AA500 User Manual
AA500 User Manual
AA500 User Manual
Analytical
Instruments
for
Science
AA500 Operation Instruction Manual
Warning labels:
Note: There are a number of warning labels attached to the instrument. Please take
notice of them.
Acetylene gas:
z Always use the correct regulator valve for the acetylene gas. Do not use pipes
made from copper, silver, mercury or their alloys in order to prevent the formation of
metal-acetylides, which could break down the pipe under the pressure.
z The acetylene gas cylinder contains dissolvable substance such as acetone. If the
primary pressure falls below 70psi, it should be replaced with a new cylinder in
order to prevent the diffuseness of the dissolvable substance.
Nitrous Oxide:
z Nitrous oxide is a colorless and sweet-tasting gas which is used to support the
acetylene flame. It is stable at normal atmospheric temperature and can be
dissolved with water, alcohol and high concentration Sulphuric Acid. Always use
adequate ventilation due of the anesthesia effect of the gas.
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AA500 Operation Instruction Manual
Oxygen:
z Oxygen should never be used.
Air:
z This should be dry and free from oil. A moisture or oil trap on the exit tube can be
installed
.
After using:
z Always turn off the gasses after using the gas instrument
.
Regulator valve:
z Periodically inspect the pressure gauges for leaks or problems
.
Pressure adjustment:
z Before installing the regulator valve, always make sure that the gas cylinder exit
tube and valve are clean and free from dirt or grease.
z The leaking of gas at the cylinder may be caused by incorrectly fitting of the
regulator valve. Do not try to install by force, replace with a new cylinder if this
situation is occurs.
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AA500 Operation Instruction Manual
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AA500 Operation Instruction Manual
z Carry out a leak check periodically before ignition. Do not ignite flame if there is a
gas leak.
z The regulator valve model is JYT-0.6, the output pressure is 2.8±0.5KPa; the
output pressure for the other model is 5KPa.
Argon cylinder:
z Carry out a leak check periodically before ignition. Do not use if there is a gas leak.
z Pay attention to the cylinder pressure when using argon, Replace the cylinder if the
pressure is lower than 70psi.
Pressure monitoring:
The flame will not operate if the pressure of air, nitrous oxide and acetylene is too high
or too low. The graphite furnace atomizer will not work if the pressure of argon is too low
or too high.
Flame monitoring:
If the flame extinguish abnormally, the instrument will give an alarm.
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AA500 Operation Instruction Manual
Emergency switch:
Press the emergency switch and turn off the gas valve in an emergency situation.
Emergency steps:
z Turn off the power supply.
z Switch off the main valve of the acetylene, nitrous oxide, LPG and argon.
z Switch off the cooling water.
z Switch off the compressor.
General Precautions:
In order to use the instrument safely, be sure to observe the following precautions.
z Use the correct burner head for different flame mode (Air-Acetylene flame, Air-LPG
flame, Nitrous Oxide-Acetylene flame).
z Never put your face or hands in the burner compartment during ignition or with
flame on. Never look directly at the flame above the chamber or put hands over the
chamber. Close the flame shield (burner compartment door and chamber) before
igniting.
z Do not ignite flame without burner head.
z Do not ignite flame without nebulizer installed.
z Do not ignite flame if the water level is too low in the liquid trap.
z Do not remove the burner head when flame is on.
z Do not touch the burner head until cool.
z Do not touch the deuterium lamp when it is lit.
z Do not put hand in the lamp tower.
z Do not put hand over the igniter and flame monitor.
z Do not put foreign objects into the lamp holder.
z Do not remove the heat protection baffle when the AA500 flame is on.
z Please check the setting of the flow rate before ignition.
z Do not touch the flame shield when flame is on.
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AA500 Operation Instruction Manual
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AA500 Operation Instruction Manual
Contents
Chapter 1 Overview ......................................................................................10
1.1 Applications ........................................................................................................... 10
1.2 Basic working principle ........................................................................................... 11
1.3 Features .................................................................................................................11
1.4 Specifications ........................................................................................................ 12
1.5 Technical descriptions ........................................................................................... 13
1.6 Standard configuration .......................................................................................... 13
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AA500 Operation Instruction Manual
Chapter 1 Overview
Preface
1. Flame only
2. Graphite furnace only
3. Flame / graphite furnace with automatic switching.
Note: the user can operate the specific configured instrument by consulting the
corresponding paragraphs and chapters of the instruction manual.
1.1 Applications
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AA500 Operation Instruction Manual
The light source of the hollow cathode lamp radiates the characteristic spectrum of
the target element which is absorbed during the atomization process. The content of the
measured element can be calculated by measuring the absorbance of the spectrum.
1.3 Features
z Automatic setting of the fuel gas flow (Acetylene, LPG) and optimizing the gas
ratio of the combustion to the supporting gas.
z Automatically identify burner head.
z Automatic switch to Nitrous Oxide-Acetylene flame.
z Automatic setting and adjusting the burner height for selecting the optimal
analytical conditions.
z Automatic loading of the element lamp through an eight-hole multiple turret holder
and simultaneously lighting two lamps with one for warm-up;
z Automatic switchover of the atomizer between the two analytical methods: flame
and graphite furnace, when the Flame/Graphite Furnace dual-mode Atomic
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AA500 Operation Instruction Manual
1.4 Specifications
Item Specification
Wavelength range 190 - 900nm;
Type Hollow cathode lamp (HCL), D2 lamp;
Modulation mode Square wave pulse;
Light
Modulation 100Hz (Self-Reversal background correction
source
frequency mode) , 400Hz (D2 lamp background correction
mode);
Model Czerny-Turner monochromator
Optical
Chromatic/optical
dispersing Planar diffraction grating;
component
Grating 1800 grooves/mm;
Blazed wavelength 250nm;
Focus 300mm;
System
Bandwidth 0.1、0.2、0.4、1.0、2.0nm;
Scan mode Automatic;
Photometer type Single beam;
Three kinds of titanium metal burner head; rot-proof
Atomization system spray chamber,high efficiency glass nebulizer;
burner height auto-adjustable;
Data Flame method, Graphite furnace method.
Measurement
Absorbance,concentration,transmittance,emission
mode
Processing intensity;
Read-out mode Continuous,peak height, peak area;
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AA500 Operation Instruction Manual
1. Main unit:
2. Software:AAWin Pro
3. Standard accessories
4. Optional configuration:
• Auto-sampler;
• Hydride unit;
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AA500 Operation Instruction Manual
The location for the instrument should be kept away from strong electromagnetic field,
strong calorific radiation or strong light. The laboratory should be situated away from
equipment or workshop that generates strong vibrations. The instrument should be kept
away from direct sunshine, smoke, dust, dirty air current and vapor. The AAS laboratory
should be separated from any chemical treatment room. The internal environment of the
laboratory should always be kept clean with appropriate temperature (15-30°C) and
relative humidity (< 70%).
The dimensions of the main unit are 1100mm X 535mm X 540mm and the dimensions of
the graphite furnace power supply are 500 X 500mm X 450mm. The laboratory bench
should be of sufficient size to install the instrument, graphite power supply (depending on
configuration). The recommended height is 0.75 meters. The bench should be stable and
solid with a flat face. A space of at least half a meter should be left around the instrument
to facilitate the operation and maintenance.
Exhaust equipment should be installed in the laboratory (see figure 2-1)
the purity should be no less than 99.9%. The acetylene cylinder should use a
special acetylene regulator valve with a flame arrestor fitted in line.
z Argon gas: The pressure from the argon cylinder should be set to 70psi and
the purity should be no less than 99.99% purity. A special gas regulator valve is
also required.
1. After unpacking the instrument, please check items against the packing list to see
whether the main unit, accessories, parts and manuals are complete. Check the
instrument for damage to the appearance. If a problem exists, please contact your local
agent promptly.
2. Carefully read the operation manual to familiarize yourself in the operating principles,
structure of the instrument, operation and installation steps.
3. Solution requirement:
z DI water, copper standard solution 2ppm, lead standard solution 5ppm, copper
standard solution 20ppb (used for graphite furnace);
4. Installation of sample tray: loosen the screws and then install the sample tray, Tighten screws
to hold the tray firmly.
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AA500 Operation Instruction Manual
Screws
Sample tray
2.3 Installation
2.3.1 Connection
Nitrous oxide: Connect one end of the blue Nitrous Oxide gas tubing, with the
appropriate length, to the outlet of the gas valve attached to the N2O gas cylinder.
Connect the other end to the N2O inlet on the back plate of atomic absorption main unit
(See Figure 2-5).
LPG: Connect one end of the orange LPG tubing, with the appropriate length, to the
outlet of the gas valve attached to the LPG cylinder. Connect the other end to the LPG
inlet on the back plate of atomic absorption main unit (See Figure 2-5).
Waste Tubing:
• Install the liquid-level monitoring device to the rear of the instrument and plug
in the electrical cable;
• Connect the transparent tubing, which is already attached to the underside of
the instrument, to the bottom connecter of the liquid-level monitoring device.
• Connect one end of the supplied transparent tubing to the upper connecter of
the liquid-level monitoring device and the other end of the tubing to a waste
liquid container. The tubing should be long enough to be put in an open top
waste container but at no time should the tubing be immersed into the waste
liquid as this could create a back pressure in the system.
• Fill the liquid-level monitoring device with De-ionized water using a wash bottle
in the fill hole.
Note: the liquid-level monitoring device must be filled with water. Please
check the level when using the flame. (The flame will extinguish if the liquid
level is too low.)
Main gas Left Steam cylinder Right Steam cylinder External gas
Water inlet Water outlet
Air
Nitrous oxide
LPG 220V AC
Acetylene Power
Control interface
Right steam cylinder
Left steam cylinder
External gas Main gas
Power supply Water inlet
Fuse
4. Electrical connections:
Connect the communication cable from the rear of the graphite furnace power supply to
the rear of the AAS main unit.
Connect the power supply cable, attached to the graphite power supply, to an
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AA500 Operation Instruction Manual
appropriate single phase plug for the 40Amp single phase supply. The wiring for this
should be only carried out by qualified personnel.
5. Installing hollow cathode lamps:
The AA500 instrument is equipped with an eight-lamp turret holder located in the light
source chamber at the upper left side of the system. Select the corresponding element
lamps according to the elements to be measured and install these lamps into the turret
before analysis. The lamp is plugged into one of the numbered sockets, then the socket
is installed into the correct numbered position at the turret.
6. Installing the heat protection baffle:
Insert the heat protection baffle between the graphite furnace atomizer head and
the flame atomizer. The heat protection baffle must be installed when using the flame.
The baffle is removed when using the graphite furnace mode.
