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固相萃取-气质联用法测定水中半挥发性有机物 被引量:8

Determination of semi-volatilization organic compounds in water with SPE-GC-MS method
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摘要 采用固相萃取(solid hase extraction,SPE)-气质联用法(GC-MS)测定水样中半挥发性有机物。水样中半挥发性有机物用Waters Porapak Rdx固相萃取柱富集、浓缩后,经DB-1701毛细管色谱柱(30 m×0.25 mm×0.25μm)分离,采用电子轰击离子源及选择离子扫描模式对样品中各组分进行定量分析。结果表明,水样中半挥发性有机物经固相萃取后得到有效富集,各化合物气相色谱分离效果较好。在0.05~0.40 mg/L浓度范围内,各组分检测响应值与浓度呈良好线性关系,相关系数均大于0.990。检出限(以基线3倍噪音计,3S/N)在0.13~15.87μg/L范围内。在空白水样的基础上用标准加入法测得各半挥发性有机物的加样回收率在70%~112%,测定结果的相对标准偏差(n=6)为2.67%~17.17%。该方法可一次性同时分析《地表水环境质量标准》和《生活饮用水卫生标准》中所列几十项SVOCs,试验结果为水质监测行业进行水质检测和进一步研究提供一定参考。 The semi-volatilization organic compounds (SVOCs) in water were determined by GC-MS method combined with solid phase extraction (SPE). SVOCs in water samples were extracted and concentrated with SPE column of Waters Porapak Rdx. The DB - 1701 capillary column (30 m ×0. 25 mm ×0.25 μm)was used to separate SVOCs, and then each compound in SVOCs was deter- mined by MS method in which an EI ion source was used and selected ion monitoring mode (SIM) was applied. The results showed that SVOCs in water samples were effectively enriched and separa- ted by SPE/GC method. A good linear relationship (R = 0. 990) was obtained between the detector respond values and concentration of SVOCs in the range of 0.05 - 0.40 mg/L, and the detection limits (3 S/N) were in the range of 0.13 - 15.87 μg/L. Recovery and precision tests were per- formed by standard addition method using a blank water sample, and gave a recovery of 70% 112% with RSD (n =6) of 2.67% - 17.17% for each semi-volatilization organic compound. Themethod is suitable for simultaneous quality standards for surface water used as references for water quality determination and standards of dozens of SVOCs contained for drinking water quality. The monitoring and further studies in environmental results could be used as references for water quality monitoring and further studies.
出处 《广西大学学报(自然科学版)》 CAS CSCD 北大核心 2012年第6期1126-1130,共5页 Journal of Guangxi University(Natural Science Edition)
基金 广西科技基础条件平台建设专项(1010827C)
关键词 固相萃取 气质联用法 半挥发性有机物 solid phase extraction ( SPE ) GC-MS semi-volatilization organic compounds (SVOCs)
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