吉正元，普学伟

(玉溪市环境监测站, 云南 玉溪 653100)

吹扫捕集-气相色谱/质谱法测定水中的乙醛、丙烯醛、丙烯腈、吡啶、松节油和丁基黄原酸

吉正元，普学伟*

(玉溪市环境监测站, 云南 玉溪 653100)

建立了一种吹扫捕集-气相色谱/质谱法同时测定水中的乙醛、丙烯醛、丙烯腈、吡啶、松节油和丁基黄原酸的分析方法。结果表明，吹扫时间、脱附时间、脱附温度和盐酸用量是影响目标化合物测定的关键因素，对吹扫捕集条件优化后，各目标化合物线性良好，相关系数均>0.998，检出限为0.13～2.22 μg/L，加标回收率为80.5%～111%，相对标准偏差为1.1%～10.9%，能够满足地表水环境质量标准的要求。

吹扫捕集；气相色谱/质谱法；乙醛；丙烯醛；丙烯腈；吡啶；松节油；丁基黄原酸

Abstract：This study established a method for determination of acetaldehyde, acrolein, acrylonitrile, pyridine, turpentine and butylxanthic acid in water by purge and trap- gas chromatography/mass spectrometry. The results indicated that the purge and trap pretreatment parameters such as purge time,desorb time, desorb temperature, chlorhydric acid dosage had dramatic effects on target compounds. The calibration curve showed a good linear relationship with correlation coefficients greater than 0.998 by optimizing pretreatment, the detection limits ranged from 0.13 to 2.22 μg/L, recoveries were between 80.5% and 111%, relative standard deviations were between 1.1% and 10.9%. The method can meet the requirements of environmental quality standards for surface water.

Keywords：Purge and trap；Gas chromatography/mass spectrometry；Acetaldehyde；Acrolein；Acrylonitrile; Pyridine; Turpentine; Butylxanthic acid

乙醛、丙烯醛、丙烯腈、吡啶、松节油是重要的化工合成原料，广泛应用于合成树脂、合成橡胶制革、造纸、制药等工业，具有很强的生物毒性[1-2]。丁基黄原酸也称丁基黄药，是多金属硫化矿泡沫浮选的捕收剂，具有恶臭和毒性，浮选废水中残留的少量丁基黄原酸，可使周围空气有异味，严重污染水源和影响水生生物生长，危害人体健康[3]。我国《地表水环境质量标准》(GB 3838—2002)中对这些项目均做了限值要求[4]。

目前，乙醛、丙烯醛、丙烯腈、吡啶和松节油的测定方法有顶空气相色谱法、吹扫捕集-气相色谱法/气相色谱质谱法、液相色谱法等[5-9]。丁基黄原酸的测定方法有铜试剂亚铜分光光度法、离子色谱法、气相色谱质谱法等[3，10-12]。由于丁基黄原酸盐不稳定，遇酸后其碳氧键断裂生成等物质的量的二硫化碳，可应用该原理，通过测定二硫化碳的量间接测定丁基黄原酸的量。