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Atomic Absorption Training Course

Flame Techniques
Practical experiments.

Varian Australia Pty Ltd 1988


Prepared by John Sanders
Version .0 (1999)

1. SETUP AND OPTIMISATION.......................................................................................2


CALIBRATION AND CURVE FIT ALGORITHM.............................................................3
2. CHARACTERISTIC CONCENTRATION AND DETECTION LIMIT............................5
3. CHEMICAL INTERFERENCES....................................................................................6
4. NON-SPECIFIC ABSORBANCE INTERFERENCE.....................................................8
5. FLAME EMISSION........................................................................................................9
6. STANDARD ADDITIONS............................................................................................10

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1. Setup and Optimisation


Aim
This experiment is designed to illustrate the techniques and operations required to
optimise for different modes of flame operation:
Air/Acetylene flames
Nitrous Oxide Acetylene Flames
Each at the following nebuliser settings
High Dissolved Solids and Maximum Sensitivity settings

Solutions

Standard Copper solutions 5ppm in 0.1% HNO 3


Standard Calcium Solution 1.0ppm in 0.1% HNO 3 2000ppm CsCl2
Standard Chromium Solution 5ppm

Procedure
Create a manual sampling worksheet with the three elements Cu, Ca, and Cr.
Select the following conditions:
Cu

Air/Acetylene Gases

Cr and Ca

Nitrous Oxide Gases

For each Gas combination determine the gas flows and nebuliser settings to provide
the following:
Max Sensitivity
Air/Acet
N2O/Acet
air
acet
N2O
acet

High Solid Setting


Air/Acet
N2O/Acet
air
acet
N2O
acet

Gas Flows
Copper
Calcium
Chromium
Absorbance
Copper
Calcium
Chromium
Discussion
1.

Describe the different readings and when to use each nebuliser mode

2.

Describe the limitations of each nebuliser setting.

3.

Would you expect to see differences in gas flow settings for the different
nebuliser settings?

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Calibration and Curve Fit Algorithm


Aim
This exercise illustrates the different calibration curvature and the algorithms used in
producing linear calibration
Solutions
Multielement standards prepared in 0.01% HNO3
Copper
2
4
6
8

Iron
5
10
15
20

Nickel
5
10
15
20

Hollow Cathode Lamps


Cu, Fe, and Ni hollow cathode lamps
Multielement Cu, Cr, Fe, Ni, Co, Mn Multielement Lamp
Setup
Create a worksheet with methods for Fe, Ni and Cu, for manual sampling with
Concentration Readout and PROMT mode with 0.5% precision
In Sequence control turn OFF the QC Tests
Procedure
Optimise each method, for maximum sensitivity.
Start an autorun and read each calibration set , read the standards as samples
After the run has finished, use the Curve Fit setting in the calibration graph and
record the results for each of the calibration algorithms. Which provide better readback
of the standards as samples? Fill in the table below for each calibration algorithm.
New

Rational

Linear

Rational
Copper
2
4
6
8
Iron
5
10
15
20
Nickel
5
10

Linear
Origin

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Quadratic

Quadratic
Origin

Cubic

Cubic
Origin

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15
20
Discussion
1. Explain the difference between the value of the standards and the readback of the
standards as samples.
2. How would you choose the "BEST" algorithm?
3. Why did we turn OFF the QC Test in the Sequence protocol?

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2. Characteristic Concentration and Detection Limit


Aim
To measure the characteristic concentration and detection limit of the instrument for
copper, iron and nickel..
Solutions
Standard Solutions: Multi Element Standard
Copper
2
4
6
8

Iron
5
10
15
20

Nickel
5
10
15
20

Procedure
Setup a worksheet with 15 samples and the three elements shown above.
Optimise each element for maximum sensitivity and run the autorun.
Using Deionised Water for the samples
From the parameters read the Characteristic Concentration for each method
Read the concentration of the DI water for all 15 samples.
Calculate the standard Deviation of each method, and calculate the Detection Limit.
Discussion
1.

What would you expect the precision of the detection limit solution?

2.

At what concentration would you limit the reading of solutions, ie the sample
reading is significantly different to a blank?

3.

At what concentration would you expect a precision of 10% RSD?

4.

Does the Characteristic Concentration differ from the published figure?

5.

What effect would you expect to see on the detection limit and characteristic
concentration if you used the high solids setting of the nebuliser?

