The analysis of nitrate-ester propellants and explosives has been performed extensively by gas chromatography for the past decade. As capillary GC technology has advanced, new opportunities for the improvement of existing methods have developed. This investigation probes several of these possibilities.
The effect on quantitation of: the solvent, the analysis time, and the use of splitless injection were investigated. Precision was shown to be improved by:
1. using a non-volatile solvent (toluene) rather than CH₂Cl₂,
2. using the most time-efficient method that will allow adequate resolution of the components,
3. using splitless injection (0.80 min. splitless time).
After these potential improvements of method were investigated, the mechanism employed in splitless injection was investigated. This mechanism is known as the SOLVENT EFFECT. The investigation showed that:
1. non-volatile components required less splitless time to achieve 100% sample transfer to the column;
2. using splitless injection improved precision over split injection;
3. injector liner design had no effect on precision;
4. column overload did not hurt precision, as long as all peaks remain baseline-resolved;
5. the initial column temperature must be below the boiling point of the solvent (how far below did not appear to be very significant);
6. quantitation is improved by using a solvent that is as non-volatile as possible;
7. varying the split ratio after the split vent has reopened (within the range of 20:1 to 500:1) has no effect on resolving peaks that occur extremely close to the solvent peak. / Master of Science
| Identifer | oai:union.ndltd.org:VTETD/oai:vtechworks.lib.vt.edu:10919/45190 |
| Date | 13 October 2010 |
| Creators | Sotack, Gregg S. |
| Contributors | Analytical Chemistry |
| Publisher | Virginia Tech |
| Source Sets | Virginia Tech Theses and Dissertation |
| Detected Language | English |
| Type | Thesis, Text |
| Format | ix, 69 leaves, BTD, application/pdf, application/pdf |
| Rights | In Copyright, http://rightsstatements.org/vocab/InC/1.0/ |
| Relation | OCLC# 21055711, LD5655.V855_1988.S667.pdf |
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