CHROMIUM SPECIATION BY ANION-EXCHANGE HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY WITH BOTH INDUCTIVELY-COUPLED PLASMA-ATOMIC EMISSION SPECTROSCOPIC AND INDUCTIVELY-COUPLED PLASMA-MASS SPECTROMETRIC DETECTION
CHROMIUM SPECIATION BY ANION-EXCHANGE HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY WITH BOTH INDUCTIVELY-COUPLED PLASMA-ATOMIC EMISSION SPECTROSCOPIC AND INDUCTIVELY-COUPLED PLASMA-MASS SPECTROMETRIC DETECTION
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DOI：
10.1016/0021-9673(95)00528-u
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发表时间：
1995-10-13
影响因子：
4.1
通讯作者：
CARUSO, JA
中科院分区：
文献类型：
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作者：
BYRDY, FA;OLSON, LK;CARUSO, JA
本文描述了一种测定Cr(III)和Cr(VI)的新方法的开发过程。在初步研究中，采用阴离子交换高效液相色谱法（HPLC）分离Cr(III)和Cr(VI)，并通过电感耦合等离子体原子发射光谱法（ICP - AES）在2766埃处进行在线检测；在最终的研究工作中，采用电感耦合等离子体质谱法（ICP - MS）在质荷比m/z 52和m/z 53处进行单离子监测。使用由硫酸铵和氢氧化铵组成的流动相，并采用一种简单的乙二胺四乙酸（EDTA）螯合程序来稳定标准溶液中的Cr(III)形态。ICP - MS的结果表明，由于流动相背景较高（主要来自SO⁺多原子干扰），使用铬同位素m/z 53而非更丰富的m/z 52同位素是可行的。通过HPLC - ICP - MS计算，在水介质中基于峰高的绝对检测限为Cr(III) 40 pg，Cr(VI) 100 pg。两种物质的线性动态范围均从5 ppb（纳克/毫升）扩展到1 ppm（微克/毫升）。通过HPLC - ICP - AES，Cr(III)的检测限为100 ng，Cr(VI)的检测限为200 ng。通过HPLC - ICP - MS在NIST - SRM 1643c（美国国家标准与技术研究院标准参考物质，水中微量元素）中检测到Cr(III)的含量为20 ppb。
Development of a new method for the determination of Cr(III) and Cr(VI) is described. Anion-exchange high-performance liquid chromatography (HPLC) was used to separate Cr(III) and Cr(VI) with on-line detection by inductively coupled plasma atomic emission spectroscopy (ICP-AES) at 2766 Angstrom in preliminary studies, and inductively coupled plasma mass spectrometry (ICP-MS) with single-ion monitoring at m/z 52 and m/z 53 for final work. A mobile phase consisting of ammonium sulfate and ammonium hydroxide was used, and a simple chelation procedure with EDTA was followed to stabilize the Cr(III) species in standard solutions. ICP-MS results indicated the feasibility of using chromium isotope m/z 53 instead of the more abundant m/z 52 isotope due to a high mobile-phase background most significantly from the SO+ polyatomic interference. The absolute detection limits based on peak-height calculations were 40 pg for Cr(III) and 100 pg for Cr(VI) in aqueous media by HPLC-ICP-MS. The linear dynamic range extended from 5 ppb (ng/ml) to 1 ppm (mu g/ml) for both species. By HPLC-ICP-AES, detection limits were 100 ng for Cr(III) and 200 ng for Cr(VI). Cr(III) was detected in NIST-SRM 1643c (National Institute of Standards and Technology-Standard Reference Material, Trace Elements in Water) by HPLC-ICP-MS at the 20 ppb level.