Experiment 7

Accelerant Identification by Gas Chromatography

Jessica Nicholson and Madi Kreitz

11/1/2017

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

an arson case based on the boiling point of each compound. Remember, shorter retention time

means that the boiling point is lower.

To find the origin of the unknowns we must run a sample of each compound through the

GC to get a reading on their retentions times, which should stay constant between different

compounds.

Experimental Procedure:

GC Method Set Up

1. Open chemstation by clicking the Instrument 1 Online icon

2. Make sure the method information and instrument/acquisition checkboxes are clicked and

then click OK

3. The Instrument | Edit | Injector: (6890) window will appear, click on the Injector box

on the far-right side to set up the injector

4. The injection volume should be 1.0 μL

 5. Click on the Inlets box to continue, set up the Front injector

6. Select mode as split or spitless from the dropdown box

7. Gas should be set to He and check the Heater, Pressure, and Total Flow boxes

8. Ensure that the GasSaver mode is checked and values are 20 mL/min and 2.00 min as

shown in the picture

9. The Columns box choose the right button

10. Mode should be set to constant flow

11. The Outlet Psi should be set to Ambient, the He Flow should be set between 0.5 and 1.5

mL/Min

12. Click the Oven box to continue

13. Click the on box, set the initial temperature and how long you would like to hold at that

temperature

14. Click on the Detectors box to continue

15. Should be set to Front or Back

16. Click the correct checkboxes

17. The Lift Offset should be set at 2.0

18. Finally click method and save method as “Partners Initials”

19. Click Start to run the sample

Sample Preparation

1. Follow your set calculations to achieve each dilution of the sample needed

2. Prepare a 100 mL 20 mM sample of toluene, n-octane, n-nonane, and n-decane and a 10

mL of a 20 mM mixture containing all four compounds in a 1:1:1:1 ratio

3. Dissolve all samples in dichloromethane before injecting into GC for analysis

 4. Label every vial

Chemical Hazards:

 All chemicals used are flammable and toxic

 No open flames should be involved with this lab

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

Results:

Sample Preparation

Compound Chemical Structure Molar Mass (g/mol) Boiling Point (°C)

Toluene 92.14 110.6

n-octane 114.23 125

n-nonane 128.2 151

n-decane 142.29 174.1

Dichloromethane Cl Cl 84.93 39.6

(Table 1)
 Compound Density Molar Mass Recipe

(g/mL) (g/mol)

Toluene 0.87 92.14

n-octane 0.708 114.23

n-nonane 0.718 128.26

n-decane 0.73 142.29

Mixture N/A N/A

(Table 2)

Sample Analysis (Unknown #1)

Peak Number Retention Time Peak Area Peak Identity

(min.) (Compound)

1 1.787 1.06231e5 Toluene

 2 3.114 7.26567e4 n-nonane

3 4.264 7.46030e4 n-decane

4 N/A N/A N/A

(Table 3)

Conclusion:

During this experiment, the job was to identify the compounds within an unknown

mixture by the use of gas chromatography. To begin, each possibly sample that may have been

present in the sample was analyzed. To begin Toluene’s retention time was found to be 1.692,

octane was found to be 1.882, nonane was found to be 2.924, and decane was found to be 4.060.

As the molecule gets more complex and as it achieves a higher boiling point the retention time

will grow along with that, as stated in the introduction, lower boiling point means a lower

retention time. So, now that these values are found it is possible to analyze the peaks found from

the unknown sample in this experiment. Three major peaks are observed in this graph that is

produced by the GC method. The first peak had a retention time of 1.787, this retention time is

close to the time that was found for toluene, so we assume that that is present in the sample. The

next peak shows a time of 3.114 which is less close to nonane, but it is closest to nonane, so we

can also assume that nonane is present in our sample. The last peak shows a retention time of

4.264 which is very close to decane, so we can assume that decane is present. In total, our

unknown contained toluene, nonane, and decane. Possible sources of contamination include the

use of the same pipette/pipette head to make multiple mixtures, keeping the sample open too

long and allowing it to evaporate, as well as not properly labeling your vials which allows for an

error. These can all be avoided with careful procedures to make mixtures and analyze them.