电感耦合等离子体原子发射光谱法测定镍基单晶高温合金中钨钽铪铼

Determination of tungsten,tantalum,hafnium and rhenium in nickel-based single crystal high temperature alloy by inductively coupled plasma atomic emission spectrometry

镍基单晶高温合金中高含量的钨、钽、铪、铼等难熔元素,不仅对样品前处理造成阻碍,而且其元素间的光谱干扰会对测定结果造成严重影响。实验采用18mL盐酸-2mL硝酸-2mL氢氟酸溶解样品,再加入酒石酸可使样品溶液长期稳定存在。通过研究单晶高温合金中钨、钽、铪、铼的谱线干扰情况,选择W 207.911nm、Ta 240.063nm、Hf 282.022nm、Re 197.312nm作为分析谱线,采用基体匹配法配制标准溶液系列绘制校准曲线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定镍基单晶高温合金中钨、钽、铪、铼。各元素在线性范围内校准曲线线性关系良好,相关系数均不小于0.9997;方法检出限为0.0001%~0.0008%。按照实验方法测定DD6单晶高温合金样品中钨、钽、铪、铼,结果的相对标准偏差(RSD,n=11)为1.0%~2.5%;加标回收率为96%~102%。

The high content refractory elements such as tungsten,tantalum,hafnium and rhenium in nickel-based single crystal high temperature alloy not only hinder the sample pretreatment,but also seriously influence the measurement results due to the spectral interference among elements.The sample was dissolved with 18mL of HCl,2mL of HNO3 and 2mL of HF.The addition of tartaric acid could stabilize the sample solution for long time.The spectral interference of tungsten,tantalum,hafnium and rhenium in single crystal high temperature alloy was investigated.W 207.911nm,Ta 240.063nm,Hf 282.022nm and Re 197.312nm were selected as analytical lines.The standard solution series were prepared by matrix matching method to draw the calibration curve.The contents of tungsten,tantalum,hafnium and rhenium in nickel-based single crystal high temperature alloy were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The linearity of calibration curves in linear range was good for all elements,and the correlation coefficients were higher than 0.9997.The limit of detection was in range of 0.0001%-0.0008%.The contents of tungsten,tantalum,hafnium and rhenium in DD6 single crystal high temperature alloy sample were determined according to the experimental method.The relative standard deviation(RSD,n=11)of determination results were between 1.0%and 25%.The recoveries were between 96%and 102%.