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AS/APR 2010/CHM510
COURSE
COURSE CODE
CHM510
EXAMINATION
APRIL 2010
TIME
3 HOURS
INSTRUCTIONS TO CANDIDATES
1.
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)
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AS/APR 2010/CHM510
QUESTION 1
a)
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)
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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)
b)
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
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)
QUESTION 4
a)
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
QUESTION 5
a)
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)
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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)
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