

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5.8 [Instrument]

Figure 5.58 : "Gas Controller Status" Dialog Box

5 [Fuel Gas Pressure] Displays whether the fuel gas pressure is appropriate or not. Menu Commands

5.8.10 [Gas Leak Check] Use this function to check for gas leaks from tubes. Follow the directions displayed on screen. For details, refer to 6.2 Checking for Gas Leaks in Tubing.

5.8.11 [Remaining Gas Combustion] This menu is used to burn up acetylene gas in the piping from the gas main valve to the instrument by closing the main valve of acetylene gas during the combustion of Air-C2H2 flame. If the flame type is set to N2O-C2H2, you can't execute this procedure. Change the flame type to Air-C2H2 and retry it. CAUTION Be sure to follow the procedure below to perform the remaining gas combustion. If the procedure is compromised, a flashback may occur.

(Procedure of Remaining Gas Combustion) (1) Set the supply pressure and setting pressure of the acetylene gas and air properly (refer to 4.8). (2) Select [Parameters]-[Edit Parameters] menu to open "Gas Flow Rate Setup" page. Set "Air-C2H2" for [Flame Type] and click on to close the page. When using the high temperature burner head, pull out the burner-recognizing pin from the hole of the burner select sensor. 5-77 AA-6200

5.8 [Instrument]

CAUTION Be sure to use Air-C2H2 flame to perform the remaining gas combustion. Using N2OC2H2 flame may cause a flashback.

(3) Press the IGNITE and PURGE buttons simultaneously to ignite a flame. (4) Select [Instrument]-[Remaining Gas Combustion] menu. The message in Figure 5.59 appears. Click on .

5

Menu Commands

Figure 5.59 : Remaining Gas Combustion - Message 1 (5) Next, the message shown in Figure 5.60 is displayed. Click on and close the main valve of the acetylene gas cylinder. At this time, don't stop the support gas (air) and continue to supply it in the proper pressure. As the acetylene gas decreases, the flame goes out. Also, the AA software displays the message "Fuel gas pressure is too low". Click on to close it.

Figure 5.60 : Remaining Gas Combustion - Message 2

NOTE When stopping the remaining gas combustion, click on in the message of Figure 5.60 without closing the main valve of the acetylene gas cylinder.

(6) Next, the message shown in Figure 5.61 is displayed. Since the support gas (air) flows out after the flame goes out, press the EXTINGUISH button of the AA main unit to stop the support gas (air).

5-78 AA-6200

5.8 [Instrument]

Figure 5.61 : Remaining Gas Combustion - Message 3 (7) Click on in the message of Figure 5.61 to close the message. With the above procedure, the remaining gas combustion is finished.

5

5.8.12 [Execute Line Search]

Menu Commands

This is used to execute the line search for the element currently set. This function is the same as that of button in the "Optics Parameters" page, but both line search and beam balance are performed by force by selecting this menu item. To refer to the result of line search/beam balance, use button in "Optics Parameters".

5.8.13 [Cleaning] This menu item is not available for AA-6200.

5.8.14 [Rinse Nozzle] This menu item is not available for AA-6200.

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5.8 [Instrument]

5.8.15 [Flame Nozzle Position] This is used to adjust the sample uptake position. Adjust the position of suction nozzle following the messages displayed step by step. To quit the position adjustment halfway, press the . Note, however, that the proper adjustment cannot be performed when the nozzle position adjustment is quitted halfway. "Please set the ASC turn table for flame measurement and remove the sample suction nozzle from the arm. The ASC nozzle moves to sample intake position if you press OK button." ↓ "Please mount the sample suction nozzle and adjust the nozzle vertical position. Please press OK button after you finish the adjustment."

5

5.8.16 [Furnace Nozzle Position] Menu Commands

This menu item is not available for AA-6200.

5-80 AA-6200

5.9

[Help]

Select this menu when using the help function.

5.9.1 [Search for Help on...] By entering a key word in "Search for Help on..." dialog box, the help of a specified item can be searched.

5.9.2 [About WizAArd...] Version and system information of this software are displayed.

5

Menu Commands 5-81 AA-6200

5.10

Rounding the absorbance and setting the decimal places for correction factors and actual concentration

5.10.1 Rounding the absorbance value [General Description] The absorbance data is displayed or printed down to the fourth decimal place. But the absorbance data kept in the internal memory is a little more precise. Although the calculation is performed more precisely when the absorbance value is not rounded, the value kept in the internal memory cannot be known instead. As the result, the WizAArd software processing is like a black box, and the calculation process cannot be verified from the outside. If the absorbance data is rounded, the rounded value is used for the calculations such as "Average", "% RSD value", "Standard deviation", "Calibration curve polynomial expression" and "Quantitation of unknown sample". Thus the processing contents in the WizAArd software can be verified by a manual calculation with a calculator.

5

Menu Commands

CAUTION 1. If the setting of rounded absorbance is changed, the calibration curve and quantitation result of the measured data are also changed. Also, if the QA/QC judgment is already executed at the time of data acquisition, the file of the data cannot be read in. Note this when changing these settings. In both cases, to recover the data at the time of the measurement, read in the file after changing the rounding settings back to the original ones used at the time of measurement. 2. When an old measurement file created in old version WizAArd (ver.1.x) is opened, the values such as absorbance and concentration on the MRT worksheet are not completely compatible and may have some differences in decimal fraction. To keep a complete compatibility, it is necessary to open the measurement file from the old version WizAArd in which the file was created(Refer to the section 5.8.3). [Operation] "Setting for rounding the absorbance" (1) Select [Instrument]-[Configuration] menu. "Configuration" dialog box is displayed.

5-82 AA-6200

5.10 Rounding the absorbance and setting the decimal places for correction factors and actual concentration

5

Menu Commands

w

q

Figure 5.62 : "Configuration" Dialog Box (2) Enter the following items. q [Use Rounded Abs. for calculation] Select this check box to round the absorbance. Then [Decimal place] can be entered. When not rounding absorbance, clear this check box. w [Decimal place] Set the decimal place when rounding the absorbance. For example, when rounding the 5 decimal places to 4 decimal places, enter "4". The enter range is "0" to "4". (3) To fix the setting, click . The message "To validate the setting, close the software once then restart it" is displayed. Follow the message and restart the AA software. [Details] The rounding method of the absorbance is as follows. 5-83 AA-6200

5.10 Rounding the absorbance and setting the decimal places for correction factors and actual concentration

1) When the figures below the specified decimal place is just 5000... When the figure in the specified decimal place is even When the figure in the specified decimal place is odd

Omission Raising to a unit

2) In other cases except the above, it is rounded normally to the specified decimal place. Example : When the specified decimal place is 4 Average between 0.1234 and 0.1235 is calculated as follows. (0.1234 + 0.1235) ÷ 2 = 0.12345000.... → 0.1234 Average between 0.1233 and 0.1234 is calculated as follows. (0.1233 + 0.1234) ÷ 2 = 0.12335000.... → 0.1234

5

Menu Commands

5.10.2 Setting the decimal places for correction factors and actual concentration value [General description] The decimal place for display is set for each of the weight correction factors (Weight Factor, Volume Factor, Dilution Factor and Correction Factor) and the actual concentration. These decimal places are used for rounding the figure, displaying the data on the screen and printing the data. The rounding method is the same as rounding absorbance (refer to the section 5.10.1). [Operation] (1) Select [Parameters]-[Edit Parameters] menu to open "Weight Correction Factors" page.

5-84 AA-6200

5.10 Rounding the absorbance and setting the decimal places for correction factors and actual concentration

w

q

5

Menu Commands

Figure 5.63 : "Weight Correction Factors" Page (2) In [Decimal Place to Display] (q), set the decimal places for Weight Factor, Volume Factor, Dilution Factor, Correction Factor and Actual Concentration. (3) Click [Apply on this dialog box] (w). The correction values in this page are displayed again according to the [Decimal Place to Display]. (4) Click to close "Weight Correction factors" page. At this time, if the decimal places newly set are smaller than the previous settings, the weight correction factors and the actual concentration value on the MRT worksheet are rounded.

5-85 AA-6200

6 Maintenance 6 Contents

AA-6200

Maintenance

6.1 Burner maintenance ………………………………………………………………6-1 6.1.1 Cleaning the burner head …………………………………………………6-1 6.1.2 Nebulizer maintenance ……………………………………………………6-2 6.1.2.1 Cleaning the Nebulizer …………………………………………………6-2 6.1.2.2 Replacing the polyethylene tube ………………………………………6-4 6.1.3 Washing the chamber………………………………………………………6-4 6.2 Checking for gas leaks in tubing …………………………………………………6-6 6.2.1 Checking for gas leaks in the gas hoses and gas piping ………………6-6 6.2.2 Checking for gas leaks in the instrument…………………………………6-6 6.3 Replacing the deuterium lamp ……………………………………………………6-8 6.4 Rinsing ……………………………………………………………………………6-10 6.4.1 Rinsing the exterior ………………………………………………………6-10 6.4.2 Rinsing the quartz window plate…………………………………………6-10 6.5 List of maintenance parts…………………………………………………………6-11 6.6 Optional accessories list …………………………………………………………6-12 6.6.1 For Flame Analysis ………………………………………………………6-12 6.6.2 Hollow cathode lamps ……………………………………………………6-12 6.6.2.1 Single element lamp……………………………………………………6-12 6.6.2.2 Multi-element lamps ……………………………………………………6-14 6.6.3 Other accessories …………………………………………………………6-14

6

Maintenance

AA-6200

6.1

Burner maintenance

If foreign matter sticks to the burner head, nebulizer, and inside of the chamber, the signal becomes unstable or absorbance sensitivity decreases. Periodic cleaning of these components is recommended. The connector between the burner head and nebulizer is sealed with O-rings. If the Orings are deformed or deteriorated, immediately replace them.

