超声辅助-邻菲罗啉/离子液体微萃取分离Cr(Ⅲ)和Cr(Ⅵ)
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摘要
以邻菲罗啉(C12H8N2)为螯合剂,1-己基-3-甲基咪唑六氟磷酸盐([C6M IM][PF6])为萃取剂,采用超声辅助-分散液液微萃取分离Cr(Ⅲ)和Cr(Ⅵ),结合电感耦合等离子体质谱法(ICP-MS)实现对铬元素形态分析。实验结果表明:邻菲罗啉浓度0. 3 mol/L、pH值为8、超声时间20 min、超声温度30℃时,Cr(Ⅲ)的萃取效果最好,Cr(Ⅵ)和Cr(Ⅲ)可以分离。通过ICPM S测定Cr(Ⅲ),由总铬减去Cr(Ⅲ)得到Cr(VI)含量。Cr(Ⅲ)浓度在0～80μg/L范围内呈现好的线性关系,检出限为0. 06μg/L,Cr(Ⅲ)的加标回收率在91. 5%～110. 2%之间,相对标准偏差(RSD)在1. 3%～4. 5%之间,表明结果可靠且符合环境水样中铬元素形态分析的要求。
The speciation of Cr(Ⅲ) and Cr(Ⅵ) were proposed by ultrasonic assisted dispersive liquid-liquid microextraction,using phenanthroline(C12 H8 N2) as chelating agent and 1-hexyl-3-methylimidazolium hexafluorophosphate([C6 MIM][PF6]) as extractant coupled with inductively coupled plasma mass spectrometry(ICP-MS). The results showed that Cr(Ⅲ) had the best extraction effect when the concentration of phenanthroline was 0. 3 mol/L,pH value was 8,ultrasonic time was20 min,and ultrasonic temperature was 30℃. Cr(Ⅵ) and Cr(Ⅲ)) could be separated. Cr(Ⅲ) was determined by ICP-MS. Cr(Ⅵ) was subtracted from total chromium to obtain Cr(Ⅵ) content. The concentration of Cr(Ⅲ) showed a good linear relationship in the range of 0-80 μg/L with the detection limit of 0. 062 μg/L,the spiked recoveries were between 91. 5% and 110. 2%,and the relative standard deviations were between 1. 3% and 4. 5%,indicating that these results were reliable and this method could meet the requirements of the chromium analysis in environmental water samples.
The speciation of Cr(Ⅲ) and Cr(Ⅵ) were proposed by ultrasonic assisted dispersive liquid-liquid microextraction,using phenanthroline(C12 H8 N2) as chelating agent and 1-hexyl-3-methylimidazolium hexafluorophosphate([C6 MIM][PF6]) as extractant coupled with inductively coupled plasma mass spectrometry(ICP-MS). The results showed that Cr(Ⅲ) had the best extraction effect when the concentration of phenanthroline was 0. 3 mol/L,pH value was 8,ultrasonic time was20 min,and ultrasonic temperature was 30℃. Cr(Ⅵ) and Cr(Ⅲ)) could be separated. Cr(Ⅲ) was determined by ICP-MS. Cr(Ⅵ) was subtracted from total chromium to obtain Cr(Ⅵ) content. The concentration of Cr(Ⅲ) showed a good linear relationship in the range of 0-80 μg/L with the detection limit of 0. 062 μg/L,the spiked recoveries were between 91. 5% and 110. 2%,and the relative standard deviations were between 1. 3% and 4. 5%,indicating that these results were reliable and this method could meet the requirements of the chromium analysis in environmental water samples.
引文
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[2] Meeravali N N,Madhavi K,Kumar S J. J. Anal. Atom. Spectrom.,2016,31(8):1582
[3] Qi X,Gao S,Ding G,et al. Talanta,2017,162:345
[4] Rezaee M,Assadi Y,Milani Hosseini M R,et al. J. Chromatogr. A,2006,1116(1/2):1
[5] Clark K D,Emaus M N,Varona M,et al. J. Sep. Sci.,2018,41(1):209
[6] Lemos V A,Oliveira L A. Food Control,2015,50:901
[7] Zeng C J,Lin Y,Zhou N,et al. J. Hazard. Mater.,2012(237–238):365
[8] Wang Z H,Wang X N. Shanghai Environ. Sci.,2014,(2):65王增焕,王许诺.上海环境科学,2014,(2):65
[9] Ren F L,Meng J,Wu Y X,et al. Chinese. J. Anal. Chem.,2009,37(4):629任凤莲,孟杰,吴元雄,等.分析化学,2009,37(4):629
[10] Li R Y,Li Y M,Wu J J. Metall. Anal.,2011,31(3):76李人宇,李咏梅,吴俊杰.冶金分析,2011,31(3):76
[11] Trzonkowska L,Les'niewska B,Godlewskaz`ykiewicz B. React. Funct. Polym.,2017,117:131
[12] Sharma N,Tiwari S,Saxena R. Rsc Adv,2016,6(13):10775
[13] Zhu X S,Jiang Z C,Hu b,et al. Chinese. J. Anal. Chem.,2003,31(11):1312朱霞石,江祖成,胡斌,等.分析化学,2003,31(11):1312
[14] Yan H,Wang H. J. Chromatogr. A,2013,1295(5):1
[15] Hu Q,He M,Mei Y,et al. Talanta,2016,163:146
[16] GB/T 27417-2017,Comformity assessment-Guidance on validation and verification of chemical analytical methods GB 27417-2017,合格评定化学分析方法确认和验证指南