206-94935A

INSTRUCTION MANUAL

Shimadzu Atomic Absorption

Spectrophotometer
AA-6300 (P/N 206-51800)

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 © Shimadzu Corporation 2002. 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.

･ Windows 2000 is trademark and trade name of Microsoft. Other product names described in this
manual are each manufacturer's trademarks or registered trademarks.
 Precautions for Safe Operation

The atomic absorption spectrophotometer is used as an analytical equipment for inorganic

elemental analysis.
To operate this equipment safely, strictly observe the following precautions. If not observed,
the safety may be compromised.

1. Do not use the equipment for any purpose other than the above-mentioned
types of analysis.

2. Follow the procedures described in the instruction manual.

3. Observe all warnings and cautions.

4. Do not disassemble or modify the equipment without the express approval of

an authorized Shimadzu Representative.

5. For internal repair of the equipment, contact your Shimadzu Representative.

6. The meshed descriptions about installation in this instruction manual are

intended for Shimadzu service personnel. Don’t use them and install the parts
by yourself because it is dangerous.

In this manual, the meanings of caution signs are provided as follows.

WARNING indicates a potentially hazardous situation, which, if not avoided,

could result in death, serious injury or moderate injury.

CAUTION indicates a potentially hazardous situation, which, if not avoided,

could result in minor injury, or may result in machine damage.

NOTE is used to increase the work efficiency or to help comprehension of

the description.

I
 Precautions on Handling High Pressure Gas

High pressure gas must be handled carefully observing the legal regulation.
Not only to the following precautions, refer to regulations and laws regarding to handle the
high pressure gas. Cautionary items in this manual should be read carefully.

1. Installation of gas cylinder

(1) Install the gas cylinders in the airy outdoors where they are not exposed to direct
sunlight.
(2) Take care that gas cylinders become no hotter than 40℃, and do not allow any
flame within 2 meters of the gas cylinders.
(3) Secure gas cylinders so that they cannot drop or fall over. Always keep liquefied gas
cylinders (acetylene, nitrous oxide, etc.) in a vertical position and do not allow them
to fall to a horizontal position.

2. Acetylene gas
(1) When using acetylene gas, please use a pressure reduction valve especially made for
use with acetylene gas. Do not allow acetylene to flow through pipes and equipment
made from copper, silver, mercury, or their alloys in order 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 reduced below 0.5MPa, it should be replaced with a new cylinder in order
to prevent the outflow of solvents.

3. Oxygen gas
Do not use oxygen gas.

4. Air
Supply the dry air. If air containing much moisture is used, the moisture may adhere to
the inside of the gas controller and prevent normal operation. Dehumidify with a drain
separator provided on the way of piping from the air supply source.

5. After use of gas

After the gas was used, be sure to close the main valve as well as the stop valve.

II
6. Pressure gauge
Periodically inspect the pressure gauge to maintain its normal function.

7. Pressure regulator
(1) Use approved pressure regulators and connectors. For details, contact your
Shimadzu Representative.
(2) When installing the pressure regulator to the cylinder, be sure to wipe the dust at the
outlet of the cylinder.
(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.

8. Cylinder opening/closing
(1) Before opening the cylinder, be sure to check 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 the hammer or spanner.
(2) After the main valve is opened, apply soapy water to the connection of the pressure
regulator to check if no gas leak is generated. Also check the connection at the main
valve.
(3) Completely open the main valve of the cylinder for nitrous oxide gas, argon gas and
hydrogen gas. If it is not completely opened, flow rate of the gas may fluctuate.
(4) When opening the main valve of the cylinder for acetylene gas, rotate it by 1
rotation or 1.5 rotations from the state of complete closing.
To prevent outflow of acetone from the inside of the cylinder, do not open the valve
exceeding 1.5 rotations from the state of complete closing. On the contrary, if the
main valve is not sufficiently opened in case of nitrous oxide-acetylene flame (high
temperature flame), flashback may be caused due to insufficient acetylene when the
flame is switched from an air-acetylene flame to nitrous oxide-acetylene flame.

III
 Precautions on Handling Hollow Cathode Lamp
Electrodes of some hollow cathode lamps contain harmful metal elements (As, Be, Hg, Se,
etc.). Some electrode metals may ignite when touched with air or water (K, Li and Na). Read
the precautions attached to the hollow cathode lamp thoroughly and handle the lamp very
carefully for safety.

1. When disposing of the lamp

If the hollow cathode lamp should be broken or its life is finished, dispose of the lamp
separately from general garbage. When disposing of the hollow cathode lamp supplied
from Shimadzu Co., select a method, which will not influence the environmental
pollution or human body, or ask a special disposal dealer.
The materials of hollow cathode lamp are as follows.
・Metals (including electrode element)
・Quartz glass
・Plastic
Some electrode contains harmful metal (Hg, As, etc.).

2. Specifications change
The specifications of the hollow cathode lamp are subject to change for improvement
without notice. In this case, set the lighting current referring to the precautions
attached to the hollow cathode lamp.

Precautions on Handling Deuterium (D2) Lamp

When disposing of the lamp

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

IV
 Handling Waste Liquid

Waste liquid discharged during measurement or pretreatment should be handled in different

ways in accordance with the solute and solvent contained in that waste liquid. The way of
handling waste liquid is different depending upon the country or region.
Be sure to dispose of waste liquid according to the location of use.

Supply Period of Replacement Parts

Replacement parts are supplied by the Shimadzu Parts Center. The supply period of these
parts is determined as below.

