Fatin najwa binti abd majid

2018695588

RAS2454A

1. Explain the following terms associated with atomic spectroscopy:

a) Atomization

- Atomization is where gaseous molecules are converted to atomic gas.

m
er as
b) Nebulization

co
eH w
- Nebulization is the transformation of a liquid into a spray of small droplets.

o.
c) Aspiration rs e
ou urc
- Aspiration is the uptake of liquid sample up to tube and into the nebulizer
chamber.
o
aC s

2. Using a simple phrase, state the function of the following devices found in a
vi y re

double beam atomic absorption spectrophotometer (AAS).

a) Hollow Cathode Lamp

ed d
ar stu

- Spectral line source and frequency turner.

b) Chopper
is

- Eliminate noise from flame emission.

Th

c) Burner
sh

-Evaporate the liquid droplets from sample solution and capacity to excite atoms
formed and cause to emit radiant energy.

This study source was downloaded by 100000792734951 from CourseHero.com on 05-19-2021 23:00:19 GMT -05:00

https://www.coursehero.com/file/60550717/tuto-chp-3docx/
 3. Explain why source modulation is employed in flame AAS.

- To modulate the output of the radiation source so that the intensity fluctuates at a
constant frequency.

4. In flame AAS:

a) Name the most common line source used.

- Hollow cathode lamp.

- Electrodeless discharge lamp.

m
er as
b) Explain the function of the chopper.

co
eH w
- To discriminate between the radiation from the hollow cathode lamp and the

o.
radiation given off by excited atoms in the flame by alternately passing through the
flame and being blocked off. rs e
ou urc
5. Explain why a stable flame is very important during atomic emission analysis.
o

- Because the heat from the stable flame evaporates the solvent and breaks
aC s

intramolecular bonds to create free atoms. The thermal energy also excites the
vi y re

atoms into excited electronic states that subsequently emit light when they return to
the ground electronic state.
ed d

6. State two disadvantages of AAS when used for elemental analysis.

ar stu

- Only solutions can be analyzed.

- Less sensitivity compared to graphite furnace.
is

- Relatively large sample quantities are required (1-3 ml).

Th

- Problems with refractory elements.

7. Explain why flame atomic emission analysis is sensitive to flame temperature.

sh

Atomic emission spectroscopy deals with excitation of atoms from the excited state
while atomic absorption spectroscopy deals with atoms in the ground state. For any
element, the ground state is much highly populated while the excited state has a
significantly low population of atoms. The population of atoms in the excited state
is given by the Boltzmann distribution and Boltzmann distribution function is

This study source was downloaded by 100000792734951 from CourseHero.com on 05-19-2021 23:00:19 GMT -05:00

https://www.coursehero.com/file/60550717/tuto-chp-3docx/
 temperature-dependent. Hence, atoms in the excited state are much highly affected
by temperature variations and thus, atomic emission spectroscopy is highly
sensitive to flame instability.

8. Hollow cathode lamp is a sharp-line source that emits specific wavelengths.

Explain why these lines are narrower than the absorption / resonance line of the
test element in a flame of Atomic Absorption Spectrometer (AAS).

Line sources emit a narrow band of radiation, which is important because they are
highly selective, provide high sensitivity which is beam power is in a narrow
wavelength band and reduce spectral interference of other elements, molecules,
atoms, or ions that have similar spectral lines.

9. What is a resonance line and why is a resonance line used in AA measurements?

m
er as
- Resonance line is the line of longest wavelength associated with a transition

co
eH w
between the ground state and excited state. Resonance line act as a light source that
produces light at a specific wavelength. It consists of a glass envelope containing a

o.
rs e
cathode which is the element to be excited and a suitable anode.
ou urc
10. Name two (2) types of interferences in atomic spectroscopy and discuss the
methods to cure each interference.
o
aC s

- Chemical interference. Methods to cure the interference are use higher flame
vi y re

temperature, add release agent and add chelating agent.

-Spectral interference. Methods to cure the interference are improve the resolution
ed d

of the spectrometer, choose another wavelength for analysis, use background

ar stu

correction based on Zeeman Effect and use two line correction method.

