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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
(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.
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.
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
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.
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
• Metals(Tungsten)
• Quartz glass
• Ceramic
• Plastic
AA-6200
Handling Waste Liquid
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.
AA-6200
Installation and operation
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
AA-6200
Warning labels indicated on the unit
WARNING!
HAZARDOUS VOLTAGE
WARNING!
HOT SURFACE
AA-6200
Warning labels indicated on the unit
WARNING!
EXPLOSION POTENTIAL
WARNING!
FLAMMABLE GAS
BE SURE TO READ the part "Igniting and Extinguish the flame" in the instruction
manual before ignition.
Warning label
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.
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
⑥ Retaining plate
⑤ O-ring
⑧ Nebulizer
② Chamber fixing screw
⑩ Mixer ⑪ O-ring
⑯ U-tube
(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.
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.
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
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
AA-6200
Table of Contents
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
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
AA-6200
AA-6200
Introduction
1
1.1 Overview of AA-6200
The Shimadzu Atomic Absorption Spectrophotometer AA-6200 is used for Flame Atomic 1
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.
For the terms and practice used in WindowsTM, refer to the WindowsTM instruction
manuals.
1-1
AA-6200
1.2 Hardware Specifications
1-2
AA-6200
1.3 Software Specifiaions
Introduction
addition, wait, pause
Determines measurement type by designating the
above actions
Data processing Linear regression analysis by least square method,
Abs = f (Conc.)
Calibration curve Dimension : first order, second order, third order,
ON/OFF of zero intercept
Select calibration curve by Curve ID
Repetitive analysis Maximum 20 analyses per sample
Accuracy enhancement Usage of average value, cancellation of abnormal
data by limitation of RSD or SD values.
Sensitivity enhancement Automatic calculation by sensitivity correction
Actual concentration calculation Automatic calculation of actual concentration by
sample volume, constant volume, and dilution
factor upon data acquisition
1-3
AA-6200
1.3 Software Specifiaions
1-4
AA-6200
1.4 Notes for when upgrading from the AA-6200 16 bit software
The main limitations and changes when upgrading to the WizAArd from the AA-6200 1
16bit software are as follows.
• Measurement and conditions files of AA-6200 16 bit software cannot be opened with
Introduction
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
[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
AA-6200
AA-6200
Installation
2
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.
Installation
Standard accessories
13 15
14
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
2
(1) The installation site should be :
(a) Away from devices that generate strong magnetic and electrical fields or high
frequencies
Installation
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).
(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
Installation
Front view
(Unit: mm)
Figure 2-2 : Instrument Placement
2-3
AA-6200
2.2 Instrument placement and site 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.
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 2
pressure does not fluctuate.
Installation
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.
2-5
AA-6200
2.2 Instrument placement and site requirements
2
Installation
2-6
AA-6200
2.2 Instrument placement and site requirements
Installation
a damper in the duct system will help create the optimum air flow.
(Unit: mm)
Figure 2-4 : Typical Ventilation System
2-7
AA-6200
2.2 Instrument placement and site requirements
for confirming the operation status of the air compressor shown in Figure 2-5.
(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
Installation
Figure 2-5 : Air Compressor Accessory
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
Installation
Use almost wide open.
Stop cock
Connecting nut
2-11
AA-6200
2.2 Instrument placement and site requirements
2.2.7.1 PC Specifications
Table 2-5 PC Specifications
Specifications
CPU Pentium 75 or faster
(Pentium 200 or faster CPU recommended)
RAM 32MB or larger
(64MB or larger recommended)
1 floppy disk drive (3.5inch size) (for installing the program)
Recording device Hard disk drive (with at least 10MB free disk space for AA
software)
Screen resolution SVGA (800 × 600 or higher)
(1024 × 768 or higher resolution recommended)
I/O port 1 serial port for AA
Monitor
Keyboard
Peripherals
Mouse or other pointing device
Printer
2-12
AA-6200
2.2 Instrument placement and site requirements
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
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
2
not filled with water, combustion gas flows out from the chamber and cause
flashback
(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.
q Burner head
e O-rings t Nebulizer retaining plate
i Capillary tube
u Sampling tube
!0 O-ring
o Chamber
(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
(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
Installation
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.
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.
CAUTION
Installation
In the case of 2-wire socket, be sure to ground the earth terminal of AC cable.
Connector
Signal Type Funcion
Pin #
Case FG Frame ground
2 TxD Output data line
3 RxD Input data line
4 SG Signal ground
Table 2-6 : Connections
2-16
AA-6200
2.2 Instrument placement and site requirements
WARNING 2
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.
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
2) Insert the AA software setup disk #1 in the floppy disk drive of the PC.
3) Select [Run...] from <START> in the task bar.
4) Input "A:¥setup" to the [Open] in the [Run] dialog box and click on <OK> (A:
Installation
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 <Next> to go ahead.
6) AA-6200 is already selected as main unit type. Click on <Next> to go ahead.
7) Check the installation destination folder. You may change the folder here, if
desired. Click on <Next> to go ahead.
9) Select the program folder. Click on <Next> 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 <OK>.
11) Finally, when the message shows that the setup is completed, click on <Finish>.
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.
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
3 Instrument configuration
Instrument configuration
Contents
AA-6200
AA-6200
Instrument configuration
3
3.1 AA-6200 configuration
Front
Instrument configuration
Right side Left side
12
Rear
3-1
AA-6200
3.1 AA-6200 configuration
3-2
AA-6200
3.1 AA-6200 configuration
Instrument configuration
When changing the lamp, hold the lamp turret rotation knob, and rotate the turret
until the latch catches.
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.