As a general rule, ten (10) years after the discontinuation of the product

Note, however, that the availability of units or parts not manufactured by Shimadzu shall be
determined by the relevant manufacturers. If Shimadzu should receive a notice of the
discontinuation of the units or parts, the necessary quantity for the above period is
immediately calculated and secured. However, such parts may cease to be available within ten
years after the discontinuation of the product, depending on the situation of the relevant
manufacturers or change of the necessary quantity.

V
 Precautions on the Installation Site and Handling

In the case of atomic absorption spectrophotometer, high pressure gas is generally used.
Therefore, it is necessary to take the utmost care for the installation site and handling.
Please observe strictly to each precaution described in this manual as well as the precautions
listed below.

1. Ventilation
The flammable gases used for the atomic absorption spectrophotometer are liable to
catch fire. 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
Be sure to prepare a ventilation duct above the atomic absorption spectrophotometer
so as to exhaust the combustion gas from the burner.

4. Condensation
Avoid using the equipment in the condition where condensation may occur. The
equipment may not work properly.

5. Power requirements
The allowable voltage range and consumption power of the atomic absorption
spectrophotometer and each attachment are shown as below. Be sure to connect them
to the power sources, which are suitable to these.

AA-6300 main unit

Voltage: AC100, 120, 230V
Allowable voltage range: ±10%
Power capacity: 230VA
Source frequency: 50/60Hz
Connections: Grounded outlet
Fuse used: 5A TYPE T 2pcs

VI
 6. High temperature burner
When using a nitrous oxide-acetylene flame, be sure to use the high temperature
burner.

7. Standard analytical conditions

The standard analytical conditions may be changed with the surrounding temperature
and humidity, replacement of the atomizer chamber and graphite tube, and sample
solution characteristics. Before starting the measurement, search the optimum
analytical conditions for each element while varying the gas flow rate in the case of
flame method and the temperature program in the case of furnace method.

8. Internal repair and maintenance

Since the ordinary maintenance can be performed without removing the main unit
cover, do not remove the unit cover. Also, don't exchange the fuses. If the repair,
which requires removing the cover, is necessary, ask it for Shimadzu Representative.

9. Gas supply hoses

Whenever using the equipment, check the gas supply rubber hoses for a crack or
deterioration caused by adhesive chemicals. If a crack or deterioration is found,
replace it with a new hose.

10. Lightening surge from the power source line

When a momentary large voltage change is given to the instrument from the power
source during using the instrument, the communication with PC is disconnected
because some function is stopped to protect the instrument.
In this case, once turn off the power of the main unit then turn on the power again and
connect it to the PC again. Then the preparation for restarting the measurement is
ready. If the instrument does not work properly when powered on, contact your
Shimadzu representative.

11. Cleaning the instrument

When cleaning your instrument, wipe off the outer cover and other portions with a dry
soft cloth. For details of cleaning method for component parts, refer to the Chapter “8
Maintenance”.

VII
 Warning Marking on the Equipment
WARNING
EXTREMELY HOT/OPEN FLAME
Avoid Burns
: Check for open flame through the flame shield window.
: Allow the burner head and walls to cool before handling.
Label, WARNING

Fig. 1

WARNING
HAZARDOUS VOLTAGE

DO NOT touch the electrodes while the instrument is active.

Label, WARNING

Fig. 2

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 WARNING
HOT SURFACE

Allow the lamp to cool to room temperature before replacement.

Label, WARNING

Fig. 3

WARNING
FLAMMABLE GAS

BE SURE TO READ the part “Igniting and Extinguish the flame” in the instruction manual
before ignition.

Label, WARNING

Fig. 4

IX
 WARNING
EXPLOSION POTENTIAL

DO NOT remove the nebulizer from the chamber during combustion.

Label, WARNING

Fig. 5

WARNING
EXPLOSION POTENTIAL

DO NOT use oxygen gas mixture.

Label, WARNING

Fig. 6

X
 Emergency Action

Take the following actions in case of emergency or when an abnormal condition is found in
the atomic absorption spectrophotometer.
Inspect the equipment before using it again and contact a service engineer if necessary.

Emergency Action
1. Turn OFF the power switch of the atomic absorption spectrophotometer.
2. Turn OFF all the power switches of accessories.
3. Close the main valves of the gas supply pipings for acetylene, air and nitrous
oxide.
4. Close the main valve of the cooling water and argon supply piping.
5. Shut OFF the power supply.
・Turn OFF the switchboard when the power cable is fixed to the switchboard
with screws.
・Disconnect the power cable when the power cable is connected with the plug.

Power switch Power cable

Fig. 7 Power Switch and Power Cable of Atomic Absorption Spectrophotometer

XI
 Inspection Procedure in Case of Flashback

Since the AA-6300 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
the following inspection procedure. Never ignite the flame before the safety is conformed as
the result of the inspection.

Cover fixing screw

Fig. 8 Burner Unit

(1) Remove the burner head ①. Note that the burner head is still hot just after the
flame is extinguished.
(2) Loosen the cover fixing screw (4 positions) and remove the chamber cover ③.
(3) If the safety bung ④ is released, check that the O-ring ⑤ of the safety valve is
not cracked or deteriorated then push the safety bung into the chamber unit ②.
Even if the safety bung is not released, push the safety bung and check that it is
properly mounted to the chamber.
(4) Check that the drain tube ⑦ is not damaged.
(5) Loosen the lock screw ⑨ on the nebulizer retaining plate ⑧ and then take out the
nebulizer ⑩.
(6) Check that the ceramic ball ⑭ in the spray assembly is not damaged.

