CHM260 LABORATORY REPORT

EXPERIMENT NUMBER: 5

TITLE: GAS CHROMATOGRAPHY (GC)

Name: Nur Amirah Binti Abdul Rahman

ID Number: 2016452798

Group member: 1. Nornazurah bt Abdul Rahman (2016604218)

2. Nur Syahirah bt Zakaria (2016452624)

3. Nuriffa Filzah bt Mohamad Zulkipli (2016490236)

4. Syazayasmin bt Sabparie (2016482258)

Group: AS1205B

Lecturer Name: Dr Yanti Yana bt Halid

Date of Submission:

1st November 2018

OBJECTIVES

1. To determine the retention times, tR of 2-propanol and n-butanol.

2. To identify the components present in a standard mixture based on the tR.
3. To identify the component(s) present in unknown sample.
4. To determine the effect of temperature on tR and Rs.

INTRODUCTION

Chromatographic analysis is used to separate complex mixtures of compounds. The

chromatographic systems have two phases which are stationary phase and mobile phase.

Stationary phase is a fixed in place in a column or a solid surface. While, the sample is

dissolved in mobile phase such as gas, liquid or supercritical liquid. As the sample passed

through the stationary phases the compound in the mixture will be separated because of the

differences in their affinities for the stationary phase, and differences in their solution in the

mobile phase.

Gas chromatography is a specifically gas-liquid chromatography which it involves a

sample being vaporised and injected onto the head of the chromatographic column. The

sample is transported through the column by the flow of the inert gaseous mobile phase. The

column itself contains a liquid stationary phase which is adsorbed onto the surface of an inert

solid.

APPARATUS

Syringe, beaker and dropper.

CHEMICALS

Propanol, butanol and mixture.

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PROCEDURE

A. Sample Handling
1. The syringe was rinsed before filling it with sample. The volume of the sample
may be more than the required volume. Air bubbles were made sure not present.
The syringe was tapped gently to remove any air bubbles.
2. The syringe was held vertically, needle up, and the plunger was pushed to require
volume at eye level.

B. Experimental
1. The instrument was switched on.
2. The GC was set using the following conditions:
a. Initial oven temperature: 70oC
b. Final oven temperature: 70oC
c. Injection temperature: 180oC
d. Detector temperature: 180oC
3. The component sample was injected and the retention time of each component
individually was determined.
4. The standard mixture was injected and each component present was determined
by comparing the retention time of each component with te retention time of each
single component determine previously.
5. The unknown sample was injected and the component(s) present in unknown
was identified.
6. The column temperature was changed as follows:
a. Initial column temperature: 100oC
b. Final column temperature: 100oC
The standard mixture was injected and the effect of reducing the temperature on
retention time and Rs of component was commented.
7. The oven temperature was changes as follows:
a. Initial oven temperature: 140oC
b. Final oven temperature: 140oC
The standard mixture was injected and the increasing the temperature on the
retention time and Rs of the components was commented.

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C. Operation of GC
1. The sample was injected into the septa (liner) for manual injection.
2. The oven column was checked. The instrument was make sure was in off mode.
3. The instrument was switched on. If the gas was not enough the warning tone will
ring.
4. ‘Instrument 1 online’ was clicked in window screen. The instrument was allowed to
setup itself.
5. ‘Method’, ‘edit entire method’ → ‘ok’ were clicked after the setup was completed.
6. The title was entered and ok was clicked.
7. ‘Manual’ was clicked to select injection. ‘back’ was clicked to select injection location.
Inlet was edited, ‘back’ was choose and kept in information.
8. ‘split’ mode was choosed if a sample is in high concentration.’splitless’ was choosed
in inlet if sample was in low concentration or in small quantities.
9. Column no. 2 was choosed at column section. Back was cossed at inlet column.
Constant pressure was coosed at mode column. Ambient was choosed at outlet
column.
10. Went to detector column. FID (front) was used.
11. Parameter was injected.
12. Ok was clicked.
13. Apply → ok → signal detail → ok → edit integration events → ok → specify report → ok
→ run time checklist → ok
14. Went to file, save, method were clicked. Command was kept.
15. Bubbles were made sure not appeared in syringe.
16. Went to run control, sample info was clicked. Name was set in operator name
column.
17. Signal 2 was set, the sample name was filled.
18. Run method was clicked and instrument waited for injection.
19. The sample was injected quickly and start button was quickly pressed on the
instrument. The syringe was quickly pulled up from the septa.
20. Went to data analysis, file then load signal was clicked.
21. Calibration was entered, new calibration table was clicked. Name was entered and
the document was printed.
22. Data analysis was clicked for next sample and steps 17-21 was repeated.

