微波消解-ICP-OES法测定哈氏C-276合金中Cr、Fe、Mo、W元素

Determination of Cr、Fe、Mo、W in Hastelloy C-276 Alloy by ICP-OES with Microwave Digestion Method

中文关键词:  微波消解  电感耦合等离子体发射光谱  哈氏C-276合金  溶解方式  Cr  Fe  Mo  W

英文关键词:microwave digestion  ICP-OES  hastelloy C-276 alloy  dissolve method  chromium  iron  molybdenum  tungsten

中文摘要:

      建立了微波消解-电感耦合等离子体发射光谱法同时测定哈氏C-276合金中Cr、Fe、Mo、W元素含量的分析方法.采用10 mL HCl-HNO₃-HF（体积比为10∶1∶1）混合酸溶解试样.研究了合金不同溶解方式、元素谱线的选择、背景校正等试验条件，并对仪器分析参数进行了优化，确定了最佳的试验条件，各元素分析谱线依次为Cr 267.716 nm、Fe 238.204 nm、Mo 202.031 nm、W 209.712 nm，建立的校准曲线各元素相关系数均在0.999 5以上.实际样品分析中，加标回收率为97.8%~102.7%，重复测定结果的相对标准偏差小于1.64%（n=6），试验测定结果与镍基标准样品标准值做对照，结果表明方法准确、快速，能够满足日常生产的检测要求.

英文摘要:

      A method for the determination of Cr, Fe, Mo and W in Hastelloy C-276 alloy using an inductively coupled plasma-optical emission spectrometer (ICP-OES) with the microwave digestion method was developed. The sample was dissolved completely with 10 mL of hydrochloric acid-hydrofluoric acid-nitric acid (with 10∶1∶1 volume ratio). Experimental conditions, including comparison of different methods for the dissolution of alloy the selection of elemental line, background correction and optimization of instruments parameters, were discussed and optimized. The analytical spectral lines for elements were selected as follows: Cr 267.716 nm,Fe 238.204 nm,Mo 202.031 nm,W 209.712 nm. The linear correlation coefficients of the calibration curves were all over 0.999 5.The relative standard deviations (RSD, n=6) of the determination results were less than 1.64%, the recovery rates were from 97.8% to 102.7%. Compared with the certified values by the standard sample of nickel base, the results showed that the method is rapid and accurate, and can satisfy with the requirements of daily testing.