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AS/APR 2010/CHM510

UNIVERSITI TEKNOLOGI MARA


FINAL EXAMINATION

COURSE

ANALYTICAL SEPARATION METHODS

COURSE CODE

CHM510

EXAMINATION

APRIL 2010

TIME

3 HOURS

INSTRUCTIONS TO CANDIDATES
1.

This question paper consists of six (6) questions.

2.

Answer ALL questions in the Answer Booklet. Start each answer on a new page.

3.

Do not bring any material into the examination room unless permission is given by the
invigilator.

4.

Please check to make sure that this examination pack consists of:
i)
ii)

the Question Paper


an Answer Booklet - provided by the Faculty

DO NOT TURN THIS PAGE UNTIL YOU ARE TOLD TO DO SO


This examination paper consists of 6 printed pages
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AS/APR 2010/CHM510

QUESTION 1
a)

Optimizing flowrate is one of the important steps in chromatographic analysis. Explain


based on van Deemter plot.
(6 marks)

b)

The separation of 4 compounds gave resolution values of 0.5, 1.8 and 10.5. Sketch
the chromatogram and comment on the efficiency of separation.
(5 marks)

QUESTION 2
a)

Give a reason for each of the following situation:


i)

In gas chromatography (GC) analysis, injection temperature is normally set higher


than column temperature.
(2 marks)

ii) Identification of compound is more confirmative by using mass spectrometer as a


detector compared to UV detector.
(2 marks)
iii) For the analysis of biological sample using HPLC, a guard column is normally
required.
(2 marks)
iv) Pressure restrictor is vital in supercritical fluid chromatography (SFC) system.
(2 marks)
b)

Discuss a suitable approach to separate a sample mixture containing volatile and


non- volatile compounds with a wide range of polarity by using:
i)

Gas chromatography (GC)


(4 marks)

ii) High performance liquid chromatography (HPLC)


(4 marks)
iii) Supercritical fluid chromatography (SFC)
(4 marks)

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AS/APR 2010/CHM510

QUESTION 3
Figure below shows a gas chromatogram of a sample mixture consisting of normal alkanes
and chlorinated benzenes separated on a bonded phase column 100 m x 250 urn x 0.25 urn
with helium as the carrier gas at 25 cm/s. The column temperature was 120 C. 1.0 uL of
sample was injected using split ratio 1/25.

1.2

1L

6 7
. <

,,

mm

a)

What does bonded phase column mean?


(2 marks)

b)

Give the internal diameter of the above column.


(1 mark)

c)

Assume that the first three peaks refer to chlorinated benzenes while the last four
peaks refer to normal alkanes.
i) Is the column used in the above separation a polydimethyl siloxane (PDMS) or
polyethylene glycol (PEG)? Explain.
(3 marks)
ii) Is the detector employed in the above separation a flame ionization detector (FID)
or electron capture detector (ECD)? Explain.
(3 marks)

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d)

AS/APR 2010/CHM510

Describe (with reason/s) the changes you expect in the chromatogram if


i)

the column temperature is increased to 160 C.


(2 marks)

ii) the carrier gas is changed to nitrogen using the same velocity.
(2 marks)
e)

Can the injection mode be changed to splitless using the same GC conditions?
Explain.
(3 marks)

f)

The retention indexes for compounds 1-3 changed when the stationary phase is
changed. However the retention indexes for compounds 4-7 remain unchanged.
Explain why.
(2 marks)

g)

Based on the above chromatogram, if compound 4 is heptane, give an approximate


value of retention index for compound 3.
(2 marks)

QUESTION 4
a)

A sample mixture containing acetophenone, phenol, 7-hydroxyphenol and methyl


benzene was analyzed using HPLC with a mobile phase system of acetonitrile/water
80/20 and a UV detector set at a wavelength of 420 nm. Quantitative analysis was
done using external standard method. Discuss the reason for each of the following
problems encountered and suggest an approach to overcome the problem.
i)

Very low detection signals were obtained.


(3 marks)

ii) The first two peaks were not separated well. (In your discussion include the
possible compounds for these peaks).
(4 marks)
iii) After doing five replicate measurements, the peak areas obtained vary
considerably.
(3 marks)

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b)

AS/APR 2010/CHM510

Suggest and describe a suitable type of a specific liquid chromatography


technique to separate two of the following samples (include the mobile phase,
stationary phase, detector and principle of separation in the description):
i)

A dam water sample with pH 3 containing several basic metals.


(6 marks)

ii) A sample containing carbohydrates namely cyclodextrin compounds.


(6 marks)
iii) A sample mixture of alpha and gamma tocopherol compounds (fat soluble
vitamins).
(6 marks)

QUESTION 5
a)

Electroosmotic flow or EOF is the bulk flow of fluid in a capillary electrophoresis


caused by migration of the dominant ions in the diffuse part of the double layer
toward the anode or cathode.
i)

If the capillary was untreated, what is the direction of the EOF?


(1 mark)

ii) EOF is pH dependent. Explain why and how does this affect the migration time?
(3 marks)
iii) Give two steps that are necessary for the analysis of anions.
(2 marks)
b)

Capillary zone electrophoresis (CZE), capillary gel electrophoresis (CGE) and


micellar electrokinetic capillary chromatography (MEKC) are three different types of
electrophoresis mainly used to separate ionic compounds. Explain how they
complement each other in their applications.
(6 marks)

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AS/APR 2010/CHM510

QUESTION 6
a)

Liquid-liquid extraction (LLE), solid phase extraction (SPE) and solid phase
microextraction (SPME) are three different techniques used to extract analytes from
liquid samples. Each of these techniques produces extract with different quality
which may or may not require clean up and pre-concentration step. Explain briefly.
(6 marks)

b)

Explain why the recovery of analytes in supercritical fluid extraction (SFE) is simple
compared to conventional solvent extraction.
(3 marks)

c)

Pressurized liquid extraction method was used to extract atrazine pesticide from an
agricultural soil sample. Methanol/water was chosen as the extraction solvents
employed at high temperature and pressure. Nitrogen gas was also used in this
method. After 10 minutes the sample extract was collected and was then filtered
before injected into HPLC system for further analysis.
i)

Why was methanol/water chosen as the extraction solvents?


(2 marks)

ii) What was the function of the nitrogen gas?


(2 marks)
iii) If the methanol/water was employed at ambient temperature and pressure, what
do you think might happen to the extraction?
(2 marks)

END OF QUESTION PAPER

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