NOTE 1. When analysis is complete, do not immediately extinguish the flame. Spray distilled water for about three to five minutes to purge the capillary of the nebulizer, burner head, and the inside of the chamber. 2. If it is difficult to remove or install the burner head and the nebulizer, apply a small amount of grease (available as an accessory) on the O-rings. CAUTION 1. O-rings are inserted into the connector between the burner head and nebulizer to prevent a gas leak. When reassembling the burner, ensure that the O-rings are correctly installed. 2. Deteriorated O-rings cause gas leaks. O-rings should be replaced on a yearly basis.

6

Maintenance

6.1.1 Cleaning the burner head If the slot of the burner head is slightly clogged, the reduction flame will have fine irregularities. When the slot is more heavily clogged, the flame splits as shown in Figure 6-1. If such a flame is produced, extinguish the flame, then remove the adhering matter by scraping the inner wall of the slot with thick paper or thin plastic plate. Sometimes an orange colored flame may flicker when the burner is ignited again after cleaning the slot. In this case, spray pure water until there is no flickering. If the flickering does not stop quickly, remove the burner head from the chamber and wash the inside with distilled water. The burner head can be removed by pulling upward. If it is extremely dirty, soak it in acid or appropriate detergent over night then brush the slot inner wall.

6-1 AA-6200

6.1 Burner maintenance

Clogged

Normal

Figure 6-1 : Flame Symptoms Due to Clogged Slot When measuring samples with high concentrations of coexistent components, such as salts, these will adhere to the inner wall of the slot. After measuring such samples, be sure to clean the slot thoroughly.

6

Maintenance

CAUTION 1. Don't use metal brushes that may scratch the burner head. 2. If the width of the slot become wider or the inner surface of the slot become coarse, replace the burner head with a new one. In the case of a high temperature burner, usage under such conditions may cause a flashback. The typical life time of burner head is about 3 years.

6.1.2 Nebulizer maintenance 6.1.2.1 Cleaning the Nebulizer If the indication value fluctuates or the absorbance sensitivity decreased during measurement, the capillary of the nebulizer may be clogged by some contaminant. Clean the nebulizer in the following procedure. (1) When the flame is extinguished completely, insert the cleaning wire into the capillary (q) to clean its inner wall (refer to Figure 6.3). (2) After removing the cleaning wire, spray distilled water. (3) Use a standard sample solution or the like to check the sensitivity and stability. (4) If the performance is not improved after performing the above operations (1) through (3), contaminants may stick between the capillary and the plastic jacket (w) at the tip of the nebulizer. In this case, perform the following procedure (refer to Figure 6.3). (5) When the flame is extinguished completely, loosen the fixing screws (q) for the nebulizer (r) to draw out the nebulizer retaining plate (w) in the right direction. Remove the SPRAY joint (e) inserted into the nebulizer and then remove the nebulizer from the chamber (t) (refer to Figure 6.2). 6-2 AA-6200

6.1 Burner maintenance

(6) After removing the nebulizer, dip the nebulizer tip into hydrochloric acid (1:1). At this time, hold the nebulizer so that only the jacket (w) is immersed and make sure that the metal part (e) is not immersed in the hydrochloric acid (refer to Figure 6.3). Subsequently, immerse the same part in distilled water to completely eliminate hydrochloric acid.

CAUTION 1. Do not remove the disperser unit. 2. Do not apply the ultrasonic cleaner to the nebulizer. Otherwise, the adhesion between the capillary and the main body may be damage. (7) Mount the nebulizer and then spray pure water. Use a standard sample solution or the like to check the absorption sensitivity and stability

6

Maintenance

rNebulizer

eSPRAY joint

Burner head

t Retaining plate q Fixing screw

t Chamber

r Nebulizer y Mixer

u Spray unit

Figure 6-2 : Burner Unit 6-3 AA-6200

6.1 Burner maintenance

q Capillary

u Polyethylene tube w Plastic jacket y Cap e Body (Metal part)

Figure 6-3 : Nebulizer

6

Maintenance

6.1.2.2 Replacing the polyethylene tube The Teflon sampling tube used to suction samples is held in place by a polyethylene tube wedged into the nebulizer capillary. If the polyethylene tube deteriorates or comes loose, it cannot hold the Teflon sampling tube in place. Should this happen, use the following procedure to replace the polyethylene tube. Refer to Figure 6-3. (1) Remove the cap (y) shown in Figure 6-3 by rotating it to the left. (2) If the old polyethylene tube is still in the capillary (q), remove it. (3) Cut the new polyethylene tube (u) to the length of the old tube (about 5mm) and insert the new tube into the capillary. Do not bend the capillary. (4) Replace the cap.

NOTE If it is difficult to fit the polyethylene tube in the capillary, enlarge the opening by inserting a pen or other thin object.

6.1.3 Washing the chamber Disassembling the chamber unit following the procedures below and completely wash it with distilled water or alcohol. (1) Remove the burner head and the nebulizer (refer to 6.1.1 and 6.1.2). (2) Remove the spray unit fixing screws (q) to remove the spray unit. Then you 6-4 AA-6200

6.1 Burner maintenance

can take the mixer out from the chamber inside. (3) Remove the chamber fixing screws (e) and remove the chamber. Then loosen the strap of the drain port (r) at the lower chamber floor and remove the Utube.

CAUTION 1. When assembling the chamber after cleaning it, be sure to check the direction of the mixer. Since the outer diameter of the mixer is slightly tapered, push it in the direction, which fits the taper of the chamber inside. 2. Before pouring water or alcohol from the burner fixing port, be sure to remove the nebulizer. Otherwise, the nebulizer may sink in the liquid and the adhesive may be damaged. 3. When disassembling the chamber unit, pay attention not to break the disperser.

6

Maintenance

e Chamber fixing screw

w Nebulizer fixing screw

q Spray unit fixing screw r Drain port

Figure 6-4 : Chamber

6-5 AA-6200

6.2

6.2 Checking for gas leaks in tubing

Perform monthly checks for gas leaks in the gas hoses, gas piping and inside the instrument according to the procedure below.

6.2.1 Checking for gas leaks in the gas hoses and gas piping Gas hoses are provided as accessories ; gas piping is provided by the user. (1) Confirm that all the hose connections and the gas piping of the cylinder and compressor are connected properly. Switch off the power to the AA-6200 main unit. (2) Open the main valve of the cylinder and compressor, wait about five seconds, and then close the valves. (3) Viewing the secondary side gauges, confirm that the pressure drop in 30 miniutes is less than 0.015MPa for fuel gas and less than 0.03MPa for oxidant gas. If the drop in pressure exceeds these values, gas is leaking. (4) If gas is leaking, apply soapy water or other leak detector to the connections to the cylinder, compressor and gas piping (provided by user) and to the gas hoses (provided as accessories) to determine the location of the leak. (5) If a gas leak occurred in a connection, try refitting the connection. (6) If a gas leak occurred in a gas hose, immediately replace it with a new gas hose.

6

Maintenance

6.2.2 Checking for gas leaks in the instrument If there is no gas leaks in the gas hose and gas piping, perform the following steps to check for a gas leak inside the instrument. (1) Switch the instrument on and start the AA-6200 software. Press to exit the “Wizard Selection” dialog box. Then select [connect] from the [Instrument] menu to establish communications to the AA-6200 main unit. (2) On the PC screen, select [Instrument] - [Gas Leak Check]. Follow the message in the dialog box, and then select . (3) Disconnect the spray tube and the fuel tube connected to the spray unit. Connect these two tubes to each other with the seal joint. And select (refer to figure 6.5). (4) Open the main valve of the compressor to supply air at a rate of 0.35MPa. Keep the gas flow adjusting knob at its normal position. If the knob is rotated fully to the right, rotate it 3 rotations to the left. (5) Close the main valve of the compressor, or rotate the secondary pressure adjusting handle of the compressor to the left enough to close it. Select . (6) Watching the secondary side gauge, confirm that the pressure drop in 30 minutes is less than 0.03MPa. If the drop in pressure exceeds these values by 6-6 AA-6200

6.2 Checking for gas leaks in tubing

0.03MPa, gas is leaking inside the instrument. Select to proceed to the next screen. (7) Reconnect the spray tube and fuel tube as they were before. Finally select to close the dialog box. If a gas leak is detected inside the instrument, immediately stop operations and contact your service representative.

CAUTION Replace the standard accessory gas hose every year to prevent a gas leak.

Fuel gas

Oxidant gas

Gas hoses Gas piping

6

Maintenance

Inside the instrument

Fuel tube

Spray tube Seal joint

Figure 6-5 : Checking for Gas Leaks

6-7 AA-6200

6.3

Replacing the deuterium lamp

WARNING The deuterium lamp and the lamp housing are very hot when the lamp is lit. Never touch the lamp when it is lit or shortly after turning it off. Before replacing the lamp, ensure that the power is off and the lamp has cooled sufficiently.

CAUTION Take care not to directly handle or touch the window of the deuterium lamp. Use a clean tissue or wear a clean glove when handling the lamp. If the window is smudged with fingerprints etc., light transmission is reduced, causing noise in the measurement. Immediately remove the dirt with alcohol.