3-3
AA-6200
3.1 AA-6200 configuration
CAUTION
Since the deuterium lamp radiates ultraviolet light, which is harmful to the eyes,
keep the lamp cover closed while the lamp is on.
3-4
AA-6200
3.1 AA-6200 configuration
Instrument configuration
q Burner head
y Drain tank
t U-tube
11 Chamber
mixed with the combustion gas in this chamber.
Mixing of the particles and combustion gas is
12 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
13 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
14 Drain discharge port
discharged from this port.
15 Chamber fixing screw Burner height is changed by loosening this screw.
When optional hydride vapor generator or mercury
16 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
!0 Retaining plate 3
!3 Safety bung !2 Mixer o Disperser
!0 Fixing screw
i Nebulizer
Instrument configuration
!1 Chamber !4 Drain discharge port
3-7
AA-6200
3.1 AA-6200 configuration
P.M.T
Monochromator
3 Chopper
mirror Deuterium lamp
Instrument configuration
Reference beam
Sample beam
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
Deuterium lamp
3
SAMPLE Analog signal processor
Monochrometer
Instrument configuration
Hollow cathode lamp Detector
Burner
CPU
PC
Gas control unit
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
AA-6200
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 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
Basic Operation
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
Basic Operation
AA-6200
AA-6200
Basic Operation
4
4.1 Switching On the Power and Starting the Software
Basic Operation
set the power switch located at the front lower right of main unit to the " O " position.
q Power switch
4-1
AA-6200
4.1 Switching On the Power and Starting the Software
4
Basic Operation
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.
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 <Edit Parameters> button in the
"Element Selection" page.
4-3
AA-6200
4.2 Software Basic Operation
4
Basic Operation
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 <OK>. Then
the "Element Selection" page will appear.
4-4
AA-6200
4.2 Software Basic Operation
(1) First, click on the <Select Elements>. Then the "Load Parameters" will appear.
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 <Periodic Table> 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 <OK>. 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 <Select Elements> button again to select the next
element. Repeat the procedure below as required.
Click on <Select Elements> button → Select an element → Click on <OK>
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 <Delete>. 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 <Edit Parameters> button, refer to the section 5.5.1 in Chapter 5.
Here, you can go ahead without using it.
(10) Click on <Next> button. Although another message appears, go ahead by
clicking on <Cancel> button. Then "Preparation Parameters" page will appear.
NOTE
4 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 <Up> or <Down> to move the row. If the
[Meas. element] at the right lower of the page is different from the first row
Basic Operation
element, the measurement is started from the [Meas. Element] and the elements
upper than it are not to be measured.
First, select the row of the element to be set by clicking on its row to highlight it,
then click on <Edit> button. The "Preparation Parameters" page will appear. Set
the parameters as below.
4-6
AA-6200
4.2 Software Basic Operation
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.
4 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
Basic Operation
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.
(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 4
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
Basic Operation
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.
(9) After setting the parameters, click on <OK> 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 <Edit> and set the parameters in the same way.
(10) When completing all the settings, click on <Next>. 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
(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
<Collective Setup>. Then the "Sample ID Collective Setup" dialog box will
appear.
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 <OK> 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 4
using the ASC, this is not required.
(5) After completing the settings, click on <Next>. Then the "Sample Selection"
page will appear.
Basic Operation
4.2.1.6 Sample Selection
In this Sample Selection page, the samples to be measured for each element are
selected.
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 <Next> to proceed to the "Connect
to Instrument/Send Parameters" page.
4
4.2.1.7 Connect to Instrument/Send Parameters
Basic Operation
Check that the power of the AA is already ON and click on <Connect/Send Parameters>.
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 <OK> to close the message. After completing the initialization, click
on <OK> 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
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 <OK>.
After completing the inspection, click on <OK> to close the dialog box. Then, click
on <Next> in the "Connect to Instrument/Send Parameters" page to proceed to the
"Optics Parameters for Lamp Position Adjustment" page.
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
Basic Operation
(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
<Close> button to return to the previous dialog box ("Optics Parameters for
4-15
AA-6200
4.2 Software Basic Operation
NOTE
Basic Operation
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 <Edit Parameters> button in the
"Element Selection" page.
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AA-6200
4.2 Software Basic Operation
Basic Operation
Figure 4-14 : Lamp Position Adjustment Dialog Box
(4) When fine adjustment of the lamp position is complete, click on the <Next>
button to proceed to the "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.
Emission mode
This mode measures concentrations by measuring the light emission energy of
4 the substance. Use this mode to adjust the position of the hollow cathode lamp
as well.
Non-BGC mode
Basic Operation
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 <Line Search...> 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 <Close> button.
(4) Click the <Next> 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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AA-6200
4.2 Software Basic Operation
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.
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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 <Finish> button. The Wizard ends
4 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.
Basic Operation
CAUTION
Before igniting the flame, carefully read 4.8 Igniting and Extinguishing the Flame
and check safety precautions.
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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 <Save> button. "Save As" dialog box is closed and the template file is
saved.
4
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.
4
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
Basic Operation
[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.
If the standard or unknown samples are measured after executing the blank
measurement, their measured values (absorbance or energy) are indicated 4
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
Basic Operation
[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 <START> 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 <START> 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).
If <START> 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.
If you want to make the size of MRT (Measurement Result Table) work sheet
Basic Operation
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.
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.
Basic Operation
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AA-6200
4.4 Saving/Printing/Deleting the Data
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
4 it out before ending the AA software.
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
<OK>. 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.
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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
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
4 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
Basic Operation
!0 Function buttons
!1 Status bar
e ru y i
q
w
!0
!1
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.
