微波消解-丁二酮肟分光光度法测定钴铬钨系合金粉末中镍  

Determination of nickel in cobalt-chromium-tungsten alloy powder by dimethylglyoxime spectrophotometry with microwave digestion

作　　者：许洁瑜 王芳 张永进 XU Jieyu;WANG Fang;ZHANG Yongjin(Center of Industrial Analysis Testing,Guangdong Academy of Science,Guangzhou 510651,China)

机构地区：[1]广东省科学院工业分析检测中心,广东广州510651

出　　处：《冶金分析》2022年第6期80-84,共5页Metallurgical Analysis

基　　金：2021年省属科研机构改革创新领域稳定支持项目(202102020626)。

摘　　要：钴铬钨(CoCrW)系合金是钴基硬质合金的一种,具有优异的耐磨粒磨损、耐冲蚀磨损、耐高温磨损、抗高温氧化和热疲劳等综合性能。目前钴铬钨系合金粉末尚无对应的检测标准,国内外相关的论文报道也较少。镍作为钴铬钨系合金粉末的主要成分,迫切需要开发其检测方法为生产、使用和贸易等方面提供指导。采用10 mL盐酸、3 mL硝酸和2 mL氢氟酸对样品进行微波消解,以酒石酸钾钠作掩蔽剂,在氢氧化钠的强碱性介质中,以过硫酸铵作氧化剂,镍与丁二酮肟生成可溶性的酒红色络合物,于分光光度计530 nm波长处进行测定,建立了丁二酮肟分光光度法测定钴铬钨系合金粉末中镍的方法。根据样品中各元素的含量范围,按照共存元素含量最大值的2或5倍加入共存元素进行干扰试验。结果表明:镍的回收率为100%~101%,说明样品中共存元素不干扰镍的测定。将实验方法应用于钴铬钨系合金粉末实际样品中镍的测定,结果的相对标准偏差(RSD,n=11)为0.26%~1.8%,加标回收率为97%~102%。根据样品中各元素的组成范围,合成钴铬钨系合金粉末模拟样品,按照实验方法进行测定,镍的测定值与理论值相符。Cobalt-chromium-tungsten(Co-Cr-W) alloy is a kind of cobalt-based hard alloy. It has excellent comprehensive performance including abrasive wear resistance, erosive wear resistance, high temperature wear resistance, high temperature oxidation resistance and thermal fatigue resistance. So far, there is no related detection standard method for Co-Cr-W alloy powder, and there are also only few reports about this at domestic and abroad. Nickel is the major component in Co-Cr-W alloy powder, and it is urgent to develop a method for determination of nickel, thus providing guidance for the production, use and trade of Co-Cr-W alloy. The sample was treated by microwave digestion with 10 mL of hydrochloric acid, 3 mL of nitric acid and 2 mL of hydrofluoric acid. Potassium sodium tartrate was selected as the masking agent and ammonium persulfate was selected as the oxidant. Nickel could form a soluble wine-red complex with dimethylglyoxime in a strong alkaline medium of sodium hydroxide. The complex was determined with spectrophotometer at 530 nm. Thus, a method for determination of nickel in Co-Cr-W alloy powder was established by dimethylglyoxime spectrophotometry. According to the content range of each element in sample, the interference tests of coexisting elements were conducted by adding 2 or 5 times of maximum content. The results showed that the recoveries of nickel were between 100% and 101%, indicating that the coexisting elements in sample had no interference with the determination of nickel. The experimental method was applied for determination of nickel in actual sample of Co-Cr-W alloy powder, and the addition standard recovery test was conducted. The relative deviations(RSD, n=11) of determination results were between 0.26% and 1.8%, and the recoveries were between 97% and 102%. According to the composition range of elements in sample, the simulated samples of Co-Cr-W alloy powder were synthesized and determined by the experimental method. The results of nickel content were consistent with the theoretical va

关 键 词：微波消解 钴铬钨(CoCrW)系合金粉末 镍 丁二酮肟 分光光度法 

分 类 号：O657.32[理学—分析化学] TF031[理学—化学]