(1) Check that the power supply of the instrument is off and confirm that the lamp housing unit is sufficiently cooled. (2) Remove the two screws of the lamp housing cover to open the cover, as shown in Figure 6-6. (3) After checking that the lamp is completely cooled, slowly pull out the lamp. (4) Insert a new deuterium lamp firmly into the socket. (5) Loosen the two screws that fix the deuterium lamp base by a half turn. If you loosen them too much, completely re-tighten the screws, then loosen them again. (6) Verify that the lamp base can slide smoothly to the right and left—use a screwdriver to rotate the position adjusting screw on the right side of the main unit. It the lamp base does not move smoothly, loosen the base fixing screws an additional quarter turn each. (7) Center the deuterium lamp so all the light passes through the aperture. (8) When installation is complete, close the lamp cover, and fix it with the two screws. (9) Switch the instrument on and start the AA-6200 software. Press Cancel to exit the "Wizard Selection" dialog box. Then select [Connect] from [Instrument] menu to establish communications to the AA-6200 main unit. (10) Select [Instrument] - [Maintenance] - [D2 Lamp Position]. Monitoring the optical value of the deutrium lamp, use the position adjusting screw to adjust the lamp until the optical value equals the lowest value. The deuterium lamp position adjusting screw is located on the right side of the main unit.

6

Maintenance 6-8

AA-6200

6.3 Peplacing the deuterium lamp

Lamp base

Two screws

Position adjusting screw

6 Aperture plate

Maintenance

Figure 6-6 : Replacing the Deuterium Lamp

6-9 AA-6200

6.4

Rinsing

6.4.1 Rinsing the exterior If the cover or the burner compartment is dirty, wipe it off with a soft cloth or tissue paper. If it still is not completely clean, wet the cloth and use detergent.

6.4.2 Rinsing the quartz window plate Wipe the quartz window plates on both sides of the burner compartment with a dry soft cloth or cotton swab. If the plates are still dirty, use a cloth soaked with ethanol.

6

Maintenance 6-10 AA-6200

6.5

List of maintenance parts Part number 206-50226-92 206-50362-92 206-50363-91 206-50370-91 036-15551-16 036-11222 036-11203 036-11217 036-11215 036-11237 201-79229-01 206-50438-91 016-02101-04 016-02101-03 016-02101-01 037-61019 016-43201-02 200-31328-01 206-51389 035-65268-02 062-65055-05 016-43200-08 206-50486

Note Disperser Polypropylene Standard burner head Used in burner socket Used in burner socket Used in nebulizer Used in nebulizer and safety bung Used in drain joint Used in jacket mounted on chamber For cleaning the capillary in nebulizer Teflon tube for sample uptake For support gas (Air) For fuel gas (C2H2) For support gas (N2O) Hose band Drain tube For sealing the capillary in nebulizer For securing the nebulizer Connecting nebulizer to spray tube D2 lamp U-tube

6

Maintenance

Part name Nebulizer ASSY Jacket ASSY Chamber ASSY 10cm Burner head ASSY O-ring AS568-116 4D O-ring 4D P22 O-ring 4D P5 O-ring 4D P16 O-ring 4D P12 O-ring 4D P35 Cleaning Wire Sampling tube Hose, 8 × 2B-BK Hose, 8 × 2B-R Hose, 8 × 2B-G Wire band, for 16mm PE tube, 8 × 1 Polyethylene Capillary No.3 Retaining plate Elbow, 31020600 Lamp, L6380 Tube, super corn-ace 9 × 13 Mixer

6-11 AA-6200

6.6

Optional accessories list

6.6.1 For Flame Analysis Part Name High Temperature Burner Head Air Compressor (50Hz) Air Compressor (60Hz) Low Noise Air Compressor Drain Separator DS-02 Precision gas pressure regulator YR-71 Precision gas pressure regulator MAF-85S

Part No. 206-50300-91 200-33897-01 200-33897-02 200-64051 200-64020 040-72020-01 040-72019-11

Remark for N2O-C2H2 flame For AC100V For AC100V For AC100V, 50/60Hz For acetylene gas For nitrous oxide gas

6.6.2 Hollow cathode lamps 6.6.2.1 Single element lamp

6

Maintenance

Element Symbol Ag Al As Au B Ba Be Bi Ca Cd Co Cr Cs Cu Dy Er Eu Fe Ga Gd Ge Hf Hg Ho In Ir 6-12 AA-6200

Element Name Silver Aluminum Arsenic Gold Boron Barium Beryllium Bismuth Calcium Cadmium Cobalt Chromium Cesium Copper Dysprosium Erbium Europium Iron Gallium Gadolinium Germanium Hafnium Mercury Holmium Indium Iridium

Part No. 200-38422-02 200-38422-01 200-38422-42 200-38422-25 200-38422-39 200-38422-03 200-38422-04 200-38422-43 200-38422-05 200-38422-06 200-38422-09 200-38422-07 200-38422-27 200-38422-08 200-38422-60 200-38422-61 200-38422-62 200-38422-10 200-38422-40 200-38422-63 200-38422-11 200-38422-64 200-38422-28 200-38422-65 200-38422-48 200-38422-66

Product Name L233-47NQ L233-13NB L233-33NQ L233-79NQ L233-5NQ L233-56NB L233-4NQ L233-83NQ L233-20NU L233-48NQ L233-27NU L233-24NB L233-55NB L233-29NB L233-66NB L233-68NB L233-63NB L233-26NB L233-31NU L233-64NB L233-32NU L233-72NU L233-80NU L233-67NB L233-49NB L233-77NQ

6.6 Optional accessories list

Potassium Lanthanum Lithium Lutetium Magnesium Manganese Molybdenum Sodium Niobium Neodymium Nickel Osmium Lead Palladium Praseodymium Platinum Rubidium Rhenium Rhodium Ruthenium Antimon Scandium Selenium Silicon Samarium Tin Strontium Tantalum Terbium Tellurium Titanium Thallium Thulium Vanadium Tungsten Yttrium Ytterbium Zinc Zirconium

200-38422-22 200-38422-29 200-38422-30 200-38422-67 200-38422-12 200-38422-13 200-38422-31 200-38422-14 200-38422-32 200-38422-68 200-38422-15 200-38422-69 200-38422-21 200-38422-41 200-38422-70 200-38422-20 200-38422-33 200-38422-44 200-38422-49 200-38422-45 200-38422-24 200-38422-71 200-38422-46 200-38422-16 200-38422-72 200-38422-18 200-38422-34 200-38422-35 200-38422-73 200-38422-47 200-38422-17 200-38422-74 200-38422-75 200-38422-19 200-38422-36 200-38422-76 200-38422-77 200-38422-23 200-38422-37

L233-19NB L233-57NB L233-3NB L233-71NB L233-12NU L233-25NU L233-42NB L233-11NB L233-41NB L233-60NB L233-28NQ L233-76NU L233-82NQ L233-46NQ L233-59NB L233-78NU L233-37NB L233-75NB L233-45NB L233-44NB L233-51NB L233-21NB L233-34NB L233-14NU L233-62NB L233-50NQ L233-38NB L233-73NU L233-65NB L233-52NQ L233-22NB L233-81NU L233-69NB L233-23NB L233-74NU L233-39NB L233-70NB L233-30NQ L233-40NB

6

Maintenance

K La Li Lu Mg Mn Mo Na Nb Nd Ni Os Pb Pd Pr Pt Rb Re Rh Ru Sb Sc Se Si Sm Sn Sr Ta Tb Te Ti Tl Tm V W Y Yb Zn Zr

6-13 AA-6200

6.6 Optional accessories list

6.6.2.2 Multi-element lamps Elements Ca,Mg Fe,Ni Na,K Si,Al Si,Ba

Part No. 200-38422-51 200-38422-53 200-38422-50 200-38422-52 200-38422-54

Product Name L733-202NU L733-204NQ L733-201NB L733-203NU L733-205NU

6.6.3 Other accessories Autosampler (ASC-6100F) Hydride Vaporizer generator (HVG-1) Mercury Vaporizer Unit (MVU-1A) Gas Flow Cell Cell Holder

6

Maintenance 6-14 AA-6200

206-50100-30 For AC100/120V 206-50100-39 For AC230/240V 206-17143 204-21932-01 201-98687 For MVU-1A 202-35867 For MVU-1A

7 Troubleshooting

Contents

AA-6200

7

Troubleshooting

7.1 Troubleshooting 7.1.1 Power supply indicator lamp does not light when the power switch of the spectrophotometer is switche on………………7-1 7.1.2 Communications between the PC and the AA-6200 do not initialize properly ……………………………………7-1 7.1.3 Wavelength origin error occurs at initialization …………………………7-1 7.1.4 Cannot recognize the autosampler at initialization ……………………7-1 7.1.5 Photometric value is abnormal ……………………………………………7-1 7.1.6 Noisy beseline (S/N is poor) ………………………………………………7-2 7.1.7 Error occurs in line search/beam balance ………………………………7-2 7.1.8 Flame does not ignite ………………………………………………………7-3 7.1.9 Air-C2H2 does not change over to N2O-C2H2 ……………………………7-3 7.1.10 Flame is not stable …………………………………………………………7-3 7.2 Error Messages ……………………………………………………………………7-4

7

Troubleshooting

AA-6200

7.1

Troubleshooting

To maintain a high level of performance in your atomic absorption spectrophotometer, replace consumable parts as needed, perform routine maintenance and inspection, and always treat the instrument with care. If you are experiencing any difficulties operating the instrument, follow the troubleshooting tips below. If the cause of malfunction is still not clear, contact your Shimadzu service representative.

7.1.1 Power supply indicator lamp does not light when the power switch of the spectrophotometer is switched on (1) Ensure that the power cable is firmly plugged in. (2) If the fan in the back is rotating, power is being supplied to the instrument. The power indicator light may be broken. Contact your Shimadzu service representative to schedule a repair.

7.1.2 Communications between the PC and the AA-6200 do not initialize properly

7

Troubleshooting

(1) Make sure the AA-6200 main unit power is on. (2) Check that the communication cable between the AA main unit and the PC is installed properly. See 2.2.10 Cable Connections for more details. (3) Ensure that the communication port is set correctly. See 5.8.3 Configuration.

7.1.3 Wavelength origin error occurs at initialization Remove any obstacles blocking the optical path in the atomizer unit.

