Procedure instrumentation and reporting of Inorganic sample By AAS

1. Principle:

Atomic absorption spectroscopy (AAS) principle is based on the absorption of light at

specific, unique wave lengths by atoms in the gaseous state, The amount of light absorbed at
this wavelength is directly proportional to the concentration of the absorbing ions or atoms
present in solution.

In GFAAS, a type of electro thermal atomization, a sample is placed in a hollow graphite

tube which is heated until the sample is completely vaporized. GFAAS is much more
sensitive than FAAS and can detect very low concentrations of metals (less than 1 ppb) in
smaller samples. Using electricity to heat the narrow graphite tube ensures that all of the
sample is atomized in a period of a few milliseconds to seconds. The absorption of the atomic
vapor is then measured in the region immediately above the heated surface. Naturally, the
detection unit does not have to contend with spectral noise, leading to improved sensitivity.

Formation of Atomization, hollow cathode lamp, mono chromator and detector are the main
components in atomic absorption spectroscopy instrumentation.

2. Applications:
The AAS is used for identification, detection, determination of metal elements
1. Ag(Silver)
2. Al(Aluminium)
3. As (Arsenic)
4. Au (Gold)
5. B (Boron)
6. Ba(Brium)
7. Be(Berelium)
8. Bi (Bismuth)
9. Ca(Calcium)
10. Cd(Cadmium)
11. Co (Cobalt)
12. Cr (Chromium)
13. Cs (Cesium)
14. Cu(Copper)
15. Dy (Dysprosium)
16. Er (Erbium)
17. Eu (Europium) 33. Mo(Molybdinum)
18. Fe(Iron) 34. Na(Sodium)
19. Ga (Gallium) 35. Nb (Niobium)
20. Gd (Gadolinium) 36. Nd (Neodymium)
21. Ge (Germanium) 37. Ni(Nickel)
22. Hf(Hafnium) 38. Pb(Lead)
23. Hg(Mercury) 39. S(Sulpher)
24. Ho(Holmium) 40. Sb (Antimony )
25. In (Indium) 41. Se(selenium)
26. Ir (Iridium) 42. Si(silica)
27. K (Potassium) 43. Sn(tin)
28. La (Lanthanum) 44. Sr(strontium)
29. Li (Lithium) 45. V(vanadium)
30. Lu (Lutetium) 46. Ti(titanium)
31. Mg (Magnesium) 47. Zn(zinc)
32. Mn(Manganese) 48. Zr(zirconium)
Procedure instrumentation and reporting of Inorganic sample By AAS

3. Safety:
Laboratory should provide the following personnel protective equipment’s to the testing
personnel’s
Cartridge mask
Gloves
Heat resistant gloves
Tongs
Eye washer
Safety shower

4. Machine Operation:
Steps to be followed to analysed Sample:
a. Switch on the fume hood
b. Switch on the air Pump System(330 to 370kpa) 2.4 l/min
c. Switch on the computer
d. Turn on the Acetylene gas(55 to 96 kpa),1.2 L/min
e. Switch on the AAS System
f. Ignite the burner and leave the system for 30 min for optimization
g. The working area must be completely clear of all hazardous materials including
corrosive liquids and flammable solvents.
h. The liquid trap is filled with the same solvent as will be used in the sample matrix.
i. The drain tubing is positioned sloping downwards and is free of kinks or sharp bends
so that the waste liquid can drain freely into the vessel. The end of the tube must be
above the expected level of waste liquid in the vessel.
j. Vent tube is installed, if necessary..
k. The exhaust system is operating.
l. Gasses are turned on and set to the correct pressures as per the specifications.
m. If fitted, the heater on the N2O regulator is turned on.
n. The correct burner is fitted.
o. The flame shield, front panel and chimney have been fitted.
p. The pressure relief bung has been lubricated with distilled water and installed
correctly.
q. All O-rings have been inspected. Immediately replace any O-rings that are cracked or
deformed.

