流动注射在线预富集——离子色谱法同时测定饮用水中痕量I~-、SCN~-、ClO_4~-及草甘膦
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摘要
目的建立了一种以活性碳纤维为吸附剂,采用流动注射在线预富集—离子色谱法测定饮用水中I~-、SCN~-、Cl O_4~-及草甘膦含量的方法。方法采用圆柱型吸附柱现场采样分析技术实现了连续现场富集水样中痕量的I~-、SCN~-、Cl O_4~-和草甘膦,并采用流动注射—离子色谱(FIA-IC)联用技术对吸附柱中富集的I~-、SCN~-、ClO_4~-和草甘膦的含量进行测定。采用Ion Pac AS19(250 mm×4 mm)色谱柱分离,KOH梯度淋洗,流速1.0 mL/min,抑制电导检测,外标法定量。结果 I~-、SCN~-、Cl O_4~-和草甘膦的线性范围为2.0~100.0μg/L,相关系数分别为0.9997、0.9998、0.9998和0.9999;以信噪比S/N=3计算检出限,I~-、SCN~-、Cl O_4~-和草甘膦的检出限为0.21~0.42μg/L;样品加标回收率为94.9%~99.6%。结论该方法用于饮用水的分析,灵敏度较常规离子色谱提高了40倍,适用于饮用水中痕量I~-、SCN~-、Cl O_4~-和草甘膦的测定,结果准确、可靠。
Objective To establish a method for the simultaneous determination of I~-,SCN~-,Cl O_4~-and glyphosate in drinking water by flow injection on-line preconcentration and ion chromatography with active carbon fiber as the adsorbent.Methods The trace of I~-,SCN~-,Cl O_4~-and glyphosate in drinking water were continuously on-line enriched by cylindrical adsorption column field sampling analysis technique;then the contents of I~-,SCN~-,Cl O_4~-and glyphosate enriched in adsorption columns were determined by the flow injection-ion chromatography(FIA-IC)multiple techniques.The chromatographic column Ion Pac AS19(250 mm×4 mm)was used to separate with gradient elution of KOH solution at a flow rate of1.0 m L/min.The detection was performed by a suppressed conductive detector.The external standard calibration curve was used for the quantitative analysis.Results The linear range of the method for trace I~-,SCN~-,Cl O_4~-and glyphosate was 2.0~100.0μg/L,and the correlation coefficients were 0.9997,0.9998,0.9998 and 0.9999 respectively;the detection limit was calculated of noise-signal ratio(S/N=3),and the detection limits of I~-,SCN~-,Cl O_4~-and glyphosate were 0.21~0.42μg/L;the average recoveries of sample addition was 94.9%~99.6%.Conclusion The sensitivity of the method in the determination of the trace I~-,SCN~-,Cl O_4~-and glyphosate in drinking water increased by 40 times than that of the conventional ion chromatography,and the result is accurate and reliable.
Objective To establish a method for the simultaneous determination of I~-,SCN~-,Cl O_4~-and glyphosate in drinking water by flow injection on-line preconcentration and ion chromatography with active carbon fiber as the adsorbent.Methods The trace of I~-,SCN~-,Cl O_4~-and glyphosate in drinking water were continuously on-line enriched by cylindrical adsorption column field sampling analysis technique;then the contents of I~-,SCN~-,Cl O_4~-and glyphosate enriched in adsorption columns were determined by the flow injection-ion chromatography(FIA-IC)multiple techniques.The chromatographic column Ion Pac AS19(250 mm×4 mm)was used to separate with gradient elution of KOH solution at a flow rate of1.0 m L/min.The detection was performed by a suppressed conductive detector.The external standard calibration curve was used for the quantitative analysis.Results The linear range of the method for trace I~-,SCN~-,Cl O_4~-and glyphosate was 2.0~100.0μg/L,and the correlation coefficients were 0.9997,0.9998,0.9998 and 0.9999 respectively;the detection limit was calculated of noise-signal ratio(S/N=3),and the detection limits of I~-,SCN~-,Cl O_4~-and glyphosate were 0.21~0.42μg/L;the average recoveries of sample addition was 94.9%~99.6%.Conclusion The sensitivity of the method in the determination of the trace I~-,SCN~-,Cl O_4~-and glyphosate in drinking water increased by 40 times than that of the conventional ion chromatography,and the result is accurate and reliable.