7.1.4 Cannot recognize the autosampler at initialization (1) Make sure the autosamler power is on. (2) Check that the communication cable between the AA main unit and the autosampler is installed properly. See 2.2.10 Cable Connections for more details.

7.1.5 Photometric value is abnormal (1) Verify that the hollow cathode lamp of the target element is located in the correct turret position. (2) Check the analysis wavelength. Select [Parameters] - [Edit Parameters], then choose the "Optics Parameters" tab. On the "Optics Parameters" page, select to examine the analysis wavelength. You can change the analysis wavelength using in "Wavelength Memory Setup" dialog box. See the section 5.5.6.3 for more information. 7-1 AA-6200

7.1 Troubleshooting

(3) If was accidentally pressed during analysis, stop aspirating samples and press . Then start measurement again. (4) Check the sample preparation. (5) If the nebulizer is clogged, clean the capillary with the supplied cleaning wire. (6) If the polyethylene tube covering the capillary of the nebulizer is broken, replace it. Refer to the section 6.1.2.2.

7.1.6 Noisy beseline (S/N is poor) (1) Check to see if the hollow cathode lamp is broken or not properly inserted. Place a piece of white paper on the optical path of the atomizer unit. If the spot of light that shines on the paper is orange, the hollow cathode lamp is lit. If the light is purple, only the D2 lamp is lit. If no orange light is visible, make sure the hollow cathode lamp is properly seated in the lamp socket. If it still does not light, the lamp is broken. Replace it with a new lamp. (2) If the light is dim, check the total lighting hours by selecting [Instrument] [Lamp History]. If the hollow cathode lamp has exceeded the manufacturer's recommended lighting hours, replace the bulb. (3) Check the optical axis of the lamp by placing a piece of white paper on the optical path of the atomizer unit. The light should be focused directly above the burner slot. If it does not, adjust the optical axis of the lamp, as described in the section 4.2.1.8. (4) Ensure that the slit width is set correctly. Firmly switch the setting on the left side of the instrument to either 0.2nm or 0.7nm, depending on the element being measured. (5) Execute a line search. See the section 5.5.6.2. (6) Remove any dirt the surface of the quartz window plate of the atomizer unit with a dry soft cloth or cotton swab. If the plates are still dirty, use a cloth soaked with ethanol.

7

Troubleshooting

7.1.7 Error occurs in line search/beam balance (1) Remove any obstacles blocking the optical path of the atomizer unit. (2) Make sure the hollow cathode lamp element is the same as the element set in the "Meas. Element" field on the "Element Selection" dialog box. This dialog box is accessed from the [Parameters] - [Element Selection Wizard] menu item. (3) Check that the proper slit width is selected (using the selector on the left side of the instrument). (4) BGC-D2 (background correction with the deuterium lamp) mode may have 7-2 AA-6200

7.1 Troubleshooting

been performed in a wavelength range that should not use D2 lamp energy. If so, select non-BGC mode. See the section 5.5.6 for more information on lamp modes. (5) If the Wavelength Memory setting was performed with the wrong wavelength, clear the Memory Wavelength setup. See the section 5.5.6.3 for more information. (6) Ensure that the proper lamp current value is set on the "Optics Parameters" page. This page is accessed from the [Parameters] - [Edit Parameters] menu item.

7.1.8 Flame does not ignite (1) Ensure that communications are established between the PC and the AA-6200 by starting the AA-6200 software and choosing [Connect] from the [Instrument] menu. (2) Perform Element Selection Wizard or open a measurement file on AA software so that the AA main unit is ready for the ignition. (3) When the following error messages are displayed on the AA software, the AA main unit is locked so that the ignition cannot be done. To release this lock, solve the problems in the instrument settings then close all the error messages displayed on the software. While the error message is displayed, the ignition cannot be done. - Fuel gas pressure is too low. - Support gas pressure is too low. - Flame has been extinguished. (4) Ensure that the acetylene supply pressure is set to 0.09MPa and air to 0.35MPa. (5) Is the main gas valve open? (6) Check the gas flow rate.

7

Troubleshooting

7.1.9 Air-C2H2 does not change over to N2O-C2H2 (1) Ensure N2O gas is being supplied. If it is not, open the main valve of the gas cylinder and supply N2O gas with correct gas pressure. (2) Is N2O-C2H2 selected as the Flame type on the "Gas Flow Rate Setup" page? This page is accessed from the [Parameters] - [Edit Parameters] menu item. (3) Ensure that the burner-recognizing pin is properly inserted.

7.1.10 Flame is not stable (1) Remove the burner head and clean the inside of the slot. (2) Use a new gas cylinder if the fuel gas cylinder is nearly empty. 7-3 AA-6200

7.2

Error Messages

NOTE Before contacting your Shimadzu service representative, record the following items. • Content of error message • Status in which the error message is displayed (indication screen, performed operation, measurement file, "wizaa.ini" file in windows folder, etc.) • Instrument information displayed at the upper in the initialization screen (model names of AA/ASC, ROM version and serial No.) • AA software version No. ([Help]-[About WizAArd] menu)

Error Message Number

Cause/Details

x,x,x,...This lamp ID is already in use. Please select another ID.

Remedial Measure • Select [None] for the Element field to clear the overlapped lamp in "Lamp Position Setup" dialog box. • When using plural lamps of the same element and type simultaneously, register each of the lamps in [Instrument][Lamp History].

A ACK has not been accepted from ASC.

7

Communication protocol with ASC was not completed. (:A)

AD Converter returned invalid data.

Troubleshooting

Analytical Line is not found.

Switch on the AA main unit again. If the error occurs again, contact your Shimadzu service representative. Line Search has failed. The following causes are considerable. (1) The lamp is not properly mounted to the lamp turret. (2) The wavelength shift has occurred in the monochromator.

ASC arm motor slipped.

ASC arm rotation position cannot be initialized.

ASC arm vertical position cannot be initialized.

7-4 AA-6200

(1) Verify that the lamp is correctly mounted to the socket and the lamp turret position. (2) Perform the wavelength correction in [Instrument][Maintenance]-[Wavelength Adjustment].

• Verify that the ASC arm movement is not impeded. • Switch on the ASC again and connect the ASC in [Instrument]-[Option Connect] menu. (1) The origin detector didn't detect the origin correctly. (2) The arm rotation drive motor doesn't operate.

(1), (2) Switch on the ASC main unit again. If the error occurs again, record the status in which this error message appears and contact your Shimadzu service representative.

(1) The origin detector didn't detect the origin correctly. (2) The vertical arm drive motor doesn't operate.

(1), (2) Switch on the ASC main unit again. If the error occurs again, record the status in which this error message appears and contact your Shimadzu service representative. Remove the cause of error and switch on the ASC power again. Then connect the ASC in [Instrument]-[Option Connect] menu and try this operation again.

ASC Error occurred during action. Press Cancel to close this dialog box. Resolve the ASC problem then retry. ASC I/F port is used for another device.

Verify the ASC power supply and the cable connection between ASC and AA main unit, then connect the ASC in [Instrument]-[Option Connect] menu.

Communication with ASC is unstable.

Verify the ASC power supply and the cable connection between ASC and AA main unit, then connect the ASC in [Instrument]-[Option Connect] menu.

7.2 Error Messages

Error Message

Cause/Details

Remedial Measure

ASC is disconnected, or ASC is set not to be used in sequence parameter settings.

• Switch on the ASC and use [Instrument]-[Option Connect] The ASC is not connected or menu to connect the ASC. the setup for using ASC is not • To make a setting to use the ASC, select [Using ASC] check made, although [ASC Sample box in the Sequence page. Pos. for EMISSION Line Search] for Emission mode is selected in the Optics Parameters page to execute the Line Search/Beam Balance in Emission mode.

ASC table cannot be initialized.

(1) The origin detector didn't detect the origin correctly. (2) The turntable drive motor doesn't operate.

ASC table motor slipped.

ASC Timedout.

(1), (2) Switch on the ASC main unit again. If the error occurs again, record the status in which this error message appears and contact your Shimadzu service representative. • Verify that rotation of the ASC table is not impeded. • Switch on the ASC again and connect the ASC in [Instrument]-[Option Connect] menu.

The ASC doesn't response on the way of the communication. The communication cable with ASC has a problem.

Verify the ASC power supply and the cable connection between ASC and AA main unit, then connect the ASC in [Instrument]-[Option Connect] menu.

B (1) • Increase the hollow cathode lamp current (Low) (pay attention to the max. current). • When the lamp mode is BGC-D2, narrow the slit width. (2) • Set [Wavelength] correctly in Optics Parameters page. • If the wavelength shift has occurred in the monochromator, perform the wavelength correction in [Instrument][Maintenance]-[Wavelength Adjustment]. (3) Change the hollow cathode lamp.

7

Troubleshooting

Background signal is too Beam Balance failed because the light intensity of BG large to execute Beam measurement is too greater Balance. than the light intensity of hollow cathode lamp. The following causes are considerable. (1) The light intensity of the hollow cathode lamp becomes too smaller than the light intensity of BG measurement as the result of change in the Optics Parameters, etc. (2) The Line Search failed to catch the correct analytical line. (3) The light intensity becomes smaller because of the exhaustion of hollow cathode lamp.

7-5 AA-6200

7.2 Error Messages

Error Message

Cause/Details

Background signal is too Beam Balance failed because small to execute Beam the light intensity of hollow Balance. cathode lamp is too greater than the light intensity of BG measurement. The following causes are considerable. (1) The light intensity of hollow cathode lamp becomes too greater than the light intensity of BG measurement as the result of change in the Optics Parameters, etc. (2) The Line Search failed to catch the correct analytical line. (3) The light intensity becomes greater because of the exhaustion of hollow cathode lamp. [When the lamp mode is BGC-D2] (4) The light intensity of BG measurement becomes smaller because of the exhaustion of D2 lamp. (5) The optical axis of D2 lamp is shifted.