2.4 Acceptance
After installation, the instrument can be adjusted and tested for acceptance. For testing
methods and acceptance please refer to the IQOQPQ instruction manual.
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AA500 Operation Instruction Manual
The AA500 has a PC system built into the electronics. The software is pre-installed so
there is no requirement for installation
The main AAWin Pro software interface includes four sections: the operation control
section (Menu, Tool bar, dynamic data display), the graphics display section (Calibration
curve, Real time graph/Peak profile), data display section (Measured results table) and
status display section (Status bar). See Figure 3-1.
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AA500 Operation Instruction Manual
The operation control section integrates all the system control functions of AAWin Pro
software system. That is, with the functions provided here, you can accomplish all kinds
of operations concerning the measurement. This section will include three parts: menu
bar, tool bar and dynamic data display bar.
The menu bar is located on the top of the main interface of the AAWin Pro application
window, and provides access to the commands used in this software. There are eight
menus included in the menu bar: File, Edit, View, Measure, Instrument, Setup,
Applications and Help. See Figure 3-2.
1. “File” menu: The “file” menu includes all the functions concerning the operations of the
measure files.
z “New”:This menu item allows you to create a blank measurement file. After
selecting this command, all data in the current measurement table will be removed
together with the measurement curves and graphs. If you need to perform sample
measurement, select [Setup]—[Sample setup guide] from the menu for sample
setup. After you set your measuring samples, measurement can then be performed.
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AA500 Operation Instruction Manual
z “Open”:This is used when you want to open an existing measurement file. Select
“Open”, the “Open a file” dialog box will open referring to Figure 3-3. Highlight the
name of the file you wish to open from the file list and click the “Open” button to open
the file or by double clicking on the file name to activate it.
z “Save”:This is used to store the measurement data from the current measurement
table into a file. Selecting the “Save” command, system will pop up the “Save a file”
dialog box, as shown the Figure 3-4. Enter the file name to be saved in the edit box
of file name and click the “Save” button, the system will store the measurement data
in the file you specified. If the file name you entered already exists, the system will
prompt asking whether you want to overwrite it or not. When you choose “Yes”, the
existing file will be overwritten by the new data. Otherwise, the system will return to
the former window without any file operation.
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AA500 Operation Instruction Manual
z “Save as”:This function allows you to store the measurement data in a file with a
new name. If the measurement data has not been saved before, this command has
no difference with the “Save” command in function. In the case that you have stored
the measurement data, however, system will store the current data in a new file when
you select the “Save as” function. Nevertheless, you have to specify a file name for it.
After that, all the operations you performed will act on the new file.
z “Newly created files”:This command provides you with the function to reload the
newly created files. You may directly select the file name to be opened from the
newly created file list to activate it.
z “Print”:This function provides you with outputting your data and graphs to the
printer. Selecting “Print”, “Select the content to be printed out” box will open. See
Figure 3-6. Specify the content you wish to print out and click “print”, the content will
be directly printed out. When you need to preview the content to be printed, click the
preview button to open the “Print preview” window. Refer to Figure 3-6.
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AA500 Operation Instruction Manual
instrument.
To print out directly, click the“ ”button. In the case that a measured table is selected,
you can use the“ ”or“ ”button to browse through the entire measurement data in the
table. Click“ ”to close the “Print preview” window.
z “Page setup”:This is for setting the size of the printing graphs, the font type and
size of the characters. See Figure 3-7.
z “Output file”:This allows you to transfer the contents of the measurement table into
other types of files and output. The AAWin software provides three types of output
files: Microsoft Word files, Microsoft Excel files and text files. When you select a type
of file, the system will pop up the “Save file” dialog box. After you enter the file name,
click the “Save” button, the system will start to perform the transformation and output
the file. Refer to Figure 3-8.
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AA500 Operation Instruction Manual
z “Export to database”: This provides the interface between the AAWin Pro and
database (support SQL-Server only). There are two steps to export data to database,
they are “connecting settings” and “upload”. The function of “connecting settings” is
to connect the PC with the database server and to adjust the sequence of upload
data, shown as Figure 3-9.
Note: Only after “Testing connection” successful the next step setting can be carry
on, shown in Figure 3-10 Uploading interface.
z “Exit”:This provides you with the function to quit from the AAWin software. In the
case that you have not stored your current measured results, the system will prompt
to save the data. After exiting the software system, follow the correct instrumental
shut-down procedures to switch off the instrument
.
2. “Edit” menu
The [edit] menu is used for performing table editing functions in the Measured Results
window. You may copy data from a selected range of cells in the measurement table to
the clipboard through the “Copy” command in the edit menu, and use the “Insert/Add”
and/or “Delete” etc function to edit the data rows in the measurement table. You can also
perform data finding through the [Find] command when needed. See Figure 3-11.
z “Copy” : This allows you to copy data from a selected range of cells in the
measurement table to the clipboard and paste them to third party software like
word processor or spread sheet.
z “Add”:This inserts an empty row for an unknown sample at the end of the
measurement table.
z “Delete”:This will delete the current row in which the cursor is located, from the
measurement table.
z “Find”:This allows you to search in the current column of the measurement table
where the cursor is located.
z “Calculator:It will open the application program of the system calculator (Calc.exe).
3. “View” menu
The [View] menu provides the functions concerning the system display operations.
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AA500 Operation Instruction Manual
Through these functions you may perform the setup to display or hide the tool bar, status
bar, calibration curve and entries of the measurement table, see Figure 3-12.
z “Tool bar”:To provide the function concerning the “Tool bar” display operation,
including the “Title display” and the “Hidden” two sub-menus. The “Title display”
submenu allows you to make a changeover between “display” and “hidden” of the
toolbar titles. The “Hidden” submenu provides the switchover between “display” and
“hidden” of the toolbar.
z “Status bar”:This allows you to make a changeover between “display” and “hidden”
of the status bar.
z “Table entries”:The [Table entries] menu provides you the switchover between
“display” and “hidden” entries (columns) in the measurement table. You may also set
the display format of the measure date and time through this function, Refer to
Figure 3-13. You can select the columns you wish to display from the “Column
display option” window, in which “Sample type”, “Sample ID” and “Absorbance”
must be specified, i.e. the above three items must be marked and you can not
remove the check marks beside them. These three entries will have to be displayed
in the measurement table. You can choose the format of the measure date and time
from the “format option” window. There are three types of date format: “yyyy/mm/dd”,
“mm/dd/yyyy” and “dd/mm/yyyy”. Likewise, there are two kinds of time format:
“hour-minute-second” and “hour-minute”.
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AA500 Operation Instruction Manual
You may modify the regression order for equation of the calibration curve to fit the points,
and use the “Hidden” check box to make a changeover between the “Display” and
“Hidden” of the calibration curve. If you need to print the calibration curve, click the “Print”
button.
z “Signal profile”:After a measurement is complete, you can check and browse the
individual sampling signal profiles by clicking the “Signal profile” to open the “signal
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AA500 Operation Instruction Manual
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AA500 Operation Instruction Manual
beneath the toolbar respectively and press “Enter”, the system will adjust the scopes of
the coordinate axes according to your setup. You can also use the two check boxes of
the “X-axis coordinate scale” and “Y- axis coordinate scale” to realize a changeover
between “display” and “hidden”.
4.“Measure”menu
The “Measure” menu includes three kinds of functions, namely Measure, Zeroing and
Renew analysis. See Figure 3-17.
5. “Instrument”menu
This menu is mainly used for setting the various parameters concerning the
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AA500 Operation Instruction Manual
instrumental performance. Through this menu you can set the working wavelength,
band width, lamp current, negative high-voltage, measure mode, background correction
mode, furnace heat program, element lamp, measurement parameters and measure
samples etc. see Figure 3-18.
z “Online”:When you are in “Offline” mode, you may use this function to realize the
communication with the AA instrument. On the contrary, you can also disconnect
the AAWin Pro software from the AA main unit when you perform in the online mode.
If the current mode is online, there will be a check mark beside the “online” entry.
6. “Setup” menu
This menu mainly provides the function to set the measurement parameters, the sample
setup guide and some control options concerning the system setup. Refer to Figure 3-19
.
unknown samples.
z “Options”:Click on this menu, the system will pop up a dialog box allowing you to
set the optional parameters. It comprises three optional pages. The first page is for
the regular parameter setup. See Figure 3-20.
¾ “Use the default file path”:When this check box is selected, the system
will use the default file path (Program directory\Data\) to save your files. If not,
the system will allow you to specify a file path or directory. You can enter the full
file path in the input box of “Save location” or click the “Directory” button for
selection.
¾ “List the newly created files”:When you have selected this check box,
the system will list all the newly created files in the “File / Newly created files”
menu. The amount of the newly created files to be displayed can be specified
through the input box behind. If you cancel the selection of this check box, the
system will not display the newly created files. You may use the “Clear” button to
remove the file list in the “newly created files” menu.
The second page is used to set the communication port of the instrument referring to
Figure 3-21. You can choose a communication port from the pull down box “Port” and
click “Apply”, the system will perform the communication connection with the AA main
unit through the selected port. When the communication is accessed, an “Operating
online” message will appear on the status bar of “state”, otherwise, an “Operating offline”
message will be displayed. The same message will also be displayed at the status bar of
the software master interface window. When you are first running the AA software and
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AA500 Operation Instruction Manual
can’t access the instrument communication connection, you can use this optional
function to change the communication port.
The third page is for the decimal digit setup referring to Figure 3-22. In this page you can
set the decimal digits for the table entries on display. When double clicking a table entry
in the list, a setup window will pop up. You can select a value from the pull down box or
enter a number in the edit box and click “Confirm” to activate the decimal digit setup. You
can also use the default setup by checking the “Use the default values” check box
followed by pressing the “Confirm” button. In this case, the system will display all the
table entries in the default decimal digits. When you modify the decimal digits of the table
entries in the list, the “Use the default values” check box should not be selected.
7. “Application” menu
The “Application” menu provides a variety of functions for system application including
energy adjustment, wavelength scan / line search, wavelength correction, exchange the
graphite tube, ignition, initialization, experimental records and options etc. See Figure
3-23.
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AA500 Operation Instruction Manual
z “Energy adjustment”:To display the current energy state and make adjustments in
steps.
z “Wavelength scan / peak search”:To dynamically scan the wavelength at the
range of 190~900nm and make a line search for the current wavelength.
z “Wavelength correction”:When a larger error (beyond ±0.3nm) is obtained in line
search, you can use this “Wavelength correction” function to make a correction to
the wavelength.
z “Experiment records”:This function allows you to take records for experiments,
such as the name of measured element, sample name, operator and
remark/comment entry. All the above items will be saved together with the measure
file and available for printing when printing the tables, see Figure 3-24.