5. Preparation of Standard:

Prepare the standard linearity solutions as per the test method.

6. Preparation of samples
Prepare the samples as per the test method along with method blank, reagent blank, QC
and Spike

7. Operational Software :

To start the SpectrAA software double-click

on the desktop SpectrAA icon (created
during the installation of the software). .
Procedure instrumentation and reporting of Inorganic sample By AAS

Index Page:

When start the SpectrAA software, the first screen to appear is the introductory screen. The
Index page contains four buttons: Worksheet, Reports, Administration, and Exit.

The function of each button is as follows: Worksheet Opens the Worksheet window

Reports opens the reports window allows to generate a report for the current worksheet or
any of the worksheets saved in the system. The Reports window consists of four tabbed
pages: Worksheet, Select, Settings, and Report. To select a particular

Administration Opens the Administration window The Administration window allows to:
migrate worksheets into the system (such as old worksheets on CD-ROM, etc.); delete
worksheets and library methods; and activate and modify password protection of the system.
The Administration window also allows to configure system.

Exit Shuts down the SpectrAA software..

Click on the Worksheet and will see a pop-up window.

The Worksheet window allows to develop and

edit methods, sequences and labels, and initiate
sample analysis. The worksheet is the
fundamental file type for SpectrAA, containing
one or more methods, sample labels, sequence
information, and analytical results. load an
existing worksheet or develop a new one. The
Worksheet window consists of four tabbed
pages: Filing, Develop, Labels, and Analysis. To access a particular page, click on the
appropriate page tab appearing under the menu bar.

Select one of the options to open or create a work

sheet. It contains filling page, develop page, labels
page and analysis page

The Filing page

Use the Filing page to perform basic worksheet

operations such as opening, saving, and closing
worksheets, creating a template from a worksheet,
and loading worksheets. view information about the
worksheet currently open.

The Develop page

Procedure instrumentation and reporting of Inorganic sample By AAS

Use the Develop page to add, delete, review and modify methods, modify sequence
parameters, change the order of methods and copy methods to the Method Library.

Refer page no 4

The Labels page

Use the Labels page to set up solution labels, weights, volumes, and dilution
factors and to configure SPS or PSD samplers.

The Analysis page

Use the Analysis page to control the AA and initiate analysis. Data is presented in
the form of a spread sheet, with one row per sample. The sample labels are
displayed in the left-hand column with concentration results for each element
across the remaining columns.

The SpectrAA software enables to have up to a maximum of 10 worksheets open at the same
time. The Worksheet tab at the bottom of the Analysis page enables to switch between
worksheets.

Worksheet menus
When viewing the worksheet, the following menu items are available:
File
This menu allows to perform filing tasks such as opening, saving and renaming files.
Edit
The Edit menu allows to copy and paste information, Edit Replicates and Go To certain parts
of a worksheet.
View
The View menu enables to nominate what is displayed on the Analysis page.

Instrument This menu enables to perform many Instrument functions such as Optimization,
Reslope, and Zero.

Options

The Options menu enables to alter the displays on the Analysis page.

Window This menu enables to quickly move around the

software.

Help This menu enables to access the Help topics

Go to the Develop folder. If you are working with a new

worksheet, now you need to add a method. Select the
element that you are going to test and make sure that the
Flame box is checked (Our instrument is a flame AAS)
Procedure instrumentation and reporting of Inorganic sample By AAS

If working with a worksheet created from a template, you can also add a method to your
worksheet.

In the Develop folder, select the Edit Method to

set up the measurement parameters.

Labels folder gives the ability to label each of sample.

After entering the weight and volume in labelling

window Go to the Analysis window.

Clean the burner by inserting an index card

(provided) into the slit and sliding the card left and
right for a few times until it is clean.

Light up the flame by press the black flame button

that is located at the lower left corner on the front
panel of the instrument.

Note: (a) wait until a stable flame is established before measurement. (b) Press the red
button next to the flame button will turn off the flame.(c) The flame can be lit up only when
open a worksheet.

