Determination Of Particular Pollutants In Petrochemical Wastewater By Solid-phase Extraction Followed By GC/MS

By gas chromatographic analysised of petrochemical waste water, had picked out13kinds of semi volatile organic compounds in the phenol wastewater with eight kinds oforganic sulfide in the petrochemical wastewater analysised by solid-phase extractionfollowed by GC/MS A method was respectively built to simultaneously determine thecontent of thirteen kinds of emi-volatile organic compounds in phenol productionwastewater and eight kinds of Organosulfur Compounds in petrochemical wastewaterby solid-phase extraction followed by GC/MS. The detected emi-volatile organiccompounds in phenol production wastewaterare that isobutyric acid,2-methyl butyricacid,2-cyclohexen-1-ol, cumene, phenol,2-phenyl-1-propene,2-chlorocyclohexanol,dl-1-phenethylalcohol, acetophenone,2-phenyl-2-propanol,2-phenylpropionaldehyde,benzoic acid,2-phenyl-1,2-propanediol. And the detected organosulfur compounds inpetrochemical wastewater are thiazole, trimethyl thiazole, sulfolane, tetramethylthiourea,1,3,5-trithiane,3,3’-thiodipropionitrile,2-methylmercaptobenzothiazole, phenothiae.Had Chosed LC-C18solid phase extraction Colum to extract Organosulfur Compoundsand Chosed LC-C18alonge with PHE solid phase extraction connected in series toextract emi-volatile organic compound. The influences of amount of methanol, pH,extractant proportion, dosage of extractant, the flow rate of sample through theclumn,the flow rate of elution,amounts of NaCl, nitrogen blowing conditions,vacuumizing time on the effect of0xtraction were investigated，at the same time thechromatographic conditions were investigated too.The results indicated that the results indicated that the best solid-phase extractionconditions of emi-volatile organic compounds were that added0.5mL methanol in100mL sample, adjust the pH of sample to3, V(dichloromethane):V(hexane）=9:9asextractant proportion, the flow rate of sample through the clumn was4mL/min, thedosage of extraction for10mL, taken gravity elution. Under the optimum conditionsand in a relatively broad linear range, the standard work curves of targets had a goodlinear relationship and liner correlation between0.993to0.999. The relative standarddeviations for the samples were less than4%(n=7), minimum determination limits werein the range of0.05~0.94mg/L for each compound and average recovery varied from4.1%~97.2%. The best solid-phase extraction conditions of Organosulfur Compounds were thatadded1.0mL methanol in100mL sample, adjust the pH of sample to5,V(dichloromethane):V(hexane）=7:3as extractant proportion, the flow rate of samplethrough the clumn was6mL/min, the dosage of extraction for11mL, taken gravityelution. Under the optimum conditions a relatively broad linear range of0.5~80.0mg/L,the standard work curves of targets had a good linear relationship and liner correlationbetween0.9953to0.9999. The relative standard deviations for the samples were lessthan4%(n=7), minimum determination limits were in the range of0.05~0.22mg/L foreach compound and average recovery varied from31.0%~102.3%.Quick operation, high sensitivity, good accuracy, safe and environmental protectionof corresponding method could be used to detect the content of OrganosulfurCompounds in petrochemical wastewater and the content of emi-volatile organiccompounds in phenol production wastewater.