ICP-MS Combined with Ionic Liquid Microextraction and Back-Extraction of Nitric Acid for Speciation Analysis of Chromium
摘 要
200 mL水样经硝酸(3+97)溶液0.1 mL酸解15 min。移取样品溶液5 mL,用硝酸(3+97)溶液定容至10 mL,用电感耦合等离子体质谱法(ICP-MS)测定总铬。另取样品溶液5 mL,依次加入pH 5的乙酸-乙酸钠缓冲溶液1 mL,30 g·L-1的二乙基二硫代氨基甲酸钠溶液0.5 mL,1-己基-3-甲基咪唑六氟磷酸盐离子液体100 μL,于30℃超声处理15 min,离心。在下层有机相中加入2 mol·L-1硝酸溶液2 mL,超声处理15 min,离心后,将上层液用硝酸(3+97)溶液定容至10 mL,用ICP-MS测定Cr(Ⅵ)。以总铬含量减去Cr(Ⅵ)含量得到Cr(Ⅲ)的含量。Cr(Ⅵ)和总铬的线性范围均为0~80 μg·L-1,检出限(3s/k)分别为0.061,0.034 μg·L-1。Cr(Ⅵ)的加标回收率在96.4%~105%之间,测定值的相对标准偏差(n=6)在2.1%~5.9%之间。
Abstract
The sample (200 mL) was digested with 0.1 mL of HNO3 solution (3+97) for 15 min. An aliquot (5 mL) of the sample solution was taken and diluted to 10 mL with HNO3 solution (3+97), and total chromium was determined in this solution by ICP-MS. Another aliquot of 5 mL was taken from the sample solution, and 1 mL of pH 5 acetate buffer solution, 0.5 mL of 30 g·L-1 sodium diethyldithiocarbamate solution and 100 μL of 1-hexyl-3-methylimidazolium hexafluorophosphate were added and the mixture was treated ultrasonically for 15 min at 30℃. After centrifuging, the lower organic phase was separated, and 2 mL of 2 mmol·L-1 HNO3 solution were added. The mixture was treated ultrasonically for 15 min. After centrifuging, the upper aqueous layer was separated and diluted to 10 mL with HNO3 solution (3+97). Content of Cr(Ⅵ) was determined in this solution by ICP-MS. Content of Cr(Ⅲ) of the water sample was found by substracting value of Cr(Ⅵ) content from the total chromium. Linearity ranges of Cr(Ⅵ) and total chromium were same within 80 μg·L-1 and values of D.L. (3s/k) were 0.061, 0.034 μg·L-1 respectively. Recovery rates of Cr(Ⅵ) obtained by standard addition method were in the range of 96.4%-105% and the RSDs (n=6) were in the range of 2.1%-5.9%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201709023
所属栏目 专题报道(形态分析)
基金项目 国家质检总局科技项目(2015IK217)
收稿日期 2016/8/15
修改稿日期
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备注冉丽敏(1989-),女,河南平舆人,硕士研究生,主要从事前处理方法的研究
引用该论文: RAN Limin,LIU Shu,YANG Yong,SHEN Kangjun,LIN Miao. ICP-MS Combined with Ionic Liquid Microextraction and Back-Extraction of Nitric Acid for Speciation Analysis of Chromium[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(9): 1094~1098
冉丽敏,刘曙,杨勇,沈康俊,林苗. 离子液体微萃取-硝酸反萃取结合电感耦合等离子体质谱法用于铬元素的形态分析[J]. 理化检验-化学分册, 2017, 53(9): 1094~1098
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【5】洪锦清,李敬,程玉龙,等.离子色谱-电感耦合等离子体质谱法检测纺织品中六价铬[J].质谱学报, 2012,33(5):290-314.
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【10】VALFREDO A L, LUANA A O. Ultrasound-assisted temperature-controlled ionic liquid microextraction for the preconcentration and determination of cadmium content in mussel samples[J]. Food Control, 2015,50:901-906.
【11】MOHSEN Z, MOHAMMAD R G, PARVIZ N. Preconcentration and trace determination of chromium using modified ionic liquid cold-induced aggregation dispersive liquid-liquid microextraction:Application to different water and food samples[J]. Food Anal Method, 2013,6:1398-1406.
【12】宋志军,蔡美强.离子液体-K2HPO4超声双水相萃取预富集-高效液相色谱法测定水产品中组胺含量[J].理化检验-化学分册, 2015,51(12):1639-1643.
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