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AA-6200
4.6 Explanation of Main Window
New : All the data and parameters are cancelled and parameters are set
Basic Operation
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)
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AA-6200
4.6 Explanation of Main Window
4
Basic Operation
(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 <Reset> 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.
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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 <OK>. The real time waveform currently displayed will be printed.
Basic Operation
displayed. Specify their colors in the [Graph] on the MRT work sheet.
(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
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AA-6200
4.6 Explanation of Main Window
the five graph. Clicking on <Reset> 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
4 [Minor Grid Line].
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
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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 <OK>.
Only the selected peak profile will be printed. 4
Basic Operation
displayed.
(1) Calibration Curve Display
If you want to check a calibration curve other than the currently displayed one,
set the <Latest> 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 <Type> button. Clicking on <Type> opens
the "Change Calibration Curve Condition" dialog box where you can change
order of calibration curve and permission of zero intercept.
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AA-6200
4.6 Explanation of Main Window
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.
4 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.
Basic Operation
(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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AA-6200
4.6 Explanation of Main Window
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.
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AA-6200
4.6 Explanation of Main Window
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 <OK>. Then the calibration curve currently displayed
is printed out. This menu is not displayed when no calibration curve exists.
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.
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AA-6200
4.6 Explanation of Main Window
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 Flame
Manual Auto(using ASC)
<AUTO ZERO> O O
<BLANK> O ×
<START> O O
<RINSE> × ×
O = Available × = Not available
Clicking on <AUTO ZERO> 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 <RINSE> 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 <STOP> stops the measurement. However, while acquiring the data,
the measurement is stopped after the data acquisition is finished.
<TEST MEAS.> is not available for AA-6200.
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AA-6200
4.6 Explanation of Main Window
q w e r t y
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.
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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.
As the measurement procedure, prepare the sample shown in the [Action] column and
click on <START>. You can proceed the measurement in the order from top row to
Basic Operation
down.
When a repeat measurement is set, rows for repetition are inserted at the time of
measurement.
(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.
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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
4 of each QC type in "QA/QC Setup" page.
Basic Operation
Basic Operation
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 AA-
6200.
PAUSE : Specifies temporary stop until the <OK> 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.
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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 4
Value] column heading, the unit specified in the "Preparation Parameters" page
is automatically displayed.
(9) [Abs.]
Basic Operation
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
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.
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.
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AA-6200
4.7 Operating the MRT work sheet
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.
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AA-6200
4.7 Operating the MRT work sheet
4
Basic Operation
[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).
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AA-6200
4.7 Operating the MRT work sheet
Basic Operation
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.
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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
eWhen completed, click on <OK> to close the "Collective Edit" dialog box.
Settings are changed and the actual concentration is recalculated
simultaneously and the work sheet is renewed.
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AA-6200
4.7 Operating the MRT work sheet
Basic Operation
measurement.
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.
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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 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
Basic Operation
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.
4.7.6.1 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.
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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.
Basic Operation
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.
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.
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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.
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AA-6200
4.8 4.8 Igniting and extinguishing the flame
PURGE
Basic Operation
EXTINGUISH
The burner select sensor for the high temperature burner head for N2O-C2H2 flame
is located at the lower left of the chamber.
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.
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4.8 Igniting and extinguishing the flame
CAUTION
Before igniting a flame, check that the ignition buttons work properly.
4
<Checking procedure>
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 10-
Basic Operation
minute 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.
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AA-6200
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 4
before the ignition.
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
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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.
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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AA-6200
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. 4
Six or seven seconds after the Air-C2H2 flame ignites. the C2H2 flow rate
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
Basic Operation
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.
CAUTION
1. Always use the high temperature burner head when using a nitrous oxide-
acetylene 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
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AA-6200
4.8 Igniting and extinguishing the flame
Carbon deposit
Blue
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.
Basic Operation
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.
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4.8 Igniting and extinguishing the flame
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. 4
Absorbance
Basic Operation
Standard addition concentration
Concentration of unknown sample
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.
Absorbance
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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.
(Analysis example)
Basic Operation
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 <Edit>. 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)
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AA-6200
4.9 Standard Addition Method and Simple Standard Addition Method
Basic Operation
(8) When completing the setup, click on <OK>. Then "Preparation Parameters"
page is displayed again. When measuring plural elements, make setup for other
elements in the same procedure.
(9) Click <Next> 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
<Finish> button to end the Wizard. The measurement procedure as shown in
Table 4.3 is set on the MRT worksheet.
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 Description
MSA Indicates standard addition method.
Indicates the concentration of unknown sample calculated
MSA-RES
from the result of measuring a set of standard addition samples.
Indicates simple standard addition method. Unknown sample
SMSA is measured using a calibration curve created by another
sample for standard addition method.
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.
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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) 4
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
Basic Operation
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.
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AA-6200
4.9 Standard Addition Method and Simple Standard Addition Method
4-66
AA-6200
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.
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 <Lamp Pos. Setup> 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 <Lamp Pos. Setup> button to display the "Lamp Position Setup"
dialog box.
2. For an arbitrary [Socket #], select "*" in the [Element] and "Normal" in the
[Lamp Type].
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AA-6200
4.10 Conditions and Operation for Flame Emission Analysis
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 <START> 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 <Next> button to proceed to the "Gas Flow Rate Setup" page first.
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AA-6200
4.10 Conditions and Operation for Flame Emission Analysis
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 N2O-
C2H2 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.
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AA-6200
4.10 Conditions and Operation for Flame Emission Analysis
(3) While spraying the sample, click on <Line Search> 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 <Close> to return to the "Optics
Parameters" page. Then click on <Next> 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).
