Determination of Petroleum Ether Residue in API by Headspace Gas Chromatography
Establish a headspace gas chromatography method for detecting petroleum ether residue in API.Method:A capillary column with 6%cyanopropyl benzene and 94%dimethyl siloxane as the stationary phase(Agilent DB-624 60.0 m*0.250 mm,1.40 μm,or similar polarity)was used as the chromatographic column.The initial column temperature is 40℃,maintained for 10 minutes,increased to 140℃at a rate of 3℃per minute,and then increased to 220℃at a rate of 30℃per minute,maintained for 2 minutes.The equilibrium temperature of the headspace bottle is 100℃,the equilibrium time is 30 minutes,and the detector is FID,with a detector temperature of 250℃;The temperature of the injection port is 200℃.Result:Using this method,the blank solvent has no interference,high sensitivity,linear regression equation is y = 142 237.032 6 x + 28 009.810 9(n = 7),correlation coefficient(r)0.999 7,recovery rate between 91.99%and 103.47%,RSD of 9 determination results is 3.45%,specificity,precision,and durability are all good,and the solution is stable within 24 hours,both meets the requirements of analytical method validation.This method was proved to be simple,repeatable,and suitable for the determination of petroleum ether residue in API.
gas chromatographyheadspaceAPIcatalystpetroleum ether residue
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