7

Remedial Measure (1) • Decrease the hollow cathode lamp current (Low). • When the lamp mode is BGC-D2, widen the slit width (pay attention to the neighboring line). (2) • Set [Wavelength] correctly in Optics Parameters page. • Narrow the slit width so as not to catch the neighboring line. • If the wavelength shift has occurred in the monochromator, perform the wavelength correction in [Instrument][Maintenance]-[Wavelength Adjustment]. • If the neighboring line is selected in line search because of its higher peak than the analysis line peak, set Wavelength Memory in order that correct analysis line may be selected. (3) Change the hollow cathode lamp. (4) Change the D2 lamp. (5) Adjust the D2 lamp position in [Instrument]-[Maintenance][D2 Lamp Position].

Troubleshooting

Before the new memory wavelength is set, clear the current memory wavelength and execute Line Search.

Only one memory wavelength can be set for one actual wavelength.

Click in "Wavelength Memory Setup" dialog box to set [Memory Wavelength] to "NONE" then set a new memory wavelength.

BG signal is too large.

Beam Balance failed because the light intensity of BG measurement is too greater than the light intensity of hollow cathode lamp. The following causes are considerable. (1) The light intensity of the hollow cathode lamp becomes too smaller than the light intensity of BG measurement as the result of change in the Optics Parameters, etc. (2) The Line Search failed to catch the correct analytical line. (3) The light intensity becomes smaller because of the exhaustion of hollow cathode lamp.

(1) • Increase the hollow cathode lamp current (Low) (pay attention to the max. current). • When the lamp mode is BGC-D2, narrow the slit width. (2) • Set [Wavelength] correctly in Optics Parameters page. • If the wavelength shift has occurred in the monochromator, perform the wavelength correction in [Instrument][Maintenance]-[Wavelength Adjustment]. (3) Change the hollow cathode lamp.

7-6 AA-6200

7.2 Error Messages

Error Message BG signal is too small.

Cause/Details

Remedial Measure

Beam Balance failed because the light intensity of hollow cathode lamp is too greater than the light intensity of BG measurement. The following causes are considerable. (1) The light intensity of hollow cathode lamp becomes too greater than the light intensity of BG measurement as the result of change in the Optics Parameters, etc. (2) The Line Search failed to catch the correct analytical line. (3) The light intensity becomes greater because of the exhaustion of hollow cathode lamp. [When the lamp mode is BGC-D2] (4) The light intensity of BG measurement becomes smaller because of the exhaustion of D2 lamp. (5) The optical axis of D2 lamp is shifted.

(1) • Decrease the hollow cathode lamp current (Low). • When the lamp mode is BGC-D2, widen the slit width (pay attention to the neighboring line). (2) • Set [Wavelength] correctly in Optics Parameters page. • Narrow the slit width so as not to catch the neighboring line. • If the wavelength shift has occurred in the monochromator, perform the wavelength correction in [Instrument][Maintenance]-[Wavelength Adjustment]. • If the neighboring line is selected in line search because of its higher peak than the analysis line peak, set Wavelength Memory in order that correct analysis line may be selected. (3) Change the hollow cathode lamp. (4) Change the D2 lamp. (5) Adjust the D2 lamp position in [Instrument]-[Maintenance][D2 Lamp Position].

7

Execute the blank measurement after the repeat measurements are finished.

Buffer Overflow.

Amount of the acquired data is larger than the communication buffer of AA software.

Switch on the PC power and the instrument power again. If the error occurs again, check the following items. • Set all of the PC BIOS setup and the electric power saving function of control panel to OFF. • Don't start up other application software simultaneously.

Burner select sensor is out of order! Please call a service engineer.

(1) When the AA-6200 was initialized, the burnerrecognizing pin was inserted in burner select sensor located at the lower left of the burner chamber. (2) At the time of initialization, the defective of burner select sensor was detected.

(1) Remove the burner-recognizing pin from the burner select sensor then start the initialization. (2) Stop using the N2O and contact your Shimadzu service representative.

Calibration Curve cannot be created.

The calibration curve order doesn't match with the number of standard samples.

When the Zero Intercept is not selected, set the calibration curve order below the number of standard samples. When the Zero Intercept is selected, set the calibration curve order below the number of standard samples or the same.

Calibration Curve does not exist!

Standard samples (STD or MSA) have not been measured.

Set up STD, in the case of calibration curve method, and MSA, in the case of standard addition method or simple standard addition method, on the MRT work sheet and measure them.

Troubleshooting

Blank cannot be inserted Inserting a blank measurement here. row between the repeat measurement rows was tried.

C

7-7 AA-6200

7.2 Error Messages

7

Error Message

Cause/Details

Remedial Measure

Calibration Curve is not valid !

The calibration curve order doesn't match with the number of standard samples.

When the Zero Intercept is not selected, set the calibration curve order below the number of standard samples. When the Zero Intercept is selected, set the calibration curve order below the number of standard samples or the same.

Can't find drive X:

The setup disk of AA software is broken (at the time of installation).

Try to recover the setup disk using the scan disk of Windows.

Communication Timeout. The communication between AA software and AA main unit has a problem.

Switch on the PC power and the instrument power again. If the error occurs again, check the following items. • Set all of the PC BIOS setup and the electric power saving function of control panel to OFF. • Fix all the communication cables (AA-PC, AA-ASC) with screws to avoid an insufficient contact and ground level mismatch of communication port.

Communication was aborted from the spectrophotometer side.

The communication between AA software and AA main unit has a problem.

Switch on the PC power and the instrument power again. If the error occurs again, check the following items. • Set all of the PC BIOS setup and the electric power saving function of control panel to OFF. • Fix all the communication cables (AA-PC, AA-ASC) with screws to avoid an insufficient contact and ground level mismatch of communication port.

Current measurement schedule cannot be selected.

The lamp of current measurement element cannot be selected as warm-up lamp.

Select [Lamp ON] check box in the Optics Parameters page to light on the lamp of current measurement element.

D Troubleshooting

D2 lamp energy is too low (1) The light intensity becomes smaller as the result of D2 lamp exhaustion. (2) The optical axis of D2 lamp is shifted.

(1) Change the D2 lamp. (2) Adjust the D2 lamp position in [Instrument]-[Maintenance][D2 Lamp Position].

D2 lamp energy is too low Beam balance failed. The following causes are considerable. (1) The light intensity becomes smaller as the result of D2 lamp exhaustion. (2) The optical axis of D2 lamp is shifted.

(1) Change the D2 lamp. (2) Adjust the D2 lamp position in [Instrument]-[Maintenance][D2 Lamp Position].

(1) Light path is obstructed. D2 lamp zeroth order (2) D2 lamp energy is light was not found. Please make sure that no insufficient. object in light path.

(1) Check that the light path is not obstructed. (2) • Check that the D2 lamp is lit on. • Exchange the D2 lamp if it has been used for a long time.

Default lamp of X is NOT set in Lamp History dialog box. Please set one lamp as default lamp for each element. Otherwise the used time don't be counted up.

7-8 AA-6200

When the Lamp Position Setup is not used, the default lamp whose used time is automatically accumulated is necessary.

In [Instrument]-[Lamp History] menu, select [Default] of the normal lamp of the listed element. If the lamp of the element has not been registered, register it newly.

7.2 Error Messages

Error Message

Cause/Details

Remedial Measure

Default lamp is not set for the following elements. -x,x,x,...Please set default lamp correctly. Otherwise lamp used time can't be count up correctly. Are you going to back to Lamp History dialog box?

When the Lamp Position Setup is not used in AA-6200, the default lamp whose used time is automatically accumulated is necessary.

Press in the message to return to the "Lamp History" dialog box. Select [Default] field of the normal lamp of the listed element. If the lamp of the listed element has not been registered, register it newly.

Although the ASC is to be used to execute Line Search/Beam Balance in Emission mode in the setting, [ASC Sample Pos. for EMISSION Line Search] in Optics Parameters page is set to "NONE".

Set the position of sample to be sprayed at the time of Line Search/Beam Balance in [ASC Sample Pos. for EMISSION Line Search]. Entry for [ASC Sample Pos. for EMISSION Line Search] is available when the [Lamp Mode] is set to "EMISSION" and [Lamp Current (Low)] to "0".

E Emission vial position has not been set in the following measurement.

Expired Lamp is The lamp selected in "Lamp selected. Reestablish the Position Setup" dialog box has setting ? a relation "(Life Time) < (Used Time)".

• Although the "Used Time" is one of the signs to change the lamp, a lamp used for longer than the life time can be used if Line Search/Beam Balance is performed successfully and if the noise level required for the analysis is satisfied. • Select [Instrument]-[Configuration] menu and clear the check box of [Show lamp used time over operating life message] not to display this message.

7

F When the number of Element Schedules on the MRT work sheet exceeds 20, the excess schedules cannot be read out on the MRT.

Delete unnecessary Element Schedules in "Element Selection" page. Also, clear the check box of unnecessary element in [Element Selection] list when reading out parameters in the Template page of "Load Parameters" dialog box.

Failed to detect wavelength motor origin.

(1) The origin detector couldn't detect the origin correctly. (2) The wavelength drive motor doesn't operate properly.

(1), (2) Switch on the AA main unit again. If the error occurs again, record the status in which this error message appears and contact your Shimadzu service representative.

Failed to extinguish the flame.

EXTINGUISH button of the instrument was not pressed while executing the remaining gas combustion.

Press the EXTINGUISH button following the instruction displayed while executing the residual gas combustion.

Troubleshooting

Failed to Add New Schedule.

Delete the "cookbook.ref" file and install it again. Failed to load Cookbook The "cookbook.ref" file in the folder in which the AA software is installed cannot be read in. The version of "cookbook.ref" doesn't match the execution file, or the file is broken. Failed to load document. Measurement file or template file cannot be read out in Wizard Selection dialog box.