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AA-6200
5 Menu Commands
5
Menu Commands
This chapter explains items and functions displayed on the screen of PC software that
controls the AA instruments.
Contents
AA-6200
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
5.3.6 [Clear Measurement Result] ……………………………………………5-20
5.3.7 [Copy] ……………………………………………………………………5-20
5.3.8 [Paste] ……………………………………………………………………5-20
Menu Commands
AA-6200
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
5.8 [Instrument] ………………………………………………………………………5-57
5.8.1 [Connect] …………………………………………………………………5-58
5.8.2 [Option Connect] …………………………………………………………5-60
Menu Commands
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
5.8.6 [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
5.8.14 [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 <Cancel> closes this dialog box, and clicking on <Wizard> at left
lower of the main window displays this dialog box again.
Menu Commands
Figure 5.1 : "Wizard Selection" dialog box
[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]
5 from the menu.
A data file 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.
5
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).
Menu Commands
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]).
5-3
AA-6200
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 <Open>.
5
Menu Commands
<Comment>
If a comment has been written with the file to be opened, the comment can be
read. Enter [File name] and click on <Comment>, 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]
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.
Menu Commands
Figure 5.4 : "Save As" Dialog Box
<Comment>
This button is used to record your comment. Click on <Comment> button, then
"File Comment" dialog box opens. Write your comment and click on <OK>. The
comment is saved with the file.
5-5
AA-6200
5.2 [File]
(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]
5
(1) Select [File]-[Additional Load] menu. "Merge File" dialog box is displayed.
Menu Commands
(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 <Open>.
(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.
5-6
AA-6200
5.2 [File]
NOTE
Only the data on the MRT work sheet can be output to text file. Measurement
5
parameters and waveform data cannot be output.
Menu Commands
Figure 5.6 : "Select Schedule" Dialog Box
5-7
AA-6200
5.2 [File]
[Operation]
(1) Select [File]-[Export Items] menu. "Export Items" dialog box is displayed.
5
Menu Commands
(2) Select the item you want to output and click the <OK> button.
5-8
AA-6200
5.2 [File]
[Operation]
(1) Select [File]-[Auto Save] menu. "File Auto Saving and Exporting" dialog box
is displayed.
q w
Menu Commands
r
e
5-9
AA-6200
5.2 [File]
NOTE
5
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.
5-10
AA-6200
5.2 [File]
w
r
e
5
t
y o
Menu Commands
u
i
[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".
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.
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AA-6200
5.2 [File]
[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
5
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.
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.
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AA-6200
5.2 [File]
5 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
Menu Commands
Menu Commands
Figure 5.11 : "Print Style Setup" page
Put check marks to the items or contents you want to print. Clicking on <Details>
displays more detail items.
In the [Data Print Mode], you can select it from the following three.
5-15
AA-6200
5.2 [File]
5
Menu Commands
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".
5-16
AA-6200
5.2 [File]
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.
5.2.14 [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.
5-17
AA-6200
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
NOTE
Insertion and deletion of a row next to current measuring row can't be done during
measurement.
[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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AA-6200
5.3 [Edit]
In this dialog box, select the element schedule of copy source and click the <OK>
Menu Commands
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.
[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 <OK> to close the [Collective Edit] dialog
box. The change is executed and the actual concentration is recalculated to
renew the worksheet.
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AA-6200
5.3 [Edit]
5
Menu Commands
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.
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AA-6200
5.4 [Refer to Parameters]
Menu Commands
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.
5-21
AA-6200
5.5 [Parameters]
5
Figure 5.18 : Drop-down Menu of [Parameters]
5-22
AA-6200
5.5 [Parameters]
Each Wizard is composed of the pages shown below. Clicking on <Next> in each
page opens the next page. You can close the Wizard by clicking on <Finish>
when the settings are completed on each page.
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 <Next> 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.
5-23
AA-6200
5.5 [Parameters]
5
Menu Commands
<Select Elements>
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.
<Edit Parameters>
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.
<Up>
Select an element row and click on this button. Then the row moves up one row
upper.
<Down>
Select an element row and click on this button. Then the row moves down one
row lower.
5-24
AA-6200
5.5 [Parameters]
<Delete>
If you want to delete a row, click on the row to make its color reversed and then
click on <Delete>. 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.
<Connect>
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.
5
5.5.1.1 "Cookbook" page
In the "Cookbook" page, select the target element from the drop-down list. Also,
Menu Commands
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.
5-25
AA-6200
5.5 [Parameters]
<Periodic Table>
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.
In the "Template" page, a template (*.taa) already created can be read. Click on
<Browse> to open the "Open" dialog box. Then specify the [Look in] and [File
name] and click on <Open>. 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 <OK> 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.
Menu Commands
Double-click on the element to be edited, or select the element row and click on
<Edit> to open the "Edit Preparation Parameters" dialog box.
5-27
AA-6200
5.5 [Parameters]
5
Menu Commands
[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.
<Repeat Conditions>
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.
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 5
brought up to a specific volume.
[Dilution Factor]
Menu Commands
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.
[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]
[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.
<Collective Setup>
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 <OK>.
[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
Menu Commands
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".
<Connect/Send 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.
<Connect Options>
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.
5
5.5.6 "Optics Parameters" Page
Wavelength, slit width, socket number, lamp current, lamp mode, lamp ON/OFF are
Menu Commands
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.
[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.
5 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.
Menu Commands
Conversely, if the light intensity of the hollow cathode lamp is too great, widen
the slit width.
NOTE
When a neighboring line exists, note that the neighboring line may not be separated
if the slit width is widened.
Menu Commands
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 <Line Search> button is pressed
5-35
AA-6200
5.5 [Parameters]
setting is valid only when the lamp mode is EMISSION and [Lamp Current] is "0".