Click the Optimize button and follow the instructions

provided by the software to optimize the lamp
position. In order to obtain the best signal-to-noise
level, try to adjust the lamp position using two screws
at the bottom of the lamp base to get the highest HC
lamp (the green bar) with the lowest Gain.

The lamp will be turned on at this time if it is not in the

on status. Click the rescale button after adjustment of
lamp position.
This is needed to reset the gain.
 Procedure instrumentation and reporting of Inorganic sample By AAS

Adjust the flame height to gives the optimum signal intensity.

After performed the optimization, measure the

samples by selecting analysis window.

Clicking the Start button. The software gives

instructions to proceed further steps.

(a) Firstly, the instrument measures the

absorbance of standard solution to
create a calibration. For example, if
standard concentration is 50µg/ml, and
specify 4 standard counts, the SIPS
dilutes standard to 25 %, 50 %, 75 %
and 100 % of standard concentration to
measure the corresponding absorbance and obtain 4 data point to establish a
calibration curve.

(b) Next, place sample solution for test. If the concentration of sample solution is below
the standard, the result is obtained and shown in the Analysis window. If sample is in
the over range, the SIPS will perform a dilution to make the concentration of the
testing analyte within the standard range, then a test is done and the concentration of
sample is recorded. However, if the concentration of sample is beyond the largest
dilution factor that the SIPS can do, the calibration will fail. In this case, an error flag
will be displayed in the data cell, for example, “1366.89D”.
After measurement of samples, make sure to save results. The software will
automatically save worksheet with results when close the worksheet or exit the
SpectrAA.
Inject distill water after sequence completion as a maintenance procedure. It just
rinses the capillary tube, the liquid trap, the spray chamber and the burner to remove
any residual of previous sample.
Turn off the flame by press the red button next to the flame button. When turn off
the flame, a warning message on the screen telling that the SIPS is stopped because
the flame is off. This is normal.
view or print result. To do so, go to the Window menu and select the Report, then
select worksheet and Report, window like this will generates
 Procedure instrumentation and reporting of Inorganic sample By AAS

There is no software control to turn off the lamps except switch the lamp. The lamp is off
when exit SpectrAA.

8. Exit SpectrAA.
9. Turn off the power of the instrument.
10. Close the Acetylene valve and turn off the Air valve.
11. Clean up all testing solutions.
12. After 10 min turn off fume hood.

The detail information about the use of the software and some explanations about the use of
this instrument can be found in the on-line help in the SpectrAA.

Calculation
Total lead (Pb) content, mg/kg = (C/W) × V × F
% = (C/W) × V × F × (1/10000)
where C = concentration of Pb in the sample solution ( mg/L)
V = volume of sample solution (mL)
F = dilution factor if necessary
W = sample weight (g)

13. Reporting Criteria

10.1. Requirement
Total lead content should not exceed 100 mg/kg (0.06%) or 90 mg/kg (0.009%)* for paints
and surface coating materials.
 Procedure instrumentation and reporting of Inorganic sample By AAS

(Note: * The Consumer Product Safety Improvement Act of 1008 (CPSIA) requires the
regulatory limit for lead in paint and other similar surface coatings to be reduced from
0.06% to 0.009% on August 14, 2009.)
Remarks:
1.If total lead content is greater than the requirement, the result shall be verified by another
technique (e.g. ICP-MS, see Appendix 2).
2.Any sample possibly having greater than 80% of the limit for lead in paint in any of the
composited paints should be retested individually.

10.2. Reporting Limit for total lead content is 10 mg/kg or 0.001%.

14. Trouble Shooting:

(a) For Low sensitivity
Alignment should be checked – gain setting should be consistent
Lamp type can improve performance e.g. using high intensity UltrAA lamp
Burner position must be optimized (vertical, horizontal & rotational positioning)
Check the lamp current

(b) System Cleanness issues

Deposits in nebulizer can reduce sample uptake rate
Solid material on burner slot reduces path length and increases noise
Contamination in spray chamber impacts on aerosol formation – increases noise

(c) On Flame systems, also clean the front panel and flame shield. If necessary, use a mild
detergent to clean the cover. Do NOT use an abrasive cleaner. When analyzing biological
samples, wipe the instrument with chlorhexidine in 95% ethanol.

