离子色谱柱切换在线前处理法同时测定皮革及织物中的三价铬与六价铬离子  

Simultaneous Determination of Chromium (Ⅲ),Chromium (Ⅵ) in Leather and Cloth by Ion Chromatography with On-line Sample Pretreatment Column-Switching Technique

作　　者：贺婕[1] 余家胜[1] 黄忠平[1] 朱作艺[1] 王慕华[2] 王娜妮[1] 张嘉捷[1] 张培敏[1] 李刚 朱岩[1] 

机构地区：[1]浙江大学西溪校区化学系,杭州310028 [2]浙江丽水学院化学系,丽水323000 [3]浙江绍兴市环境保护局,绍兴312000

出　　处：《分析化学》2014年第8期1189-1194,共6页Chinese Journal of Analytical Chemistry

基　　金：国家重大科学仪器设备开发专项(No.2012YQ09022903);浙江省自然科学基金(Nos.Y4110532;Z14B070002);浙江省公益性科技计划(分析测试)项目(No.2012C37038);国家海洋局海洋-大气化学与全球变化重点实验室基金(Nos.GCMAC1208;GCMAC1109);浙江省公益性技术应用研究计划项目(No.2013C37073)资助项目~~

摘　　要：采用一根NG1反相色谱柱作为前处理柱在线去除样品中的水溶性有机基质,建立了离子色谱柱切换技术同时测定CrⅢ与CrⅥ的方法。进样前,先将待测样品水溶液与一定浓度的乙二胺四乙酸（EDTA）溶液充分反应,使其中的CrⅢ络合生成阴离子产物,该阴离子产物在可见光范围内有较强吸收;进样后,样品中的离子经前处理柱分离后被收集在2 mL接收环内,通过柱切换技术,淋洗液将接收环内的离子带至阴离子分析柱中分离,CrⅥ与1,5-二苯卡巴肼（DPC）溶液进行衍生化反应后与CrⅢ的EDTA络合物在同一波长下有较强吸收,由此可完成对两种离子的同波长测定。在优化的实验条件下,CrⅢ与CrⅥ的线性范围分别为0.3~10 mg/L（r=0.9991）,0.05~2 mg/L（r=0.9992）,检出限分别为80.78和6.67μg/L（信噪比S/N=3）,将3 mg/L CrⅢ与0.3 mg/L CrⅥ标准溶液连续进样6次,得到的色谱保留时间及峰面积相对标准偏差均小于3%;将本方法应用于皮革中CrⅢ与CrⅥ的检测,加标回收率为88.7%~108.5%。实验结果表明,本方法用于皮革及织物中铬离子的检测,具有快速、灵敏、选择性好等优点。A new analytical method has been developed for the simultaneous determination of CrⅢand CrⅥusing on-line sample pretreatment valve-switching ion chromatography. The organic matrix in leather was removed by using a reverse-phase column as the pretreatment column. Before injection, EDTA was added into sample solution to react with the CrⅢto form anion which could absorb visible light strongly. After injection, the ions separated by the pretreatment column were received in a collection loop. Then the ions were delivered into an analytical column and separated. CrⅥ then was derived with the derivatization reagent 1, 5-diphenylcarbazide （ DPC） , and detected together with CrⅢ-EDTA complex by a UV-Vis detector. Under the optimum conditions, the linear range of the method for CrⅢ and CrⅥ was 0. 3-10 mg/L （r=0. 9991） and 0. 05-2 mg/L （ r = 0. 9992 ）, whereas detection limits （ S/N = 3 ） were 80. 78 μg/L and 6. 67 μg/L, respectively. The recoveries were in the range of 88. 7%-108. 5% with the relative standard deviations for retention time and peak area less than 3%. The method could be applied to determine CrⅢ and CrⅥ in leather and cloth effectively and quickly.

关 键 词：离子色谱 柱切换 在线前处理 铬 

分 类 号：O657.7[理学—分析化学]