气相色谱-质谱联用法同时测定工作场所空气中44种挥发性有机物

Simultaneous determination of 44 volatile organic compounds in workplace air by gas chromatography-mass spectrometer

目的建立了一种同时测定工作场所空气中44种挥发性有机物的溶剂解吸-气相色谱质谱联用法。方法采用溶剂解吸型活性炭管对工作场所的空气采样,二硫化碳解吸后经HP-VOC石英毛细管色谱柱(60 m×0.20 mm×1.12μm)分离,质谱检测器检测,标准曲线法定量。结果被测组分线性相关系数均大于0.99,检出限在0.10~0.95μg/ml之间,相对标准偏差小于9.80%,平均解析率为61.23%~118.50%。应用该方法对33份样品进行分析,结果分别检出19种挥发性有机物,含量在0.10~604.43 mg/m^(3)之间,其中超出职业接触限值的有苯乙烯(62.32~114.54 mg/m^(3))、甲苯(50.11~604.43 mg/m^(3))和二甲苯(79.61 mg/m^(3)和91.55 mg/m^(3))三种有机物;并对5种原料进行定性识别,两种结果相符。结论该方法具有较高的灵敏度和精密度,各项指标均满足工作场所空气中44种挥发性有机物分析的要求。

Objective To establish a method for simultaneous determination of 44 volatile organic compounds in the air of workplace by solvent desorption-gas chromatography/mass spectrometer.Methods The solvent desorption activated carbon tube was used for sampling the target analyte.After desorption with carbon disulfide,the desorbed solution was injected into the gas chromatography,separated by HP-VOC capillary column,and detected by MS detector.The external standard method was used for quantitation.Results The correlative coefficients of the target analyte were greater than 0.99,and the detection limits between 0.10μg/ml and 0.95μg/ml.The relative standard deviations were lower than 9.80%,and the average desorption efficiencies ranged from 61.23%to 118.50%.The method established was used to analyze 33 samples,and 19 kinds of volatile organic compounds were detected,with the concentration ranging from 0.10 mg/m~3 to 604.43 mg/m~3.Styren(62.32-114.54 mg/m~3),toluene(50.11-604.43 mg/m~3)and xylene(79.61 mg/m~3 and 91.55 mg/m~3)were above the occupational exposure limits.Five kinds of raw materials were identified qualitatively,and the two results were consistent.Conclusion This method is highly sensitive and precise,and the indexes meet the requirements specified in the limits of 44 volatile organic compounds in workplace air.