8. “Help” menu:
“Help” menu provides the function of help, including register information and version
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AA500 Operation Instruction Manual
In addition, if you need to modify the user logon information, please click “Modify the user
logon information”, then you can open the logon information window, see figure 3-26.
You can input your name and the company’s name, which will be printed out.
The “Tool bar” is located on the second top of the master/main interface of the AAWin
Pro application windows just beneath the menu bar. It comprises of a variety of tool bar
buttons allowing you to realize the same operation functions as the related menus.
:This button is used to create a blank measurement file. Its function is the same as
the menu command operation “File”Æ “New”.
:Open a measurement file. Its function is the same as the menu command
operation “File”Æ “Open”.
:Save the current measurement file in a file name. It is the same function as the
menu command operation “File”Æ “Save”.
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AA500 Operation Instruction Manual
:Open the “print option” dialog box with the same function as “File”Æ “Print”.
:Open the sample setup guide with the same function as “Setup”Æ “Sample
setup guide”.
:Open the “measurement parameter setup” dialog box with the same function as
“Setup”Æ “Measurement parameters”.
:Open the “Wavelength scan/line search” window with the same function as
“Application”Æ“Wavelength scan/line search”.
:Open the “energy status” window with the same function as “Application”Æ
“Energy adjustment”.
:Open the “element lamp setup guide” with the same function as “Setup”Æ “Set
the element lamp”.
:Ignite the burner in flame when measured in flame absorption or flame emission
with the same function as the menu command operation “Application”Æ
“Ignition”.
:Open the furnace body when measured in furnace mode with the same function
as “Application”Æ“Exchange the graphite tube”. You can replace the graphite
tube when the furnace body is open after pressing this button, and then click
“ok” to close the furnace body.
:Open the “furnace heat program setup” window when measuring in furnace mode
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AA500 Operation Instruction Manual
with the same function as the menu command operation “Setup”Æ“Set the
furnace heat program”. You may set the furnace temperature program in the
pop up window.
The “dynamic data display bar” provides you with the function of displaying a variety of
data including the measurement element, working wavelength, absorbance and
background values in real time referring to Figure 3-27. When the measuring element
and the working wavelength are changed, the contents of the above “dynamic data
display bar” will also be correspondently adjusted. The time interval of refreshing for the
absorbance and background value is 0.5 second.
The graphics display section provides the function of editing and dynamically displaying
both the calibration curve and the real time graph for the measurement. Before making
an introduction to these two types of graphics, learn how to set the graph color,
coordinate scale graphics parameters.
In AAWin Pro software system, the graph setup function is incorporated in almost all the
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AA500 Operation Instruction Manual
graphs except in the real time graph, where the graph setup parameters are the same as
those in the peak profile, i.e. once you set up the parameters for the peak profile, the
parameters for the real time graph will also be fixed.
By clicking the right mouse button while the mouse pointer is positioned within the
boundaries of the graph, a pop-up window with the “graph setup” menu will open. Click
on the “graph setup” item to open the graph setup box. You will see two optional pages in
this dialog box, the first one is for the regular parameter setup, see Figure 3-28.
In this regular parameter setup page, you may enter the coordinate scale limits of both
the horizontal and vertical axes in the “Maximum” and “Minimum” input boxes, select the
rotation angles for the titles of both the horizontal and the vertical axes from the pull down
boxes or enter the values in the edit boxes in the “Rotation angle” items, and choose the
grid line types of the horizontal and vertical coordinate axes in the “Grid line” box,
together with marking in their check boxes for “display” or canceling the mark for
“hidden”.
The second page is used for the color setup. Refer to Figure 3-29.
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AA500 Operation Instruction Manual
In this page, you may choose the object and color from the setup list box. When making
a color setup for different types of graphs, the contents in the setup list box may also be
changed. Furthermore, in the case of color setup of the calibration curve, you may also
choose the shape of the standard points from the “Shape of standard points” pull down
box.
The calibration curve graph is located on the left of the graph display section. It is used to
display the current calibration curve, see Figure 3-30. When clicking the right mouse
button while the mouse pointer is positioned within the boundaries of the graph, a pop-up
menu will open, from which the graph settings can be made. Refer to Figure 3-31.
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AA500 Operation Instruction Manual
The real time graph is located on the right of the graph display window. It is mainly used
to dynamically display the measurement signal profile referring to Figure 3-34. Clicking
the right mouse button while the mouse pointer is positioned within the boundaries of the
real time graph, a pop-up menu for setup will open. See also Figure 3-35. Click on the
“signal profile” item from this menu to open the signal profile display window.
The data display section mainly consists of a table called the measurement table. See
Figure 3-36. Each column in the measurement table will have a different meaning, in
which the leftmost column is used as the flag column where the mark is labeled to
indicate the current row of the measurement table and is the same color as that of the
flag column. In the process of measurement, when the sample of the current row is
finished, the flag of the current measurement row will jump to the next row for you to
measure another sample. When the current measurement row becomes the last row of
the table, the system will automatically add a new sample in the measurement table in
order for you to continue the measurement.
Clicking the right mouse button while the mouse pointer is positioned within the
boundaries of the measurement table, a pop-up menu for setup will open. See Figure
3-37. The function of the menu items are as follows:
z “Edit” : This [Edit] menu is used for performing table-editing functions in the
measurement table. The table entries to be editable are “Sample ID”, “Weight”,
“Volume”, “dilute ratio”, “Modification/ Correction factor” and “Sample position”.
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AA500 Operation Instruction Manual
z “Copy”:This copies data from a selected range of cells in the measurement table to
the clipboard.
z “Add” : This adds an empty row for an unknown sample at the end of the
measurement table.
z “Delete”:This deletes the current sample row in which the cursor is located, from the
measurement table. If you are finished with all the standard measurements and the
calibration curve preparation, the calibration curve will be re-fitted when you delete a
standard sample from the measurement table. If there is only one standard sample
left in the measurement table, you will not be able to delete it.
z “Renew analysis”:This allows you to measure the sample of the row in which the
cursor is located in the measurement table for a second time.
z “Table setup”:This opens the “table setup” dialog box referring to Menu barÆView
menuÆTable entries for more details.
z “Sample attributes”:Clicking on the “Sample attributes” menu item, the “Sample
attributes” dialog box will be open, see Figure 3-38. This dialog box is mainly used to
give a detailed description of the sample in the measurement table which the cursor
is located, including concentration value, unit, standard deviation, relative standard
deviation, measurement time, mean value, duplicate number and the individual
measured results. You may click on the “Print” button to print them out.
z
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The status display section, namely the status bar, is mainly responsible for the dynamic
display for information of the system running status including the measure mode, energy
status, the run mode of AAWin Pro software and the notation item of the menu, refer to
Figure 3-39. The menu entry is used to display some detailed information about the
current menu. The measure mode entry is for display of the current measure method
employed. You can use the mouse to open the measure mode setup window by double
clicking on this item. Once you have modified the measure mode, the content displayed
in this entry will also be correspondently changed. The lamp energy and background
state entries are used to dynamically display their current energy status respectively. You
may also open the energy setup window by double clicking on the item. The run mode
entry is to display the current run mode of AAWin Pro software. If you are running the
software in offline mode, the system will display “ ” in the run mode entry,
otherwise a “ ” information will be displayed.
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When you start up AAWin Pro software, you will see firstly a starting headline window as
Figure 3-40. This starting window will soon disappear when you turn on the power for the
AA instrument and connect the communication cable. If it is not the case, a message box
will open reminding you to check the connections. Make sure that all the connections are
normal, click “Retry” for re-communication with the AA main unit. The starting window
goes away after the communication with the AA main unit is successfully attached. You
can also click “Cancel” directly to enter into the offline mode.
A run mode selection box will open next for you to choose a run mode. Refer to figure
3-41. You may check “Online” or “Offline” from the dropdown box for a run mode
selection.
z “Online”:To make an AA analysis, you can select “Online” and then click “Confirm”,
the system will switch to the instrumental initialization and set all the initial
instrumental parameters.
z “Offline”:If you want to get familiar with the AAWin Pro software operations or need
to output the former measure results, you may check the “Offline” and click
“Confirm”, the system will start up in offline mode. In this case, you cannot control
the instrument.
z “Exit”:If you do not want to run the AAWin Pro software, click “Exit” to close the
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3.9 Initialization
When you select the online mode for running the software, the system will initialize the
instrument. See figure 3-42. The instrumental initialization is mainly aimed at the setup of
initial parameters of the individual drive motors including D2 lamp motor, HCL lamp motor,
atomizer motor, burner motor, slit width motor and wavelength motor. When an entry is
successfully initialized, a check mark will appear on the left beside the item; Otherwise,
a cross sign will appear. If any one of them fails to be successfully initialized, the
whole instrumental initialization will fail. In this case, a message box will open after the
initialization for you to choose whether you want to try again or not. You may enter “Yes”
to continue or press “No” to exit the AAWin Pro system. Note that the above message
box will open only in the online run mode. When you choose [Application]—[Initialization]
from the menu to carry out the instrumental initialization, the above message box will not
appear.
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AA500 Operation Instruction Manual
When the instrumental initialization is finished, the system will open the element lamp
setup guide, which will allow you to make lamp and its element parameter settings step
by step. The guide contains four pages. In the first page you can set the working lamp
and the warm-up lamp as Figure 3-43. You may select a working or warm-up lamp from
its dropdown box respectively, or you can also make exchange of them through the
exchange button.
When you need to modify the lamp element, double click the element lamp entering into
the element selection dialog box. See Figure 3-44.
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AA500 Operation Instruction Manual
The element selection box has two optional pages, the first of which is provided with an
elementary periodic table allowing you to make an element selection. In this periodic
table elements are marked with different color and designs, which indicates the analytical
methods available for the element. All the three AA analytical methods are marked with
color, in which the white color“ ”stands for the flame method (FA), the
green“ ”indicates the furnace method (GFA), and the pink“ ”is for the hydride
generation method (HGA). For example, the element tungsten is marked with “ ”,
showing that tungsten can be measured by flame method; Copper is labeled with “ ”,
indicating that cupper can be measured by both flame and furnace method; Mercury is
marked with “ ”,which means that all the three AA analytical methods can be used to
measure this element. For the element hydrogen, however, there is no mark at all, the
color being the same as its background color, which means, none of the three AA
methods can be used for this element.
In the second page for the element selection box some detailed information about the
element is displayed in the form of a list, providing you with a variety of standard
reference conditions for the elements including the specific wavelengths, band width,
lamp current, and the fuel flow rate. Hence, you can easily choose a condition for your
measure element from the said expert information system. Refer to Figure 3-45.