5-36
AA-6200
5.5 [Parameters]
Menu Commands
the <Line Search> 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.
<Close>
When this button is clicked on, this dialog box is closed to return to previous screen.
<Stop>
If this button is clicked on during execution of line search, beam balance
execution stops.
<Do Line Search>
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
5 optimization of detector sensitivity (beam balance) are performed. When the
sensitivity setup is finished, "Beam Balance: OK" is indicated.
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.
<Print>
The result of Line Search is printed out.
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]
5
Select a wavelength used as the analysis line from the [Detected Peaks] list box.
The wavelength set here is stored in the AA software.
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.
5-39
AA-6200
5.5 [Parameters]
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.
5
Menu Commands
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.
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.
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.
5-41
AA-6200
5.5 [Parameters]
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.
5
[Measured Data]
The current measurement data is displayed. In the background correction
Menu Commands
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.
<Auto Zero>
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 <OK>. To cancel the setting
halfway, click on <Cancel>. Then the settings return to the previous conditions 5
before changed.
Menu Commands
5-43
AA-6200
5.6 [Edit Parameters]
5
Menu Commands
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.
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)
Menu Commands
Figure 5.36 : Repetition Sequence (SM-SM-...)
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]
[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
5 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
Menu Commands
better repeatability.
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]
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.
5 [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
Menu Commands
RSD : RSD = σ
µ ×100(%)
5-48
AA-6200
5.6 [Edit Parameters]
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]
5 Enter a unit for actual concentration.
[Decimal Place]
Set a decimal place for displaying and rounding the Weight Factor, Volume Factor,
Menu Commands
Dilution Factor, Correction Factor and Actual Conc. This decimal place is used
for actual concentration calculation, the display on the screen and data print.
5-50
AA-6200
5.6 [Edit Parameters]
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.
5-51
AA-6200
5.6 [Edit Parameters]
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.
5
Menu Commands
r= N Σxiyi−ΣxiΣ yi
[NΣxi2−(Σ xi)2] [NΣyi2−( Σyi)2]
1 1
2 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".
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.
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.
[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").
[Conc. Unit] 5
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).
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AA-6200
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.
5
5.7.3 [Graph]
"Graph Default Scale" dialog box is opened. The ordinate scale and the time width
Menu Commands
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.
5-56
AA-6200
5.8 [Instrument]
Menu Commands
Figure 5.44 : "Instrument" Drop-Down Menu
5-57
AA-6200
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
<OK> 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
5
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.
Menu Commands
After closing the "Initialize" dialog box, "Instrument Check List for Flame Analysis"
is displayed.
5-58
AA-6200
5.8 [Instrument]
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 <OK>. After completing the inspection, click on <OK>
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).
5-59
AA-6200
5.8 [Instrument]
5
Figure 5.47 : "Option Connect" Dialog Box
<Connect>
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.
[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]
5
This function is used to set the baseline to zero frequently in the flame
measurement with ASC.
Menu Commands
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.
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].
[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
5 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
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.
[Decimal place] 5
This sets a decimal place to which the absorbance is rounded.
The rounding method is as follows.
Menu Commands
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.
5-63
AA-6200
5.8 [Instrument]
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.
Menu Commands
q
(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 <OK> button and
close "Configuration" dialog box to fix the setting.
5-65
AA-6200
5.8 [Instrument]
Figure 5.50 : Management of Lamp Used time when the Lamp Position Setup function is not used
5
(1) Selecting the measurement lamp
Select the measurement element in the Element Selection dialog box. At this
Menu Commands
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.
5-66
AA-6200
5.8 [Instrument]
Figure 5.51 : Management of Lamp Used time when the Lamp Position Setup function is used
Menu Commands
After turning off the lamp, select [Instrument]-[Lamp Position Setup].
"Lamp Position Setup" dialog box is displayed.
q w e r
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
5
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).
Menu Commands
After finishing the settings, click on the <OK> to fix the settings. The
lamp position setup information is saved in "lampplace.ref" file.
(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.
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
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.
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AA-6200
5.8 [Instrument]
9 Default
each element when the lamp position setup function is not used.
10 Comment Comment can be freely entered (up to 25 characters).
This is used to lock or release the lamp data edit. When the used
11 Lock
time accumulation is started, this is automatically selected.
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).
5
[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.
Menu Commands
(2) Click <Clear> (!2).
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
(2) To display the message, select [Show lamp used time over operating life
message] check box (q) and click <OK>.
If you don't want to display the message, clear this check box and click <OK>.
5-72
AA-6200
5.8 [Instrument]
5.8.6 [Maintenance]
Selecting this menu allows you to use the functions for maintenance of the instrument.
[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 <OK>.
5
(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 <OK>. The D2 lamp is lit on and the
beam balance is executed. When the beam balance has succeeded, "D2 lamp
Menu Commands
Adjustment" dialog box is displayed.
If the error message "D2 lamp energy is too low. Please adjust D2 lamp
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.
(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.
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 <Start Measurement> in this dialog box ignores the waiting time and starts
5
measurement.
Menu Commands
Figure 5.57 : "Warmup Waiting" Dialog Box
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.
NOTE
Menu Commands
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 <OK>.
[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 <OK> and close the "Sequence" page.
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AA-6200
5.8 [Instrument]
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.
CAUTION
Be sure to follow the procedure below to perform the remaining gas combustion. If
the procedure is compromised, a flashback may occur.
5-77
AA-6200
5.8 [Instrument]
CAUTION
Be sure to use Air-C2H2 flame to perform the remaining gas combustion. Using N2O-
C2H2 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 <OK>.