XII
 (7) Check that the mixer ⑪ in the chamber is not damaged.
(8) Check that the O-ring ⑫ 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.
(9) Fix the nebulizer firmly with the retaining plate.
(10) Check that the gas tube ⑬ connected with the chamber is not damaged.
(11) Insert the gas tube connected with the quick-connect joint ⑭ and check that it is
not disconnected by pulling it.
(12) Mount the chamber cover and fix it firmly with the screws.
(13) Check that burner head slot is not clogged, if clogged, clean the burner head.
(14) Check that the O-rings ⑯ of the burner head fixing port ⑮ are not cracked or
deteriorated. Then mount the burner head to the port.
(15) When checking the drain sensor, start up the AA unit and WizAArd software
beforehand. Remove the drain tank ⑰ lid and take out the liquid level sensor ⑱
from the drain tank. Check that an error message appears on the PC screen.
Finally put the liquid level sensor back into the drain tank and close the lid.

Chamber

Drain tube

Drain container

Fig. 9 Drain Tank

XIII
 General Precautions

In order to use the atomic absorption spectrophotometer safely, be sure to observe the
following cautions. If not observed, the safety of this equipment may be compromised.

WARNING

1. When pressing the ignition button (at igniting), never put your face or
hands in the burner compartment (combustion chamber). Do not look into
from above the combustion chamber and do not hold your hands over the
combustion chamber.
When N2O-C2H2 flame is ignited, the flame goes up to the level of
approx.40cm from the top of the equipment. Care should be taken.
Before igniting a flame, be sure to close the flame shield (combustion
chamber door).
2. Do not ignite a flame unless the burner is mounted to the chamber.
3. Do not ignite a flame 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 a flame when the drain tube is removed from the chamber.
6. Do not remove the nebulizer from the chamber during combustion.
7. Do not remove the drain tube from the chamber during combustion.
8. Do not remove the burner during combustion.
9. Do not touch the burner while it is hot.
10. Do not touch the deuterium lamp while it is hot.
11. Do not touch the end of cleaning wire for nebulizer capillary directly by
hand. Wire may stick your finger.
12. Do not touch the flame shield during combustion. It is very hot by the heat
of flame and dangerous.
13. 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.

XIV
 CAUTION

1. Do not use the flame for other purpose than analysis.

2. Do not hold any substance over the flame.
3. Do not remove the chimney (funnel) when using the atomic absorption
spectrophotometer in flame method. If the chimney (funnel) is removed,
heat of flame is introduced to the instrument inside and measurement may
be unreliable.
4. Check the setting of gas flow rate before igniting a flame.
5. Do not use the standard burner (10 cm slot burner) when the recognizing
key is still left in the hole of the burner select sensor (BURNER SELECT).
6. Do not put any foreign objects in the hole of the burner select sensor.
7. Do not put any foreign objects in the lamp socket.
8. Do not connect the power cable to the outlet that is not provided with
grounding terminals.
9. Do not put your fingers or hands in the hold of lamp turret, igniter and
flame monitor.

Moving or Transporting the AA-6300

To move or transport the installed AA-6300, contact our sales office or representative.
If the AA-6300 is move or transported without the above contact, the warranty will not be
applied to any failure.

Warning on Sample to Be Measured

Do not measure any explosive sample.

Such measurement not only could cause a failure in or damage to the AA-6300, but also
might endanger the user's safety.

XV
 CONTENTS

Chapter 1 Overview

1.1 Overview of AA-6300 ........................................................................................1-1

1.2 Specifications......................................................................................................1-2

Chapter 2 Installation

2.1 Parts Inspection (AA-6300 Standard Parts)........................................................2-1

2.2 Instrument Placement and Site Requirements ....................................................2-4
2.3 Equipment Requirements....................................................................................2-7
2.3.1 Power Requirements................................................................................................ 2-7
2.3.2 Water Supply Requirements .................................................................................... 2-7
2.3.3 Gas Requirements.................................................................................................... 2-8
2.3.4 Ventilation System ................................................................................................. 2-10
2.3.5 Use of an Air Compressor...................................................................................... 2-11
2.3.6 General Precautions for Handling Gas Cylinders.................................................. 2-13
2.3.7 Installing Pressure Regulators (Optional) and Checking for Leaks....................... 2-14
2.3.8 Software Operation Minimum Requirements (provided by user) ......................... 2-16
2.4 Assembling the AA-6300 .................................................................................2-17
2.4.1 Connecting the Drain Tube.................................................................................... 2-17
2.4.2 Assembling the Burner .......................................................................................... 2-18
2.4.3 Cable Connections ................................................................................................. 2-19
2.4.4 Hose Connections .................................................................................................. 2-20
2.4.5 Replacing the Atomizer ......................................................................................... 2-22
2.4.6 Installation of PC software .................................................................................... 2-24
2.5 Mounting a Hollow Cathode Lamp ..................................................................2-25

Chapter 3 Instrument Constructions

3.1 AA-6300 Configurations ....................................................................................3-1

3.1.1 Operation Switches.................................................................................................. 3-1
3.1.2 Hollow Cathode Lamp Turret.................................................................................. 3-2
3.1.3 Deuterium Lamp...................................................................................................... 3-3
3.1.4 Burner Module......................................................................................................... 3-4
3.1.5 Burner ...................................................................................................................... 3-5

i
 3.1.6 Optical System......................................................................................................... 3-7
3.1.7 Photometric System ................................................................................................. 3-8

