连续流动法测定水中阴离子表面活性剂含量
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摘要
利用连续流动分析方法建立以亚甲蓝比色法为基础的MBAS分析方法。方法中标样及水样利用自动进样器进样,碱性亚甲蓝试剂、氯仿试剂和样品被泵入模块,在内径为1 mm的玻璃圈中有机相和水相相互混合反应。生成的蓝色有机物质在混合过程中溶入有机相。利用相分离器分离有机相和水相,达到在线萃取目的。再经过酸性亚甲蓝去除大多数干扰离子的影响后流入检测池,在660 nm波长下检测样品或标样中的阴离子表面活性剂的浓度。MBAS标准溶液测定线性范围为0～5 mg/L,相关系数(r~2)大于0.999;方法检出限(DL)为0.002 mg/L。相对标准偏差(n=6)均小于1.0%,在不同浓度样品中添加适量标样,样品处理后MBAS回收率可达90.0%～96.6%。
The objective of this paper is to establish a method for the determination of MBAS in water by continuous flow analysis(CFA) and spectrophotometry method. In the method, the standard sample and the water sample are injected by the autosampler. Alkaline methylene blue(MB), chloroform and sample are pumped into the manifold. The organic phase and the aqueous phase are mixed with each other in a glass ring having an inner diameter of 1 mm. The resulting blue compound is dissolved in chloroform after mixing. On-line extraction was conducted by phase separator for separation of organic and aqueous phases. Over-acidic methylene blue removes most interfering ions and flows into the detection cell, the concentration of anionic surfactants in a sample or standards are detected at 660 nm. The absorbance of chloroform is proportional with the concentration of MBAS in standards and samples. When detecting the MBAS in drinking water, surface water, waste water and underground water with this method, it has high sensitivity, fast speed, less contamination and less reagent requirement, and less harmful to human body. The test range of MBAS by this method is 0-5 ppm, and the linearity r2>0.999 of MBAS standards, the detection limit(DL) of this method is about 2 ppb. The relative standard deviations(RSDs, n=6) were below 1.0%, the recoveries of MBAS at 3 different spiked concentration samples were range from 90.0% to 96.6%.
The objective of this paper is to establish a method for the determination of MBAS in water by continuous flow analysis(CFA) and spectrophotometry method. In the method, the standard sample and the water sample are injected by the autosampler. Alkaline methylene blue(MB), chloroform and sample are pumped into the manifold. The organic phase and the aqueous phase are mixed with each other in a glass ring having an inner diameter of 1 mm. The resulting blue compound is dissolved in chloroform after mixing. On-line extraction was conducted by phase separator for separation of organic and aqueous phases. Over-acidic methylene blue removes most interfering ions and flows into the detection cell, the concentration of anionic surfactants in a sample or standards are detected at 660 nm. The absorbance of chloroform is proportional with the concentration of MBAS in standards and samples. When detecting the MBAS in drinking water, surface water, waste water and underground water with this method, it has high sensitivity, fast speed, less contamination and less reagent requirement, and less harmful to human body. The test range of MBAS by this method is 0-5 ppm, and the linearity r2>0.999 of MBAS standards, the detection limit(DL) of this method is about 2 ppb. The relative standard deviations(RSDs, n=6) were below 1.0%, the recoveries of MBAS at 3 different spiked concentration samples were range from 90.0% to 96.6%.
引文
[1] 国家环境保护局规划标准处.GB/T 7494-1987 水质阴离子表面活性剂的测定亚甲蓝分光光度法[S].北京:中国标准出版社,1987.
[2] 中华人民共和国卫生部、建设部、水利部、国土资源部、国际环境保护总局等.GB5749-2006 生活饮用水卫生标准[S].北京:中国标准出版社,2006.
[3] 杜瑞华,周明松.连续流动分析法在烟草分析中的应用[J].中国测试技术,2007(3):55-58.
[4] 刘萤,刘熙岩,韩深,等.连续流动-水杨酸盐分光光度法测定葡萄酒及葡萄汁中氨氮含量[J].食品安全质量检测学,2015 (11):4318-4323.
[5] 王玉杰,关胜,郝电.碳棒涂膜电极流动注射法测定环境水样中的阴离子表面活性剂[J].分析化学,2002 (30):1455-1458.
[6] Technical Committee ISO/TC147,Water quality,Subcommittee SC2.ISO 16265-2009 Water quality-Determination of the methylene blue active substances(MBAS) index-Method using continuous flow analysis (CFA)[S].Switzerland:ISO,2009.
[7] Technical Committee ISO/TC147,Water quality,Subcommittee SC2.ISO 11732-2005 Water quality-Determination of ammonium nitrogen-Method by flow analysis (CFA and FIA) and spectrometric detection[S].Switzerland:ISO,2005.
[8] U.S.EPA Environmental Protection Agency.Revision1.11 U.S.EPA,40 CFR,Part 136,App.B—Definition and procedure for the determination of the method detection of the method detection limit[S].USA:Federal Register,1984.
[2] 中华人民共和国卫生部、建设部、水利部、国土资源部、国际环境保护总局等.GB5749-2006 生活饮用水卫生标准[S].北京:中国标准出版社,2006.
[3] 杜瑞华,周明松.连续流动分析法在烟草分析中的应用[J].中国测试技术,2007(3):55-58.
[4] 刘萤,刘熙岩,韩深,等.连续流动-水杨酸盐分光光度法测定葡萄酒及葡萄汁中氨氮含量[J].食品安全质量检测学,2015 (11):4318-4323.
[5] 王玉杰,关胜,郝电.碳棒涂膜电极流动注射法测定环境水样中的阴离子表面活性剂[J].分析化学,2002 (30):1455-1458.
[6] Technical Committee ISO/TC147,Water quality,Subcommittee SC2.ISO 16265-2009 Water quality-Determination of the methylene blue active substances(MBAS) index-Method using continuous flow analysis (CFA)[S].Switzerland:ISO,2009.
[7] Technical Committee ISO/TC147,Water quality,Subcommittee SC2.ISO 11732-2005 Water quality-Determination of ammonium nitrogen-Method by flow analysis (CFA and FIA) and spectrometric detection[S].Switzerland:ISO,2005.
[8] U.S.EPA Environmental Protection Agency.Revision1.11 U.S.EPA,40 CFR,Part 136,App.B—Definition and procedure for the determination of the method detection of the method detection limit[S].USA:Federal Register,1984.
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