CHEM 340 2021

TUT 3 : Gas Chromatography

1. Examine the figure of the GC shown below.

B
A

Column

a. Identify the parts labelled A and B.

A – injector
B – detector

b. Give and discuss the two configurations for the part labelled A.
Split mode: the split vent remains open during analysis. This allows for samples with
high concentration, usually greater than 1% to be analysed without overloading the
column. In this way, up to 99% of the sample goes to waste.
Splitless mode: the split valve is closed during injection. This allows for a greater
proportion of the sample to enter the column and thus reach the detector. Used for
samples with low analyte concentration (trace analysis, less than 0,1%).
 c. The column shown is a capillary column. How is this different from a
packed column?

Packed column Capillary column

Solid support is packed into column Solid support is coated on column wall

Larger internal diameters (2-4mm) Very small internal diameter (down to

0.1mm)

Tend to be short (1.5 to 10m) Tend to be long, up to 100m in length

Usually constructed from stainless steel Constructed from polymer and glass

Typically used to analyse for permanent Used to analyse most organic compounds

gases

d. If you had to analyse an air sample, would this column be suitable? Give
a reason for your answer.
No. Air consists of permanent gases such as O2 and N2 and a packed column is
required to analyse it. Capillary columns contain a stationary phase which does not
interact with these gases.

2. Based on the working principle of the FID, explain why organic compounds are
more easily detected by this detector.
Based on the working principle with organic compounds such as hydrocarbons, the
gas stream from the column is mixed with hydrogen and burned. Positive ions (e.g.
CH3+ or CHO+) and electrons are produced in the flame when organic substances
are present.
The ions are collected at electrodes and produce a small, measurable current.
The current is proportional to the amount of Carbon in the gas stream. Since the
amount of carbon is being measured, inorganic compounds or permanent gases
cannot be detected.

3. You obtained a sample that contains organochlorine pesticides, which will be

analysed by GC. With reasons, explain which detector is most suited for this
analysis. Explain how it would function to detect the compound.
This detector exhibits high intensity for halogen containing compounds, which is what
the pesticide contains. With an ECD, a beta emitter such as radioactive tritium or 63Ni
is used to ionize the carrier gas. Fast beta particles generated by the radioactive
source collide with the molecules of the carrier or make-up gas. By impact ionization,
free slow-moving electrons are produced, which generates a measurable and steady
current. If the GC effluent contains organic molecules with electronegative functional
groups, such as halogens, phosphorous and nitro groups, electrons will be captured
and the current will be reduced. The reduction in electron flow is proportional to the
quantity of the analyte.

4. The chromatograms shown are of the same six compounds, but using two
different oven temperature programmes. Explain in detail why there is poor
separation in Figure 1 and similarly why the separation has improved in Figure
2.

Figure 1

Figure 2

An Isothermal temperature programme has been used in Figure 1. This is likely a

high temperature programme where there is poor separation at the front-end and
improved separation for lower volatility compounds at the tail end.
The separation can be improved by using a stepped temperature programme or
changing the rate of the temperature increase. This is the case in Figure 2. Since the
temperature is increased at varying rates, the separation is improved since the
compounds are subject to different temperature effects throughout the run.

5. How will the stationary phase affect the performance of a GC column?

Increasing the thickness of the stationary phase allows the separation of larger
sample sizes
Increasing the thickness of the stationary phase reduces efficiency
Increasing the thickness of the stationary phase is better for separation of highly
volatile compounds due to increased retention.