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首页> 外文期刊>Journal of Environmental Science and Health. A, Toxic/Hazardous Substances & Environmental Engineering >Separation and Quantification of Tl(Ⅰ) and Tl(Ⅲ) in Fresh Water Samples
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Separation and Quantification of Tl(Ⅰ) and Tl(Ⅲ) in Fresh Water Samples

机译：淡水样品中Tl（Ⅰ）和Tl（Ⅲ）的分离与定量

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摘要

The two oxidation states of thallium, Tl(Ⅰ) and Tl(Ⅲ), were quantified by IC-ICP-MS using complexation of Tl~(3+) with DTPA (penta-carboxymethyl-diethylenetriamine) and separation on a cation exchange column according to a modification of the method devised by Coetzee et al. In order to avoid successively lowered separation efficiency and loss of resolution during a run, a gradient elution was made using HCl instead of HNO_3. With an ultrasonic nebuliser instead of a Ⅴ-groove nebuliser the limit of detection for Tl(Ⅰ) and Tl(Ⅲ) could be lowered from 25 ng/L and 3.0 ng/L to 9.0 ng/L and 0.7 ng/L, respectively, which is adequate for many fresh water systems. The stability of Tl(Ⅲ) in acidic solutions was found to be concentration dependent, with an initially high reduction rate of Tl(Ⅲ). Exposure of the sample to light further increased the reduction rate. Addition of DTPA (0.01 mM) and acid (HNO_3, 1%) to a sample with 1 μg/L Tl(Ⅲ) stabilised the Tl(Ⅲ) content for at least 48 h. Analysis of field samples showed that only acidification is inadequate to maintain the original distribution of Tl(Ⅰ) and Tl(Ⅲ). Internal calibration (standard addition) and correction of the analytical signal (~(205)Tl) with a non-ionic internal standard (~(11)B) yielded almost quantitative recoveries of both Tl(Ⅰ) and Tl(Ⅲ). A scheme for field sample preparation is proposed, including sampling, storage and pre-analysis treatment.
机译：l（3+）与DTPA（五羧甲基-二亚乙基三胺）的络合并在阳离子交换柱上分离，采用IC-ICP-MS定量测定th的两种氧化态Tl（Ⅰ）和Tl（Ⅲ）。根据Coetzee等人设计的方法的修改。为了避免运行中连续降低分离效率和分离度，使用HCl代替HNO_3进行梯度洗脱。用超声波雾化器代替Ⅴ槽雾化器，可将Tl（Ⅰ）和Tl（Ⅲ）的检出限分别从25 ng / L和3.0 ng / L降低到9.0 ng / L和0.7 ng / L ，足够用于许多淡水系统。发现Tl（Ⅲ）在酸性溶液中的稳定性与浓度有关，最初具有较高的Tl（Ⅲ）还原率。样品暴露于光下进一步降低了还原速率。在具有1μg/ L Tl（Ⅲ）的样品中添加DTPA（0.01 mM）和酸（HNO_3，1％）可使Tl（Ⅲ）含量稳定至少48 h。现场样品分析表明，仅酸化不足以维持Tl（Ⅰ）和Tl（Ⅲ）的原始分布。内部校准（标准添加）和使用非离子内标（〜（11）B）对分析信号（〜（205）T1）的校正几乎可以定量回收Tl（Ⅰ）和Tl（Ⅲ）。提出了一种野外样品制备方案，包括采样，存储和分析前处理。

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