Abstract: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 values.
[1] 王丹,孙莹,马洪波.电感耦合等离子体原子发射光谱法测定钴铬钨合金中钨镍铁钒[J].冶金分析,2018,38(2):42-46. WANG Dan,SUN Ying,MA Hongbo.Determination of tungsten, nickel, iron and vanadium in cobalt chromium tungsten alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2018,38(2):42-46. [2] 付海阔,何海梅.丁二酮肟沉淀分离-EDTA滴定法测定镍钴锰三元氢氧化物中镍[J].冶金分析,2020,40(7):47-51. FU Haikuo,HE Haimei.Determination of nickel in nickel-cobalt-manganese composite hydroxide by EDTA titration after precipitation separation using dimethylglyoxime[J].Metallurgical Analysis,2020,40(7):47-51. [3] 王素梅,张慧珍,蒋天怡,等.氨水沉淀分离EDTA络合滴定法测定镧镍合金废渣中的镍[J].稀土,2018,39(4):119-124. WANG Sumei,ZHANG Huizhen,JIANG Tianyi,et al.Determination of nickel in waste lanthanum-nickel alloy by EDTA titrimetry after separation by precipitation with ammonia[J].Chinese Rare Earths,2018,39(4):119-124. [4] 祁玉静,范丽新.Na2EDTA返滴定法测定铜镍合金中的镍含量[J].中国无机分析化学,2021,11(2):62-65. QI Yujing,FAN Lixin.Determination of nickel in crude copper by Na2EDTA back titration[J].Chinese Journal of Inorganic Analytical Chemistry,2021,11(2):62-65. [5] 明帮来,谢英豪,钟敏方,等.酒石酸掩蔽-丁二酮肟重量法测定二次电池废料中镍[J].理化检验(化学分册)(Physical Testing and Chemical Analysis(Part B:Chemical Analysis)),2021,57(4):370-373. [6] 陈兰,胡军凯,潘晓玲,等.硫代硫酸钠掩蔽铜-丁二酮肟重量法测定含铜工业硫酸镍中镍[J].冶金分析,2018,38(2):66-69. CHEN Lan,HU Junkai,PAN Xiaoling,et al.Determination of nickel in copper-containing industrial nickel sulfate by dimethylglyoxime gravimetry after masking copper with sodium thiosulfate[J].Metallurgical Analysis,2018,38(2):66-69. [7] 王彤,冯振华,徐进勇,等.分光光度法测定高铁、高镁红土镍矿中的镍[J].中国无机分析化学,2012,2(2):20-23. WANG Tong,FENG Zhenhua,XU Jinyong,et al.Determination of nickel in laterite-nickel ore with high iron and high magnesium by spectrophotometry[J].Chinese Journal of Inorganic Analytical Chemistry,2012,2(2):20-23. [8] 刘宪彬,罗辉,路宁宁.丁二酮分光光度法测定高炉冶炼镍基体料中镍[C]//第十六届国际冶金及材料分析测试学术报告会论文集.北京:中国金属学会,2012(化学分册):428-431.