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AA500 Operation Instruction Manual
In this page all the elements which can be measured in AA analysis are listed on the left
table, presenting you the element symbol, serial number, name, atomic weight and the
measure method suitable for the element. In the method column of this table, some
abbreviation symbols are used, in which“F”stands for the flame method,“G”shows the
furnace method, and “H” indicates the hydride generation method. You can click the
headline of each column in the list to sort the data ascending or descending. See Figure
3-46 and 3-47.
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AA500 Operation Instruction Manual
Below the element list table on the left will be provided with the description of related
measure methods available to the element selected in the list. For example, when the
element copper (Cu) was highlighted in the list, the following message will be displayed:
“Flame: air⎯acetylene, oxidative (blue)”. On the right of element list table are the
characteristic spectral lines of the selected elements. The user can use the scrollbar to
read. See fig.3-48.
When you finish selecting the elements, click “Confirm”. The system will allow you to
modify the element you just selected on the current lamp position. In this case, you may
click “Next” entering into the element lamp parameter setup page. See Figure 3-49.
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AA500 Operation Instruction Manual
In this page, you can set the lamp parameters for the selected element, which will include
working current, warm-up current, bandwidth and the negative high-voltage. Both the
working current of the lamp and the bandwidth are taken from the database of the expert
information system as the default setting values. You may also enter other values if you
do not want to use the default ones. Click “Next”, the system will make the adjustment to
the instrument according to your settings. Refer to Figure 3-50.
Note:This window will always be applied in the AAWin software system, when
needed to deliver the control parameters for the instrument. You can click “stop”
to quit from the execution of this instruction.
After you finish the above settings, you may switch to the wavelength setup page. In this
page, you can choose the characteristic wavelength for the specified element and
perform the peak searching refer to Figure 3-51.
Select a line from the dropdown box of wavelength, and click “Peak-search” to perform
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AA500 Operation Instruction Manual
the peak searching (For detailed information, see Section 3.11 Peak search and
wavelength scan). When peak search is complete, you will end up with the element lamp
setup. Click “Finish” to close the setup guide. If you did not perform the peak-search, the
system will remind you to do so when you click the “Next” button. As you have already
changed the parameters for the element lamp, the optimal position of the wavelength
may also have changed, therefore a peak search is recommended in this case. You can
choose “Yes” for peak search or “No” to skip. If you do not need reminding, click
“Cancel”.
After completion in the element lamp setup, you can carry out peak search and scan the
wavelength profile. Select [Application]—[Wavelength scan / Peak-search] from the
menu or click the“ ”button from the toolbar to open the wavelength scan and peak
search dialog box. See Figure 3-52.
Click the “Peak search” button in this box to set the peak position of the current
wavelength. If you need to make a peak search for other characteristic wavelengths of
the specified element, select the corresponding wavelength from the dropdown box and
click the “Peak search” button. The result for peak search will be dynamically displayed
on the wavelength scan graph and the maximum energy position (Peak position) will be
displayed below the wavelength scan graph, after the fine adjustment to the instrumental
energy. See Figure 3-53. If you want to check the current energy state of the instrument,
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AA500 Operation Instruction Manual
click the “Energy” button to open the energy adjustment window. Refer to Section 3.13
for more information.
Sometimes you need to scan a range of wavelengths in order to get more detailed
information about the wavelength profile within that range. In this case, you may enter
the starting point and end point of the wavelength separately in each of the input box and
input the lower and upper limits of the energy (the vertical coordinate axis) in the
respective input box. Click “Scan” to perform wavelength scanning within the specified
range. Note: The values of the wavelength should be at the range of 190~900nm. If you
enter a value out of that range, the system will open an error message and allow you to
enter it again. You can also read out the coordinates of the peak profile graph. Right click
on the graph, select [Coordinate readout] from the popup menu to get the coordinates of
peak position. If you need to lock the readout coordinates, check the “Lock” option from
the above popup menu. To unlock the readout coordinates, re-check the “Lock” option.
Refer to Figure 3-54.
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AA500 Operation Instruction Manual
If you want to terminate the instrumental operation in the process of wavelength scan or
peak search, click the “Stop” button to quit from the current operation. Note: Abnormal
termination of the instrument may affect the accuracy of measurement. Hence, this
function will here not be recommended.
The peak search or wavelength scan graph will be saved by the AAWin Pro system in
order to be examined when needed. You may also click “Print” to print out. The scan
graph will not be removed until you perform the peak search or wavelength scanning for
a second time. In that case, a new scan graph will open to substitute the old one.
If you have a large wavelength error (more than ±0.3nm) while you perform the peak
search, you may use the wavelength correction function to calibrate the wavelength.
Select [Application]—[Wavelength correction] from the menu to open the wavelength
correction box. Refer to Figure 3-55.
Choose the turret number of the lamp used for wavelength correction from the element
lamp setup list. Note: Only a calibration element lamp (Hg) can be applied to the
wavelength correction. Therefore, the calibration lamp has been specially labeled
with“ ”in the element lamp list. You can only perform the wavelength correction with the
labeled element lamp; otherwise, the wavelength correction will not proceed. You can
use the element lamp setup guide to set the lamp parameters for the element (See
Section3.10 Set the element lamp).
After you have selected the element lamp, click “Start” to perform the wavelength
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AA500 Operation Instruction Manual
correction. If you want to terminate the operation while the wavelength correction
proceeds, you may click the “Stop” button. See Figure 3-56. If an error message appears
during the correction process: “Wavelength error is too large, correction cannot proceed”,
it indicates that the wavelength error of the instrument is out of the limitation range or the
AA instrument is not in a normal state. In this case, you can check if the atomizer or the
burner head is correctly set on the AA optical path or if they are blocking the light path.
You need to re-set the position of the burner head or of the atomizer in the case of light
blocking until the light can pass through smoothly. Click “Reset” to restore the initial
parameters of the wavelength setup, and then perform the wavelength correction again.
If the error message appears again, you need to readjust the optical path of the
instrument. In this case, please contact with your local dealer for repair or advice.
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AA500 Operation Instruction Manual
When you need to check the energy state of the instrument or make an adjustment of
energy, select [Application]—[Energy adjustment] from the menu or click the“ ”button
from the toolbar to open the energy adjustment box, see Figure 3-57. In this box, a sector
(fan-shaped) plate meter with different color needle indicators are used to indicate the
current energy state of the AA and BG signals, in which the green color shows the AA
energy signal, and the red color shows the BG energy signal. If no BG correction mode is
used, the green energy indicator is only displayed. You can enter a value for the negative
high voltage in the input box (within the range of 0~1000V) followed by a “Enter” key to
make an adjustment of the negative high voltage, or press the“ ”or“ ”button to
increase or decrease the high voltage value with the amplitude of 0.25 V for each step.
When you need to re-adjust the lamp current, you can enter a current value (within the
range of 0~20mA) in the lamp current input box followed by the “Enter” key,or use
the“ ”or“ ”button to make fine adjustments with the amplitude of 0.1mA for each step.
Use the same method as above to adjust the D2 lamp current or the wide and narrow
pulse currents, when the D2 lamp or SR lamp BG mode is selected. Refer to Figures 3-58
and 3-59.
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If you cannot perform a successful beam balance manually, click the “Auto beam balance”
button for an automatic adjustment. In this case, the system will automatically adjust the
instrument to the beam balance state.
You can also make an advanced adjustment to the instrumental parts in the energy
adjustment box. Click “Advanced adjustment” to open the advanced adjustment box.
Select one entry from the advanced adjustment option box, use the four buttons on the
lower right of the box to make adjustments. For the “burner motor” and the “slit motor”, no
zeroing can be performed, and the “zero-order spectra line search” is the unique function
for the “wavelength motor”. If you select D2 lamp as a background correction, the D2
lamp mirror motor can become active in the advanced adjustment box. You can use the
“positive rotation” or “Reverse/Back turn” button to adjust the light path of the D2 lamp
until the beam spot of the D2 lamp becomes fully overlapped with that of the element
lamp.
Note: The advanced adjustment function should be of limited use in the
practical work of measurement. When there is no special need, the frequent
use of this function should be avoided.
In this section, it will show how to set the parameters for the instrumental hardware
portions. As these parameters are tightly (closely) related to the hardware driving system
of the instrument, any negligence or carelessness in the parameter settings may cause
damage of the instrument, users should carefully read the following sections and
become familiar with their operations before performing the parameter settings.
When you need to set the working wavelength, bandwidth and the negative high voltage,
select [Instrument]—[Optical system] from the menu to open the optical parameter setup
box, refer to Figure 3-60. You can select the working wavelength from the wavelength
dropdown box or enter the value of the current working wavelength in the input box. The
wavelength you entered should be in the range of 190~900nm, If not,the system will
open a message box with a warning.
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AA500 Operation Instruction Manual
You can choose the bandwidth from the dropdown box. The bandwidths available are:
2.0nm, 1.0nm, 0.4nm, 0.2nm and 0.1nm.
You can enter the current negative high voltage in the high voltage input box, the value of
which should be in the range of 0~1000V. If it is out of the range, the system will show a
warning message.
After regular parameter settings, click “Determine” for the system to transfer your
settings to the AA instrument. The instrumental parts will be adjusted according to your
settings. When the adjustment is finished, the system will close the above dialog box. If
you do not want to close the dialog box, you can click “Execute” instead of “Determine”.
In this case, the system can also deliver your settings to the instrument, but will not close
the dialog box after adjustment, allowing you to make a further adjustment to the
instrument.
When you want to modify your current measure method, select [Instrument]—[measure
method] from the menu to open the measure mode setup box, see Figure 3-61. Before
doing so, you should make sure that all the measure results in the measure table have
been properly saved or printed in case they are lost, because all the data in the measure
table will be removed once you have changed your current measure method.
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AA500 Operation Instruction Manual
You can set the measure method from the dialog box according to your measure
requirements. The methods that are available in the box are listed as follows: flame
absorption, flame emission, graphite furnace atomization and hydride generation
method. For example, if you need to change your current measure mode from flame to
furnace method and exchange the graphite tube, you can select “Graphite Furnace” from
the “Measure method” list box, and then click “Execute”. After the switchover is complete,
click the “Exchange the graphite tube” button to open the furnace body, allowing you to
replace a new graphite tube. After you finish the replacement, click [ok] to close the
furnace body.
Note: Before switching to the Graphite furnace mode, remove the heat baffle plate
between the burner head and the furnace body, lift up the sample support stand
and the combustion chamber door in case of any damage in the instrument during
the process.
