Experiment 1: Introduction to Gas Chromatography
Jessica Nicholson
9/5/19
Results:
Table 1: Retention Times for Compounds on Chromatograph
Compound Retention Time Retention Time Retention Time Retention Time Retention Time
(min) (min) (min) (min) (min)
Chromatograph Chromatograph Chromatograph Chromatograph Chromatograph
A B C D E
Acetone 1.697 1.697 1.698 1.697 1.697
i-propanol n/a 1.827 n/a 1.827 1.827
n-butanol n/a n/a n/a 2.544 no peak
t-pentanol n/a n/a 2.334 2.345 2.353
Cyclohex. n/a n/a n/a 4.503 no peak
Table 2: Peak Areas for Compounds on Chromatograph
Compound Peak Area PeakArea Peak Area Peak Area Peak Area
(pA*s) (pA*s) (pA*s) (pA*s) (pA*s)
Chromatograph Chromatograph Chromatograph Chromatograph Chromatograph
A B C D E
Acetone 24.011 23.758 23.175 23.766 27.340
i-propanol n/a 1.519 n/a 1.514 1.513
n-butanol n/a n/a n/a 26.551 no peak
t-pentanol n/a n/a 350.9 90.763 39.785
Cyclohex. n/a n/a n/a 17.996 no peak
Discussion:
To identify the peaks within each of the chromatograms we have to take into
consideration the different boiling points of the acetone and alcohols. The compounds
should elute out of the GC in this order: Acetone (56 °C), i-propanol (97-98 °C), t-
pentanol (101-103 °C), n-butanol (116-118 °C), and cyclohexanol (161.8 °C). So, the
peaks and retention times that associate with the different compounds should be simple
to identify. The peak shapes in our chromatographs displayed a perfect shape, they
were curved, they came to a distinct point after a steady incline and ended as well in a
completely parallel slope down. There we no irregularity. The acetone peak was always
much smaller than the others around it. We would expect between the 15 mM and 7.5
mM solutions that the peaks for the same compound should have the same retention
times but different peak areas, the 7.5 mM should have lower peak areas due to the
concentration being halved, since the peak area is directly proportional to concentration.
During our lab we did not fully get that desired result.
Between the chromatographs B (i-propanol) and chromatograph C (t-pentanol)
and chromatograph D (15 mM mixture) the retention times were basically identical. In
chromatograph B, i-propanol is seen to have a retention time at 1.827 minutes and then
in chromatograph D, i-propanol has a retention time that is completely identical. In the t-
pentanol chromatograph, its retention time is recorded at 2.334 minutes and in
chromatograph D it is just 0.011 minute off at 2.345 minutes. This outcome does not
deviate at all from what would be expected. Retention times re not dependent on the
amount of a compound, they completely rely on the boiling point of a compound. So,
since the compounds i-propanol and t-pentanol both do not have a change in boiling
point from the three separate chromatographs, retention times are all suspected to stay
the same, as they did.
Unfortunately, our undiluted and diluted solutions did not produce results that
were as favorable. The peak areas, as discussed before, for the 15 mM solution and the
7.5 mM should differ from one another by the factor of 0.5. Our only good data point for
this section was t-pentanol. On chromatograph D (15 mM) this alcohol had a peak area
of 90.763 pA*s and then on chromatograph E (7.5 mM) it had a lower retention time of
39.785 pA*s which shows ideal data points and the expected outcome. For the other
points we did not get the same result. The i-propanol peak areas between both
chromatographs was the same exact number. Our other two alcohols: n-butanol and
cyclohexanol sis not even create peaks during our run of our 7.5 mM solution which can
be related to machine error that will be discussed later. The main outtake of this section
of the lab is that the GC machine is very sensitive to concentrations of chemicals.
During this lab the error that we faced was due to human error during the
creation of our 7.5 mM mixture as well as some machine error during the same 7.5 mM
mixture. The machine error is very simple and easy to explain and fix in the future
experiments we will perform. Due to the low concentrations of cyclohexanol and n-
butanol they were not fully sensed and recorded by the GC machine; this does fall on
human error as well. The biggest error we faced was not properly planning for the
dilution of our 15 mM solution. In this lab we made four separate solutions for each of
our alcohols and then joined those together in equal volumes in a GC vial. So, when
diluting these it was hard to gather exactly how to go about it, it would have been much
more beneficial to have just made a stock solution of 15 mM to start our experiment.
This error has been recognized and will not happen again now that it has been dealt
with.
In this lab, our goal was to analyze the mixture of alcohols in a qualitative as well
as a quantitative manner, to relate the retention times of compounds to their molecular
structure, as well as to get more familiar with using the Gas Chromatography Machine.
The last point was achieved with ease during this lab, the functions of the GC machine
were thoroughly explained and understood during the procedure. Through the use of
gas chromatography and analyzation of the chromatographs that our mixtures produced
we were able to learn that the qualities of our peaks were standard, we did not produce
any odd shapes or incredibly sharp peaks in our data. Quantitatively the retention times
produced in our lab were ideal and all matched up with their same compound across the
5 chromatographs that we composed. This confirmed that retention times are solely
proportional to the boiling point of the compound which is proportional to the molecular
complexity of that specific compound. The only error that was experienced during this
lab was human error as well as slight machine error and not an error produced by
systematics. Overall, our experiment was a success beside a few humans made errors.
Appendix:
Equation 1: Initial Calculations for 15 mM solution
a. i-propanol
𝑔
0.015 𝑀 × 60.09 = 0.90135 𝑔/𝐿
𝑚𝑜𝑙
𝑔
0.90135 × 0.05 𝐿 = 0.045 𝑔
𝐿
0.045 𝑔
= 0.056 𝑚𝐿
0.803 𝑔/𝑚𝐿
b. n-butanol
𝑔
0.015 𝑀 × 74.12 = 1.118 𝑔/𝐿
𝑚𝑜𝑙
𝑔
1.118 × 0.05 𝐿 = 0.0559 𝑔
𝐿
0.0559 𝑔
= 0.069 𝑚𝐿
0.81 𝑔/𝑚𝐿
c. t-pentanol
𝑔
0.015 𝑀 × 88.15 = 1.322 𝑔/𝐿
𝑚𝑜𝑙
𝑔
1.322 × 0.05 𝐿 = 0.0661 𝑔
𝐿
0.0661 𝑔
= 0.082 𝑚𝐿
0.805 𝑔/𝑚𝐿
d. cyclohexanol
𝑔
0.015 𝑀 × 100.158 = 1.502 𝑔/𝐿
𝑚𝑜𝑙
𝑔
1.502 × 0.05 𝐿 = 0.0751 𝑔
𝐿
0.0751 𝑔
= 0.078 𝑚𝐿
0.9624 𝑔/𝑚𝐿
Chemical Hazards and Waste:
PPE are required at all times while a lab is being performed
Do not use gloves when using the computer
Chemicals being used in this lab are flammable; no open flames in the lab
Dispose of all solutions into the hazardous container labeled hazardous organic
waste container
Works Cited:
Forensic Chemistry Faculty and Staff. (n.d.). Advanced Forensic Chemistry Laboratory
Manual. University at Albany.
Libretexts. (2019, June 5). Gas Chromatography. Retrieved from
[Link]
Analytical_Chemistry)/Instrumental_Analysis/Chromatography/Gas_Chromatography
