电感耦合等离子体发射光谱法测定钨铼合金中铼的含量

Determination of rhenium content in tungsten-rhenium alloys by inductively coupled plasma emission spectrometry

建立了电感耦合等离子体发射光谱测定钨铼合金中质量分数为0.50%~26.00%的铼含量的方法。以硝酸和氢氟酸溶解样品,优化了仪器工作参数和实验条件,考察了WRe0.5, WRe2, WRe5和WRe25 4牌号的钨铼合金样品的方法精密度和正确度,并委托8家实验室开展协同试验。经统计分析,4个牌号样品中铼含量的平均值分别为0.514%, 2.048%, 5.058%和26.22%,测定结果的相对标准偏差为0.22%~2.4%,加标回收率为97.9%~102.5%,重复性限分别为0.023%, 0.077%, 0.193%和0.501%,再现性限分别为0.032%, 0.145%, 0.235%和0.623%。采用丁二酮肟分光光度法进行比对验证,经F检验和t检验分析,2种方法具有较好的一致性。

A method was established for the determination of rhenium content in tungsten-rhenium alloys with mass fraction ranging from 0.50% to 26.00% by inductively coupled plasma emission spectrometry. After dissolving with nitric acid and hydrofluoric acid, the working parameters of the instrument and the experimental conditions were optimized. The precision and accuracy of the method were tested with the tungsten-rhenium alloy samples of WRe0.5, WRe2, WRe5 and WRe25. Eight laboratories were commissioned to carry out collaborative tests. Through statistical analysis, the total average values of the four grades of samples were 0.514%, 2.048%, 5.058% and 26.22%, respectively, the relative standard deviations were 0.22%-2.4%, and the recoveries were 97.9%-102.5%. The repeatability limits were 0.023%, 0.077%, 0.193% and 0.501%, and the reproducibility limits were 0.032%, 0.145%, 0.235% and 0.623%, respectively. Butanedione oxime spectrophotometry was used for comparison and verification. Both F test and t test showed that the two methods had good consistency.