Chapter 4 Basic Operration

4.1 Switching On the Power and Starting Up the Software .....................................4-1

4.1.1 Switching ON the Power to Hardware .................................................................... 4-1
4.1.2 Starting Up the Software ......................................................................................... 4-3
4.2 Software Basic Operation ...................................................................................4-4
4.2.1 Software Basic Operation (Flame Continuous Method).......................................... 4-4
4.2.1.1 Operation Flowchart (Flame Continuous Method) ....................................... 4-4
4.2.1.2 Logging in WizAArd..................................................................................... 4-5
4.2.1.3 Wizard Selection ........................................................................................... 4-5
4.2.1.4 Element Selection.......................................................................................... 4-6
4.2.1.5 Preparation Parameters................................................................................ 4-10
4.2.1.6 Connect to Instrument/Send Parameters ..................................................... 4-17
4.2.1.7 Initializing the instrument ........................................................................... 4-18
4.2.1.8 Instrument Check List for Flame Analysis.................................................. 4-19
4.2.1.9 Optics Parameters........................................................................................ 4-20
4.2.1.10 Atomizer/Gas Flow Rate Setup................................................................. 4-22
4.2.2 Software Basic Operation (Flame Micro Sampling Method) ................................ 4-24
4.2.2.1 Operation Flowchart (Flame Micro Sampling Method).............................. 4-24
4.2.2.2 Logging in WizAArd................................................................................... 4-25
4.2.2.3 Wizard Selection ......................................................................................... 4-25
4.2.2.4 Element Selection........................................................................................ 4-26
4.2.2.5 Preparation Parameters................................................................................ 4-31
4.2.2.6 Connect to Instrument/Send Parameters ..................................................... 4-40
4.2.2.7 Initializing the instrument ........................................................................... 4-41
4.2.2.8 Instrument Check List for Flame Analysis.................................................. 4-42
4.2.2.9 Optics Parameters........................................................................................ 4-43
4.2.2.10 Atomizer/Gas Flow Rate Setup................................................................. 4-45
4.2.3 Software Basic Operation (Furnace Method) ........................................................ 4-47
4.2.3.1 Operation Flowchart (Furnace Method)...................................................... 4-47
4.2.3.2 Logging in WizAArd................................................................................... 4-48
4.2.3.3 Wizard Selection ......................................................................................... 4-48
4.2.3.4 Element Selection........................................................................................ 4-49
4.2.3.5 Preparation Parameters................................................................................ 4-54
4.2.3.6 Connect to Instrument/Send Parameters page............................................. 4-64

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 4.2.3.7 Initializing the instrument ........................................................................... 4-65
4.2.3.8 Bypass the Instrument Check List for Flame Analysis ............................... 4-66
4.2.3.9 Optics Parameters........................................................................................ 4-67
4.2.3.10 Furnace Program ....................................................................................... 4-69
4.3 Saving the Template..........................................................................................4-72
4.4 Measurement Procedures..................................................................................4-73
4.4.1 Measurement Operation (for Flame Method)........................................................ 4-74
4.4.2 Measurement Operation (for Furnace Method) ..................................................... 4-77
4.4.3 Completing the Measurement................................................................................ 4-78
4.5 Saving and Printing the Data ............................................................................4-79
4.5.1 Saving the Data...................................................................................................... 4-79
4.5.2 Printing the Data .................................................................................................... 4-80
4.6 Explanation of Main Window...........................................................................4-82
4.6.1 Menu bar................................................................................................................ 4-83
4.6.2 Standard tool bar.................................................................................................... 4-83
4.6.3 Measurement element tool bar............................................................................... 4-84
4.6.4 Absorbance digital display .................................................................................... 4-84
4.6.5 Real time graph (and furnace program graph)....................................................... 4-85
4.6.6 Peak Profile (Latest four measurements and overlay display)............................... 4-87
4.6.7 Calibration Curve Display ..................................................................................... 4-89
4.6.8 MRT work sheet .................................................................................................... 4-93
4.6.9 Function buttons .................................................................................................... 4-94
4.6.10 Status bar ............................................................................................................. 4-96
4.7 Operating the MRT work sheet.........................................................................4-97
4.7.1 Fields of MRT work sheet ..................................................................................... 4-98
4.7.2 Right Mouse Button Menu .................................................................................. 4-105
4.7.3 Right Mouse Button on Summary Table ............................................................. 4-110
4.7.4 Inserting and Deleting the Measurement Row .................................................... 4-110
4.7.5 Active Cell Movement by Shortcut Key and Cell Selection ............................... 4-111
4.7.5.1 Moving an Active Cell .............................................................................. 4-111
4.7.5.2 Selecting Cells........................................................................................... 4-111
4.7.6 Copy and Paste .................................................................................................... 4-112
4.7.6.1 Copy .......................................................................................................... 4-112
4.7.6.2 Paste .......................................................................................................... 4-113
4.7.7 Changing Column Width and Column Header Height of MRT Worksheet......... 4-114
4.8 Igniting and Extinguishing the Flame............................................................. 4-115
4.8.1 Operation Locations ............................................................................................ 4-115
4.8.2 Safety Precautions Prior to Ignition..................................................................... 4-115

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 4.8.3 Igniting and Extinguishing Air-C2H2 flame ....................................................... 4-116
4.8.4 Igniting and Extinguishing N2O-C2H2 flame..................................................... 4-118
4.8.5 Flame Conditions When Analyzing Organic Solvent Samples ........................... 4-121
4.9 Standard Addition Method and Simple Standard Addition Method ...............4-122
4.9.1 Setting the “Preparation Parameters” page......................................................... 4-123
4.9.2 Measurement Procedures on MRT worksheet ..................................................... 4-128
4.10 Conditions and Operation for Flame Emission Analysis..............................4-130
4.10.1 “Optics Parameters” Page.................................................................................. 4-130
4.10.2 “Atomizer/Gas Flow Rate Setup” Page............................................................. 4-133
4.10.3 Line Search and Beam Balance ......................................................................... 4-135
4.11 Specifying Optimal Conditions for Flame....................................................4-136
4.11.1 Setting the Optimum Condition of Burner Height............................................. 4-137
4.11.2 Setting the Optimum Condition of Fuel Gas Flow Rate.................................... 4-138

