Process-accompanying analysis of solid intermediate and end products in the manufacturing process of high-purity tungsten by ETV-ICP-OES

Many solids from the production of high-purity tungsten are challenging to analyze due to their insolubility and tungsten's high spectral line density, which causes interferences in many spectroscopic methods. To address this, electrothermal vaporization (ETV) coupled with inductively coupled plasma optical emission spectrometry (ICP-OES) was optimized for the direct multi-element analysis of various tungsten-based materials, including ammonium paratungstate ((NH4)10(H2W12O42) ∙ 4 H2O), yellow tungsten oxide (WO3), blue tungsten oxide (WO2+x), tungsten metal powder (W) and tungsten carbide (WC). The method focused on detecting critical contaminants like Al, B, P, S and Si as well as O in W and WC, which affect the characteristics of final products.高纯钨生产过程中产生的诸多固体物料因难溶性以及钨本身极高的谱线密度，易对多数光谱分析方法造成干扰，因此分析难度极大。为此，研究人员针对电热蒸发（electrothermal vaporization, ETV）与电感耦合等离子体光发射光谱法（inductively coupled plasma optical emission spectrometry, ICP-OES）联用技术进行优化，以实现多种钨基材料的直接多元素分析，所涉物料包括仲钨酸铵((NH4)10(H2W12O42)·4H2O)、黄色氧化钨(WO3)、蓝色氧化钨(WO2+x)、金属钨粉(W)以及碳化钨(WC)。该方法重点检测会影响最终产品性能的关键污染物，包括钨及碳化钨中的铝(Al)、硼(B)、磷(P)、硫(S)、硅(Si)以及氧(O)。