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Gas chromatography (GC), liquid chromatography (LC), and supercritical fluid chromatography
(SFC) are three types of separation methods with different mobile phases.

a) Compare and discuss how each mobile phase affects

i) the B term of van Deemter in each of the above separation method.

(6 marks)

ii) the types of sample that are suitable for each of the above separation method.

(6 marks)

b) For each of the above separation methods, discuss one main parameter (exclude flow
rate) that can be manipulated to improve the separation of analytes.
(6 marks)

(Q2 OCT 2010)


a) Explain the effect of the followings on a gas chromatographic peak.

i) Introducing too much sample into the injection port.

(3 marks)

Too much sample vented out, small amount of sample flow into the column (1), hence
small peak (1) and not reproducible (1).

ii) Too high split ratio was set for a split mode injection of a split/splitless injector.
(3 marks)

b) Consider the gas chromatographic separation of 10 hydrocarbons with large boiling

points (80-280C). Using an isothermal column temperature of 180C, the first 4 peaks
were not well separated while the last 3 peaks were broad and took a long time to elute
from the column.

i) Discuss the reasons for the above observation.

(4 marks)

ii) Would increasing the isothermal column temperature to 250C improve the
separation? If not, suggest an approach to improve the separation.

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(6 marks)

c) In the analysis of phenols using gas chromatography (GC), discuss the followings :

i) The sample of phenols was added with N,0-bis(trimethylsilyl)trifluoroacetamide

(BSTFA) reagent prior to GC analysis.
(4 marks)

ii) Mass spectrometry was chosen as the detector out of other common GC detectors.
(3 marks)

(Q2 JAN 2012)


The analysis of polyaromatic hydrocarbons was carried out with the following GC conditions:
column, poly(phenylmethyl)siloxane (5% phenyl); injection, split 1:20, detector, mass
spectrometry; column temperature, 100C for 2 min then programmed to 350C at 10C/min.
The chromatogram is shown below.

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i) Which of the polyaromatic hydrocarbon compound is the most polar? Explain.

(3 marks)

ii) Is it possible to decrease the rentention time of naphthalene by increasing the initial
column temperature to 200C without affecting the separation of other compounds?
(4 marks)

iii) Suggest another possible detector for this analysis? Verify your choice.
(3 marks)

b) What is the significance of each of the following terminology in GC separation.

i) Bonded phase column

ii) Derivatization
iii) Split injection
(9 marks)

(Q2 JUN 2012)

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c) i) Figure 1 shows the separation of hydrocarbons achieved using the following GC

conditions; Column: polydimethyl siloxane (PDMS), initial temperature 100 C at
rate 15 Cmin-1. Name the phenomena observed at retention time before 20
minutes and briefly discuss the cause of the phenomena.
(3 marks)

Figure 1

ii) Figure 2 shows a typical chromatogram observed for the separation of polar
analytes using PDMS column. Explain the cause of the observed peak tailing.
Suggest an approach to avoid this problem.

(3 marks)

Figure 2

d) The analysis of drug in urine was analyzed using a gas chromatography with
split/splitless injector. The drug was extracted using solid phase extraction and elution

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was achieved using methanol. Suggest a suitable injection mode for this analysis.
(3 marks)

(Q1 JAN 2013)


c) The chromatogram in Figure 2 was obtained in the analysis of chlorpyrifos in contaminated

soil extracted using dichloromethane. Prior to gas chromatography (GC) analysis,
chlorpyrifos was extracted into dichloromethane and 0.5 L of the aliquot was injected
into a GC with electron capture detector (ECD) using split injection with split ratio 1:20.

Explain why a split injection mode is not suitable for this analysis. Suggest an alternative
approach for sample injection in order to improve the separation of chlorphrifos.

(Q1c-f JUN 2013)


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iii) Suggest a suitable carrier gas for the analysis. Verify your answer.
(3 marks)

(Q1a, c Jun 2014)

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