11. Ionization interference is one type of interference in AAS.

is

a) Explain what is meant by 'ionization interference',

Th

- Ionization interference is a phenomenon which shows a change in emission

intensity, causing the ionization equilibrium to shift, when coexisting elements
sh

include easily ionizable elements such as Na, K, Rb, and Cs.

b) State one (1) method to cure this type of interference.

- Adding an excess of an element which is easily ionized.

This study source was downloaded by 100000792734951 from CourseHero.com on 05-19-2021 23:00:19 GMT -05:00

https://www.coursehero.com/file/60550717/tuto-chp-3docx/
 12. Why are releasing agents such as La3+ added during the analysis of calcium
using flame absorption or emission methods.

- To reacts preferentially with the chemical interference and preventing its

interaction with the analyte.

13. What is the purpose of adding CsCl solution when conducting an atomic
spectroscopy experiment?

Increase the electron concentration in flame and drive back the ionic form to
ground state.

14. SO42- and PO43- hinder the atomization of Ca2+ by forming non-volatile
salts.

m
er as
a) Name the type of interference described above.

co
eH w
- Chemical interference

o.
rs e
b) State two methods which can be used to prevent this type of interference.
ou urc
- Add a releasing agent
o

- using higher flame interference

aC s
vi y re

15. In the analysis of potassium in blood samples, it is recommended that the

solutions used contain 1000 ppm of CsCI. What is the function of the CsCI
solution?
ed d
ar stu

Increase the electron concentration in flame and drive back the ionic form to
ground state.
is

16. The determination of sodium and potassium in blood was done by flame
Th

emission spectroscopy. The accuracy of this analysis depends on flame stability.

Explain.
sh

- Atomic emission spectroscopy deals with excitation of atoms from the excited
state while atomic absorption spectroscopy deals with atoms in the ground state.
For any element, the ground state is much highly populated while the excited state
has a significantly low population of atoms. The population of atoms in the excited
state is given by the Boltzmann distribution and Boltzmann distribution function is

This study source was downloaded by 100000792734951 from CourseHero.com on 05-19-2021 23:00:19 GMT -05:00

https://www.coursehero.com/file/60550717/tuto-chp-3docx/
 temperature-dependent. Hence, atoms in the excited state are much highly affected
by temperature variations.

17. The amount of sodium and potassium in blood can be determined using flame
emission spectroscopy. Explain why the accuracy of atomic emission analysis such
as this depends on flame stability.

-Atomic emission spectroscopy deals with excitation of atoms from the excited
state while atomic absorption spectroscopy deals with atoms in the ground state.
For any element, the ground state is much highly populated while the excited state
has a significantly low population of atoms. The population of atoms in the excited
state is given by the Boltzmann distribution and Boltzmann distribution function is
temperature-dependent. Thus, atom in the excited state are much highly affected by
temperature variations.

m
er as
18. The atomic absorption signal for iron in a flame atomic absorption

co
eH w
spectrometer (AAS) is found to decrease in the presence of large concentrations of
sulfate ions. Suggest an explanation for this observation

o.
rs e
ou urc
-Sulfate ion prevents interference by forming stable but volatile species with the
analyte.
o

19. Suggest and explain two possible methods for overcoming the potential
aC s

interference of sulfate in a quantitative determination of iron.

vi y re

20. Answer the following questions based on the table given below, which
represents the operating condition for the determination of lead (Pb) in blood using
ed d

a Graphite Furnace Atomic Absorption Spectrometer (GFAAS).

ar stu

a) From the temperature conditions given, identify which are the:

is

i) Drying stage(s)
Th

stage 1 and 2

ii) Ashing stage(s)

sh

stage 3

This study source was downloaded by 100000792734951 from CourseHero.com on 05-19-2021 23:00:19 GMT -05:00

https://www.coursehero.com/file/60550717/tuto-chp-3docx/
 iii) Atomizing stage(s)

stage 5

b) Explain why the gas flow needs to be stopped during stage 4.

To prevent atomization of remaining analyte.

c) State the main purpose of switching on the gas flow at stage 5.

To ensure atomization of remaining product.

