电感耦合等离子体原子发射光谱法测定铝钨合金中钨

以盐酸和过氧化氢溶解样品,电感耦合等离子体原子发射光谱法(ICP-AES)测定了铝钨合金中钨。着重研究样品的溶解条件,确定了先加入盐酸至铝基质颗粒反应完全后再加入10 mL过氧化氢的试剂加入顺序。过氧化氢用量随着样品中钨含量的不同而不同,但对于溶解钨含量为0.10%~15%铝钨合金样品,过氧化氢加入量在100 mL以下对测定结果无影响。钨的质量浓度在500 mg/L内校准曲线的线性关系良好,相关系数为0.999 5。基体铝对测定的影响采用基体匹配方法消除。方法应用钨质量分数不同的铝钨中间合金分析,钨的测定值与辛可宁重量法测定值一致,回收率在98％～102％之间,相对标准偏差(RSD,n=9)为2.8％～5.1％。方法能满足科研与生产的快速检测需要。

Determination of tungsten in aluminum-tungsten alloy by inductively coupled plasma atomic emission spectrometry

The sample was dissolved with hydrochloric acid and hydrogen peroxide. Then, the content of tungsten in aluminum-tungsten alloy was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The sample dissolution conditions were studied in detail. The following addition sequence of reagents was obtained: the aluminum-based particles were firstly dissolved in hydrochloric acid; after complete reaction, 10 mL of hydrogen peroxide was added. The dosage of hydrogen peroxide was different for samples with different tungsten contents. However, for aluminum-tungsten alloy samples with tungsten content of 0.10 %-15.00%, the dosage of hydrogen peroxide had no influence on the determination results when more than 100 mL of hydrogen peroxide was added. The linearity of calibration curve was good when the mass concentration of tungsten was within 500 mg/L. The correlation coefficient was 0.999 5. The effect of matrix aluminum could be eliminated by matrix matching method. The proposed method was applied to the analysis of aluminum-tungsten intermediate alloys with various mass fraction of tungsten. The found results were consistent with those obtained by cinchonine gravimetric method. The recoveries were between 98% and 102%. The relative standard deviation (RSD, n=9) was 2.8%-5.1%. This method could meet the requirements of rapid analysis for scientific research and production.