柱切换离子色谱法测海水中的草酸根离子
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摘要
建立了柱切换离子色谱法测海水中草酸根离子的方法。采用Dionex Ion Pac AS11-HC(4 mm×250 mm)阴离子分离柱和AG11-HC(4 mm×50 mm)保护柱分离海水中草酸根,采用20 mmol/L KOH淋洗液,流速为1.0 m L/min等度淋洗,通过柱切换除去海水中大部分的高浓度阴离子(Cl~-、SO_4~(2-)和Br~-),分离出的C_2O_4~(2-)收集于富集柱,然后经过阀切换,将目标离子从富集柱上洗脱,进入阴离子分析柱分离,此时淋洗液换成30 mmol/L Na OH溶液,流速为0.8 m L/min等度淋洗,电导法检测。结果表明,在线性范围为0.5~10.0 mg/L内其相关系数为0.999 4,相对标准偏差为1.48%(n=6),最低检出限为4.35μg/L(S/N=3),所得样品回收率为85.3%~110.0%。该实验方法简单方便,且具有较好的重现性和较低的检出限,可用于检测海水中的草酸根离子。
A method for determination of oxalate in seawater by ion chromatography coupe of column switching was established.Sample separation method was as follows: firstly,seawater was injected on an analytical column( Dionex Ion Pac AS11-HC,4 mm×250 mm) and a guard column( AG11-HC,4 mm×50 mm),the elution was 20 mmol/L KOH at a 1. 0 m L/L flow rate.Secondly,high concentration anions( Cl~-,SO_4~(2-) and Br~-) and matrix in seawater were removed by setting an appropriate valve switching time,while the C_2O_4~(2-) was collected a concentrator column. Thirdly,the C_2O_4~(2-) in concentrator was eluted on a Dionex Ion Pac AS19( 4 mm×50 mm) and a AS19( 4 mm×250 mm) column by another valve switching,the elution was 30 mmol/L Na OH at a 0. 8m L/L flow rate.Finally,the C_2O_4~(2-) was separated by chosen column and detected using conductivity detection.Under the separation conditions,the method showed good linearity( r = 0. 999 4) in the range of 0. 5 ~ 10. 0 mg/L and satisfactory repeatability( RSD =1. 48%,n = 6).The limit of detection was 4. 35 μg/L( S/N = 3).The utilization of the method was demonstrated by the analysis of seawater,with satisfactory spiked recoveries of ammonium between 85. 3% and 110. 0%. The result showed that the single pump column-switching system was convenient and practical for the determination of low level.
A method for determination of oxalate in seawater by ion chromatography coupe of column switching was established.Sample separation method was as follows: firstly,seawater was injected on an analytical column( Dionex Ion Pac AS11-HC,4 mm×250 mm) and a guard column( AG11-HC,4 mm×50 mm),the elution was 20 mmol/L KOH at a 1. 0 m L/L flow rate.Secondly,high concentration anions( Cl~-,SO_4~(2-) and Br~-) and matrix in seawater were removed by setting an appropriate valve switching time,while the C_2O_4~(2-) was collected a concentrator column. Thirdly,the C_2O_4~(2-) in concentrator was eluted on a Dionex Ion Pac AS19( 4 mm×50 mm) and a AS19( 4 mm×250 mm) column by another valve switching,the elution was 30 mmol/L Na OH at a 0. 8m L/L flow rate.Finally,the C_2O_4~(2-) was separated by chosen column and detected using conductivity detection.Under the separation conditions,the method showed good linearity( r = 0. 999 4) in the range of 0. 5 ~ 10. 0 mg/L and satisfactory repeatability( RSD =1. 48%,n = 6).The limit of detection was 4. 35 μg/L( S/N = 3).The utilization of the method was demonstrated by the analysis of seawater,with satisfactory spiked recoveries of ammonium between 85. 3% and 110. 0%. The result showed that the single pump column-switching system was convenient and practical for the determination of low level.
引文
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[16]CHEN Mei-lan,YE Ming-li,HU Zhong-yang,et al.Determination of trifluoroacetic acid and chloride in celecoxib drug[J].Asian J.Chem.,2014,26(18):5 943-5 946.
[2]STEINBERG S M,BADA J L.Oxalic,glyoxalic and pyruvic acids in eastern Pacific ocean waters[J].J.Marine Res.,1984,42(3):697-708.
[3]TEDETTI M,KAWAMURA K,CHARRIERE B,et al.Determination of low molecular weight dicarboxylic and ketocarboxylic acids in seawater samples[J].Anal.Chem.,2006,78(17):6 012-6 018.
[4]YANG Xiao-hua,LEE C,SCRANTON M I.Determination of nanomolar concentrations of individual dissolved low molecular weight amines and organic acids in seawater[J].Anal.Chem.,1993,65(5):572-576.
[5]ZHONG Fu-jin,CHEN Xiao-qing,ZHANG Shu-chao,et al.Organic acids and inorganic anions in Bayer liquors by ion chromatography after solid-phase extraction[J].J.Cent.South.Univ.,2007,14(2):191-195.
[6]CHOVANCEK M,CHOO P,MACKA M.Development of a fully buffered molybdate electrolyte for capillary electrophoresis with indirect detection and its use for analysis of anions in Bayer liquor[J].Electrophoresis,2004,25(3):437-443.
[7]XIAO Jian-bo.Determination of nine components in Bayer liquors by high performence ion chromatography with conductivity detector[J].J.Chil.Chem.Soc.,2006,51(3):964-967.
[8]赵丽辉,王菊思.含酚废水中有机酸的气相色谱测定[J].环境化学,1989,(3):70-79.
[9]KAWAMURA K,IKUSHIMA K.Seasonal changes in the distribution of dicarboxylic acids in the urban atmosphere[J].Environ.Sci.Technol.,1993,27(10):2 227-2 235.
[10]成霈,刘佳,顾慧莹,等.离子色谱法测定果酒中的有机酸[J].食品与发酵工业,2011,37(8):175-177.
[11]杨泽蓉,金吉祥.有机酸的离子色谱分析[J].分析化学,1984,(7):15-18.
[12]陈梅兰,叶明立,范云场,等.离子色谱抑制电导测定尿液中草酸根、磷酸根及枸橼酸根离子[J].药物分析杂志,2009,(9):1 466-1 469.
[13]周梅素,陈亮.单柱离子色谱法测定痕量草酸根离子[J].分析测试技术与仪器,1995,(1):43-46.
[14]WANG Na-ni,WANG Rui-qi,ZHU Yan.Novel ion chromatography cycling-column-switching system for the determination of low-level chlorate and nitrite in high salt matrices[J].J.Hazard.Mater.,2012,235/236(2):123-127.
[15]ZHANG Jia-jie,ZHU Hai-bao,ZHU Yan.Determination of trace inorganic anions in anionic surfactants by singlepump column-switching ion chromatography[J].Chin.Chem.Lett.,2012,23(7):835-838.
[16]CHEN Mei-lan,YE Ming-li,HU Zhong-yang,et al.Determination of trifluoroacetic acid and chloride in celecoxib drug[J].Asian J.Chem.,2014,26(18):5 943-5 946.