21. In reference to Graphite Furnace AAS (GF-AAS):

a) The atomization process occurs in three steps. Name these three steps and

m
er as
briefly explain the processes occurring at each of these steps.

co
eH w
- Desolvation. The solvent evaporates to produce a finely divided solid molecular

o.
aerosol.
rs e
ou urc
- Volatilization. Solid aerosol is converted to gaseous molecules.

- Dissociation. Gaseous molecules are converted to atomic gas.

o
aC s

b) Briefly discuss a significant advantage of GF-AAS over flame AAS.

vi y re

- Slurries and solid samples can be analyzed in addition to samples in solution

- It shows greater sensitivity than AAS
ed d

- Smaller quantities of sample are required (normally 5-60 μL)

ar stu

- The atomization process is more efficient comparing to AAS

is
Th
sh

This study source was downloaded by 100000792734951 from CourseHero.com on 05-19-2021 23:00:19 GMT -05:00

https://www.coursehero.com/file/60550717/tuto-chp-3docx/
 22. A standard addition method was used in the determination of Cu(ll) in a waste
water sample using atomic absorption spectroscopy. 5.00 mL aliquots of the waste
water sample were pipetted into each of five 50.0 mL volumetric flasks. Different
volumes of a 2.5 ppm Cu(ll) standard solution were added into the volumetric
flasks as shown below. All resultant solutions were diluted to the mark and
absorbances measured at the maximum wavelength gave the following readings.

Plot the appropriate graph and determine the amount of Cu(ll) in the waste water
sample. Clearly show all the calculation steps.

Absorbance versus Volume of standard solution added, mL

14

12

m
er as
10

co
Absorbance

eH w
6

o.
4
rs e
ou urc
2

0
0.5 1 1.5 2 2.5 3 3.5 4 4.5 5 5.5
o

Volume of standard solution added, mL

aC s
vi y re

Cs = 2.5 ppm
ed d
ar stu

Vt = 5.00ml

Vx = 50.0ml
is
Th

m = (12.00-0.00) ÷ (1.040-0.215)

= 14.5454
sh

B = 0.215

Cx = (0.215 × 2.5ppm) ÷ (14.5454/ml × 5.00ml)

= 0.007391 ppm of Cu 2+

This study source was downloaded by 100000792734951 from CourseHero.com on 05-19-2021 23:00:19 GMT -05:00

https://www.coursehero.com/file/60550717/tuto-chp-3docx/
 23. A standard addition method was used in the determination of chromium in an
aqueous sample using atomic absorption spectroscopy. Ten milliliters of the
unknown were pipette into each of five 50.0-mL volumetric flasks. Various
volumes of a standard containing 12.2 ppm chromium were added to the flasks,
following which the solutions were diluted to volume.

m
A linear equation of y = mx + c was obtained from the data.

er as
co
a) Plot the appropriate graph and determine m and c value from the equation.

eH w
o.
rs e
Graph Absorbance versus Volume of standards, ml
ou urc
45
40
40
o

35
30
aC s

30
Absorbance

vi y re

25
20
20
15
10
10
ed d

5
0
ar stu

0
0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1 1.1
Volumes of standards, ml
is
Th

M = (40.0- 0.00) ÷ (1.009-0.240)

sh

= 52.0156/ml

C = 0.24 based on graph

This study source was downloaded by 100000792734951 from CourseHero.com on 05-19-2021 23:00:19 GMT -05:00

https://www.coursehero.com/file/60550717/tuto-chp-3docx/
 b) Determine the amount of chromium in an aqueous sample. Clearly show all the
calculation steps.

Vt = 10.0ml B = 0.240

Vs = 50.00ml

Cs = 12.2 ppm

Cx = ( 0.240 × 12.2 ppm) ÷ ( 52.0156/ml × 10.0ml)

= 0.005629 ppm

m
er as
co
eH w
o.
rs e
ou urc
o
aC s
vi y re
ed d
ar stu
is
Th
sh

This study source was downloaded by 100000792734951 from CourseHero.com on 05-19-2021 23:00:19 GMT -05:00

https://www.coursehero.com/file/60550717/tuto-chp-3docx/
Powered by TCPDF (www.tcpdf.org)