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Sensitive determination of iodine species, including organo-iodine, for freshwater and seawater samples using high performance liquid chromatography and spectrophotometric detection

机译:使用高效液相色谱和分光光度检测法灵敏测定淡水和海水样品中的碘,包括有机碘

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摘要

In order to more effectively use iodine isotope ratos, ~(129)I/~(127)I, as hydrological and geochemical tracers in aquatic systems, a new high performance liquid chromatography (HPLC) method was developed for the determination of iodine speciation. The dissolved iodine species that dominate natural water systems are iodide, iodate, and organic iodine. Using this new method, iodide was determined directly by combining anion exchange chromatography and spectrophotmetry. Iodate and the total of organic iodine species are determined as iodide, with minimal sample preparation, compared to existing methods. The method has been applied to quantitatively determine iodide, iodate as the difference of total inorganic iodide and iodide after reduction of the sample by NaHSO_3, and organic iodine as the difference of total iodide (after organic decomposition by dehydrohalogenation and reduction by NaHSO_3) and total inorganic iodide. Analytical accuracy was tested: (1) against certified reference material, SRM 1549, powdered milk (NIST); (2) through the method of standard additions; and (3) by comparison to values of environmental waters measured independently by inductively coupled plasma mass spectrometry (ICP-MS). The method has been successfully applied to measure the concentrations of iodide species in rain, surface and ground water, estuarine and seawater samples. The detection limit was approx 1 nM (0.2 ppb), with less than 3% relative standard deviation (R.S.D.) for samplets determined by standard additions to an iodide solution of 20 nM in 0.1 M NaCl. This technique is one of the few methods sensitive enough to accurately quantify stable iodine species at nanomolar concentrations in aquatic systems across a range of matrices,and to quantitatively measure organic iodine. Additionally,this method makes use of a very dilute mobile phase, and may be applied to small sample volumes without pre-column concentration or post-column reactions.
机译:为了更有效地使用〜(129)I /〜(127)I碘同位素作为水生系统中的水文和地球化学示踪剂,开发了一种新的高效液相色谱(HPLC)方法来测定碘的形态。在自然水系统中占主导地位的溶解碘物种是碘化物,碘酸盐和有机碘。使用这种新方法,可以通过结合阴离子交换色谱法和分光光度法直接测定碘。与现有方法相比,只需最少的样品制备即可确定碘化物和有机碘的总量。该方法已用于定量测定碘化物,碘化物为样品中总无机碘化物与碘化钠之差,再用NaHSO_3还原,有机碘为总碘化物(经脱卤化氢分解后再用NaHSO_3还原)之差。无机碘化物。分析准确性的测试:(1)以认证标准物质SRM 1549,奶粉(NIST)为对照; (2)通过标准添加的方法; (3)与通过电感耦合等离子体质谱(ICP-MS)独立测量的环境水的值进行比较。该方法已成功地用于测量雨水,地表水和地下水,河口和海水样品中碘化物的浓度。样品的检出限约为1 nM(0.2 ppb),相对样品的相对标准偏差(R.S.D.)小于3%,该样品是通过向20 nM的0.1 M NaCl碘化物溶液中标准添加而确定的。这项技术是为数不多的灵敏度极高的方法之一,可以准确地定量分析一系列基质中水系统中纳摩尔浓度的稳定碘物种,并定量测量有机碘。此外,该方法利用了非常稀的流动相,可用于小体积样品,而无需进行柱前浓缩或柱后反应。

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