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LINEAR PROGRAMMED TEMPERATURE GAS CHROMATOGRAPHY
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8. ANALYSIS OF AROMATIC COMPOUNDS Until recently, the application of gas chromatography to aromatic com pounds derived from coal tar was re stricted to mixtures boiling below 300° C1'3. Due to the complex and wide-boiling nature of these mixtures, several chromatograms had to be run at different constant column tempera tures to separate all of the compo nents. Much of the gas chromato graphic detail for the higher boiling components is lost due to peak spread ing and it is difficult to use the data either qualitatively or quantitatively. The use of linear programmed tem perature gas chromatography, how ever, enables analysis of such complex mixtures in a single run and also facilitates both qualitative and quanti tative analysis. The chromatogram at the left illustrates this for the analysis of a 17-component mixture of aro matic hydrocarbons ranging from xylene (b.p. 139°C) to chrysene (b.p. 448°C). The accuracy of the analysis is shown in the following table.
UNEAR PROGRAMMED^HIG^TEMPERATURE
GAS CHROMATOGRAPH-MODEL 500 FEATURING • Independent operation to 500° C—column, detec tor, ond injection port. • 18 linear heating rates. • Circulating air oven for columns to 50 ft. • Fast-heating, fast-cooling • 6 min.-change column ond re-establish baseline.
QUANTITATIVE ANALYSIS Compound Added, % Found, % Xylene 5.9 5.5 Mesitylene 5.9 6.4 Pseudocumene 2.9 2.9 Hemimellitene 1:1 f 147 14.0 Indan Napthalene 8.8 9.7 Diphenyl 2.9 3.5 1,2-Demerhylnaphthalene 5.9 5.9 Acenaphthene 8.8 9.6 Diphenylene oxide 5.7 6.0 Fluorene 2.9 3.3 Phenanthrene 48:!}i3.2 11.9 Carbazole Fluoranthene 5.9 6.5 Pyrene 8.8 9.7 1,2-Benza fluorene 1.4 1.1 Chrysene 5.9 4.9
The last column lists the amounts of each compound determined by sim ple peak area summation. The ex cellent results are attributed largely to the good separation and the sharp peaks obtained by temperature pro gramming a well-conditioned Apiezon L column. This analysis was made on a Model 500 Linear Programmed High Tem perature Gas Chroma tograph2. This unit uses stable, hot-wire thermal con ductivity detection for operation to 500° C. Separate and independent temperature controls for the column, detector, and injection port are also featured. LITERATURE CITED (1.)
Dupire, F., Z. Anal. Chem., 170, 317326 (1959). (2.) *Martin, A. J., Bennett, C. E., and Martinez, F. W. Jr., "Linear Program med Temperature Gas Chromatography," presented at the Cleveland ACS Meeting, April 1960. (3.) Ta-Chuang Lo Chang, and Karr, C , Anal. Chim. Acta, 21, 474-490 (1959).
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