引文
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[10]侯艳霞,刘丽萍,杜振霞.高效液相色谱-电感耦合等离子体质谱法测定饮用水中碘酸根和碘离子[J].理化检验-化学分册,2011,47(11):1262-1265.
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[12]刘贵花,韩德满,梁华定,等.流动注射在线预富集-高效液相色谱法测定水产品中4种磺胺类药物[J].分析化学,2012,40(3):432-436.
[13]黄文锋,张骊,肖琳.离子色谱法测定饮用水中四种阴离子与传统化学法的比较[J].中国卫生检验杂志,2013,25(2):309-315.
[14]肖志雯,周睿,劳宝法,等.固相萃取净化-离子色谱法测定水产品中的6种阴离子含量[J].中国食品卫生杂志,2012,24(6):550-553.
[15]王永根,陈淑莎,王剑波,等.离子色谱-电导检测发测定饮用水中13种阴离子的研究[J].中国卫生检验杂志,2012,22(7):1495-1501.
[16]章骅,赵婷,宋文华.双系统离子色谱同时测定饮用水中氨氮、亚硝酸和硝酸盐的含量[J].中国食品卫生,2013,25(6):525-527.
[2]周娟.离子选择性电极法测定碘强化饮料中的碘[J].中国卫生检验杂志,2012,22(9):2054-2059.
[3]侯艳霞,刘丽萍,杜振霞.高效液相色谱-电感耦合等离子体质谱法测定饮用水中碘酸根和碘离子[J].理化检验-化学分册,2011,47(11):1262-1265.
[4]张慧芳,郭探,李权,等.双波长分光光度法同时测定溶液中的硝酸根和碘离子[J].中国无机分析化学,2011,1(4):24-28.
[5]胡继业,赵殿英,宁君.气相色谱-氮磷检测器测定草甘膦在土壤和苹果中的残留量[J].农药学学报,2007,9(3):286-290.
[6]曹赵云,牟仁祥,陈铭学.液相色谱-串联质谱法测定稻米中的草甘膦和氨甲基膦酸残留[J].色谱,2010,28(8):743-748.
[7]诸力,陈红平,周苏娟,等.超高效液相色谱-串联质谱法测定不同茶叶中的草甘膦、氨甲基膦酸及草铵膦的残留[J].分析化学,2015,43(2):271-276.
[8]李茂国,王广凤,高迎春,等.纳米银修饰电极对痕量硫氰根的测定[J].理化检验-化学分册,2005,41(5):305-309.
[9]张萍,史亚利,蔡亚歧,等.大体积进样离子色谱法测定环境水样中高氯酸根[J].分析化学,2006,34(11):1575-1578.
[10]侯艳霞,刘丽萍,杜振霞.高效液相色谱-电感耦合等离子体质谱法测定饮用水中碘酸根和碘离子[J].理化检验-化学分册,2011,47(11):1262-1265.
[11]李联鑫,黄静,陈娜,等.表面增强拉曼光谱技术检测高氯酸根离子[J].环境污染与防治,2013,35(8):20-22.
[12]刘贵花,韩德满,梁华定,等.流动注射在线预富集-高效液相色谱法测定水产品中4种磺胺类药物[J].分析化学,2012,40(3):432-436.
[13]黄文锋,张骊,肖琳.离子色谱法测定饮用水中四种阴离子与传统化学法的比较[J].中国卫生检验杂志,2013,25(2):309-315.
[14]肖志雯,周睿,劳宝法,等.固相萃取净化-离子色谱法测定水产品中的6种阴离子含量[J].中国食品卫生杂志,2012,24(6):550-553.
[15]王永根,陈淑莎,王剑波,等.离子色谱-电导检测发测定饮用水中13种阴离子的研究[J].中国卫生检验杂志,2012,22(7):1495-1501.
[16]章骅,赵婷,宋文华.双系统离子色谱同时测定饮用水中氨氮、亚硝酸和硝酸盐的含量[J].中国食品卫生,2013,25(6):525-527.