5
Menu Commands
(5) Next, the message shown in Figure 5.60 is displayed. Click on <OK> 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 <OK> to close it.
NOTE
When stopping the remaining gas combustion, click on <Cancel> 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]
(7) Click on <OK> in the message of Figure 5.61 to close the message.
5
5.8.12 [Execute Line Search]
This is used to execute the line search for the element currently set. This function is
the same as that of <Line Search> button in the "Optics Parameters" page, but both
Menu Commands
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 <Line Search> button in
"Optics Parameters".
5.8.13 [Cleaning]
This menu item is not available for AA-6200.
5-79
AA-6200
5.8 [Instrument]
"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.
5
Please press OK button after you finish the adjustment."
5-80
AA-6200
5.9 [Help]
Menu Commands
5-81
AA-6200
5.10 Rounding the absorbance and setting the decimal places for correction factors and actual concentration
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.
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AA-6200
5.10 Rounding the absorbance and setting the decimal places for correction factors and actual concentration
Menu Commands
q w
(3) To fix the setting, click <OK>. 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.
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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 Omission
When the figure in the specified decimal place is odd Raising to a unit
5.10.2 Setting the decimal places for correction factors and actual
Menu Commands
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.
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AA-6200
5.10 Rounding the absorbance and setting the decimal places for correction factors and actual concentration
w q
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 <OK> 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
Maintenance
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
AA-6200
AA-6200
Maintenance
6
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 O-
rings 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 6
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.
Maintenance
2. Deteriorated O-rings cause gas leaks. O-rings should be replaced on a yearly basis.
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
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.
(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
r Nebulizer
t Chamber
y Mixer u Spray unit
6-3
AA-6200
6.1 Burner maintenance
q Capillary
u Polyethylene tube
w Plastic jacket
y Cap
e Body
(Metal part)
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.
(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
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.
Maintenance
e Chamber fixing screw w Nebulizer fixing screw
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.
6 (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.
Maintenance
(6) If a gas leak occurred in a gas hose, immediately replace it with a new gas hose.
(1) Switch the instrument on and start the AA-6200 software. Press <Cancel> 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 <OK>.
(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 <OK>
(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 <OK>.
(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 <OK> to proceed to the
next screen.
(7) Reconnect the spray tube and fuel tube as they were before. Finally select
<OK> 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.
Gas hoses
Fuel gas Oxidant gas Gas piping
6
Maintenance
Fuel tube
Spray tube
Seal joint
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
6 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.
Maintenance
(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.
6-8
AA-6200
6.3 Peplacing the deuterium lamp
6
Aperture plate
Maintenance
6-9
AA-6200
6.4 Rinsing
6
Maintenance
6-10
AA-6200
6.5 List of maintenance parts
Maintenance
Retaining plate 206-51389 For securing the nebulizer
Elbow, 31020600 035-65268-02 Connecting nebulizer to spray tube
Lamp, L6380 062-65055-05 D2 lamp
Tube, super corn-ace 9 × 13 016-43200-08 U-tube
Mixer 206-50486
6-11
AA-6200
6.6 Optional accessories list
6-12
AA-6200
6.6 Optional accessories list
Maintenance
Ru Ruthenium 200-38422-45 L233-44NB
Sb Antimon 200-38422-24 L233-51NB
Sc Scandium 200-38422-71 L233-21NB
Se Selenium 200-38422-46 L233-34NB
Si Silicon 200-38422-16 L233-14NU
Sm Samarium 200-38422-72 L233-62NB
Sn Tin 200-38422-18 L233-50NQ
Sr Strontium 200-38422-34 L233-38NB
Ta Tantalum 200-38422-35 L233-73NU
Tb Terbium 200-38422-73 L233-65NB
Te Tellurium 200-38422-47 L233-52NQ
Ti Titanium 200-38422-17 L233-22NB
Tl Thallium 200-38422-74 L233-81NU
Tm Thulium 200-38422-75 L233-69NB
V Vanadium 200-38422-19 L233-23NB
W Tungsten 200-38422-36 L233-74NU
Y Yttrium 200-38422-76 L233-39NB
Yb Ytterbium 200-38422-77 L233-70NB
Zn Zinc 200-38422-23 L233-30NQ
Zr Zirconium 200-38422-37 L233-40NB
6-13
AA-6200
6.6 Optional accessories list
6-14
AA-6200
7 Troubleshooting
Contents
7
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
Troubleshooting
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
AA-6200
AA-6200
Troubleshooting
7
7.1 Troubleshooting
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.
Troubleshooting
7.1.3 Wavelength origin error occurs at initialization
Remove any obstacles blocking the optical path in the atomizer unit.
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.
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.
Troubleshooting
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.
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)
Analytical Line is not Line Search has failed. (1) Verify that the lamp is correctly mounted to the socket and
found. The following causes are the lamp turret position.
considerable. (2) Perform the wavelength correction in [Instrument]-
(1) The lamp is not properly [Maintenance]-[Wavelength Adjustment].
mounted to the lamp turret.
(2) The wavelength shift has
occurred in the
monochromator.
ASC arm motor slipped. • Verify that the ASC arm movement is not impeded.
• Switch on the ASC again and connect the ASC in
[Instrument]-[Option Connect] menu.
ASC arm rotation (1) The origin detector didn't (1), (2) Switch on the ASC main unit again.
position cannot be detect the origin correctly. If the error occurs again, record the status in which this error
initialized. (2) The arm rotation drive message appears and contact your Shimadzu service
motor doesn't operate. representative.
(1) The origin detector didn't (1), (2) Switch on the ASC main unit again.
