摘要
称取镍基单晶高温合金0.100 0g于聚四氟乙烯烧杯中,先令其与盐酸9mL和硝酸1mL加热反应,待反应缓慢时滴加氢氟酸2mL并继续加热使样品完全溶解。加入500g·L^-1酒石酸溶液2mL,冷却至室温,在塑料容量瓶中加水定容至100.0mL。按仪器工作条件采用电感耦合等离子体原子发射光谱法测定其中5种合金元素(Mo、W、Ta、Re、Ru)的含量,选择分析谱线依次为204.598,207.911,240.063,197.312,240.272nm。结果发现:除了Re外,其余4种元素的测定中均受共存元素的光谱干扰,严重影响了测定结果的准确性。为克服其干扰,除了采用基体匹配法消除镍的基体干扰外,试验采用混合校正系数矩阵法对测定结果进行校准。通过一系列试验计算得到混合校准系数矩阵K,并应用于模拟样品的分析。结果表明:经过矩阵K的校准,所测定的5种元素的准确度显著提高,达到了消除共存元素之间光谱干扰的目的。通过精密度试验,测得上述5种元素测定值的相对标准偏差(n=11)均在1.5%以下,并通过标准加入法进行回收试验,测得5种元素的回收率为97.0%~105%。
A portion(0.100 0 g)of the Ni-based single crystal supper alloy sample was dissolved in a PTFE beaker with 9 mL of HCl and 1 mL of HNO3 and 2 mL of HF successively by heating.The solution was cooled and 2 mL of 500 g·L^-1 tartaric acid solution were added and the solution was diluted to 100.0 mL with water in a plastic volumetric flask.Five alloy elements(Mo,W,Ta,Re and Ru)were determined this sample solution by ICP-AES under the working condition of the instrument.Analytical spectral line chosen for these elements were 204.598,207.911,240.063,197.312,240.272 nm respectively.It was found that besides Re,spectral interferences were encountered in the determination of the 4 remainder elements,leading to serious errors of the analytical results.To overcome this trouble,in addition to the elimination of matrix effect due to Ni,by the matrix matching method,the matrix method of mixed correction coefficients was tested to correct the spectral interferences.Base on the known values of mass concentrations of the testing elements and their ICP-AES determined values in mass concentrations,values of matrix K of mixed correction coefficients were calculated according to the given formula,and by applying the values of matrix K,the errors encountered could be corrected.Precision and recovery of the ICP-AES method after correction by the matrix method of mixed correction coefficients were tests,giving RSDs(n=11)for the 5 elements less than 1.5%and values of recovery obtained by standard addition method in the range of 97.0%-105%.
作者
朱天一
冯典英
李本涛
黄辉
李颖
巩琛
ZHU Tianyi;FENG Dianying;LI Bentao;HUANG Hui;LI Ying;GONG Chen(Institute of China North Industries Group,Jinan 250000,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2020年第4期443-448,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
