Final Project

Case #3

Jessica Nicholson and Madi Kreitz and Joe and Sazzad

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

that the boiling point is lower.

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-

butanol, iso-butanol, and tert-butanol.

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

see which are contained in the methanol.

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

the way up with methanol

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

amounts of µL based on the chart in table 1

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

observe and print your findings

Chemical Hazards and waste:

 Gloves, goggles, and lab coat must be worn at all times

 Methanol: highly flammable, no open flames should be used in this lab, keep away from

eyes, mouth, and nose, it is a toxic solution

 Toluene: keep away from eyes, nose, and mouth because inhalation or contact with these

things will cause heavy irritation

  N-butanol, Sec-butanol, Iso-butanol, and Tert-butanol: all should be kept away from

nose, mouth, and eyes due to the potential of irritation

Table 1: Calculations

Compound Density Molar Mass Recipe

N-butanol 0.810 74.121 g 74.121 𝑔 1 𝑚𝐿

0.02 𝑚𝑜𝑙 × ×
1 𝑚𝑜𝑙 0.810 𝑔/𝑚𝑜𝑙
20 𝑚𝑀 =
g/mol 1𝐿
1.83 𝑔
= × 0.1 𝐿 = 183𝜇𝐿
1𝐿

Sec-butanol 0.806 74.122 g 74.122 𝑔 1 𝑚𝐿

0.02 𝑚𝑜𝑙 × ×
1 𝑚𝑜𝑙 0.806 𝑔/𝑚𝑜𝑙
20 𝑚𝑀 =
g/mol 1𝐿
1.84 𝑔
= × 0.1 𝐿 = 184𝜇𝐿
1𝐿

Iso-butanol 0.802 74.122 g 74.122 𝑔 1 𝑚𝐿

0.02 𝑚𝑜𝑙 × ×
1 𝑚𝑜𝑙 0.802 𝑔/𝑚𝑜𝑙
20 𝑚𝑀 =
g/mol 1𝐿

1.85 𝑔
= × 0.1 𝐿 = 185𝜇𝐿
1𝐿

Tert- 0.781 74.122 g 74.122 𝑔 1 𝑚𝐿

0.02 𝑚𝑜𝑙 × ×
1 𝑚𝑜𝑙 0.781 𝑔/𝑚𝑜𝑙
20 𝑚𝑀 =
butanol g/mol 1𝐿
1.90 𝑔
= × 0.1 𝐿 = 190𝜇𝐿
1𝐿
Conclusion:

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

goes down, so does retention times.

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

have to be brought up about this solution and the persons in question.

Works Cited:

Huynch, L., Henck, C., Saxton, K., & Wang, J. (n.d.). Introduction to Forensic Chemistry:

Laboratory Manual (Vol. 1). University at Albany.

1-Butanol. (n.d.). Retrieved December 06, 2017, from

http://www.chemicalbook.com/ChemicalProductProperty_EN_CB9113046.htm