In the measurement of atomic absorption analysis, if the matrix of the measured sample
is too complicate which gives a large background absorption causing a serious problem
of spectral interference, or the content of the element to be measured is too low, where
high sensitivity is required and the atomic absorption signal needs to be more accurately
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AA500 Operation Instruction Manual
corrected. In this case you need to use the background correction mode for
measurement. The background correction modes that are available for AA500 series
atomic absorption spectrophotometer are as follows: D2 lamp-BGC and SR lamp-BGC
mode. You can select [Instrument] — [Background correction mode] from the menu to
open the background correction mode selection box, refer to Figure 3-62.
You can choose the background correction mode from the list box and click [ok] or
[Execute], the system will immediately set the background correction mode you selected
as the current mode. If you select the D2 lamp to perform the background correction, an
input box for D2 lamp current will open on the right side of the BGC mode list box,
allowing you to set the lamp current values according to your own requirements. When
you choose SR lamp to perform the background correction, there will be two input boxes
open on the right of the BGC mode list box, allowing you to enter the wide and narrow
pulse current values for the SR lamp. Refer to Figure 3-63.
Based on the measured elements, the default values for the D2 lamp current or the SR
lamp currents (the wide and narrow pulse current) may be different which are all taken
from the database of the expert information system or cook book. When you set the D2
lamp current, the value you entered should be at the range of 0~120mA. When set the
SR lamp currents, the value of the wide pulse current should be controlled within
0~20mA, and the narrow pulse current within 0~10mA. If the values you entered are out
of the limitation range, the system will open an error message warning.
Note: When the D2 lamp is used to perform the background correction, the current
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should not be used at its maximum power (lamp current =120mA) for a long time.
When it is not used for a long period, shut down the lamp power as soon as
possible in order to extend its useful life period.
When you need to change the working lamp and/or the warm-up lamp current, Select
[Instrument]—[Lamp current] from the menu to open the lamp current setup box, see
Figure 3-64. You can enter the current values for the working lamp and/or the warm-up
lamp in the respective input box, and click [ok] or [Execute] to transfer your settings. The
current value you entered should be controlled within 0~20mA. If it is out of this limitation
range, the system will open a warning message. If you are now using the D2 lamp to
perform the background correction, you can also enter a current value for the D2 lamp in
the D2 lamp current box.
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When setting the instrumental wavelength to a certain value, you can use the
“wavelength location” function. Select [Instrument]—[Wavelength location] from the
menu or press F3 key to open the wavelength location window, refer to Figure 3-65. You
can choose the wavelength value from the dropdown box or directly enter it into the
wavelength box, and then click [ok] to perform.
The analysis of some elements must use the function of wavelength locating,
such as Cr analysis. First the user should search the peaks to get peak-searching
spectrum, then read the wavelength of the second peak by using coordinate
readout. And then locate the wavelength to the main sensitive line. See 3.11 for
peak searching and wavelength scan.
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Choose “Burner head Identification” from “Instrument” menu on flame absorption mode
to identify the current type of burner head. There are three kinds of burner head, such as
“Air-Acetylene”, “Air-LPG”, “Nitrous Oxide-Acetylene”. It will show you “No burner head”
without burner head fitted.
Air-Acetylene mode:
Replace with the Air-Acetylene burner head first, and press “Flame” to gain access to “Choosing
Flame Interface”. Then ignite the Air-Acetylene flame by this interface.
Air-LPG mode:
Replace with the Air-LPG burner head first, and press “Flame” to gain access to “Choosing Flame
Interface”. Then ignite the Air-LPG flame by this interface.
Press “Status Checking” button to check the pressure status of all the equipment. It will
show “ON” for the normal status, “OFF” for the error status. Ignition can be carried on
when all the status show “ON”.
When you are using the furnace mode to perform measurements, you have to set the
furnace parameters, including the furnace heat program parameters and the position of
the furnace atomizer.
Before measuring in furnace mode, you need to set the heat program for the furnace.
Select [Instrument]—[Set furnace heat program] from the menu to open the furnace
heat program setup box, see Figure 3-66.
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In this dialog box you are allowed to set a maximum of 9 stages of temperature
conditions for the furnace temperature program. Click the check box beside each serial
number of stage in the serial number column to activate that stage to perform the heat
program setup.
z “Target temperature” is the set value of the end temperature for the current stage,
which should be controlled within the range of 20~2700#.
z “Heating time” refers to the time period taken by the heat stage in which the
furnace temperature is elevated from the set value in the former stage to the target
in the current stage. The value for the heating time should be at the range of 0~255
seconds.
z “Hold time” is defined by the time period during which the furnace temperature is
set to keep constant after elevated to the target temperature. The value for the hold
time should be also controlled within the range of 0~255 seconds.
z “Atomization” is used to set the atomizing stage for the furnace heat program in
order for the system to perform data sampling at that stage. You can click the check
box in the step to select as the atomizing stage. Please note that this “Atomization”
function can be set at only one stage for the heat program.
z “Inner gas flow rate” allows you to regulate the gas flow passing through the inside
of the graphite tube during each stage. It adopts a gas line system with “none”, “low”,
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“medium” and “high” four-level flow control. The “none” level is mainly used for the
atomizing step, during which the inner gas flow rate is totally cut off. The “Low” level
refers to the gas flow state where the inner gas flow rate is set to a low value with
about 150mL/min. For the “Medium” level, a middle inner gas flow rate with about
300mL/min has been regulated. With the “High” level inner gas flow rate,
approximately a 450mL/min gas flow rate is allowed to pass through the inside of the
graphite tube.
Note:When the furnace temperature is set to 2000~2500#, the total time used for
heating and hold in this stage should be less than 25 seconds. If a 2500~2700#
furnace temperature is selected, the total time for heating and hold should be
controlled to no more than 15 seconds. If the value is out of the limitation range,
the system will open a warning message. Heat steps to be set in a furnace
program should be logical and coherent, no blank stage is allowed in the furnace
program.
If you need to modify the cooling time for the furnace body, you can enter the value in the
input box of the “cool-down time” which should be within the range of 20~99seconds.
After you finish setting the heat program, click [ok] to transfer your settings to the
instrument and exit the setup window.
When performing measurements in the furnace mode, a problem for the offset of the
atomizer may sometimes occur, causing the light path from the element lamp not to pass
through the center for the graphite furnace atomizer. In this case, you need to re-set the
furnace atomizer position. Select [Instrument]—[Set the atomizer position] from the
menu to open the atomizer position setup box, refer to Figure 3-67.
You can use the left mouse key to drag the scroll bar for adjustment. Once you have set
the scroll bar to a new position, click [ok] or [Execute] to activate your setting.
The software will save the heating times automatically when measuring by the graphite
furnace method. If you choose “Times limitation” and input the value, it will show “The life
time of the GF tube is over, please replace with a new tube”.
If your instrument is fitted with an auto-sampler, you can set it by selecting “auto-sampler”
from “instrument”. There are two different setups for the auto-sampler, for flame analysis
and graphite furnace analysis respectively. If you use flame analysis, the setup window
will be for the flame auto-sampler, refer to 3.18.1. If you select graphite furnace analysis,
the setup window will be for the graphite furnace auto-sampler, refer to 3.18.2. If you
select “start auto-sampler”, connect the power supply cable and communication cable,
then click “offline”, the auto-sampler will be in online mode. If the connection failed, you
can try selecting other communication ports. When the connection is ok, click “initialize”
to initialize the auto-sampler.
z Wash time: The wash time before each sampling. The unit is “second”.
z Interval of repeat: The interval of each repeat measurement. The unit is “second”.
z Spray time: The waiting time before each sampling. The unit is “second”. Because
the length of the capillary can be different, the time from sampling to the burner head
is also different. If your capillary is long, you can set the pre-spray time a little longer
to ensure the sufficient combustion.
z Wash time: Set the wash time before each sampling. The unit of the cleanout time
is “second”.
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z Interval of repeat: The interval of each repeat measurement. The unit is “second”.
z The total samples: The total samples means the sampling volume of each sample.
You can click “setup” to open the setup window.
Basic sampling: Basic sampling means the sampling volume of each specified
sample. It is also called “fix sampling”.
Mix sampling: You can set three kinds of mix samples, specify the location of
the cuvettes and the sampling volume. In addition to the samples of fix sampling,
you can mix four solutions to measure. You can also dilute the samples. The
volume of the graphite tube is limited, so the total sampling is limited. If the total
volume you set is beyond the maximum, the system will prompt you to modify it.
Position adjustment: In order to position the auto-sampler more accurately,
the position adjustment program of the auto-sampler is added to the software.
You can adjust the position to make the sampling more accurate. Refer to 3-68.
Note: Please refer to the Auto sampler user’s manual for more information.
The position of the sample needle should be re-adjusted if replacing the GF tube
or the atomizer position is changed.
The auto dilution function will be active if you choose “Connect ASC” on Graphite furnace
mode. Choose the “Sample” button to go to the Sample wizard. Click the “Auto Dilution”
check box from the Concentration setting page and go to the “Auto dilution parameters
setting page”. Set the main liquid concentration, position, carrier liquid position, matrix
developed agent volume and position on this page.
After the setting up is finished, the auto sampler begins to auto dilute.
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3.19 Measurement
Set up the measurement parameters before measuring. Choose the “Parameters” from
“Setting” main menu to open this. There are four pages for the measurement
parameters.
In this page, you can set the display boundary of absorbance in the measuring graphs,
i.e. the lower and upper limits of the vertical / longitudinal axis of the measuring graphs. If
you are selecting “Flame emission” as your current measurement mode, then you may
also set the display range of energy. See also figure 3-71.
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“Refresh time”is the maximum time period during which the real time profile can
continuously display in flame mode, i.e. the threshold of time axis (the horizontal) in the
measuring graph. For example, if you set the “Refresh time”as 10 seconds, then the
maximum display period of time coordinate axis will be 10 seconds during the
measurement, and the real time profile will be refreshed or renewed every 10 seconds,
the former curves will be cleared out. You can adjust the display range of your horizontal
coordinate through the “graph display setup” function, i.e. you may display your former
graph for the second time. The graph will be removed when you begin to make a second
measurement. Note that the “Refresh time” can only be active in Flame mode. When you
are using Furnace mode for making measurement parameter settings, it will not be
displayed.
z Signal processing
After making the display setup, you can select the third page “Data processing” for signal
processing parameter settings (See figure 3-72). In this page, you can check the data
calculation mode from the “Calculation mode” pull-down menu box. The calculation
mode you may select is as follows: continuous, peak height, and peak area. However,
you can only choose two of them: peak height or peak area for the selection of
calculation mode in furnace analysis.