ASC arm vertical
detect the origin correctly. If the error occurs again, record the status in which this error
position cannot be
(2) The vertical arm drive message appears and contact your Shimadzu service
initialized.
motor doesn't operate. representative.
ASC Error occurred Remove the cause of error and switch on the ASC power again.
during action. Press Then connect the ASC in [Instrument]-[Option Connect] menu
Cancel to close this and try this operation again.
dialog box. Resolve the
ASC problem then retry.
ASC I/F port is used for Communication with ASC is Verify the ASC power supply and the cable connection
another device. unstable. between ASC and AA main unit, then connect the ASC in
[Instrument]-[Option Connect] menu.
7-4
AA-6200
7.2 Error Messages
Troubleshooting
considerable. • If the wavelength shift has occurred in the monochromator,
(1) The light intensity of the perform the wavelength correction in [Instrument]-
hollow cathode lamp [Maintenance]-[Wavelength Adjustment].
becomes too smaller than (3) Change the hollow cathode lamp.
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
Before the new memory Only one memory wavelength Click <Clear> in "Wavelength Memory Setup" dialog box to set
wavelength is set, clear can be set for one actual [Memory Wavelength] to "NONE" then set a new memory
the current memory wavelength. wavelength.
wavelength and execute
Line Search.
BG signal is too large. Beam Balance failed because (1)
the light intensity of BG • Increase the hollow cathode lamp current (Low) (pay
measurement is too greater attention to the max. current).
than the light intensity of • When the lamp mode is BGC-D2, narrow the slit width.
hollow cathode lamp. (2)
The following causes are • Set [Wavelength] correctly in Optics Parameters page.
considerable. • If the wavelength shift has occurred in the monochromator,
(1) The light intensity of the perform the wavelength correction in [Instrument]-
hollow cathode lamp [Maintenance]-[Wavelength Adjustment].
becomes too smaller than (3) Change the hollow cathode lamp.
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.
7-6
AA-6200
7.2 Error Messages
Troubleshooting
Blank cannot be inserted Inserting a blank measurement Execute the blank measurement after the repeat
here. row between the repeat measurements are finished.
measurement rows was tried.
Buffer Overflow. Amount of the acquired data is Switch on the PC power and the instrument power again. If the
larger than the communication error occurs again, check the following items.
buffer of AA software. • 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 (1) When the AA-6200 was (1) Remove the burner-recognizing pin from the burner select
out of order! Please call initialized, the burner- sensor then start the initialization.
a service engineer. recognizing pin was (2) Stop using the N2O and contact your Shimadzu service
inserted in burner select representative.
sensor located at the lower
left of the burner chamber.
(2) At the time of initialization,
the defective of burner
select sensor was detected.
C
Calibration Curve The calibration curve order When the Zero Intercept is not selected, set the calibration
cannot be created. doesn't match with the number curve order below the number of standard samples.
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 Standard samples (STD or Set up STD, in the case of calibration curve method, and MSA,
not exist! MSA) have not been measured. in the case of standard addition method or simple standard
addition method, on the MRT work sheet and measure them.
7-7
AA-6200
7.2 Error Messages
7-8
AA-6200
7.2 Error Messages
Troubleshooting
Schedule. Schedules on the MRT work page. Also, clear the check box of unnecessary element in
sheet exceeds 20, the excess [Element Selection] list when reading out parameters in the
schedules cannot be read out Template page of "Load Parameters" dialog box.
on the MRT.
Failed to detect (1) The origin detector couldn't (1), (2) Switch on the AA main unit again.
wavelength motor detect the origin correctly. If the error occurs again, record the status in which this error
origin. (2) The wavelength drive motor message appears and contact your Shimadzu service
doesn't operate properly. representative.
Failed to extinguish the EXTINGUISH button of the Press the EXTINGUISH button following the instruction
flame. instrument was not pressed displayed while executing the residual gas combustion.
while executing the remaining
gas combustion.
Failed to load Cookbook The "cookbook.ref" file in the Delete the "cookbook.ref" file and install it again.
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 Check that the file tried to load actually exists.
file cannot be read out in
Wizard Selection dialog box.
Failed to open the serial The PC serial port cannot be Check the following points.
port. used. • [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.
7-9
AA-6200
7.2 Error Messages
7-10
AA-6200
7.2 Error Messages
Troubleshooting
(6) The emission intensity of
the standard sample of the
highest concentration is too
small.
I
Instrument is not ready! (1) A command was tried to (1) Set the communication with the instrument to ON from
send when the [Instrument]-[Connect] menu.
communication between the (2) Close this message box and wait until the command
instrument and PC is OFF. currently executed in the instrument is finished. Perform
(2) While the instrument is the target operation again after "READY" is displayed at the
executing the command, the right lower of the status bar.
next command was tried to
send.
Instrument is still busy. The operation that cannot be Close this message and wait until "READY" is displayed at the
executed during BUSY status of right lower of the status bar. Then perform the target operation
instrument was tried. again.
Invalid ASC Command. A command that is not Verify that the AA software supports the your ASC.
supported by the ASC was sent
from the AA software.
Invalid ASC Parameter. Parameters that are not Verify that the AA software supports the your ASC.
supported by the ASC were
sent from the AA software.
J,K
7-11
AA-6200
7.2 Error Messages
7-12
AA-6200
7.2 Error Messages
Troubleshooting
O
Other program is using "lamphist.ref" file is a data file (1) "lamphist.ref" can be renewed from the AA software firstly
lamphist.ref file. Lamp for lamp history. The following started up but cannot be renewed from the AA software
data will not be saved. causes are considerable when secondly started up. Therefore, use the AA software firstly
this message is displayed. started up to perform measurement. There is no problem to
(1) The second AA software has use the AA software secondly started up to edit parameters.
been started up. (2) Turn the read-only attribute of "lamphist.ref" file in AA
(2) The file attribute of software folder OFF.