Windows Clean the sample compartment windows and the lamp compartment window
with a gentle stream of filtered air, or a puffer brush, like those used to clean camera
lenses.
If the windows are dirty, wipe them using an optical tissue held between tweezers and
dampened with a 50% ethanol/water solution.
Filters Check the filter in the air compressor supply line and clean if necessary

15. Recommended Maintenance :

Furnace AA
Rec. Maintenance Schedule Daily:
Empty waste container
Check exhaust system
Check condition of the graphite tube – replace as necessary – When replacing the
tube, check the condition of the electrodes
Clean the work head around the sample injection hole
Check dispensing capillary “free” and syringe
Top up rinse reservoir as required.

Gas cylinders
Change gas cylinders according to the instructions supplied by the manufacturer. When
changing gas cylinders:
Procedure instrumentation and reporting of Inorganic sample By AAS

Inspect all gas supply pipes and hoses. Replace any hose showing signs of damage or
deterioration.
Test all connections for leaks using a commercial leak testing solution, a mild dish washing
soap solution, or an electronic leak detector.
Test the operation of all regulators.
Ensure that shut off valves are correctly functioning.

AAS Maintenance Schedule

Daily – before operation
 Check that the exhaust system has positive extraction
 Check the gas supplies
 Check all hoses and connections for damage, leaks and wear
 Ensure end of the drain tube in not immersed below the liquid level in the drain vessel
Daily – after operation
 Clean the instrument
 Clean the burner (Flame systems only)
 Rinse out the spray chamber and liquid trap (Flame systems only)
 Check graphite components including the shroud, electrode, and tube (Furnace/Zeeman
systems only)
 Clean the electrodes (Furnace/Zeeman systems only)
 Replace the tube if necessary (Furnace/Zeeman systems only)
 Empty the drain vessel
 Turn off the gas supplies at the regulator

Weekly
 Check for O-ring deterioration:
Three O-rings inside the burner, spray chamber, and the bung

 Two o-rings that seal the gas inlets to the spray chamber
 Procedure instrumentation and reporting of Inorganic sample By AAS
16. Error Codes description:
30601 - Instrument fault
30602 - Power failure
30603 - Chopper sync error
30604 - Wavelength invalid for
PMT
30605 - Low HC lamp energy
30606 - High HC lamp energy
30607 - Instrument status
message
30608 - Low lamp energy
30609 - High lamp energy
30610 - No peak detected
30611 - Lamp turret home
fault
30612 - Lamp turret sensor
fault
30613 - Lamp turret fault
30614 - Lamp turret home
sensor fault
30615 - Invalid position
30616 - Lamp not recognized
30617 - EHT over-range
30618 - Magnet overheated
30619 - Low D2 lamp energy
30620 - High D2 lamp energy
30621 - Magnet not connected
30622 - Mono home sensor
fault
30623 - Slit drive home sensor
fault
30624 - Slit drive home not
found
30625 - Slit drive detents not
found
30626 - Invalid slit settings
30627 - Slit drive detent sensor
fault
30628 - No burner fitted
30629 - Wrong burner
30630 - Spray chamber fault
30631 - Flame shield open
30632 - High air reservoir
pressure
30633 - Low air pressure
30634 - Oxidant pressure fault
30635 - Low oxidant pressure
30636 - Flame sensed
30637 - Flame out
30638 - Flame failed to ignite
30639 - Flame control offline
30640 - Autoadjuster home
sensor fault
30641 - Autoadjuster home
sensor not found
30642 - Flame pressure relief
bung
30643 - Liquid trap not ready
30644 - No lamp current
detected
30645 - Background lamp
failed
30646 - Background lamp
interlock