Chapter 5 User Administration

5.1 GxP Support Functions.......................................................................................5-1

5.1.1 Overview of GxP Support Functions....................................................................... 5-1
5.1.1.1 What is GLP/GMP? ...................................................................................... 5-1
5.1.1.2 What is FDA 21 CFR Part 11? ...................................................................... 5-1
5.1.2 GxP Support Functions............................................................................................ 5-2
5.2 System Administration........................................................................................5-4
5.2.1 Reviewing System Administration .......................................................................... 5-4
5.2.1.1 What is System Administration? ................................................................... 5-4
5.2.1.2 System Administration Application............................................................... 5-7
5.2.1.3 System Administration Flow ......................................................................... 5-8
5.2.1.4 Designing a System Administration Policy................................................... 5-8
5.2.2 Using the System Administration Tools to Set Available Items ............................ 5-11
5.2.3 Starting the System Operation ............................................................................... 5-13
5.2.3.1 Setting User Administration Policies .......................................................... 5-13
5.2.3.2 Registering (Changing/Deleting) Rights Groups ........................................ 5-17
5.2.4 Registering (Changing/Deleting) Users................................................................. 5-19
5.2.5 Short Time after System Operation Has Been Started........................................... 5-22
5.2.5.1 Viewing the History of System Administration........................................... 5-22
5.2.5.2 Changing Passwords ................................................................................... 5-24
5.3 Using the Security Support Functions ..............................................................5-26
5.3.1 Login Authentication ............................................................................................. 5-26
5.3.2 Current User Display ............................................................................................. 5-28
5.3.3 Restricting the Operations according to User Rights............................................. 5-28
5.3.4 Protecting an Analytical Task by Locking the Screen ........................................... 5-30

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 5.4 Audit Trail.........................................................................................................5-31
5.4.1 Referencing a Record in a Data File...................................................................... 5-31
5.4.2 Viewing the History of System Changes ............................................................... 5-32
5.5 Performing Software Validation .......................................................................5-34
5.5.1 Performing Program Checks.................................................................................. 5-34
5.5.2 Performing the Function Check............................................................................. 5-36
5.6 Data Administration..........................................................................................5-37
5.6.1 Reviewing the Long-Term Storage of Data ........................................................... 5-37
5.6.1.1 Managing the Print Images.......................................................................... 5-37
5.6.1.2 Storing a Data File for a Long Period of Time ............................................ 5-37
5.6.1.3 Devising a Data Storage Method................................................................. 5-39
5.6.1.4 Using a Print Image..................................................................................... 5-40
5.7 Other System Management Tools.....................................................................5-41
5.7.1 Performing the Maintenance of System Management Database ........................... 5-41
5.7.1.1 Using the Database Maintenance Tool ........................................................ 5-41
5.7.2 Managing the System on the Network................................................................... 5-43
5.7.2.1 Using Shimadzu User Authentication Tool on the Network ....................... 5-43
5.7.2.2 Using the Maintenance of Instrument Information Tool ............................. 5-44

Chapter 6 QA/QC Setup

6.1 What is QA/QC?.................................................................................................6-1

6.1.1 Overview of QA/QC................................................................................................ 6-2
6.2 QA/QC Check Items and Their Settings.............................................................6-3
6.2.1 Calibrating the instrument (creating a calibration curve) ........................................ 6-4
6.2.2 ICV and ICB ............................................................................................................ 6-7
6.2.3 CCV and CCB ......................................................................................................... 6-8
6.2.4 CRA (CRDL for AA)............................................................................................... 6-9
6.2.5 PB (Preparation Blank).......................................................................................... 6-10
6.2.6 LCS (Laboratory Control Samples)....................................................................... 6-12
6.2.7 S (Spike: Spike test) .............................................................................................. 6-13
6.2.8 D (Duplicate Sample Analysis) ............................................................................. 6-15
6.2.9 IDL (Instrument Detection Limit Determination) ................................................. 6-16

Chapter 7 Hardware Validation

7.1 Hardware Validation ...........................................................................................7-1

7.2 Necessary Items ..................................................................................................7-1
7.3 Outline of Standard Test Item .............................................................................7-2