You can input the integration time for the measuring data in the “Integration time” box.
The integration time you enter should be at the range of 0.1 to 100 seconds. In Furnace
analysis, the “Integration time” box will become grey (inactive). The system will
automatically take the total sum of the heating time in the atomization stage and the last
three seconds in the former step (Ashing stage) in the furnace temperature program as
the default integration time.
“Range extend” is the extended times of the received data. It should be controlled at the
range of 0.01~100 times.
“Filter factor” is a constant which needs to be given to filter the acquired data. It should
be controlled at the range of 0.01~10. For the graphite furnace analysis, the factor should
be set to 0.1.
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z Quality control
Quality control is added to the software in order to cooperate with the auto-sampler. The
user can monitor the measure results by using this function, and also can set control
options by using this function. See Fig. 3-73.
1. Upper value and lower value:Set the upper value and the lower value of the
quality control.
2. Deal with ultra-upper value and ultra- lower value: Set the processing method
when the measure result is upper value. The user can choose “continue”, “stop”, or
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“re-measure”. In addition, the user can choose to mark, which will be marked in the
upper value grid of the measure table, for the upper value.
3. Deal with out of range for the second time: Set the processing method when
the measure result is out of range for the second time. The user can choose “stop” or
“continue”.
4. Control range of Abs: the user can choose effective monitoring range for Abs.
Quality control can only monitor the data when the Abs is in the range.
Before making a measurement, you need to set the measuring samples. Select
[settings]—[Guide to the sample setup] from the menu or just press the button “ ” from
the toolbar to open the “Guide to the sample setup” dialog box. It includes three pages
allowing you to make measurement sample settings step by step. The first page is meant
for standard sample settings referring to Figure 3-74.
“Correction method” is used to select the correction method for standard samples. The
method to be selected is as follows: calibration curve, standard addition or interpolate
method.
“Regression equation” is the calculation formula selected for the regression of
calibration curve of the standard samples, including “linear A=K1[C]+K0”, “linear
C=K1[A]+K0”, “square C=K2[A]2+K1[A]+K0” and “cubic C=K3[A]3+K2[A]2+K1[A]+K0” etc.
This section allows you to select a regression order for the calibration curve.
“Concentration unit” is the unit used for the sample concentration. It may be as follows:
“ng/μl”, “ng/ml”, “μg/μl”, “μg/ml”, “mg/l”, “ppb”, “ppm”, “mol/l” etc. You can also enter the
unit by yourself in the case of no unit existing in the concentration unit list.
“Sample identification (ID)” and ”Serial number” generally make up the sample
number. For example, Sample no. “S1” stands for the sample which has a Sample ID ”S”
and a Serial number “1”.
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“start error correction”:It can effectively reduce the measure error. If your measure
result is not accurate, you can choose this option.
“Auto-upgrade equation”: It can monitor the standard equation according to the
minimum relativity you set. Once the relativity is less than the minimum relativity you set,
the system will upgrade the standard equation from linear equation to nonlinear equation
and calculate again. The function is effective only when the curvilinear equation is first
order equation.
After you have made standard parameter settings, click the “Next step” button entering
the page for standard concentration setup referring to figure 3-75. You can enter the
concentration values in the concentration boxes of the standard list. Click “Increase”
button to add the standard samples, you may add totally 8 samples in the standard list.
Click “Decrease” to remove/delete standard samples, you should leave at least one
standard sample in the list.
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After finishing the standard concentration setup, click the “Next step” button for the
auto-analysis setup referring to figure 3-76. In this page, you may check some
auto-analysis functions and make the corresponding parameter settings for the
measurement.
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z Sensitivity correction: There may be some errors exist called “drift”. Sensitivity
correction function is added in the software in order to reduce errors. It needs to
measure the standard sample, and then correct the sensitivity according to the
measurement result. The user needs to select the serial number of the standard
sample and correction cycle.
z Auto-save: Set the sample interval for storing measurement data in case that the
measurement data will not be totally lost when the computer is switched off by
accident. You can set a cycle, then the system will auto save your sample by your
set cycle.
After you complete the auto-analysis setup, click the “Next setup” button entering the last
page of this sample setup guide — the “Unknown sample settings” section.
In this page, the following items will be set: number of unknown samples, sample ID and a
variety of coefficients or factors needed for concentration calculation or correction. In the
result table, one column entitled ” Actual concentration” is listed. Its calculation formula is as
follows:
Conc * VF * DF * CF
Actual Conc.=
WF
You can input factors according to the sample, and then calculate the concentration.
When you start the sample setup guide, the default factor is 1. That is to say, if you don’t
make a setup, the “real concentration” is equal to “concentration” in the sample table
after measurement. If you need to modify the above factor, you can use the edit function
of the measurement table.
After you finish all the above sample parameter settings, you can make some changes
through clicking the “former step” button and editing the contents of the former pages.
When you confirm that you have made all the sample parameter settings and click the
“Finish” button, the system will transform your settings into a measurement table. Now
you can start to make a measurement.
In AAWin Pro software system, different analytical methods need to take different
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procedure and require different preparations to carry out. The following shows both the
analytical procedure for Flame method and that for Furnace method. Please read the
related contents carefully in case any safety problem occurs.
Note: Insert the baffle between the flame burner head and the graphite furnace
before ignition.
In the case of flame analysis, you should carefully check all the tubing for gas leaks
before operating the instrument. Select [Instrument]—[Ignition] from the menu for igniting
the flame. When the flame height is too high or too low or if the burner is not set in the
correct position, carry out the adjustments.
After igniting the flame and making adjustments to the burner parameters, you can now
start to make a measurement. To do so, first select [Measurement]-[Start] from the menu
or click the button“ ”from the toolbar or just press F5 key to open the measurement
window, then the analog signal will start in the real time graph. Refer to Figure 3-77.
Now you can click the [Start] button for sampling. If you have chosen a Manual mode to
make the measurement in the measurement parameter-setting window, you will have to
push the [Start] button again for another measurement. In the case of Automatic mode,
however, the system will automatically take the sampling process according to your
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setting of the “Time interval”. After finishing the samplings, the system will display the
results in the measurement window, standard deviation (SD) and relative standard
deviation (RSD) values will also be calculated and displayed in the window after the third
repetitive reading. After you complete all the readings, set by the duplicate number in the
measurement parameter dialog box, the system will calculate the mean value of the
measurement results and display it in the correct cell (unit element) of the measurement
table. See also Figure 3-77.
During the measurement a timer is placed on the upper right of the measurement window
from which you can check the total time used for your analysis. You can also insert a
blank before each sample for zero check. Click the “Zero” button to make zero
adjustment. Press the “End” button when the measurement is finished, see also figure
3-78. If you have selected D2 lamp or SR mode for the background correction, AA and
BG values will be displayed together with the absorbance in the measurement window. In
the mean time, the AA and BG curves will also appear in the real time graph. In this case,
the absorbance is the difference subtracting the BG value from the AA value (Abs. = AA
- BG). If no background correction is used, the system will display the absorbance and
provide the Abs Curve only. In this situation, the abs. is equal to the AA value (Abs. = AA).
Curve color in the real time graph can be set through the function of the Graph Setup. In
the case of default, Abs. Curve takes blue, AA curve is light green and BG curve for red.
1. Absorbance(Net value)
2. Atomic absorption value(AA value)
3. Background value(BG value)
4. Standard deviation
5. Relative standard deviation
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6. Measurement timer
7. Results for continuous integration mode
8. Results for peak height calculation mode
9. Results for peak area calculation mode
Use the up and down buttons for the changeover of the calculation mode between
continuous, peak height and peak area.
In the AAWin Pro software system, the measurements are made sequentially according
to the measurement table. After you finish your current sample, click “Start” from the
measurement window for the next sample. The current measuring sample in the
measurement table will be automatically changed to the next. If you are measuring the
last sample as the current sample, the system will add a new unknown sample in the
measurement table.
In the case of calibration curve preparation, system will draw up each point of the
standard samples on the graph of the calibration curve after sampling, and display the
final calibration curve together with the regression calculation results when all the
standards you have set in the measurement table are finished. See Fig. 3-77.
Next, you can measure the unknown samples. The measurement results will be
auto-filled into the measurement table. When you finish all the measurement of samples,
you may close the measurement window. If you need to save your measurement results,
select [File]—[Save] from the menu or click the toolbar“ ”。When you want to print them
out, select [File] —[Data Print] from the menu or click the toolbar“ ”for output, then
choose “from” in the pop-up window as for data source confirm.
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As furnace methods can provide sample analysis with much higher sensitivity than flame
method, please turn to the furnace method when you need to make measurements with
trace or super trace levels, where high sensitivity is preferred for analysis. Different from
flame method, furnace analysis does not require ignition but you need to make more
connections for gas tubing or water hoses. Before measurement, please carefully check
all the tubing for leaks. If you are making the first measurement for furnace analysis, after
you switch on the power of the instrument, you need to set the heat program first. Set the
temperature program, select [Measurement]—[Start] from the menu or click the
toolbar“ ”or just press F5 key. The system will change to the measurement window.
For furnace analysis, there will not be a signal profile displayed in the measurement window as
for flame method before you click the [Start] button from the window. From the first you
need to correctly load your sample into the graphite tube, you can then click “Start” for
running the furnace temperature program. In this time, signals begin to appear in the
measurement window, and the current furnace temperature, heat stage together with a
timer, which will indicate the time left for the heat stage, will also be displayed in the
window. Refer to Figure 3-80.
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injection can be performed. During this period, you cannot make any other operations through the
software. You can make a further measurement only when the timer is over. See Figure 3-81.
Like with the flame method, the standard deviation (SD) and relative standard deviation
(RSD) values will also be displayed after the third measurement (It is so called sampling
in flame method) in furnace analysis. As there may be a variety of factors including the
status of the instrument affecting the repeatability of the measurement results during
furnace process, some measure results may be unacceptable. In this case, you can
measure the sample for one extra time. You can just reload the sample, click with the left
key of the mouse on the last measure result and drag it onto the [Start] button and then
release the mouse to make a repetitive measurement of the sample. The former result
will then be overwritten by the newly measured result, the standard deviation (SD) and
relative standard deviation (RSD) values will also be re-calculated, refer to Figure 3-82.
Note that only when you have performed measurement of the same sample for 3 times
(inclusive) can you make a repetitive measurement. This can also be applied to the flame
method. However, as the flame method can generally give much better repeatability than
furnace method, this function may not be so commonly used especially in the “Automatic”
mode.
As furnace analysis may take you a much longer time for the measurement, you are
strongly recommended to follow the procedure exactly. After you complete your
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measurements, you can save your measure results or print them out. Other measure
steps are similar to that of the flame method.
