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Case #3
12/06/2017
Mike Miller
Introduction:
Gas Chromatography (GC) is a common type of chromatography used for separating and
analyzing compounds that can be vaporized without decomposition. A sample gets loaded and is
injected into a heated column and immediately vaporized and mixed with the carrier gas (mobile
phase), this gas carries the injected compounds through a very thin, long packed column
(stationary phase) containing liquid or polymer placed in an oven. The sample will either have an
affinity for the mobile phase or the stationary phase. Low boiling points will flow through the
exit column first (shorter retention time). In this experiment, the identity of the peaks of standard
samples provided and compare to the peaks of unknown sample collected from a crime scene of
a case based on the boiling point of each compound. Remember, shorter retention time means
The given case deals with a research scientist, Bernard Laurence, that is suspected to have
messed with the research of a fellow scientist, Michael Johnson. During Johnson’s reactions
failed countless times he suspected that his solvents were not pure. From this analysis he realized
that his methanol contained countless unnecessary compounds, including n-butanol, sec-
In order to test the scientist’s theory, there must be sample solutions of each contaminating
compound. These contaminating compounds must be run using GC analysis separately so there
is an idea around where each peak will be located. After that, the unknown that is provided by
the scientist will be run, this GC analysis will be compared to each contaminating compound to
Experimental Procedure:
1. Start by preparing a 100 mL solution of methanol and 183 µL of n-butanol (calculations
found in Table 1)
2. Get a 100 mL volumetric flat round bottom glass and using a glass funnel fill it 80% of
3. Then pipette 183 µL of n-butanol into the volumetric flat round bottom flask and fill up
the rest of the flask with methanol until it is filled up to the 100 mL line
4. Repeat steps 1-3 with sec-butanol, iso-butanol and tert-butanol using their different
5. Then pipette the same about of each of the compounds (table 1) into a 100 mL volumetric
flat round bottom flask and fill the rest with methanol
6. Then fill 4 Gas chromatography (GC) vials, one with each of the mixtures ¾ of the way
full
7. Then place each of them along with the unknown given by your TA into the GC and
Methanol: highly flammable, no open flames should be used in this lab, keep away from
Toluene: keep away from eyes, nose, and mouth because inhalation or contact with these
Table 1: Calculations
1.85 𝑔
= × 0.1 𝐿 = 185𝜇𝐿
1𝐿
In this experiment, the goal was to see if a scientist’s sample was contaminated by one of
his fellow workers. Through the use of gas chromatography, we were able to get retention times
of all of the molecules that were in question to be contaminating the sample given. The
molecules looked at were n-butanol which had a retention time of 2.585 as seen on table 2, next
iso-butanol had a retention time of 2.429 as seen on table 3, sec-butanol has a retention time of
2.349 as seen on table 4, and final tert-butanol has a retention time of 2.128 as seen on table 5.
As you can see, as the value in front of the butanol gets higher the retention time gets smaller
because the bonds become easier to be broken, as boiling point plays a hand in this due to gas
chromatography it is important to mention them. Their boiling points follow in the same order
the molecules were stated previously, 117.7 °C, 108 °C, 99 °C, and 82.2 °C. As boiling point
In table 6, the unknown mixture is put through the GC analysis and many different peaks
are taken note of. The first two peaks on the graph are the methanol which is meant to be the
only thing within the mixture. Interestingly, the next four peaks that follow all have very similar
retention times to the previously analyzed molecules. The third peak on the graph has a retention
time of 2.184, very close to that of tert-butanol. The fourth peak on the graph has a retention time
of 2.368, very close to that of sec-butanol. The fifth peak on table 6 has a retention time of 2.491,
close to iso-butanol. Then, the last important peak, the sixth, has a retention time of 2.717, close
to that of n-butanol.
What is concluded from this analysis is that the unknown mixture has been in some way
contaminated. There is no proof or support for the claim that Bernard Laurence was the one who
committed this crime against his fellow scientist, Michael Johnson. These results are
presumptive and not confirmatory, so in order to get further with this case, more tests and ideas
Works Cited:
Huynch, L., Henck, C., Saxton, K., & Wang, J. (n.d.). Introduction to Forensic Chemistry:
http://www.chemicalbook.com/ChemicalProductProperty_EN_CB9113046.htm