Check that the file tried to load actually exists.

Failed to open the serial port.

Check the following points. • [COM port] in [Instrument]-[Configuration] is properly set. • Other application software (communication software, FAX software, etc.) is not used. • The resource of the communication port doesn't compete with other device.

The PC serial port cannot be used.

7-9 AA-6200

7.2 Error Messages

Error Message

Cause/Details

Remedial Measure

Failed to send parameters to the instrument. Wait until the instrument becomes READY then retry it.

Close this message and wait until "READY" is displayed at the right lower of the status bar. Then perform the target operation again.

Flame monitor couldn't be set Failed to set Flame Monitor Safety Device to OFF while executing the residual gas combustion. OFF.

Stop using the instrument, switch on the power again and connect it with the PC again. If the item "Flame Monitor ON" becomes NG, contact your Shimadzu service representative.

Failed to turn OFF the gas pressure monitor.

The gas pressure monitor couldn't be set OFF while executing the residual gas combustion.

Stop using the instrument. Then switch on the power again and reconnect it with the PC. If NG is displayed for the item "Gas Pressure Monitor ON" on the initialization screen, contact your Shimadzu service representative.

Failed to turn ON the gas pressure monitor.

The gas pressure monitor couldn't be set ON when the residual gas combustion was finished or cancelled.

Stop using the instrument. Then switch on the power again and reconnect it with the PC. If NG is displayed for the item "Gas Pressure Monitor ON" on the initialization screen, contact your Shimadzu service representative.

Flame has been extinguished.

The flame monitor detected that the flame is extinguished although the EXTINGUISH button is not pressed.

• Verify that nothing obstructs the flame monitor. • Remove the cause that make flame go out.

Flame Monitor Safety Device was not set.

Flame monitor couldn't be set ON while executing the residual gas combustion.

Stop using the instrument, switch on the power again and connect it with the PC again. If the item "Flame Monitor ON" becomes NG, contact your Shimadzu service representative.

Fuel gas pressure is too low.

(1) The supply pressure of fuel gas (C2H2 or H2) or support gas (Air or N2O) has decreased. (2) The PURGE button on the gas controller panel of AA main unit was pressed.

(1) Open the stopcock and check the supply pressure of fuel/support gas by the meter of pressure regulator. If the required pressure is not satisfied, change the fuel/support gas cylinder, check/adjust the air compressor operation or perform other appropriate treatment. (2) This doesn't mean an abnormal status. Close the message and continue the operation.

Sufficient light intensity of hollow cathode lamp could not be obtained during the wavelength adjustment. The following causes are considerable. (1) The optical axis has a problem. (2) The light intensity of the hollow cathode lamp becomes too small as the result of change in the Optics Parameters, etc. (3) The Line Search failed to catch the correct analytical line. (4) The light intensity becomes smaller because of the exhaustion of hollow cathode lamp.

(1) • Verify that the atomizer or any other thing doesn't obstruct the optical axis. • Verify that the lamp is correctly mounted to the socket and the lamp turret position. • Rotate the hollow cathode lamp and adjust the optical axis. (2) • Increase the hollow cathode lamp current (Low) (pay attention to the max. current). • Widen the slit width (pay attention to neighboring lines). (3) Set [Wavelength] correctly in Optics Parameters page. (4) Change the hollow cathode lamp.

7

Troubleshooting

G H HC Lamp Energy is insufficient.

7-10 AA-6200

7.2 Error Messages

Error Message HC lamp energy is too low.

Cause/Details

(1) • Verify that the socket to which the lamp is mounted and the lamp turret position are correctly set. • Rotate the hollow cathode lamp to adjust the optical axis (2) Verify that there is no obstacle on the light path. (3) Increase the lamp current or widen the slit width in the Optics Parameters page. (4) • Set [Wavelength] correctly in Optics Parameters page. • If the wavelength shift has occurred in the monochromator, perform the wavelength correction in [Instrument][Maintenance]-[Wavelength Adjustment]. (5) Change the hollow cathode lamp. (6) • Use a proper flame type. • Use a standard sample of higher concentration.

7

Troubleshooting

The light intensity of the hollow cathode lamp (or emission intensity in the case of flame emission analysis) is small and the Line Search/Beam Balance failed. The following causes are considerable. [In the case of atomic absorption analysis] (1) The hollow cathode lamp is not set in the lamp turret correctly. (2) The optical path is obstructed. (3) The light intensity of the hollow cathode lamp becomes too smaller as the result of change in the Optics Parameters, etc. (4) The Line Search failed to catch the correct analytical line. (5) The light intensity becomes smaller because of the exhaustion of hollow cathode lamp. [In the case of flame emission analysis] (6) The emission intensity of the standard sample of the highest concentration is too small.

Remedial Measure

I Instrument is not ready!

(1) Set the communication with the instrument to ON from (1) A command was tried to [Instrument]-[Connect] menu. send when the communication between the (2) Close this message box and wait until the command currently executed in the instrument is finished. Perform instrument and PC is OFF. the target operation again after "READY" is displayed at the (2) While the instrument is right lower of the status bar. executing the command, the next command was tried to send.

Instrument is still busy.

Close this message and wait until "READY" is displayed at the The operation that cannot be executed during BUSY status of right lower of the status bar. Then perform the target operation again. instrument was tried.

Invalid ASC Command.

A command that is not supported by the ASC was sent from the AA software.

Verify that the AA software supports the your ASC.

Invalid ASC Parameter.

Parameters that are not supported by the ASC were sent from the AA software.

Verify that the AA software supports the your ASC.

J,K

7-11 AA-6200

7.2 Error Messages

Error Message

Cause/Details

Remedial Measure

L Lamp energy is too low to execute Beam Balance.

Beam Balance failed because the light intensity of hollow cathode lamp is too small. The following causes are considerable. (1) The light intensity of the hollow cathode lamp becomes too small as the result of change in the Optics Parameters, etc. (2) The Line Search failed to catch the correct analytical line. (3) The light intensity becomes smaller because of the exhaustion of hollow cathode lamp.

To edit the lamp history data, display the Lamp History dialog box when no schedule exits on the MRT work sheet.

Lamp history data can't be edited when an element schedule is on MRT work sheet.

7

(1) • Increase the hollow cathode lamp current (Low) (pay attention to the max. current). • Widen the slit width (pay attention to neighboring lines). (2) • Set [Wavelength] correctly in Optics Parameters page. • If the wavelength shift has occurred in the monochromator, perform the wavelength correction in [Instrument][Maintenance]-[Wavelength Adjustment]. (3) Change the hollow cathode lamp.

Troubleshooting

Lamp History data file (lamphist.ref) cannot be found.

(1) Check whether the name "lamphist.ref" was changed or not (1) "lamphist.ref" file doesn't and whether it has been moved to other folder or not. If so, exist in the folder in which set it back to original condition. If "lamphist.ref" file doesn't the AA software is installed. exist in the install folder, the AA software creates a new file. (2) Execution file (wizaa.exe) (2) Be sure to execute "wizaa.exe" from the install folder. was copied in the folder other than the installation folder and was executed.

Lamp ID is not valid. Register the proper lamp in Lamp History dialog box, then set the lamp turret position.

In "Lamp Position Setup" dialog Select [Instrument]-[Lamp History] menu and register the lamp to be used. box, select a lamp to be used from the lamps registered in "Lamp History" dialog box. Therefore, register the lamp in "Lamp History" dialog box when using a lamp that is not registered.

Lamp Socket # is not [Socket #] in the Optics Execute the blank measurement after the repeat selected in this schedule. Parameters page of the element measurements are finished. for warm-up is set "NONE". Lamp Socket # is wrong. [Socket #] of the element for This schedule cannot be warm-up in the Optics selected for warmup Parameters page is set "NONE". lamp.

Lamp socket# is not specified! Please set socket# for the following elements.

7-12 AA-6200

Set up the Socket # in the Optics Parameters page. When the Socket # you wish to set is not displayed in the list, set up the lamp mounted to the Socket # in . (If the Lamp ID of the lamp you wish to set is not displayed in the "Lamp Position Setup" dialog box, register the lamp in [Instrument]-[Lamp History].) In the Optics Parameters page of the element named in the message, set the socket number. If the aimed socket number is not displayed on the list, set the lamp mounted to the aimed socket number in . (Furthermore, if the lamp of aimed element and type is not displayed on the list in "Lamp Position Setup" dialog box, register the lamp in [Instrument]-[Lamp History].)

7.2 Error Messages

Error Message Lamp Used Time exceeded the Life Time

Cause/Details In "Lamp History" dialog box, the lamp to be used has a relation "(Life Time) < (Used Time).

Remedial Measure • Although the "Used Time" is one of the sign to change the lamp, a lamp used for longer than the life time can be used if Line Search/Beam Balance is performed successfully and if the noise level required for the analysis is satisfied. • Select [Instrument]-[Configuration] menu and clear the checkbox of [Show lamp used time over operating life message] not to display this message.

M Memory Lock Failure

More than two default lamps are set for the following elements. Only one default lamp must be set for each element..x,x,x,...-

The memory reserved for Switch on the PC power and the instrument power again. If the communication by AA software error occurs again, check the following items. couldn't be locked. • Set all of the PC BIOS setup and the electric power saving function of control panel to OFF. • Don't start up other application software simultaneously. In "Lamp History" dialog box, clear [Default] field so that default lamps of listed elements are not overlapped.

N [Socket #] in the Optics Set up the Socket # in the Optics Parameters page. When the Parameters page is set "NONE". Socket # you wish to set is not displayed in the list, set up the lamp mounted to the Socket # in . (If the Lamp ID of the lamp you wish to set is not displayed in the "Lamp Position Setup" dialog box, register the lamp in [Instrument]-[Lamp History].)