"lamphist.ref" is read-only.
Other program is using "lampplace.ref" file is a data file (1) "lampplace.ref" can be renewed from the AA software
lampplace.ref file. Lamp for lamp position setup. The firstly started up but cannot be renewed from the AA
data will not be saved. following causes are software secondly started up. Therefore, use the AA
considerable when this software firstly started up to perform measurement. There
message is displayed. is no problem to use the AA software secondly started up
(1) The second AA software has to edit parameters.
been started up. (2) Turn the read-only attribute of "lampplace.ref" file in AA
(2) The file attribute of software folder OFF.
"lampplace.ref" is read-only.
P
Periodic Blank If an invalid value that is not usually entered has been entered
Preparation Parameters in the Blank Samples table of the "Edit Preparation
is Invalid. Parameters" dialog box, enter a correct value.
7-13
AA-6200
7.2 Error Messages
S
Sample Preparation If an invalid value that is not usually entered has been entered,
Parameters is Invalid. 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 Select the measurement element and set up the measurement
ASC, Element schedule has not procedure in [Action] fields on the MRT work sheet.
been selected, or the
measurement procedure has
not been set up although the
element schedule exists.
Serial Port Error. The PC serial port has a Switch on the PC power and the instrument power again. If the
problem. 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
Troubleshooting
remaining gas combustion may cause a
combustion. flashback.
T
Termination has not Communication protocol with Verify the ASC power supply and the cable connection
been accepted from ASC was not completed. (:T) between ASC and AA main unit, then connect the ASC in
ASC. [Instrument]-[Option Connect] menu.
The following lamps The data mismatching between Click on <Yes> and delete the data from the lamp position
exist in the Lamp the lamp history and the lamp setup. Register the necessary lamps in [Instrument]-[Lamp
Position Setup Dialog position setup was detected at History]. Next, make a setting of the lamp mounted to each
Box, but do not exist in the time of starting up the AA socket in [Instrument]-[Lamp Position Setup].
the Lamp History Dialog software.
Box. Please update the
Lamp History Dialog
Box or delete lamps
from the Lamp Position
Setup Dialog Box.
Socket #x,x,x,…
The selected area cannot In [Instrument]-[Lamp Position Setup] menu, select [NONE] for
be cleared as the [Element] field of the lamp ID you wish to clear, and click on
information is stored in <OK>. Then clear the target lamp in "Lamp History" dialog box.
the Lamp Position Setup
Dialog Box.
The selected area cannot In [Instrument]-[Lamp Position Setup] menu, select [NONE]
be deleted as the for [Element] field of the lamp ID you wish to delete, and click
information is stored in on <OK>. Then delete the target lamp in "Lamp History" dialog
the Lamp Position Setup box.
Dialog Box.
7-15
AA-6200
7.2 Error Messages
executed while the measurement element. Use [Lamp ON] check box in the case
hollow cathode lamp is lit of measurement lamp and <Warmup Lamp> button in the case
ON. Please retry it after of warm-up lamp. Then, execute the aimed operation.
you turn off the lamp.
Timer cannot be created. The number of timers currently Start up the PC again. Also, don't start other applications.
After closing other used exceeds the limit of the
applications, try it again. Windows system.
Too many schedules. When executing [File]- When the Element schedule you wish to add is located in the
Failed to add all [Additional Load], the excess latter part of the original file of adding, start up another AA
schedules. schedules cannot be read out software and load the original file for adding and move the
on the MRT work sheet if the order of target Element schedule. Or take out only the element
number of Element Schedules schedule and save it as different file name to create an original
on the MRT work sheet file for adding.
exceeds 20.
U
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: An error that is not defined in Switch on the PC power and the instrument power again. If the
/(Error Code) the AA software inside has error occurs again, record the number indicated in the error
occurred. message and the status in which the errors occurred. Then
contact your Shimadzu service representative.
Usage time has exceed When registering the lamp in It is possible to input the values as "(Life Time) < (Used Time)".
lamp life time. "Lamp History" dialog box, the If the values are not wrong, continue the input.
input values has a relation
"(Life Time) < (Used Time)".
7-16
AA-6200
7.2 Error Messages
Troubleshooting
7-17
AA-6200
8 Appendix
Contents
Appendix
AA-6200
8
Appendix
AA-6200
8.1 Measurement conditions for Flame Atomic Absorption analysis
Appendix
Ho 410.4 14 0.2 N2O-C2H2 7.0 High Temp 1.2
Ir 208.8 20 0.2 Air-C2H2 2.2 Standard 1.5
K 766.5 10 0.7 Air-C2H2 2.0 Standard 0.012
La 550.1 18 0.7 N2O-C2H2 7.5 High Temp 70
Li 670.8 8 0.7 Air-C2H2 1.8 Standard 0.03
Lu 360.0 14 0.7 N2O-C2H2 7.0 High Temp 15
Mg 285.2 8 0.7 Air-C2H2 1.8 Standard 0.0035
Mn 279.5 10 0.2 Air-C2H2 2.0 Standard 0.028
Mo 313.3 10 0.7 N2O-C2H2 7.0 High Temp 0.5
Na 589.0 12 0.2 Air-C2H2 1.8 Standard 0.006
8-1
AA-6200
8.1 Measurement conditions for Flame Atomic Absorption analysis
8-2
AA-6200
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.
Appendix
8-3
AA-6200
8.2 Analysis line wavelengths for Flame Emission analysis
† : Band Spectrum
8-4
AA-6200