The “Renew analysis” function is different from what we called the “Re-measurement” in
the above section. Re-measurement can be defined by the replacement or update of the
individual results for the duplicate measurements of one sample. The re-measurement
results will be taken for the calculation of the final result of the sample. Renew analysis;
however, can be regarded as the re-determination of the sample, which has already
been measured for a final result, i.e. the replacement or update of the final result.
If you find that some results are unacceptable or need to be further improved after you
have finished all the measure samples, turn to the renew analysis function of AAWin Pro
software. To do so, you first highlight the sample in the measurement table with the
mouse, then select [Measurement]—[Renew analysis] from the menu or right click on the
measurement table and select [Renew analysis] from the pop-up menu to make the
renew analysis. After the measurement, you may also leave the window open and click
[Start] again to make the renew analysis for a second time if you are not satisfied with
your measure result. You can keep doing so again and again until the measure result is
acceptable.
When you are satisfied with your renew analysis result, click the [End] button to close the
measurement window. If you continue making renew analysis of other samples, click the
toolbar button “ ”after you quit from the last renew analysis window.
While you make renew analysis of standard samples, the calibration curve will be
recalculated and refitted according to your renew analysis results.
When you have finished all the measurements and made a print-out of the measure
results or saved them to the disk, you can select [File]—[Exit] from the menu to quit from
the AAWin Pro software system. Before closing AAWin Pro system, a message box will
open to remind you to follow the proper procedure to shut down the instrumental system.
This warning message will always open every time you close the AAWin Pro software
system in case that you may forget to shut down the water, gas or electricity supply or
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take some safety precaution measures after you complete your measurement. Therefore,
you are assumed to follow exactly the shut-down procedure to quit from the analysis, i.e.
after finishing measurement and closing the AAWin Pro software, switch off the water,
gas and power supply immediately in case of any accident.
Through the reading of the former chapters, you are sure to understand the AAWin Pro
operation system for AA500 series atomic absorption spectrophotometer. In the next, we
will show a full measure procedure through an example.
Firstly, you should define the elements that need to be measured in the unknown
samples. We will here take the measurement of the Cu element in the sample as an
example to provide you the full measure procedure of the AA analysis. Prepare the Cu
element lamp, Cu standard solutions, blank and the unknown sample solutions. Check if
the pressures of the acetylene gas cylinder and/ or the argon gas cylinder are correct for
use. Before making a measurement, you should carry out all these preparations.
When the preparation work is ready, you can follow the following procedures to perform
the instrumental operations.
Step 1:Instrumental initialization
When you start up the AAWin Pro software, switch on the power of the AA computer and
run WINDOWS operating system first, and then double click the AAWin Pro software
icon on the desktop or click the AAWin Pro entry under the group of “AAWin Pro for
AA500” from the program group. The system will run the AAWin Pro software, and a
start window as below will open on the computer screen.
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This starting window will soon disappear when you turn on the power for the AA
instrument and connect the communication cable. If it is not the case, a message box will
open reminding you to check the connections. When all the connections are correct, click
“Retry” for re-connection with the AA main unit. The starting window goes off after the
communication with the AA main unit is successfully accessed.
A run mode selection box will open next for you to choose a run mode of the software
shown as below. Select “Online” from the dropdown box for a run mode selection and
click “OK” to enter into the instrumental initialization.
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The instrumental initialization is mainly aimed at the setup of initial parameters of the
individual drive motors including D2 lamp motor, HCL lamp motor, atomizer motor, burner
motor, slit width motor and wavelength motor. When an entry is successfully initialized, a
check mark will come up on the left beside the item; Otherwise, a cross sign will pop
up. If any one of them fail, the whole instrumental initialization will fail. In this case, a
message box will open after the initialization for you to choose whether you want to try it
again or not. You may enter “Yes” to continue or press “No” to exit the AAWin system.
Note: When you want to run the AAwin Pro software for a second time after you
exit the software without the cutoff of the AA main unit power, you can start it up
without a further instrumental initialization, supposed that you have already
performed the instrumental initialization successfully in the first time. In this case,
you can select the “Offline” mode from the pull down box for the run mode
selection and click “ok” to skip the initialization procedure and directly enter into
the operation system. Next you select “Online” mode from the [Application] menu
to make communication with the AA instrument. On the contrary, you can also
disconnect the AAWin software from the AA main unit when you perform in the
online mode. If the current mode is online, there will be a check mark beside the
“online” entry, otherwise, the check mark will not appear. In addition, the
specified element lamp needs to be lit up during the instrumental initialization,
and the light beam from the element lamp should pass through the atomizer
smoothly, otherwise, the wavelength motor initialization will fail. In that case, you
can’t perform the line search and therefore can’t make measurement.
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You can load the copper HCL lamp in the No.1 lamp turret and set it as the working lamp,
choose another turret number for the next element to be measured as the warm-up lamp,
then click “Next step” to set the element lamp parameters. If there is no Cu lamp mark
coming up in the lamp turrets, you can select one turret number (e.g. No.1) and unplug
the element lamp in this turret then insert the Cu lamp. Move your mouse to the turret
number position (No.1) and double click the turret icon entering into the element
selection box, see figure as below.
Point the mouse to the Cu element position in the periodical table and make a double
click or click the Cu element followed by pressing the ”ok” button in the popup box to
return to the element lamp selection window. You will see that the Cu element has
already been set on the No.1 lamp turret. Afterwards, click “Next step” to switch to the
element lamp parameter window.
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The parameters shown as above can provide a reference when setting the instrumental
parameters. You may set the instrument following the above values, or make a
modification according to the requirement for the measurement. The parameters needed
to be set are: the working lamp current, the warm-up lamp current, bandwidth and the
negative high voltage. Click the “Next step”, system will send the above parameters you
have set to the AA main unit through the instruction transfer window as follows:
After you have finished the above settings, the system will switch to the
wavelength setup page (see figure below). In this page, you can choose the
characteristic wavelength for the specified element and perform the peak
search. Select a resonance line from the dropdown box of wavelength and click
the “Peak-search” button, the system will perform the peak search for the
specified wavelength.
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Window for the peak search of the specified wavelength is shown as below:
When peak search is complete, click “Close” to quit from the wavelength setup window.
Press the “Finish” button to end up the element lamp setup and exit the setup guide.
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Use the left mouse key to drag the scroll bar back and forth for adjustment. After you
have set a position for the scroll bar, click [ok] to activate your setup. Check the
instrumental energy state until it shows the maximum value. If the energy exceeds 120%,
lower the instrument energy to 100% and then make adjustment to the atomizer position
until the energy indicates a maximum value.
“Correction method” is used to set the correction method for the standard samples.
The methods that are available are given as follows: calibration curve, standard
addition and interpolate method.
“Regression equation” is the calculation formula selected for the regression of
calibration curve of the standard samples, including “linear A=K1[C]+K0”, “linear
C=K1[A]+K0”, “square C=K2[A]2+K1[A]+K0” and “cubic C=K3[A]3+K2[A]2+K1[A]+K0”. This
section allows you to select a regression order for the calibration curve. Usually, a linear
(first-order) regression of the calibration curve is used for calculation of the measure
results.
“Concentration unit” is the unit used for the sample concentration. The units that can
be used are as follows: “ng/μl”, “ng/ml”, “μg/μl”, “μg/ml”, “mg/l”, “ppb”, “ppm”, “mol/l”. You
can also enter the unit by yourself.
“Sample identification (ID)” and ”Serial number” generally make up the sample
number. For example, Sample no. “S1” stands for the sample which has a Sample ID ”S”
and a Serial number “1”.
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After you finish the standard parameter settings, click “Next step” entering the page for
standard concentration setup referring to the following figure. You can enter the
concentration values into the concentration column of the standard list. Click “Increase”
to add the standard samples, you may add up to 8 samples in the standard list. Click
“Decrease” to remove standard samples, you should leave at least one standard sample
in the list.
After finishing the standard concentration setup, click “Next step” to enter into the
last page of the sample setup guide— the “unknown sample setup” page, see
figure as follows:
In this page, the following items will be set: number of unknown samples, sample ID and
a variety of coefficients or factors needed for concentration calculation or correction. In
the measure result table, one column entitled “Actual concentration” is listed. Its
calculation formula is as follows:
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You can carry out the calculation of the actual concentrations through the selection of
individual factors according to the sample situation. When you first open the sample
setup guide, all the factors or coefficients are set to 1.000 as the default values, i.e. if you
do not make any changes, the actual concentration will be the same as that calculated
from the absorbance of the sample. If you need to modify your settings, click the “former
step” button to edit the contents of the former pages. When you confirm that every
sample parameter has been correctly set and click the “Finish” button, the system will
transfer your settings into a measure table. You may next start to make a measurement.
Step 6: Set the measure parameters
Before making a measurement, you need to set the measure parameters first. Select
[Settings] — [Measurement parameters] from the menu or click the button from the
toolbar and you will open a dialog box for measure parameter settings. The dialog box
contain three optional pages, the first page is used to make regular parameter settings.
See Figure as follows:
You may set duplicate numbers for the “Standard” and “Unknown” samples in the
“Repeat number for measurement” section, the value of which is usually 1~3. If you set
the measure method to the Flame Analysis (Flame absorption, Flame emission, Hydride
generation) method, you can select “Manual” or “Automatic” as the “Operation mode”.
In the “Manual” mode, you need to press the keyboard manually to perform every
individual measurement. In the “Automatic” mode, however, the system will
automatically finish all the repetitive measurements through pressing the keyboard only
once at the very beginning. If you have chosen the “Automatic” mode, you need to set
the “Time interval” and ”Sampling delay” parameters.
“Time interval” is the waiting time for each sample uptake, it is usually set to be of 1~3
seconds.
“Sampling delay” is the waiting time taken before auto-sampling, i.e. the pre-spraying
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In this page, you can set the display boundary of absorbance in the measure graphs, i.e.
the lower and upper limits of the vertical / longitudinal axis. Generally, a lower limit with –
0.1 and an upper limit with 0.6 are set.
“Refresh time” is the maximum time period during which the real time profile can
continuously be displayed in the measure graph in flame mode, namely the threshold of
the time axis. It is generally set to be 300 seconds, that is, the real time profile will be
renewed every 300 seconds,
The third page “Data processing” is used to set the signal processing parameters, refer
to the following figure:
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In this page, you can choose the data calculation mode from the “Calculation mode”
pull down menu box. In flame mode, the calculation mode “continuous” is commonly
used; in furnace mode, however, “peak height” or “peak area” is often selected.
