分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2014年
8期
1190-1195
,共6页
贺婕%余家胜%黄忠平%朱作艺%王慕华%王娜妮%张嘉捷%张培敏%李刚%朱岩
賀婕%餘傢勝%黃忠平%硃作藝%王慕華%王娜妮%張嘉捷%張培敏%李剛%硃巖
하첩%여가성%황충평%주작예%왕모화%왕나니%장가첩%장배민%리강%주암
离子色谱%柱切换%在线前处理%铬
離子色譜%柱切換%在線前處理%鉻
리자색보%주절환%재선전처리%락
Ion chromatography%Column switching%On-line pretreatment%Chromium
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。
採用一根NG1反相色譜柱作為前處理柱在線去除樣品中的水溶性有機基質,建立瞭離子色譜柱切換技術同時測定CrⅢ與CrⅥ的方法。進樣前,先將待測樣品水溶液與一定濃度的乙二胺四乙痠( EDTA)溶液充分反應,使其中的CrⅢ絡閤生成陰離子產物,該陰離子產物在可見光範圍內有較彊吸收；進樣後,樣品中的離子經前處理柱分離後被收集在2 mL接收環內,通過柱切換技術,淋洗液將接收環內的離子帶至陰離子分析柱中分離,CrⅥ與1,5-二苯卡巴肼(DPC)溶液進行衍生化反應後與CrⅢ的EDTA絡閤物在同一波長下有較彊吸收,由此可完成對兩種離子的同波長測定。在優化的實驗條件下,CrⅢ與CrⅥ的線性範圍分彆為0.3~10 mg/L(r=0.9991),0.05~2 mg/L(r=0.9992),檢齣限分彆為80.78和6.67μg/L(信譟比S/N=3),將3 mg/L CrⅢ與0.3 mg/L CrⅥ標準溶液連續進樣6次,得到的色譜保留時間及峰麵積相對標準偏差均小于3%；將本方法應用于皮革中CrⅢ與CrⅥ的檢測,加標迴收率為88.7%~108.5%。實驗結果錶明,本方法用于皮革及織物中鉻離子的檢測,具有快速、靈敏、選擇性好等優點。
채용일근NG1반상색보주작위전처리주재선거제양품중적수용성유궤기질,건립료리자색보주절환기술동시측정CrⅢ여CrⅥ적방법。진양전,선장대측양품수용액여일정농도적을이알사을산( EDTA)용액충분반응,사기중적CrⅢ락합생성음리자산물,해음리자산물재가견광범위내유교강흡수；진양후,양품중적리자경전처리주분리후피수집재2 mL접수배내,통과주절환기술,림세액장접수배내적리자대지음리자분석주중분리,CrⅥ여1,5-이분잡파정(DPC)용액진행연생화반응후여CrⅢ적EDTA락합물재동일파장하유교강흡수,유차가완성대량충리자적동파장측정。재우화적실험조건하,CrⅢ여CrⅥ적선성범위분별위0.3~10 mg/L(r=0.9991),0.05~2 mg/L(r=0.9992),검출한분별위80.78화6.67μg/L(신조비S/N=3),장3 mg/L CrⅢ여0.3 mg/L CrⅥ표준용액련속진양6차,득도적색보보류시간급봉면적상대표준편차균소우3%；장본방법응용우피혁중CrⅢ여CrⅥ적검측,가표회수솔위88.7%~108.5%。실험결과표명,본방법용우피혁급직물중락리자적검측,구유쾌속、령민、선택성호등우점。
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.
