Determination of 8 Phenolic Pollutants in Wastewater by Gas Chromatography-Mass Spectrometry Coupled with Ultrasound-Assisted Emulsion Extraction
By optimizing extraction and chromatographic conditions,the title method was proposed to determine 8 phenolic pollutants in wastewater,including phenol,o-chlorophenol,o-cresol,p-cresol,2,5-dimethylphenol,3,5-dimethylphenol,2,4-dimethylphenol,and quinoline.After settling and filtering the wastewater sample,20 mL of the sample was taken.Then 4.0 g of sodium chloride was added,and the mixture was shaken for 2 min.After 20 mL of dichloromethanen was added,ultrasonic emulsification extraction was performed for 5 min.The mixed solution was placed into a separating funnel to settle for 5 min.The organic phase was taken,and concentrated to 2-3 mL at 10 ℃.The concentrated solution was diluted to 5 mL by dichloromethane,and 1 g of anhydrous sodium sulfate was added.The mixture was settled for 10 h to remove the moisture,and the resulting solution was introduced into the gas chromatograph-mass spectrometer.Program temperature separation of 8 phenolic pollutants in the sample solution was conducted on the Agilent DB-VRX chromatographic column(30 mm×0.25 mm,1.4 μm).Qualitative and quantitative analysis was performed by full scan(SCAN)and selective ion monitoring(SIM)modes,respectively.It was shown that linear relationships between values of the mass concentration and peak area of 8 phenolic pollutants were kept in the range of 0.50-500.00 μg·L-1,with detection limits(3S/N)in the range of 0.02-0.07 μg·L-1.Test for recovery was made according to the standard addition method,giving recoveries in the range of 76.8％-114％,and RSDs(n=6)of the determined values not more than 10％.The proposed method was used for the analysis of surface water and coal chemical wastewater samples,2.40 μg·L-1 phenol and 1.3 μg·L-1 p-cresol were detected in surface water,and 8 phenolic pollutants were detected in coal chemical wastewater with detection amounts in the range of 1.21-30.63 μg·L-1.
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