Related compounds
Internal standard solution
Transfer 30 mg of dibenzyl to a 10-mL volumetric flask, and dissolve in and dilute with methylene chloride to volume.
Test stock solution
Transfer about 5.0 g of Dibutyl Phthalate to a 50-mL volumetric flask, and dissolve in and dilute with methylene chloride to volume.
Test solution 1
Transfer 5.0 mL of Test stock solution to a 10-mL volumetric flask, and dilute with methylene chloride to volume.
Test solution 2
Transfer 5.0 mL of Test stock solution to a 10-mL volumetric flask, add 1.0 mL of Internal standard solution, and dilute with methylene chloride to volume.
Standard solution
Transfer 1.0 mL of Test solution 1 to a 100-mL volumetric flask, add 10.0 mL of the Internal standard solution, and dilute with methylene chloride to volume.
Chromatographic system (see Chromatography 621)
The gas chromatograph is equipped with a flame-ionization detector and contains a 4-mm × 1.5-m column packed with 3% liquid phase G3 on support S1A. The carrier gas is nitrogen, flowing at a rate of about 30 mL per minute. The column temperature is maintained at 190
, and the injection port temperature and the detector temperature are maintained at 225
. Chromatograph the
Standard solution, and record the peak responses as directed for
Procedure: the elution order is the internal standard peak followed by the dibutyl phthalate peak; and the resolution,
R, between these peaks is not less than 12. Chromatograph
Test solution 1, and verify that there is no peak with the same retention time as the internal standard. If a peak observed in the chromatogram for
Test solution 1 has the same retention time as that for the internal standard, make any necessary correction for factors of dilution, and then determine the area due to the interfering component that must be subtracted from the area of the internal standard peak appearing in the chromatogram recorded for
Test solution 2, as directed for
Procedure.
Procedure
Inject 1-µL portions of Test solution 2 and the Standard solution successively into the gas chromatograph, record the chromatograms for three times the retention time of dibutyl phthalate, and measure the responses of the peaks. From the chromatogram of the Standard solution, calculate the peak area ratio of dibutyl phthalate to the internal standard, A. From the chromatogram of Test solution 2, calculate the peak area ratio of the sum of all peaks, excluding the main peak, the solvent peak, and the internal standard peak, to the internal standard peak: this ratio is not greater than A (1.0%).
Assay
Transfer about 0.75 g of Dibutyl Phthalate, accurately weighed, to a flask, add 25.0 mL of 0.5 N alcoholic potassium hydroxide VS, attach a reflux condenser to the flask, and boil in a water bath for 1 hour. Add 1 mL of phenolphthalein TS, and titrate immediately with 0.5 N hydrochloric acid VS. Perform a blank determination (see
Residual Titrations under
Titrimetry 541). Each mL of 0.5 N potassium hydroxide is equivalent to 69.59 mg of C
16H
22O
4.