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CDB 3093 Analytical Chemistry Laboratory Sep 2017 P age |1



The purpose of this experiment is to determine the composition of an unknown alcohol

mixture by using gas chromatography.


A gas chromatograph is an instrument that allows separation of the components of a volatile

mixture. The time required for the peak to appear, the retention time, can be used to

identify the components. Areas under the peaks can be used to measure the relative

quantities of the components.


Gas Chromatography (Model: Shimadzu)


Methanol CH3OH Ethanol CH3CH2OH

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Figure 1: Gas-chromatography (Model: Shimadzu) in the Laboratory 04-02-09.


Warm up the GC (see the operating manual for the instruments) and read the instructions for

operation of the instruments thoroughly before beginning the experiment.

A. Setting up the Gas Chromatograph (Done by the instructor)

1. Turn on the GC.

2. Start the software.

3. Set the following conditions for sample analysis.

Start 40 C. Hold 3 minutes.

Ramp 10 C / min until the temperature is 70 C

CAUTION: The gas chromatograph is like an oven, so the port may be hot.

B. Running Known Alcohols (Standard sample)

1. Inject methanol using auto sampling injection and start the data collection.
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2. When the peak in the chromatogram returns to baseline, the run may be stopped by

pressing the end button on the computer.

3. After the peak is obtained, record data and print the graph as instructed.

4. Repeat Step 1- 3 by replacing methanol with ethanol.

C. Running Unknown Alcohol Mixture

1. Obtain an unknown alcohol mixture.

2. Repeat steps above used for the known alcohol samples. When running the unknown

alcohol mixture sample, be certain to let the data collect long enough to get all possible

peaks. Record data.

3. Identify the alcohols present by comparing the retention time of the known alcohols.

4. To find the % of each alcohol in the mixture sample:

a) Record the area of each peak in the unknown alcohol mixture.

b) Record the total area.

c) % alcohol = area under the alcohol peak

total area
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A. Setting up the Gas Chromatograph

Starting temperature

Holding time

Ramping rate

Final temperature

Data collection duration

B. Running Known Alcohols

Standards Retention time (min)



C. Running Unknown Alcohol Mixture

Unknown Sample Retention Time Alcohol Area %

Peak 1

Peak 2

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1. Sketch the basic components (block diagram) of a GC.

2. Why was it necessary to run known alcohol samples?

3. If a known sample is properly injected into the gas chromatograph and several peaks are

observed, what can be concluded about the sample?

4. Why is it important to clean the syringe before inject another new sample?