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3. Chemical Interferences
AIM
To illustrate the problems seen with chemical interferences and means of reducing the
effects.
Solutions
Calcium Standards:
0,1,2,3,5 mg/L Calcium standards
0,1,2,3,5 mg/L Calcium standards each with 2000mg/L Cesium Chloride
Samples:
3mg/L Ca Solution
3mg/L Ca solution with 10mg/L P
3mg/L Ca solution with 10mg/L P, 2000mg/L Cs
3mg/L Ca solution with 10mg/L P, 2000mg/L Cs, 2000mg/l LaCl3.
3mg/L Ca solution with 100mg/L Al and 2000mg/L CsCl, and 2000mg/l LaCl3.
Procedure
Create a worksheet with four identical Calcium methods all manual sampling, use the
following method details and layout:
Method1
Gas Mixture
Air/Acetylene
Matrix/Standard Set
No Cesium
Create a label set of 13 Samples

Method 2
N2O/Acetylene
No Cesium

Methods 3
Air/Acetylene
Cesium

Method 4
N2O/Acetylene
Cesium

Using each standard set matrix record a calibration using the relevant standard
solutions and readback the standards and 3ppm samples. Record the results.

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Method1
Air/Acetylene

Method 2
N2O/Acetylene

Method 3
Air/Acetylene

Method 3
N2O/Acetylene

Standard 1
Standard 2
Standard 3
Standard 5
Standard 1+Cs
Standard 2+Cs
Standard 3+Cs
Standard 5+Cs
3 Ca
3 Ca+10P
3 Ca + 10P
+2000Cs
3 Ca + 10P
+2000Cs+2000
La
3 Ca + 100 Al
+2000Cs+2000
La

Discussion
1.

Discuss the differences in calibration curvature.?

2.

Why is there a difference in the signal noise with the different gases.?

3.

What types of interferences are shown?

4.

Would you expect the effect to increase or decrease with changes in relative
concentrations of the interferent and analyte.?

5.

Discuss the differences in the results when nitrous oxide/acetylene is used


relevant to air/acetylene?

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4. Non-Specific Absorbance Interference


Aim
To illustrate the effect of background absorbance on the analytical process.
Solutions
0, 0.1, 0.2, 0.3 Zn standards
Samples
0.2mg/L Zn
0.2mg/L Zn + 5%KBr
0.2mg/L Zn + 5%NaCl
Procedure
Create a worksheet with two Zinc methods and six samples, The only difference
between the two methods will be the OPTICS page where the second method will have
Background Correction BC=On, in the other method Background Correction BC=Off
Optimise the instrument and adjust for maximum sensitivity.
Start and autorun and read the standards and samples.
Record the results:
BC=Off

BC=On

0.1 Standard
0.2 Standard
0.3 Standard
0.2 mg/L Zn Sample
0.2mg/l Zn 5%KBr
0.2mg/l Zn 5%NaCl
Discussion
1.

What is causing the apparent difference in readings?

2.

Could the non-zero calibration algorithms be used to correct for the offset in the
results caused by the non-specific absorbance?

3.

Will the use of background correction improve the accuracy of any


measurements?

4.

What affect will background correction have on the detection limit and sensitivity
of the instrument.?

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5. Flame Emission
Aim
To illustrate the use of flame emission measurements for alkali elements
Solutions
0, 0.5, 1.0 and 1.5 mg/l Sodium solutions.
Procedure
Create a worksheet with two methods for Sodium, in one method set the Instrument
mode to Absorbance in the other set the mode to emission.
Independently optimise each method and create a calibration, reading the calibration
solutions as samples.
Rotate the burner 90o and repeat the measurements
Discussion
1.

Are the calibrations linear?

2.

What effect did burner rotation have on the calibrations and the precision of the
readings?

3.

Which method would you expect to give the better precision? Why?

4.

Which method would you expect to give the better accuracy? Why?

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6. Standard Additions.
Aim
To illustrate the use of the standard Additions calibration method and illustrate where it
can be used.
Solutions
0, 1.0, 2.0, 4.0 mg/l Iron Standards
Spiking solution
10mg/l iron standard
Samples
10% Solution of ethyl alcohol in water samples spiked with 1.0 and 2.0mg/L of iron.
Procedure
Create a worksheet with four iron methods.
In the first two use normal concentration mode for calibration one method with
background correction, the other with no background correction,
In the remaining two methods select standard additions calibration mode, one method
with background correction, the other with no background correction,
You will need to take care in using the correct label sequence and naming of solutions.
Also be careful in selecting the samples to be analysed in the worksheet.
Measure the iron concentration of the samples using both procedures.
Measure the nebuliser uptake of the blank water and the sample.
Conc Mode

Std Add Mode

Std Add + BCG

Sample
Sample + 1mg/l Fe
Sample + 2mg/l Fe
Sample + 4mg/l Fe
Discussion
1.

Are the graphs for the standard addition calibration and the normal concentration
calibration parallel? Why?

2.

Are the results different if background correction is used?

3.

Does standard additions correct for background interference?

4.

What does analytical problems does the method of standard additions correct
for?

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