v
 7.3.1 Wavelength accuracy ............................................................................................... 7-2
7.3.2 Noise level ............................................................................................................... 7-2
7.3.3 Baseline drift............................................................................................................ 7-3
7.3.4 Absorbance and repeatability (In the case of flame analysis).................................. 7-3
7.3.5 Detection limit (In the case of flame analysis) ........................................................ 7-3
7.3.6 Stability (In the case of flame analysis)................................................................... 7-4
7.3.7 Absorbance and repeatability (In the case of furnace analysis)............................... 7-4
7.3.8 Detection limit (in the case of furnace analysis) .................................................... 7-4
7.4 Basic Operation Procedures................................................................................7-6
7.4.1 Preparation............................................................................................................... 7-6
7.4.1.1 Preparation of hollow cathode lamp.............................................................. 7-6
7.4.1.2 Sample preparation........................................................................................ 7-7
7.4.2 Selecting the test items ............................................................................................ 7-8
7.4.3 Setting the ASC parameters ................................................................................... 7-11
7.4.4 Setting the warm-uptime of lamps and stabilization time for flame...................... 7-12
7.4.5 Starting the test ...................................................................................................... 7-13
7.4.6 Items with sample measurement............................................................................ 7-16
7.4.7 Stop the test............................................................................................................ 7-17
7.4.8 Print the check result ............................................................................................. 7-17
7.4.9 Saving and Loading the data.................................................................................. 7-18
7.5 Parameter change..............................................................................................7-19
7.5.1 Entering the parameter change screen ................................................................... 7-19
7.5.2 Setting the test parameters ..................................................................................... 7-20
7.5.3 Setting the scale for graph display/output of each data ......................................... 7-22
7.5.4 Saving/loading the parameters............................................................................... 7-23
7.5.4.1 When saved as the individual validation file............................................... 7-23
7.5.4.2 When saved as the auto load validation file ................................................ 7-24
7.6 Functions of operation menu ............................................................................7-25
7.6.1 Main screen............................................................................................................ 7-25
7.6.2 File ......................................................................................................................... 7-27
7.6.2.1 New ............................................................................................................. 7-27
7.6.2.2 Open ............................................................................................................ 7-27
7.6.2.3 Save ............................................................................................................. 7-27
7.6.2.4 Save As........................................................................................................ 7-27
7.6.2.5 Print Summary Report................................................................................. 7-27
7.6.2.6 Print Measured Data.................................................................................... 7-27
7.6.2.7 Print Setup ................................................................................................... 7-28
7.6.2.8 File history................................................................................................... 7-28

vi
 7.6.2.9 Exit .............................................................................................................. 7-28
7.6.3 Tests ....................................................................................................................... 7-29
7.6.3.1 Modify Batch............................................................................................... 7-29
7.6.3.2 Set Parameters ............................................................................................. 7-29
7.6.4 Configuration......................................................................................................... 7-30
7.6.4.1 Connect Spectrophotometer ........................................................................ 7-30
7.6.4.2 Check Accessories....................................................................................... 7-30
7.6.4.3 Instrument Settings...................................................................................... 7-30
7.6.4.4 Warm-up Time............................................................................................. 7-30
7.6.4.5 ASC Parameters .......................................................................................... 7-30
7.6.5 Perform .................................................................................................................. 7-31
7.6.5.1 Start ............................................................................................................. 7-31
7.6.5.2 Stop.............................................................................................................. 7-31
7.6.6 Graph ..................................................................................................................... 7-32
7.6.6.1 Set Limits .................................................................................................... 7-32
7.6.6.2 Set Y Axis in Each Test ............................................................................... 7-32
7.7 Performance Specifications ..............................................................................7-33

Chapter 8 Maintenance

8.1 Atomizer Positioning Adjustment.......................................................................8-1

8.1.1 Burner Positioning Adjustment................................................................................ 8-1
8.1.2 Furnace Position Adjustment................................................................................... 8-3
8.2 Burner Maintenance............................................................................................8-4
8.2.1 Cleaning the Burner Head ....................................................................................... 8-5
8.2.2 Nebulizer Maintenance............................................................................................ 8-6
8.2.2.1 Cleaning the Nebulizer.................................................................................. 8-6
8.2.2.2 Replacing the Polyethylene Tube .................................................................. 8-7
8.2.3 Cleaning the Chamber ............................................................................................. 8-8
8.3 Checking for Gas Leaks......................................................................................8-9
8.3.1 Gas leak check for outside of instrument................................................................. 8-9
8.3.2 Gas leak check for inside of instrument................................................................. 8-10
8.4 Replacing the Deuterium Lamp........................................................................8-12
8.4.1 Specifications of Deuterium Lamp ........................................................................ 8-12
8.4.2 Replacing Procedures of Deuterium Lamp............................................................ 8-13
8.5 Maintenance Parts.............................................................................................8-15
8.5.1 AA-6300 Maintenance Parts.................................................................................. 8-15
8.6 Special Accessories...........................................................................................8-16
8.6.1 For Flame Analysis ................................................................................................ 8-16

vii
 8.6.2 For Furnace Analysis (for GFA-EX7i) .................................................................. 8-16
8.6.3 Autosampler........................................................................................................... 8-16
8.6.4 Hollow Cathode Lamps (Single Element Lamps) ................................................. 8-17
8.6.5 Hollow Cathode Lamps (Single element lamps, Usable for SR method).............. 8-19
8.6.6 Hollow Cathode Lamp (Multi-element Lamps) .................................................... 8-20
8.6.7 Other Accessories .................................................................................................. 8-20

Chapter 9 Appendix

9.1 Measurement Conditions Table for Flame Atomic Absorption Analysis .........9-1
9.2 Analysis Line Wavelength Table for Flame Emission Analysis .......................9-4
9.3 Graphite Tube Type Selection in Furnace Method ...........................................9-5
9.3.1 When Using a High Density Graphite Tube .......................................................... 9-6
9.3.2 When Using a Pyrolytic Coated Graphite Tube ..................................................... 9-6
9.3.3 When Using the Platform Type Tube .................................................................... 9-6
9.4 Error Messages .................................................................................................9-9

viii
 Chapter 1 Contents

Chapter 1 Overview

Contents

1.1 Overview of AA-6300................................................................1-1

1.2 Specifications .............................................................................1-2

AA-6300
 1.1 Overview of AA-6300

1.1 Overview of AA-6300

The Atomic Absorption Spectrophotometer AA-6300 incorporates two background

correction functions, the D2 method (Deuterium Lamp method) and the SR method
(Self-Reversal method), enabling selection of the appropriate method for the measurement
sample.
The AA-6300 allows you to change the measurement mode while simply switching the
atomizer, thus enabling quick and easy switching back and forth between flame measurement
and furnace measurement. In addition, wide ranging measurement operations are available,
from manual operation to automatic continuous measurement of multi-elements with the use
of an auto sampler. This enables selection of the appropriate combination to match the number
of elements and samples to be analyzed as well as the skill of the operator.
The PC software controlling the AA-6300 operates on the Windows 2000TM, and using the
Wizard for parameter setting enables an operator, even a beginner of atomic absorption
spectrophotometer, to make measurement conditions easily. In addition, the hardware
validation function is available as standard to allow you to check the performance of the
AA-6300. This function is applicable to the system suitability management for IQ/OQ or the
like.

