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Suggested Answer For Tutorial 3

The document provides answers to tutorial questions on atomic absorption spectroscopy. It discusses several topics: 1) The use of cesium as an ionization suppressor to reduce interference from potassium emission lines. 2) Different types of interferences like chemical and spectral interferences and methods to address them such as using releasing agents or high resolution spectrometers. 3) Key differences between flame atomic absorption spectroscopy and flame atomic emission spectroscopy, including their light sources and measurement principles.

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351 views

Suggested Answer For Tutorial 3

The document provides answers to tutorial questions on atomic absorption spectroscopy. It discusses several topics: 1) The use of cesium as an ionization suppressor to reduce interference from potassium emission lines. 2) Different types of interferences like chemical and spectral interferences and methods to address them such as using releasing agents or high resolution spectrometers. 3) Key differences between flame atomic absorption spectroscopy and flame atomic emission spectroscopy, including their light sources and measurement principles.

Uploaded by

Echizen
Copyright
© © All Rights Reserved
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Download as PDF, TXT or read online on Scribd
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SUGGESTED

ANSWER FOR TUTORIAL 3



1. To eliminate interference caused by emission of radiation by the flame. OR: To distinguish the
signal of the flame from the desired atomic line at the same wavelength

2. Cs is more easily ionized, a high concentration of electrons are produced in the flame. In an
application of Le Chateliers principle, the ionization of K is suppressed as follows:
K(g) K+ (g) + e- (g)

3. a) Hollow cathode Lamp (HCL)


(b) Transfomation of the liquid into a spray of small droplets/a fine spray or mist called aerosol
(c) To differentiate between the signal from HCL (the source) and the atomizer (flame)
(d) The use of one lamp per element during the analysis

4. a) Chemical interference
(b) i. Add releasing agents such as EDTA, La2+ solution, 8-hydroxyquinoline
ii. Use a higher flame temperature/ fuel-rich flame

5. In emission spectroscopy, the analyte signal is due to a small number of excited atoms.
Therefore, any change/ fluctuations in flame temperature will dramatically influence the
number of excited species. Therefore, the analytical signal will also be inconsistent

6. a) To reduce the matrix effects (due to the presence of a lot of impurities in the sample)

b)







The concentration of silicon in oil sample = |-11.6 | = 11.6 ppb

7.
Flame Atomic Absorption Spectroscopy Flame Atomic Emission Spectroscopy (AES)
(AAS)
The line source is HCL
Does not use any light source to excite the
electrons (it just uses the flame)
Detector measures the energies from a light
source which are absorbed by unexcited
atoms/ ions
The flame is used to atomize the sample The flame or plasma (ICP) atomizes and
(source of energy)
excites the electrons (source of energy)
The radiation absorbed by the ground state The radiation emitted by the excited atoms
are measured
are measured

8. a) The process in which a sample is converted into a gas-phase atoms or elementary ions
(b) The transformation of a liquid into a spray of small droplets or aerosols
(c) The process by which a sample solution is drawn by suction in atomic spectroscopy

9.
Interferences
Method to cure
Spectral interferences
Use high resolution spectrometers
Chemical interference
- Add releasing agens, i.e. EDTA, 8-
hydroxyquinoline, La3+ solution OR
- Use higher temperature flame
The flame is used to atomize the sample
Use ionization supressor , i.e. CsCl

10. (a)Functions as a source modulator to differentiate signal emitted by the source (HCL) and the
signal emitted by the flame (atomizer) AND eliminate the effects of radiation from the flame
AND to distinguish between component of radiation arising from source with flame background
(b) The most common source for atomic absorption measurements that consists of a tungsten
anode and a cylindrical cathode
(c) As an atomizer, in which a part of where aerosol, oxidant and fuel are burned. The burners
used are most often premixed, laminar flow

11. (a) Standard addition analysis is done for sample with complicated matrix (When sample matrix
is high)
(b) Cx
= bCstd / mVx

= (0.2662 x 10 ppm)

(1.645 mL-1 x 20 mL)

= 0.08175 ppm

12. a)

(b) Concentration of analyte in initial solution =


Vflask
Concentration of analyte in initial solution
Vinitial unknown

Concentration of Ca in wastewater =
-CSA (Vflask/ Valiquot)
CSA = | -7 ppb |


=
7 ppb





=
7 ppb x (50/10)





=
35 ppb

(c) Principles:



Process measured

Use of flame
Beers Law
Data presentation

FAES
Excitation of neutral atoms
is brought only by the
thermal energy
Measurement of the
intensity of light emitted
when a metal is introduced
into a flame
Atomization with excitation
Not applicable
Intensity vs. Concentration

FAAS
Excitation of neutral atom
is brought only by radiation
from HCL
Measurement of the
intensity of light absorbed
when a metal is
bombarded by HCL
Atomization
Applicable
Absorbance vs.
Concentration

13. To prevent chemical interference. This could form a compound of higher stability than that
formed by analyte
Example : Ca3(PO4)2 + LaCl3 3 CaCl2 + 2 LaPO4

14.


Concentration of Pb in sample by extrapolation of graph,
= | -1.76 ppm|
= 1.76 ppm

15. a) Spectral interference: It refers to the overlap of analyte signals due to other elements or
molecules in the sample or with signals due to the flame/ atomizer
b) - Use a high resolution spectrometer
- Interference can be subtracted using D2 or Zeeman background correction
- Choose another wavelength for analysis

16. i) Use high- resolution spectrometers
ii) Use another wavelength for analysis
iii) Do a background correction method (i.e. based on Zeeman effect, two line correction, etc)

17. When the matrix effects are high

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