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Determination of total and soluble chromium(Ⅵ) in compost by ion chromatography-inductively coupled plasma mass spectrometry

机译:离子色谱-电感耦合等离子体质谱法测定堆肥中总铬和可溶性铬(Ⅵ)

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Ion chromatography coupled to inductively coupled plasma quadrupole mass spectrometry (IC-ICP-MS) was used for the specific determination of Cr(Ⅵ) in compost samples. Potential interferences from humic substances, carbon and chlorine species were avoided by chromatographic separation. Solution detection limits below 150 ng L~(-1) were obtained for injection volumes of 100 μL. Total Cr(Ⅵ) was determined by the previous alkaline digestion of the sample, following the method EPA3060A. Recoveries of pre- and post-digestion spikes (2.5 μg and 50 μgL~(-1) of Cr(Ⅵ) as potassium chromate, respectively) were better than 90%, indicating that the combined method can provide accurate results in spite of the high content of organic matter. Detection limits of 6 ng g~(-1) were obtained for the total Cr(Ⅵ) determination, the repeatability was better than 2% (at 30 μg L~(-1)), and the reproducibility between extractions was around 6%. Soluble Cr(Ⅵ) was determined by the leaching of compost samples with water (liquid-to-solid ratio 10:1). A total Cr(Ⅵ) content of 1.2 μg g~(-1) was obtained for a compost from urban solid residues, whereas the soluble Cr(Ⅵ) in the pH range 4-10 was below the detection limit of the leaching method (1 ng g~(-1)).
机译:离子色谱-电感耦合等离子体四极杆质谱(IC-ICP-MS)用于堆肥样品中Cr(Ⅵ)的特异性测定。色谱分离避免了腐殖质,碳和氯物种的潜在干扰。对于100μL的进样量,获得的溶液检测限低于150 ng L〜(-1)。按照EPA3060A的方法,通过先前的碱消解法测定了总Cr(Ⅵ)。消解前和消解后峰值(分别为2.5μg和50μgL〜(-1)的铬(Ⅵ)为铬酸钾)的回收率均优于90%,这表明尽管采用该方法,该组合方法仍可提供准确的结果高含量的有机物。测定总Cr(Ⅵ)的检出限为6 ng g〜(-1),重复性优于2%(在30μgL〜(-1)时),两次萃取之间的重现性约为6% 。通过用水浸出堆肥样品(液固比10:1)来测定可溶性Cr(Ⅵ)。从城市固体残渣中获得的堆肥的总Cr(Ⅵ)含量为1.2μgg〜(-1),而pH范围4-10中的可溶性Cr(Ⅵ)低于浸出方法的检测极限( 1 ng g〜(-1))。

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