用 ICP-AES 法测定合金钢中的硒和碲时沉积铁、钨、钼和铬的技术

A. Belozerova, A. Mayorova, M. N. Bardina
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引用次数: 0

摘要

由于所研究材料中存在的宏观成分在光谱和非光谱方面的干扰,采用电感耦合等离子体原子发射光谱法(ICP-AES)直接测定冶金材料中的硒和碲杂质含量非常困难。本研究的目标是通过初步沉淀分离微量成分(Se、Te)和宏观成分(Fe、W、Mo、Cr、Cu、Ni、Co)。研究表明,使用醋酸钡和氟化钠作为沉淀剂可有效地将 Se 和 Te 与 Fe、W、Mo 和 Cr 分离(分析溶液中的含量小于原始含量的 0.1%),并将部分 Se 和 Te 与 Cu、Ni 和 Co 分离(分析溶液中的含量为原始含量的 25 至 55%)。确定了大分子成分(铁、钨、钼、铬)沉淀的最佳条件,以及抑制硒和碲在大分子成分沉淀物上共沉淀的过程,以便随后进行 ICP-AES 测定。大分子沉淀的最佳 pH 值等于 1。沉淀剂(醋酸钡和氟化钠)的最佳质量分别为 10 克和 3 克。为抑制硒和碲在大分子沉积物上的共沉淀过程,建议使用氢氟酸。确定了氢氟酸和盐酸抑制大分子沉积物上分析物共沉淀过程的最佳体积(分别为 3 和 6 立方厘米)。使用 "尖峰 "法在合金钢标准样品上测试了所开发的从宏观成分中分离微量硒、碲的程序。该技术具有令人满意的准确性和可重复性,分离宏观成分后分析物的测定极限为 10-3 wt.%。
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A technique for depositing iron, tungsten, molybdenum, and chrome in the determination of selenium and tellurium in alloy steel by ICP-AES method
Direct determination of the content of selenium and tellurium impurities in metallurgical materials by the method of inductively coupled plasma atomic emission spectroscopy (ICP-AES) is difficult due to spectral and non-spectral interference from macrocomponents present in the materials under study. The separation of micro-(Se, Te) and macro-components (Fe, W, Mo, Cr, Cu, Ni, Co) through preliminary precipitation is the goal of the study. The use of barium acetate and sodium fluoride as precipitants are shown to provide an effective separation of Se and Te from Fe, W, Mo, and Cr (the content in the analyzed solution is less than 0.1 wt.% of the original) and partial separation from Cu, Ni, and Co (the content in the analyzed solution from 25 to 55 wt.% of the original). Optimal conditions for the deposition of macrocomponents (Fe, W, Mo, Cr) and inhibition of the process of coprecipitation of selenium and tellurium on sediments of macrocomponents for their subsequent ICP-AES determination were determined. The optimal pH for the precipitation of macrocomponents equals 1. The optimal mass of precipitants (barium acetate and sodium fluoride) is 10 and 3 g, respectively. To inhibit the process of coprecipitation of selenium and tellurium on sediments of macrocomponents, it is proposed to use hydrofluoric acid. The optimal volume of hydrofluoric and hydrochloric acids for inhibiting the process of coprecipitation of analytes on sediments of macrocomponents was determined (3 and 6 cm3, respectively). The developed procedure for separating micro-Se, Te from macro-components was tested on standard samples of alloyed steels using the «spike» method. The technique is characterized by satisfactory accuracy and reproducibility, the limit of determination of analytes after separation of macrocomponents is 10–3 wt.%.
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