微波消解-电感耦合等离子体原子发射光谱（ICP-AES）法测定镍基耐蚀合金中镍

采用微波消解法与电感耦合等离子体原子发射光谱(ICP-AES)法相结合的方式,建立了镍基耐蚀合金中镍元素含量的测定方法。试样在浓硝酸和浓盐酸中微波消解后,用电感耦合等离子体原子发射光谱仪在优化的工作参数下测定,结果表明,稀释的消解液可直接用于镍含量的测定,光谱干扰少。对镍基耐蚀合金中镍含量进行多次平行测定,相对标准偏差(RSD,n=7)为0.29%,且测得值与标准值结果一致。对不同的镍基耐蚀合金样品进行加标回收实验,加标回收率在98.5%~102%。标准物质验证实验表明,测得值与标准值一致。

Determination of nickel content in Ni-based corrosion-resistant alloys by Microwave digestion-inductively coupled plasma emission method

The analysis method of nickel in Ni-based corrosion-resistant alloys by microwave digestion-inductively coupled plasma atomic emission spectrometry was established.The sample was dissolved with nitric acid and hydrochloric acid by microwave digestion,and then measured under optimized operating parameters by inductively coupled plasma emission spectrometer.The results show that the diluted solution can be used for the direct determination of nickel content with less spectral interference.The relative standard deviation(RSD,n=7)was 0.29%,and the measured value was consistent with the standard value.The recovery of nickel base corrosion resistant alloy samples was 98.5%—102%.The verification test by using reference standard showed that the measured values are in agreement with the standard values.