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Flame Techniques
Practical experiments.
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Solutions
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
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
Gas Flows
Copper
Calcium
Chromium
Absorbance
Copper
Calcium
Chromium
Discussion
1.
Describe the different readings and when to use each nebuliser mode
2.
3.
Would you expect to see differences in gas flow settings for the different
nebuliser settings?
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Iron
5
10
15
20
Nickel
5
10
15
20
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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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.
4.
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.
2.
Why is there a difference in the signal noise with the different gases.?
3.
4.
Would you expect the effect to increase or decrease with changes in relative
concentrations of the interferent and analyte.?
5.
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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.
2.
Could the non-zero calibration algorithms be used to correct for the offset in the
results caused by the non-specific absorbance?
3.
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.
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
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.
3.
4.
What does analytical problems does the method of standard additions correct
for?
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