7

Troubleshooting

No lamps which can be used for this measurement are set. Set a lamp which is suitable for measurement element and lamp mode.

O Other program is using lamphist.ref file. Lamp data will not be saved.

(1) "lamphist.ref" can be renewed from the AA software firstly "lamphist.ref" file is a data file started up but cannot be renewed from the AA software for lamp history. The following secondly started up. Therefore, use the AA software firstly causes are considerable when started up to perform measurement. There is no problem to this message is displayed. use the AA software secondly started up to edit parameters. (1) The second AA software has (2) Turn the read-only attribute of "lamphist.ref" file in AA been started up. software folder OFF. (2) The file attribute of "lamphist.ref" is read-only.

Other program is using lampplace.ref file. Lamp data will not be saved.

"lampplace.ref" file is a data file (1) "lampplace.ref" can be renewed from the AA software firstly started up but cannot be renewed from the AA for lamp position setup. The software secondly started up. Therefore, use the AA following causes are software firstly started up to perform measurement. There considerable when this is no problem to use the AA software secondly started up message is displayed. to edit parameters. (1) The second AA software has (2) Turn the read-only attribute of "lampplace.ref" file in AA been started up. software folder OFF. (2) The file attribute of "lampplace.ref" is read-only.

P Periodic Blank Preparation Parameters is Invalid.

If an invalid value that is not usually entered has been entered in the Blank Samples table of the "Edit Preparation Parameters" dialog box, enter a correct value.

7-13 AA-6200

7.2 Error Messages

Error Message

Cause/Details

Remedial Measure

Please connect ASC.

(1) Although the auto-sampler is necessary for the operation, the ASC is not connected. (2) Although the ASC is used in the measurement conditions, the ASC is not connected.

(1) Verify the ASC power supply and the cable connection between ASC and AA main unit, then connect the ASC in [Instrument]-[Option Connect] menu. (2) When the ASC is necessary for the measurement, connect the ASC in the procedure as above. When the ASC is not necessary, clear the [Using ASC] check box in the [Parameters]-[Edit Parameters]-[Sequence].

Please connect the ASC serial interface.

The ASC power is set OFF or the communication cable between ASC and AA main unit is disconnected.

Verify the ASC power supply and the cable connection between ASC and AA main unit, then connect the ASC in [Instrument]-[Option Connect] menu. Fix the communication cable between ASC and AA with the screws. When using N2O as oxidant gas, the high temperature burner head (optional attachment) is necessary. Mount the high temperature burner head and insert the pin, which is attached to the burner head with wire, to the burner select sensor at the lower left of burner chamber.

Please mount high temperature burner head and insert burnerrecognizing pin in burner select sensor. Please select the Flame Type.

Flame type is not selected properly in Gas Flow Rate Setup page.

Select a correct flame type in Gas Flow Rate Setup page.

Please specify the lamp socket#.

Line Search/Beam Balance couldn't be executed because [Socket #] in the Optics Parameters page is set "NONE".

Set up the Socket # in Optics Parameters page of the current measurement element. When the Socket # you wish to set is not displayed in the list, set up the lamp mounted to the Socket # in . (If the Lamp ID of the lamp you wish to set is not displayed in the "Lamp Position Setup" dialog box, register the lamp in [Instrument]-[Lamp History].)

7

Troubleshooting

Q,R S Sample Preparation Parameters is Invalid.

If an invalid value that is not usually entered has been entered, enter a correct value in the Unknown Samples table in the "Edit Preparation Parameters" dialog box.

Schedule does not exist!

In the measurement using the ASC, Element schedule has not been selected, or the measurement procedure has not been set up although the element schedule exists.

Select the measurement element and set up the measurement procedure in [Action] fields on the MRT work sheet.

Serial Port Error.

The PC serial port has a problem.

Switch on the PC power and the instrument power again. If the error occurs again, check the following items. • Set all of the PC BIOS setup and the electric power saving function of control panel to OFF. • Fix all the communication cables (AA-PC, AA-ASC) with screws to avoid an insufficient contact and ground level mismatch of communication port. • To avoid overrun of PC serial port, lower the receive buffer of FIFO on the control panel.

7-14 AA-6200

7.2 Error Messages

Error Message Set the flame measurement as a current measurement.

Cause/Details

Remedial Measure

The tried operation cannot be executed unless the flame measurement mode is set in the instrument.

After changing the measurement mode of the instrument to flame, execute the target operation. Perform the following operation to change the measurement mode of the instrument to flame. [When the flame measurement exists on the MRT] Select the flame measurement from the measurement element tool bar. [When the flame measurement doesn't exist on the MRT] Select [Parameters]-[Element Selection Wizard] and add a flame measurement by in the "Element Selection" page. Then select the measurement from the [Meas. Element] drop-down list as current measurement element and click on .

Spectrophotometer has not been turned ON or cable is disconnected.

Switch on the PC power and the instrument power again. If the error occurs again, check the following items. • Verify that the communication cables between AA main unit and PC are connected properly and fixed with screws. • Set all of the PC BIOS setup and the electric power saving function of control panel to OFF.

Standard Preparation Parameters is Invalid.

If an invalid value that is not usually entered has been entered in the STD Samples table of the "Edit Preparation Parameters" dialog box, enter a correct value. The supply pressure of support Open the stopcock and check the supply pressure of support gas (Air or N2O) has decreased. gas by the meter of the pressure regulator. If the required pressure is not satisfied, change the support gas cylinder, check/adjust the air compressor operation or perform other appropriate treatment.

Switch the Flame Type to AIR-C2H2 before the remaining gas combustion.

When the support gas is N2O, executing the residual gas combustion may cause a flashback.

Set [Flame Type] to [AIR-C2H2] in Gas Flow Rate Setup page. Then execute the residual gas combustion.

Termination has not been accepted from ASC.

Communication protocol with ASC was not completed. (:T)

Verify the ASC power supply and the cable connection between ASC and AA main unit, then connect the ASC in [Instrument]-[Option Connect] menu.

The following lamps exist in the Lamp Position Setup Dialog Box, but do not exist in the Lamp History Dialog Box. Please update the Lamp History Dialog Box or delete lamps from the Lamp Position Setup Dialog Box. Socket #x,x,x,…

The data mismatching between the lamp history and the lamp position setup was detected at the time of starting up the AA software.

Click on and delete the data from the lamp position setup. Register the necessary lamps in [Instrument]-[Lamp History]. Next, make a setting of the lamp mounted to each socket in [Instrument]-[Lamp Position Setup].

7

Troubleshooting

Support gas pressure is too low.

T

The selected area cannot be cleared as the information is stored in the Lamp Position Setup Dialog Box.

In [Instrument]-[Lamp Position Setup] menu, select [NONE] for [Element] field of the lamp ID you wish to clear, and click on . Then clear the target lamp in "Lamp History" dialog box.

The selected area cannot be deleted as the information is stored in the Lamp Position Setup Dialog Box.

In [Instrument]-[Lamp Position Setup] menu, select [NONE] for [Element] field of the lamp ID you wish to delete, and click on . Then delete the target lamp in "Lamp History" dialog box.

7-15 AA-6200

7.2 Error Messages

Error Message

7

Cause/Details

Remedial Measure

The selected area contains the D2 lamp. D2 lamp row cannot be deleted.

Deleting the first row for D2 lamp in "Lamp History" table was tried.

The first row for D2 lamp is fixed and cannot be deleted.

This file cannot be loaded because instrument type is different.***Flame Type X isn't suitable for this instrument.

Measurement file (*.aa) measured in different model (AA main unit) may not be read out because of parameter mismatch.

Use the software that corresponds with the same (or compatible) model to read out the file. When reading out only the parameters, use the template file (*.taa). The parameters are read out after converted to match with the model.

This file cannot be loaded because instrument type is different.***Lamp Mode X isn't suitable for this instrument.

Measurement file (*.aa) measured in different model (AA main unit) may not be read out because of parameter mismatch.

Use the software that corresponds with the same (or compatible) model to read out the file. When reading out only the parameters, use the template file (*.taa). The parameters are read out after converted to match with the model.

This file cannot be loaded because instrument type is different.***Slit Width X isn't suitable for this instrument.

Measurement file (*.aa) measured in different model (AA main unit) may not be read out because of parameter mismatch.

Use the software that corresponds with the same (or compatible) model to read out the file. When reading out only the parameters, use the template file (*.taa). The parameters are read out after converted to match with the model.

This file is not to be loaded. Software doesn't support this file.

The extension of file is wrong.

Load a file that has the extension indicated in [Files of type] in "Open" dialog box.

Troubleshooting

This operation cannot be The operation tried cannot be executed during action executed when the instrument or measurement. is BUSY status or while the measurement is executed.

Close this message and wait until "READY" is displayed at the right lower of the status bar. Then perform the target operation again.

This operation cannot be executed while the hollow cathode lamp is lit ON. Please retry it after you turn off the lamp.

Turn off the lamp in Optics Parameters page of the current measurement element. Use [Lamp ON] check box in the case of measurement lamp and button in the case of warm-up lamp. Then, execute the aimed operation.

Timer cannot be created. The number of timers currently Start up the PC again. Also, don't start other applications. used exceeds the limit of the After closing other applications, try it again. Windows system. When executing [File][Additional Load], the excess schedules cannot be read out on the MRT work sheet if the number of Element Schedules on the MRT work sheet exceeds 20.

When the Element schedule you wish to add is located in the latter part of the original file of adding, start up another AA software and load the original file for adding and move the order of target Element schedule. Or take out only the element schedule and save it as different file name to create an original file for adding.

Unexpected file format.

The extension of file is wrong.

Load a file that has the extension indicated in [Files of type] in "Open" dialog box.

Unknown Status Code: /(Error Code)

An error that is not defined in the AA software inside has occurred.