AA-6300 1-1
Chapter 1 Overview

1.2 Specifications

AA-6300 Basic Specifications

Measurement Wavelength Range
Monochrometer
Bandwidth
Detector
Photometric Method
Measurement
System
Background Correction
Number of Lamp Sockets
Lamp Mode
Data Software Environment
Processing Parameter Setting
Measurement Mode
Concentration Conversion Mode
Repeat Measurement
Baseline Correction
Peak data processing range
Sensitivity Correction
Table Data Processing Functions
Loading Parameters
Procedure/Result Display
Result Print
185~900nm
Aberration-corrected Czerny-Turner mount
0.2, 0.7, 0.7L, 2.0L nm (4-step automatic switching)
Photo multiplier (185.0nm-600.0nm),
semiconductor (600.1nm-900.0nm)
Frame: Optical double beam
Furnace: Electrical double beam
High-speed self reversal method (BGC-SR), Optional
PMT (R787-04) is required in the range greater than
600.0nm.
High-speed deuterium lamp method (BGC-D2)
6 lamp sockets, 2 lamps simultaneously lit (1 for
warming up)
EMISSION, NON-BGC, BGC-SR, BGC-D2
Microsoft Windows 2000
Wizard Method
Flame continuous method, Flame micro sampling
method, Furnace method
・Calibration Curve (selectable among 1st, 2nd, 3rd
order function)
・Standard addition method/Simple standard addition
method (1st order function)
・Max. 20 repetitions
・Indication of Average, Standard deviation (SD) and
Relative Standard Deviation (RSD)
・Exclusion of deviant value based on SD value and
RSD value
Automatic correction of base line drift using offset
correction with peak height and peak area mode
Peak data processing range can be changed with peak
height and peak area mode.
Automatic calibration curve correction function by
sensitivity observation
Actual concentration calculation using Weight factor,
Dilution factor, Volume factor and Correction factor.
Template function
MRT Work Sheet (MRT: Measurement Result Table)
Summary Report

1-2
 1.2 Specifications

Correlation factor, %RSD, ICV/ICB, CCV/CCB, PB,

LCS, SPK, PDS, DUP
QA/QC
Pause or Mark&Continue is selected by these QA/QC
checks.
Retry/Not retry can be selected.
Automatic dilution re-measurement of unknown sample
Re-measurement
by the auto sampler (Flame micro sampling method,
Furnace method)
・User administration by login ID/password
・Limitation of assigned rights with user level
Electronic records and electric
・Recording of log
signatures
・Audit trail
・Electronic signatures
AC100, 120, 230V selectable, 230VA, 50/60Hz
Power Requirements
Additional power for personal computer is necessary.
W835× D545 × H460mm, 70kg
Dimensions, Weight
(not including funnel and protrusions)
10°C～35°C, 20%～80%
Ambient Temperature and Humidity Range
(less than 70% if temperature is over 30°C)

Flame Specifications
Type Air-cooled pre-mix type
10cm slot made of Titanium (5cm slot made of Titanium for
Burner Head
N2O-C2H2 frame is optional item.)
Pt-Ir capillary
Nebulizer Teflon orifice
Burner Unit
Impact bead made of Ceramic (Fluoric acid is usable.)
Chamber Polypropylene
Manual adjustment for back-fore position
Positioning Automatic adjustment for up-down position
Automatic searching for optimum burner height
Automatic flow rate setting for fuel gas and support gas (0.1 L/min
Flow Rate Control increments)
Automatic searching for optimum gas flow rate
・ Air/N2O auto switching with C2H2 flow rate monitor (optical
sensor)
Gas Controller ・ Flame monitor
・ Prevents usage of incorrect burner head
Safety Features
・ Gas pressure monitor
・ Drain water level monitor
・ Safety extinction by automatic detection of momentary power
failure

AA-6300 1-3
Chapter 1 Overview

Furnace Specifications
Heating Temperature Range Ambient～3000°C
・ Drying: Current control method
Heating Control Method
・ Ashing/Atomizing: Optical temperature control method
・ Max. 20 stages
・ Heating mode: RAMP/STEP
・ Inner gas type: 2-line switching
Heating Parameter settings ・ High sensitivity setting
・ Furnace concentration boost cycle: Max 20 times
・ Optimum furnace program search function
・ Inner gas flow rate: 0～1.5 L/min
・ Cooling water flow rate monitor
・ Gas pressure monitor
Safety Features
・ Over current protection (double check by breaker and optical sensor)
・ Furnace block cooling check

