Abstract

A technique for analysis of secondary tungsten-containing raw materials (tungsten-containing sludge) using inductively coupled plasma atomic emission spectrometry in combination with microwave autoclave sample preparation has been developed. The composition of the acid mixture and algorithm of microwave heating of the autoclave are chosen to provide a complete quantitative transfer of the sample into a convenient analytical form for subsequent ICP-AES determination of the main components (heating of the sample to 220°C in the acid mixture of NH₄F, HNO₃, and HCl provides a quantitative transfer of its components to be determined into the solution). Analytical lines free from spectral interference were selected to determine Ti, Cr, Fe, Co, Ni, and W. We used real industrial samples of secondary raw materials obtained in product manufacture from VK-type hard alloys [solid solution of tungsten carbide grains (WC phase) in cobalt (Co phase)] in the form of tungsten-containing powders, grinding sludge of solid sintered alloys, dust waste, defective mixtures, waste of ventilation systems, and carbide powders. Correctness of the determination of elements was proved in analysis of ferrotungsten standard samples upon determination of the matrix component (tungsten) and by the methods of additives and sample weight variation upon determination of the alloying elements and impurities. The method of internal standard (with Sc as the element of comparison) was used to improve the precision and accuracy of the tungsten determination. The relative standard deviation was thus reduced from 0.03 to 0.004. The developed precise rapid technique was tested in analysis of industrial samples of secondary tungsten-containing sludge of hard alloys. The technique is recommended to control the composition of the secondary tungsten-containing sludge of hard alloys in a wide range of concentrations.

中文翻译：

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电感耦合等离子体原子发射光谱法（ICP-AES）分析含钨污泥的技术的发展

摘要

开发了一种使用电感耦合等离子体原子发射光谱法结合微波高压釜样品制备技术分析二次含钨原料（含钨污泥）的技术。选择酸混合物的成分和高压釜的微波加热算法，以将样品完全定量转移为方便的分析形式，以便随后进行ICP-AES测定主要成分（将样品加热至220°C）。 NH ₄ F，HNO ₃的酸混合物，而HCl则可将其待确定的组分定量转移到溶液中）。选择没有光谱干扰的分析线来确定Ti，Cr，Fe，Co，Ni和W。我们使用从VK型硬质合金[碳化钨晶粒的固溶体（钴（Co相）形式的钨相，固态烧结合金的研磨污泥，粉尘废物，有缺陷的混合物，通风系统废物和碳化物粉末。在测定基体成分（钨）时分析钨铁标准样品，并在确定合金元素和杂质时通过添加剂和样品重量变化的方法证明了元素测定的正确性。采用内标法（以Sc为比较元素）提高了钨的测定精度和准确性。相对标准偏差因此从0.03降低到0.004。在分析硬质合金二次含钨污泥的工业样品时，对开发的精密快速技术进行了测试。推荐使用该技术来控制各种浓度范围的硬质合金二次含钨污泥的成分。