Space Grant Consortium - University of Wisconsin - Green Bay

The chambers were sealed and baked at 120±5ºF for 24 hours, after which analysis could be
peformed. An alkane standard was run on both gas chromatographs (GCs) before running the
actual samples to ensure proper instrument performance. Samples were also allowed to cool to
room temperature before analysis, around 75ºF. For the Autosystem, 2.0cm 3 of headspace
sample was injected, while 1.0cm 3 was injected for the 6890, both in duplicate. Standard toxic
lab procedures were used for all runs. When samples were taken from the chambers to be
analyzed, the syringe was rinsed at least three times with sample before injecting into the GC.
Two 2.0cm 3 syringes were used for all the transfers as they were graduated and could be used to
accommodate both injection volumes. For identification purposes each of the three samples was
run on GC-MS as well. A similar procedure was also used to look at the interactions between
108193 and Mix 1. The difference was 50μL of Mix 1 was used in each of the two chambers
opposed to unequal Mix volumes.
To determine response factors 10μL of Mix 1 was added to a purged 1.00L test chamber and
baked overnight. After cooling the chamber to room temperature four 1.0cm 3 samples were run
on the Agilent 6890 GC/FID and three 2.0cm 3 samples were run on the Autosystem GC/FID.
Following these runs 10μL of Mix 2 was added to the chamber and after baking for four hours
and cooling once again, three 1.0cc samples were run on the Agilent 6890 GC/FID and three
2.0cm 3 samples were run on the Autosystem GC/FID. The chamber was purged with high
quality air and 10uL of Mix 2 was added to the chamber. After allowing it to bake overnight
four 1.0cc samples were run on the Agilent 6890/FID and three 2.0cm 3 samples were run on the
Autosystem GC/FID. To identify peaks 40mL samples of Mix 1, Mix 2, and Mixes 1 and 2
combined were run on the Incos GC-MS.
In a 1.00L test chamber 10μL of Mix 1 was added and baked for four hours. After cooling to
ambient room temperature 100μL of the sample was injected in the Autosystem GC/FID. The
resulting peaks were too large, and a 25μL sample was run, which resulted in too small of peaks.
When a 50uL sample was run the peaks were ideal. Seven trials were run using one syringe for
both injections because one of the two 50μL syringes had poor airflow. The same procedure was
used in analyzing Mix 2 and six sets of data were taken for it. Incos GC-MS spectra from
previous experiments were used for identification of peaks. To quantify the detection limits an
Excel template was used.
The first sample tested was log number 108148, a green foam. A 5.0g sample was placed in a
1.00L chamber and baked for 24 hours after which it was removed from the oven and a 1.0μL
sample was injected into the Autosystem GC/FID three minutes later. Four more samples were
injected at approximately 48 minute intervals as soon as the GC cooled. The next day after
removing the chamber from the oven a run was done 19.5 hours later. Times for each run and
the temperature of the chamber were recorded at the time samples were injected into the GC. A
60mL sample was also run on the Incos GC-MS after it had cooled for about an hour for
identification purposes.
The next sample analyzed was composite material, log number 107999, three 5.0g white foam
cubes. The same basic procedure was used as before with several exceptions. Room
temperature was also recorded as the temperature fluctuated before, and air conditioning setting
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