Input the integration time for your measure data in the “Integration time” box. In flame
mode, an integration time of 1-3 seconds is usually selected. However, you need not set
the integration time in furnace mode. In that case, the system will automatically take the
total sum of the heating time in the atomization stage and the last three seconds in the
former step (the ashing stage) from the furnace temperature program as the default
integration time.
“Filter factor” is a constant which needs to be given to filter the acquired data, i.e. the
flatten factor. In flame mode, a filter factor of 0.1~1.0 is often used, in furnace mode, it is
usually set to 0.1.
Step 7: Perform Measurement
A.Flame analysis
In the case of flame analysis, before you make measurement, switch on the power of the
air compressor and regulate its pressure to 32psi, turn on the acetylene gas cylinder and
carefully check all the tubing for gas leaks. When everything is O.K, select
[Application]—[Ignition] from the menu for igniting the flame. When the flame height is
too high or too low or if the burner is not set in the correct position, turn to the “Burner
parameter setup” for adjustment. Select [Measurement]—[Start] from the menu or
click the button“ ”from the toolbar or just press F5 key to open the measurement window,
then the analog signal should be seen in the real time graph. Refer to Figure as follows:
Prepare the blanks, the standard solutions and the unknown samples in the front of,
sampling capillary into the measure sample solution until the displaying data or signal is
stable, then click the [Start] button to read samples. If you have chosen a Manual mode
from the measure parameter setup window, you need to press the [Start] button again for
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another measurement after you finish every single sampling operation. In the case of
Automatic mode, however, the system will automatically take the sampling process
according to your setting of the “Time interval”. After you finish the readings, the system
will display the results in the measure window and standard deviation (SD) and relative
standard deviation (RSD) values will also be calculated and displayed in the window after
the specified repetitive reading. After you perform the readings for the set number of
measurements, the system will calculate the mean value of the measure results and
display it in the correct cell
1. Absorbance(Net value)
2. Atomic absorption value(AA value)
3. Background value(BG value)
4. Standard deviation
5. Relative standard deviation
6. Measurement timer
7. Results for continuous integration mode
8. Results for peak height calculation mode
9. Results for peak area calculation mode
During the measurement, you can check the total time used for your analysis through a
timer placed on the upper right of the measurement window. You can also insert a blank
before each sample for zero check. Click the “Zero” button to make zero adjustment.
Press the “End” button when the measurement is finished. If you have selected D2 lamp
or SR mode for the background correction, AA and BG values will be displayed together
with the absorbance (net value) in the measurement window. The AA and BG curves will
also appear in the real time graph. In this case, the absorbance is the difference
subtracting the BG value from the AA value (Abs. = AA - BG). If no background
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correction is used, the system will display the absorbance and provide the Abs Curve
only. In this situation, the abs. is equal to the AA value (Abs. = AA). Curve color in the real
time graph can be set through the function of the “Graph Setup”. In the case of default,
Abs. curve takes blue, AA curve is light green and BG curve for red.
When measuring the standard samples, the system will draw each point of the standards
on the graph of the calibration curve, and will display the final calibration curve on the
graph when all the standards are finished. See Figure as follows:
After the measurement of your standard sample series is complete, double click the
“calibration curve” box to check the calibration curve. If there are any points showing a
large offset from your calibration curve, you can measure them for a second time. After
preparing the calibration curve, you may next perform the measurement of your unknown
samples. The measurement results will be auto-filled into the individual unit elements of
the measurement table. In the AAWin software system, measurements are made
sequentially according to the measurement table. After you finish your current sample,
click “Start” from the measurement window for the next. The current measuring sample
in the measurement table will be automatically changed to the next. If you are measuring
the last sample as the current sample, the system will add a new unknown sample in the
measurement table for you to continue your measurement.
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The furnace heat program generally includes four temperature elevation stages namely
drying, ashing, atomizing and cleaning.
Drying: temperature 100-120C, heating time 5-20s,hold time 5-20s,inner gas flow
rate is set to high;
Ashing: temperature 200-2000C (according to the measure element) heating time
1-15s,hold time 5-15s,inner gas flow rate is set to high;
Atomizing: temperature 1400-2700C (according to the measure element) heating time
0-1s,hold time 2-5s,inner gas flow rate is set to close/none;
Cleaning: temperature is set to equal to or slightly higher than the atomization
temperature heating time 0-1s,hold time 1-2s,inner gas flow rate is set to
high.
Note: After setup of the heat program, you must click “confirm” to exit.
First select [burn], from toolbar, then select [Measurement]—[Start] from the menu or
click “ ”from the toolbar or just press F5 key. The system will change to the
measurement window.
For furnace analysis, no signal profile will be displayed in the measurement window
before you click the [Start] button. Using a pipette, load your sample of 10-20µl into the
graphite tube, then click [Start] for running the furnace temperature program. In this time,
signals begin to appear in the measurement window, and the current furnace
temperature, heat stage together with a timer, which will indicate the time left for the heat
stage, will also be displayed in the window. Refer to Figure as follows:
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You can choose the D2 lamp background correction mode from the list box and click [OK]
or [Execute], the system will immediately set the D2 lamp mode as the current
background correction mode. From its current input box you can set the D2 lamp current
according to your own requirements. The D2 lamp current is usually set to a value of
20-60mA. When you choose SR lamp to perform the background correction, you can
enter the wide and narrow pulse current values for the SR lamp in their input boxes.
Refer to Figure as follows:
Note: When the D2 lamp is used to perform the background correction, it should
never be used for long period of time with high current. When your measurement
is finished, shut down the lamp power as soon as possible in order to extend its
useful life period.
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In the case of the D2 lamp as the background correction mode, you need to perform the
beam balance, adjusting the D2 lamp energy to be matched with that of the element HCL
lamp. From the system shortcut icons, click the “Energy” icon to open the energy
adjustment box. Click “Advanced adjustment” to open the advanced adjustment box,
referring to the following figure. Select the D2 lamp mirror motor and click the “positive
rotation” or “Reverse/Back turn” button to adjust the energy of the D2 lamp to its
maximum position. When finished, check the adjustment result. If the D2 lamp current is
larger than 120mA, reduce the element lamp current and click “Auto energy balance”
again for a second beam balance in order to extend the D2 lamp’s service life.
B. SR background correction
When you choose the SR background mode, click “Auto energy balance” to perform the
beam balance. See the following figure.
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You can input the lamp current and high voltage to perform an energy balance.
When you have completed the analysis with background correction, switch the current
background correction mode to no BGC mode as soon as possible to reduce lamp
deterioration.
After completing the analysis, you can perform data processing for the individual
measured results and make a report output for the total results. Contents of each
parameter setting and measurement results can be output to the printer and stored.
If you need to save your measured results in a file, select [File]—[Save] from the menu
or click the“ ”button from the toolbar, see figure as follows.
“Save”:Store the content of the current measured results table in a file. When the “Save”
function is selected, the system will open the “Save as a file” dialog box, refer to figure
above. Enter a file name to be stored in the “File name” box and click “Save”, the system
will store the measured results in the specified file. If the file name you have input already
exists, the system will prompt a warning message to ask you weather you want to
overwrite it or not. When choose “Yes”, the existing file will be overwritten. Otherwise, the
system will cancel the operation of saving the measurement results.
“Print”:This function provides you with outputting your data and graphs to the printer.
Selecting “Print”, the system will open the ”Select the output report type” box, see
figure as below. Specify the type of the output report and click “OK”, the contents of the
current output report will be printed out.
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¾ Measure curve:This function allows outputting the current measure curve to the
printer.
¾ Signal curve:Selecting this function, the current signal profile will be printed out.
¾ Calibration curve:The current calibration curve will be printed out.
¾ Search peak/Scan curve:This function is to print out the current wavelength scan
or line search graph.
¾ Selected sample:The sample data in the current cursor position of the measured
results table will be printed out.
¾ Measure table:This function will allow all data in the measured result table to be
printed out.
¾ Work parameters:This will allow you to output the current operation conditions of
the instrument together with the measure parameters to the printer. If you need to
preview the contents to be printed out, click “Preview” to open the “Print preview”
window, as shown in the following figure.
¾
When you need to print them out directly, click the“ ”button. In the case that a
measured table is selected, you can use the“ ”or“ ”button to browse through the
entire measurement data in the table. Click“ ”to close the “Print preview” window.
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When the flame analysis is complete, turn off the acetylene gas supply and spray a
blank solution for several minutes to clean the nebulizer. Switch off the air compressor.
When the graphite furnace analysis is complete, turn off the argon gas supply and
cooling water. Check and clean out all the standard and unknown samples and organize
your measured results in the report.
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D. The energy is low for peak searching and the high voltage is
overflow
Trouble-shooting
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Problem: the flame is not lit when “ignition” is selected but the igniter does discharge.
Check:
1. Check whether there is acetylene gas in the pipeline of the instrument. Check if the
acetylene gas cylinder is open and the pressure is correct; you can check whether the
acetylene gas has entered into the instrument by selecting ignition a number of times.
Sometimes it take more than 6 ignition selections to ignite the flame if it is a new
installation or the gas pipe lines are empty.
2. Check whether the burner is at the correct position.
3. Check whether the gas flow is more than 1500ml/min,open “burner parameters
setting” to confirm. .
4. Check whether the exit pressure of the air compressor is proper.
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the beams don’t coincide, then open the left cover of the instrument and adjust the
setting screw to make the beams overlap.
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4. Check if there is any salt substance on the burner blocking the burner slit.
5. Check if there is anything clogged in the drainage tubing system.
6. Check if the water sealing in the waste tubing system is defective.
7. Check if the exhaust rate for the ventilation system is set too high.
8. Check if there is any draft blowing around the instrument.
J. BGC compensation too low or insufficient in case of the D2 lamp
background correction mode.
Trouble-shooting:
1. Mainly check the two beams from the element lamp and the deuterium lamp are
completely overlapped.
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N. The wavelength has moved or its reading accuracy does not satisfy
the specification of no more than ±0.3nm
Trouble-shooting:
1. Use the “wavelength correction” button for the AAWin software system to make
adjustment. Details about the operation of wavelength correction please refer to section
5.5 wavelength correction in this instruction manual.
2. Please contact with the supplier if the deviation is still more than ±0.3nm.
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E. Gas flow path blocked, no gas can flow through or be cut off during
the furnace test
Trouble-shooting:
1. Check if the power control connections from the furnace have been correctly
attached and if there are any pin connection bent or broken.
2. Check if there are any solenoid valves (electromagnetic valve) defective or their
connections damaged by removing the power supply cover. Note: Always make
sure that the electrical power is turned off when removing the cover.
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instruments
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