Chromatographic system
(see
Chromatography
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)The gas chromatograph is equipped with a flame-ionization detector and a 2-mm × 1.8-m column packed with 10% liquid phase G41 on 100- to 120-mesh support S1A. The carrier gas is helium, flowing at a rate of about 30 mL per minute. The chromatograph is programmed as follows. Initially, the column temperature is maintained at 150
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for 2 minutes, then increased at a rate of 4
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per minute to 280
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, and maintained at 280
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for 30 minutes. Make adjustments if necessary. Chromatograph the
System suitability solution, and record the peak responses as directed for
Procedure: the resolution,
R, between dibutyl sebacate and methyl heptadecanoate, at relative retention times of about 1.0 and 0.8, respectively, is not less than 1.8; and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure
Inject about 1.0 µL of Dibutyl Sebacate into the chromatograph, record the chromatogram, and measure the peak responses. Calculate the percentage of C
18H
34O
4 in the portion of Dibutyl Sebacate taken by the formula:
100A / B,
in which
A is the peak response for dibutyl sebacate; and
B is the sum of the responses of all the peaks.