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DATA ANALYSIS

RESULT

Name and model of instrument : Perkin Elmer Clarus 680 GC with SQ 8C GC/MS

Table 4.1: Retention times of standard and unknown sample

Temperature (oC) Compounds Retention time, tR (min)

70, 100, 140 2-Propanol 1.48, 1.39, 1.33

70, 100, 140 n-Butanol 1.90, 1.52, 1.39

70 Standard mixture 1.40 1.60

Graph of 2-propanol

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 Graph of n-butanol

Graph of Standard Mixture

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QUESTIONS

1. State the type of compounds which are suitable for analysis using GC.

The type of compounds which are suitable for analysis using GC are hydrocarbons,
halogenated compounds, compounds containing halogens, sulphur or nitrogen and
organic compounds.

2. Why is FID a suitable detector for this analysis?

Flame Ionization Detector (FID) is a suitable detector for this analysis because FID is
used to detect hydrocarbons. Ionization detectors interact with solutes eluted from
gas chromatography columns to produce a current that varies in proportion to the
amount of solute present. It will not detect non-carbon containing compounds. This
detector responds to all organic compounds except formic acid and the response is
highest for hydrocarbons. Besides that, the detector is insensitive to H2, O2, N2,
SiCl4, SO2, NO2, H2O and NH3. FID requires hydrogen supply and oxygen supply.
Lastly, FID exhibits high sensitivity.

3. List two factors which can increase the efficiency of a GC column.

Factors that can increase the efficiency of a GC column by reducing the packing size
of column and by lengthen the column. Tis factors may increase the efficiency of a
GC column.

DISCUSSION

The retention time, tR is a measure of the time taken for a solute to pass through a
chromatography column. It is calculated as time from injection to detection. The retention
time for a compound is not fixed as many factors can influence it even if the same gas
chromatography and column are used. The factors that may influence them are the gas flow
rate, the temperature differences in the oven and the column, column degradation and
column length.

In this experiment, a different range of temperature are set. In set A, the temperature is
set at 70oC. While, the temperature at set B is 100oC. Lastly, at set C the temperature is
140oC. From the graph it can be seen, the higher the temperature, the longer time for the
compounds to elute. Hence, the resolution will increase resulting the increasing of the
efficiency. From the graph, in set A, at temperature 70oC the retention time for the n-butanol

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is 1.90 mins and 1.48 mins is for 2-propanol. In the second injection, the retention time for 2-
propanol is 1.39 mins and retention time for n-butanol is 1.52 mins at 100°C. At 140°C, the
retention time for 2-propanol is 1.33 mins and 1.39 mins for n-butanol. Based on the
retention time obtained, we know that at standard mixture, 1.40 min is the retention time for
2-propanol while 1.60 min retention time for n-butanol.

Some precaution are needed to avoid errors from happening to minimize the errors in
the data. First of all, all the solution need to be shaked adequately to ensure dissolution for 5
min before the injection into the chromatograph. The column was checked before injected
the mixture to prevent any clogged occurs. The syringe was rinsed and cleaned before and
after use. Lastly, bubbles formation are avoided because it may affect the reading in the
column.

CONCLUSION

In conclusion, from this experiment, the retention time can be determined where the tR of n-
butanol and 2-propanol is 1.60 min and 1.40 min respectively. Besides, we can identified the
components that is present in the mixture based on the retention time. We also learned tye
effect of temperature on the tR and Rs. the higher the temperature, the higher the retention
time. Hence, Rs also increases.

REFERENCES

1. Jim Clark (2016, July). Gas-liquid Chromatography. Retrieved from:

https://www.chemguide.co.uk/analysis/chromatography/gas.html
2. John V. Hinshaw (2005). The Flame Ionization Detector, Volume 23, Issue 12, Pg
1262-1272. Retrieved from: http://www.chromatographyonline.com/flame-ionization-
detector
3. Chromatography Today (August, 2014). Understanding the Differences Between
Retention time and Relative Retention time. Retrieved from:
https://www.chromatographytoday.com/news/autosamplers/36/breaking-
news/understanding-the-difference-between-retention-time-and-relative-retention-
time/31166

4. A. B. Littlewood, Gas Chromatography: Principles, Techniques, and Applications.

Academic Press, 2013

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