Switch on the PC power and the instrument power again. If the error occurs again, record the number indicated in the error message and the status in which the errors occurred. Then contact your Shimadzu service representative.

Usage time has exceed lamp life time.

When registering the lamp in "Lamp History" dialog box, the input values has a relation "(Life Time) < (Used Time)".

It is possible to input the values as "(Life Time) < (Used Time)". If the values are not wrong, continue the input.

Too many schedules. Failed to add all schedules.

U

7-16 AA-6200

7.2 Error Messages

Error Message V W

Cause/Details

Remedial Measure

Wavelength adjustment (first half) has failed. Please check D2 lamp and Hg lamp and retry it.

Wavelength adjustment (first (1) Go back to the preceding step and adjust the Hg lamp half) is a step that must position again. succeed. The followings are (2) Stop the wavelength adjustment sequence and adjust the D2 considerable as the causes of lamp position in [Instrument]-[Maintenance]-[D2 Lamp wavelength adjustment failure. Position]. (1) Optical axis of Hg lamp is (3) Replace the D2 lamp or Hg lamp. out of position. (2) Optical axis of D2 lamp is out of position. (3) Because the D2 lamp or Hg lamp has been deteriorated, the light intensity becomes weak.

Wavelength adjustment (latter half) has failed.

When the wavelength adjustment (first half) has succeeded, Even if the wavelength there is no problem. Click button to end the adjustment (latter half) has wavelength adjustment. failed, there is no problem because it is the adjustment for reference.

Wizard cannot be executed during measurement or when the instrument is BUSY.

Close this message and wait until "READY" is displayed at the right lower of the status bar. Then perform the target operation again.

7

X,Y,Z Troubleshooting 7-17 AA-6200

8 Appendix

Contents 8.1 Measurement conditions for Flame Atomic Absorption analysis ………………8-1 8.2 Analysis line wavelengths for Flame Emission analysis ………………………8-4

8

Appendix

AA-6200

8

Appendix AA-6200

8.1

Element

Wavelength Current Slit (nm) (mA) (nm) 328.1 7 0.7 309.3 10 0.7 193.7 12 0.7 242.8 12 0.7 249.7 16 0.2 553.5 16 0.2 234.9 16 0.7 223.1 10 0.7 422.7 10 0.7 228.8 8 0.7 240.7 12 0.2 357.9 10 0.7 852.1 16 0.7 324.8 6 0.7 421.2 14 0.2 400.8 14 0.7 459.4 14 0.7 248.3 12 0.2 287.4 4 0.2 368.4 12 0.2 265.2 18 0.2 307.3 24 0.2 253.7 4 0.7 410.4 14 0.2 208.8 20 0.2 766.5 10 0.7 550.1 18 0.7 670.8 8 0.7 360.0 14 0.7 285.2 8 0.7 279.5 10 0.2 313.3 10 0.7 589.0 12 0.2

Flow Burner 1% Abs. (l/min) Type (ppm) 2.2 Standard 0.04 Air-C2H2 7.0 High Temp 1.0 N2O-C2H2 2.0

Air-C2H2 1.8 Standard 0.2 Air-C2H2 7.7 High Temp 15 N2O-C2H2 6.7 High Temp 1.3 N2O-C2H2 7.0 High Temp 0.05 N2O-C2H2 2.2 Standard 0.25 Air-C2H2 Air-C2H2 2.0 Standard 0.07 1.8 Standard 0.012 Air-C2H2 1.6 Standard 0.06 Air-C2H2 2.8 Standard 0.12 Air-C2H2 1.8 Standard 0.03 Air-C2H2 1.8 Standard 0.04 Air-C2H2 7.0 High Temp 1.7 N2O-C2H2 7.0 High Temp 1.6 N2O-C2H2 7.0 High Temp 1.3 N2O-C2H2 2.2 Standard 0.08 Air-C2H2 1.8 Standard 1.3 Air-C2H2 7.0 High Temp 30 N2O-C2H2 7.8 High Temp 2.0 N2O-C2H2 7.0 High Temp 20.0 N2O-C2H2 By the cold vapor mercury technique 7.0 High Temp 1.2 N2O-C2H2 2.2 Standard 1.5 Air-C2H2 2.0 Standard 0.012 Air-C2H2 7.5 High Temp 70 N2O-C2H2 Air-C2H2 1.8 Standard 0.03 7.0 High Temp 15 N2O-C2H2 1.8 Standard 0.0035 Air-C2H2 2.0 Standard 0.028 Air-C2H2 7.0 High Temp 0.5 N2O-C2H2 1.8 Standard 0.006 Air-C2H2

Gas Type

8

Appendix

Ag Al As (H) Au B Ba Be Bi Ca Cd Co Cr Cs Cu Dy Er Eu Fe Ga Gd Ge Hf Hg Ho Ir K La Li Lu Mg Mn Mo Na

Measurement conditions for Flame Atomic Absorption analysis

8-1 AA-6200

8.1 Measurement conditions for Flame Atomic Absorption analysis

Element Nb Ni Os Pb (1) Pb (2) Pd Pr Pt Rb Re Ru Sb Sc Se (H) Si Sm Sn (1) Sn (2) Sr Ta Tb Te Ti Tl V W Y Yb Zn Zr Bi (H) Sb (H) Sn (H) Te (H)

8

Appendix 8-2

AA-6200

Wavelength Current Slit (nm) (mA) (nm) 334.9 24 0.2 232.0 12 0.2 290.9 14 0.2 217.0 12 0.7 283.3 10 0.7 247.6 10 0.7 495.1 14 0.7 265.9 14 0.7 780.0 14 0.2 346.0 20 0.2 349.9 20 0.2 217.6 13 0.7 391.2 10 0.2 196.0 23 0.7 251.6 15 0.7 429.7 14 0.2 224.6 14 0.7 286.3 10 0.7 460.7 8 0.7 271.5 18 0.2 432.6 10 0.2 241.3 14 0.2 364.3 12 0.7 276.8 6 0.7 318.4 10 0.7 255.1 24 0.2 410.2 14 0.2 398.8 10 0.7 213.9 8 0.7 360.1 18 0.2 223.1 10 0.7 217.6 13 0.7 286.3 10 0.7 214.3 14 0.2

Gas Type N2O-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 N2O-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 Air-C2H2 N2O-C2H2 N2O-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 N2O-C2H2 N2O-C2H2 N2O-C2H2 N2O-C2H2 Air-C2H2 N2O-C2H2 Air-C2H2 Air-C2H2 Air-C2H2 Air-C2H2

Flow (l/min) 7.0 1.6 7.0 2.0 2.0 1.8 7.0 1.8 1.8 7.0 1.8 2.0 7.0 2.0 7.7 7.0 3.0 3.0 1.8 7.0 7.0 1.8 7.8 1.8 7.5 7.7 7.5 7.5 2.0 7.5 2.0 2.0 2.0 2.0

Burner 1% Abs. Type (ppm) High Temp 30 Standard 0.08 1.8 High Temp Standard 0.12 Standard 0.28 Standard 0.09 High Temp 30 Standard 1.3 Standard 0.06 High Temp 15 Standard 0.6 Standard 0.33 High Temp 0.6

High Temp 1.8 High Temp 18 Standard 2.0 Standard 5.0 Standard 0.06 High Temp 18 High Temp 15 Standard 0.3 High Temp 3.0 Standard 0.3 High Temp 1.5 High Temp 10.0 High Temp 3.6 High Temp 0.13 Standard 0.011 High Temp 18



8.1 Measurement conditions for Flame Atomic Absorption analysis

NOTE 1. The above table shows the default measurement parameters ; however, the optimum parameters may be different, depending on the properties of the particular sample. 2. "HVG-1" indicates the Hydride Vapor Generator, offered as an optional accessory. 3. "High Temp" indictes the high temperature burner head, offered as an optional accessory. 4. In some cases an error message may be generated during the Line Search/Beam Balance indicating that the Hollow Cathode Lamp (HCL) current is too high or too low. If an error message indicates that the hollow cathode lamp current is too high, lower the Lamp Current value on the "Optics Parameters" page. (accessed from the [Parameters] - [Edit Parameters] menu item). If the current is too lower, raise the current value. 5. "1%Abs" means "1% absorption concentration" that indicates the sensitivity. This value, which differs for each element, shows the concentration of standard solution that shows the absorbance approx. 0.0044. This "1%" means the transmittance 1%, which is converted to approx. 0.0044 in absorbance. The smaller the 1% absorption concentration is, the higher the sensitivity.

8

Appendix 8-3 AA-6200

8.2

Element Ag Al As Au B Ba Be Bi Ca Cd Ce Co Cr Cs Cu Dy Er Eu Fe Ga Gd Ge

8

Analysis line wavelengths for Flame Emission analysis

Wavelength (nm) 328.1 396.2 193.7 267.6 518.0† 455.4 234.9 306.8 422.7 326.1 494.0† 345.4 425.4 455.5 324.8 404.6 400.8 459.4 372.0 417.2 622.0 265.1

Appendix

† : Band Spectrum

8-4 AA-6200

Element Hf Hg In Ho Ir K La Li Lu Mg Mn Mo Na Nb Nd Ni Os Pb Pd Pr Pt Rb

Wavelength (nm) 531.2 253.7 451.1 410.4 550.0 766.5 442.0 670.8 451.9 285.2 403.3 390.3 589.0 405.9 492.5 352.5 442.1 405.8 363.5 495.1 265.9 794.8

Element Re Rh Ru Sc Si Sm Sn Sr Ta Tb Te Ti Th Tl U V W Y Yb Zn Zr

Wavelength (nm) 346.1 343.5 372.8 402.4 251.6 476.0 317.5 460.7 474.0 534.0† 486.6 334.9 492.0 377.6 544.8 437.9 430.2 597.2 398.8 636.2 360.1