RPIC/ICP-MS测定水中的Cr(Ⅲ)和Cr(Ⅵ)
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摘要
建立了反相离子对色谱-电感耦合等离子体-质谱(RPIC/ICP-MS)联用技术测定水中痕量三价铬Cr(Ⅲ)和六价铬Cr(Ⅵ)的分析方法。通过对流动相的组成、浓度、pH值等色谱条件的实验,确定当流动相组成为0.25mmol.L-1乙二胺四乙酸二钠和2mmol.L-1四丁基氢氧化铵,5%(V/V)甲醇,pH=7.0时,成功分离了Cr(Ⅲ)和Cr(Ⅵ)离子。ICP-MS测定时选用碰撞反应接口技术(CRI)消除40Ar12C+与35Cl16OH+对52Cr+的质谱干扰,Cr(Ⅲ)和Cr(Ⅵ)的检出限分别为0.50、0.34μg.L-1,RSD<10%(n=5)。应用于湖北黄冈、黄石、襄阳等地企业废水中Cr(Ⅲ)和Cr(Ⅵ)含量的测定,加标回收率为86.1%—100.1%。与分光光度法比对,实验证明本方法能克服用分光光度法测定水中六价铬由样品本身带来的干扰。
A method was developed to determination chromium speciation simultaneously in water using reversed-phase ion-pair chromatography with inductively coupled plasma mass spectrometry(RPIC/ICP-MS).The Cr(Ⅲ) and Cr(Ⅵ) were separated well on C18 column with the mobile phase of 0.25mmol/L ethylene diamine tetraacetic acid disodium salt-2mmol/L tetrabutylammonium hydroxide-5%(V/V)methanol(pH7.0).The collision response interface was applied to eliminate the mass interferences of 40Ar12C+ and 35Cl16O1H+ in the analysis of 52Cr+.The detection limit of Cr(Ⅲ) and Cr(Ⅵ) are 0.50、0.34 μg·L-1.The recoveries of Cr(Ⅲ) and Cr(Ⅵ) ranged from 86.1%—100.1% with the relative standard deviations(RSDs) less than 10%(n=5).Cr(Ⅲ) and Cr(Ⅵ) in waste water samples which collected from Huanggang,Huangshi and Xiangyang were analyzed by this method with satisfied recovery of standard addition,this method avoid the interference which caused by sample matrix in spectrophotometry.
A method was developed to determination chromium speciation simultaneously in water using reversed-phase ion-pair chromatography with inductively coupled plasma mass spectrometry(RPIC/ICP-MS).The Cr(Ⅲ) and Cr(Ⅵ) were separated well on C18 column with the mobile phase of 0.25mmol/L ethylene diamine tetraacetic acid disodium salt-2mmol/L tetrabutylammonium hydroxide-5%(V/V)methanol(pH7.0).The collision response interface was applied to eliminate the mass interferences of 40Ar12C+ and 35Cl16O1H+ in the analysis of 52Cr+.The detection limit of Cr(Ⅲ) and Cr(Ⅵ) are 0.50、0.34 μg·L-1.The recoveries of Cr(Ⅲ) and Cr(Ⅵ) ranged from 86.1%—100.1% with the relative standard deviations(RSDs) less than 10%(n=5).Cr(Ⅲ) and Cr(Ⅵ) in waste water samples which collected from Huanggang,Huangshi and Xiangyang were analyzed by this method with satisfied recovery of standard addition,this method avoid the interference which caused by sample matrix in spectrophotometry.
引文
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[5]曹凤梅,张新申,赵欢欢.流动注射分析法测定制革排放污水中的铬()[J].化学研究与应用,2011,23(3):381—384.
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[7]Pena F,Lavilla I and Bendicho C.Immersed Single-drop Microextraction Interfaced with Sequential Injection Analysis forDetermination of Cr()in Natural Waters by Electrothermal-Atomic Absorption Spectrometry[J].Spectrochimica Acta Part B,2008,63(4):498—503.
[8]Zhang N,Suleiman J S,He M et al.Chromium()-imprinted Silica Gel for Speciation Analysis of Chromium in EnvironmentalWater Sample with ICP-MS Detection[J].Talanta,2008,75(2):536—543.
[9]苏雪妮,张志广.分光光度法测度刚六价铬影响因素概述[J].广州化工,2009,37(6):148—149.
[2]Huang X P,Chang X J,He Q et al.Tris(2-aminoethyl)Amine Functionalized Silica Gel for Solid-Phase Extraction andPreconcentration of Cr(),Cd()and Pb()from Waters[J].Journal of Hazardous Materials,2008,157(1):1—6.
[3]王松柏,万俊生,丁富新等.铬形态离子的毛细管电泳分离测定[J].分析测试学报,2006,25(6):56—59.
[4]陈松涛,闫永胜,徐婉珍等.纳米TiO2预分离/富集FAAS法同时测定Cr()和Cr()的研究[J].光谱学与光谱分析,2007,27(5):1018—1020.
[5]曹凤梅,张新申,赵欢欢.流动注射分析法测定制革排放污水中的铬()[J].化学研究与应用,2011,23(3):381—384.
[6]郭志英,于水.HPLC/ICP-MS在环境样品的痕量元素形态分析中的应用[J].质谱学报,2006,27(1):56—64.
[7]Pena F,Lavilla I and Bendicho C.Immersed Single-drop Microextraction Interfaced with Sequential Injection Analysis forDetermination of Cr()in Natural Waters by Electrothermal-Atomic Absorption Spectrometry[J].Spectrochimica Acta Part B,2008,63(4):498—503.
[8]Zhang N,Suleiman J S,He M et al.Chromium()-imprinted Silica Gel for Speciation Analysis of Chromium in EnvironmentalWater Sample with ICP-MS Detection[J].Talanta,2008,75(2):536—543.
[9]苏雪妮,张志广.分光光度法测度刚六价铬影响因素概述[J].广州化工,2009,37(6):148—149.