QUANTITATION OF AN ALCOHOL BY

GAS CHROMATOGRAPHY

PURPOSE
Utilize gas chromatography to separate butanol from methanol and analyze for the
volume percent composition of butanol in an unknown sample.

TECHNIQUES
• Gas chromatography
• Preparation and use of a standardized curve

THEORY - GAS CHROMATOGRAPHY

Gas chromatography (GC) is an analytical technique that allows volatile sample mixtures
to be separated and detected as they pass through a coiled column of packing material.
An inert carrier gas (often helium) serves as the mobile phase to push the now gaseous
substances through the porous column packing (stationary phase). Substances that spend
more time on the stationary phase will take longer to travel through the column. They
will have a longer retention time than substances that move quickly through the column.
It is often seen that lower boiling point components travel more rapidly while substances
with higher boiling points will stay on the column longer. A detector can measure how
much of a component exits the column at any given time. By comparing the "area counts"
of each component, it is often possible to quantitate the amount of each substance.

BACKGROUND – STANDARDIZED CURVE

The detectors used with gas chromatographs do not always respond equally to chemicals
of different structures. A series of samples of known concentrations can be carefully
prepared and analyzed by GC. By plotting the detector response to these known
quantities of a particular chemical, a standardized curve can be created. This curve can
then be used to predict the concentration of a substance based on how the detector
responds to a sample of unknown concentration.

PROCEDURE

1) To cut down on the time it takes to analyze samples, it is best if you work in a group
of three students. While two of your group starts to prepare your standards, one of you
should approach the instructor and ask to have an unknown alcohol mixture injected. You
and your teammates should record the unknown code. The printed chromatogram will be
given to your group when it is ready.

2) Use the burets preloaded with methanol or butanol to quantitatively prepare the
following series of standards. Each solution should be mixed in a small labeled flask and
stoppered shut. You should be able to easily calculate the "volume percent of butanol in
each standard."
(continued on other side)

S '08 v2 M. Hauser (Survival Manual 7e) Gas Chromatography of Alcohols

 Identity Volume Butanol Volume Methanol Volume Percent
(mL) (mL) Butanol
Standard 1 2 8
Standard 2 5 5
Standard 3 8 2

GAS CHROMATOGRAPHY

3) Your instructor will make a random draw of groups to determine the order that your
set of standard samples will be injected. Take the standards to the instructor at the gas
chromatograph when your turn is announced. He will instruct you on the use of the GC
and your samples will be analyzed. You should record the gas chromatograph parameters
in your lab notebook.

4) When your chromatograms are returned to you, you should be able to logically
determine the identity of each of the two major peaks.

CALCULATIONS

5) From the data for each standard, identify the peaks corresponding to butanol and
methanol. Record the area counts associated with each of these two peaks. Divide the
butanol area count by the methanol area count to get the BuOH/ MeOH ratio for each
standard. Put your data in a table similar to this one:

Standard Vol % of BuOH MeOH BuOH/MeOH

Std. area counts area counts ratio
1
2
3

6) Each of you should use graph paper to prepare a graph. The vertical axis should
indicate the BuOH/MeOH ratio for each standard, while the horizontal axis should show
volume % butanol. Plot the three standards and draw the best-fit straight line.

7) Analyze the chromatogram for your unknown sample to get the BuOH/MeoH ratio as
before. Use your newly generated standardized curve to predict the volume percent of
butanol in your unknown. The samples may be discarded in the "nonhalogenated waste."

RESULTS

In your notebook Conclusion, list the typical retention time of each alcohol. Report the
volume percent of butanol from your unknown sample (don’t forget the unknown code).
State what physical property you could use to tell which of your major peaks was butanol
and which was methanol. Tape your Standardized Curve into your notebook. A member

S '08 v2 M. Hauser (Survival Manual 7e) Gas Chromatography of Alcohols

of your group should staple and submit the chromatograms to the instructor; write each
group member's name on top of this packet.

QUESTIONS

1) Which one of the following gases do you think would be unsuitable for use as a GC
carrier gas- nitrogen, argon, or oxygen? EXPLAIN your answer.

2) If the GC oven temperature was accidentally set too low, how would this impact
retention times?

3) Suppose a student left the cap off of her prepared standard sample and the sample was
not analyzed immediately. How might this affect the GC results?

4) Suppose a student accidentally splashed a small amount of water into his sample and
then injected this contaminated sample onto a GC operating with a Flame Ionization
Detector. Would this incident impact the gas chromatogram printout? If so, how would
the chromatogram be changed?

5) When you did the GC area calculations in this lab, you made a broad assumption that
each peak we observed was not superimposed on top of another peak. This would make a
peak show a higher area count than it actually had. [Suppose another chemical in our
unknown sample had the same retention time as butanol but it was hidden from sight.
Would this make the % butanol number we report higher or lower than it actually was?]
(You need rewrite only the portion in brackets in your notebook before providing an
answer.)

GC column

S '08 v2 M. Hauser (Survival Manual 7e) Gas Chromatography of Alcohols