1-4
 Chapter 2 Contents

Chapter 2 Installation

Contents

2.1 Parts Inspection (AA-6300 Standard Parts)................................2-1

2.2 Instrument Placement and Site Requirements ............................2-4
2.3 Equipment Requirements ...........................................................2-7
2.3.1 Power Requirements............................................................................2-7
2.3.2 Water Supply Requirements ................................................................2-7
2.3.3 Gas Requirements................................................................................2-8
2.3.4 Ventilation System.............................................................................2-10
2.3.5 Use of an Air Compressor .................................................................2-11
2.3.6 General Precautions for Handling Gas Cylinders..............................2-13
2.3.7 Installing Pressure Regulators (Optional) and Checking for Leaks...2-14
2.3.8 Software Operation Minimum Requirements (provided by user) .....2-16
2.4 Assembling the AA-6300 .........................................................2-17
2.4.1 Connecting the Drain Tube................................................................2-17
2.4.2 Assembling the Burner ......................................................................2-18
2.4.3 Cable Connections.............................................................................2-19
2.4.4 Hose Connections..............................................................................2-20
2.4.5 Replacing the Atomizer .....................................................................2-22
2.4.6 Installation of PC software ................................................................2-24
2.5 Mounting a Hollow Cathode Lamp ..........................................2-25

AA-6300
 2.1 Parts Inspection

2.1 Parts Inspection (AA-6300 Standard Parts)

CAUTION
Since this instrument is installed and adjusted by person dispatched by
Shimadzu, stay and check it together.
Read and strictly observe the sections 2.2 and 2.3 to maintain the
instrument stability, to obtain the high reliability of analysis result and to use
this instrument for a long time.

Check the standard accessories referring to Table 2.1 and Fig. 2.1.
If any parts are missing or damaged, please contact your Shimadzu Representative.

AA-6300 2-1
Chapter 2 Installation

Table 2.1 Standard Accessories (AA-6300)

Item No. Parts Name Qty. Part No
1 Spectrophotometer Main Unit 1
2 Standard Accessories
2-1 Hose ASSY (for Air) 1 206-50389-91
2-2 Hose ASSY (for Acetylene) 1 206-50389-92
2-3 Cord set 1 071-60824-01
2-4 Cleaning wire 1 201-79229-01
2-5 Hose clamp, 16MM 2 037-61019
2-6 Seal joint ASSY 1 206-52039-91
2-7 Sampling tube (Teflon made) 2 204-05899-01
2-8 Sampling tube (for organic solvent sample) 1 206-50772-91
2-9 Polyethylene capillary, No. 3 500mm 200-31328-01
2-10 Drain ASSY 1 206-52033-91
2-11 PE tube, 8x1 (for drain tube) 2400mm 016-43206
2-12 Wrench, hexagonal 3 1 086-03804
2-13 Card (10 sheets) 1 206-52046-91
2-14 Grease in cup 1 206-50442-91
2-15 Funnel ASSY 1 206-52021-91
2-16 Cable, RS-232C, 9P (1) (206-50325-91)
2-17 CD-ROM, WizAArd (1) (206-52062-91)
3 Instruction manual, AA-6300E 1 206-94935
4 Inspection test report 1 206-94990
5 Certificate of compliance for ISO-9001 QA system 1 206-84934-57
6 Packing list (This document) 1 206-94992

NOTE
The hollow cathode lamps, high temperature burner head, pressure
regulator and compressor are not included in the standard accessories.

2-2
 2.1 Parts Inspection

Fig. 2.1 Standard Accessories (AA-6300)

NOTE
The instruction manual and other document sheets are not shown in the
above figure.

AA-6300 2-3
Chapter 2 Installation

2.2 Instrument Placement and Site Requirements

The instrument components are positioned as shown in Fig. 2.2.

In addition to this, the installation site for personal computer and printer is necessary.
(1) The installation site should be:
(a) Sufficiently distant from devices that generate strong magnetic and electrical fields
and high frequency
(b) Sufficiently ventilated
(c) Free from vibration
(d) Free from excessive dust and moisture and should not be exposed to corrosive gases
(e) The luminous intensity of installation site for this instrument should be below
1300Lx in the case of fluorescent lamp, below 800Lx in the case of indirect outdoor
daylight, and below 400Lx in the case of heat light source like incandescent lamp.

NOTE
The AA-6300 series are equipped with the safety system using an optical
sensor. When installing the instrument near a window, make sure that it is
not exposed to strong outdoor daylight. Exposure to strong outdoor daylight
may interfere with normal operation of the flame extinction safety system for
monitoring flame combustion (Flame Monitor). When using incandescent
lamp or other heat light sources near the main unit, select the installation
site where the luminous intensity by the light source only is below 400Lx. If
not available, don’t allow the direct light from the light source to come into
the burner compartment.

(f) Ambient temperature range: 10 to 35°C

Humidity: 20 to 80% (but less than 70% if temperature is over 30°C)

NOTE
If the temperature changes by 1°C, the absorbance may change by 0.010
Abs maximum. To carry out such long-hour measurement as may be
affected by temperature changes, execute AUTO ZERO during the
measurement if necessary.
In the case of manual flame measurement (not using ASC), you can
execute AUTO ZERO at any time by clicking on <AUTO ZERO> button on
the left lower of the main window. In the case of automatic flame

2-4
 2.2 Instrument Placement and Site Requirements

measurement (using ASC), if set “AUTO ZERO” or “RINCE” in [Action] field

on the MRT work sheet, AUTO ZERO can be executed during the nozzle
rinsing. In the case of furnace measurement, setting is not necessary
because the instrument automatically execute AUTO ZERO just before
measurement.

(g) Ground is available.

(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-6300 70kg
GFA-EX7i 44kg
ASC-6100F+ASK-6100+ASK-6300 15kg
(3) Since gas and water pipes cables are connected at the back of the AA main unit,
there must be a space of about 15 to 20cm from the back of the AA main unit to a
wall.

(4) Install the personal computer with a clearance of about 15 to 20 cm from the left or
right side of the AA-6300 so that the HCL cover on the right side of the AA-6300
can be opened/closed and that the connectors can be connected to the left side of the
AA-6300.

AA-6300 2-5