电感耦合等离子体原子发射光谱法测定锆铪合金中磷铁铪

Determination of phosphorus,iron and hafnium in zirconium-hafnium alloy by inductively coupled plasma atomic emission spectrometry

锆铪合金性能优异、应用广泛,其化学成分须准确测定。试验采用10 mL盐酸-2 mL氢氟酸-1 mL硝酸消解样品,选择P 178.221 nm、Fe 239.562 nm、Hf 277.336 nm为分析线并采用两点校正法扣除背景,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定锆铪合金中磷、铁、铪的分析方法。各元素校准曲线线性良好,相关系数均不小于0.999;方法测定范围为:0.002%~0.036%磷,0.01%~0.36%铁,1.00%~5.00%铪。方法中各元素检出限为0.000032%~0.0019%(质量分数)。按照实验方法测定1个锆铪合金样品中磷、铁、铪,测定结果的相对标准偏差(RSD,n=10)小于3%;回收率为94%~107%。

Zirconium-hafnium alloy has excellent properties and it has been widely used.The chemical composition of zirconium-hafnium alloy should be determined accurately.The sample was dissolved with 10 mL of hydrochloric acid-2 mL of hydrofluoric acid-1 mL of nitric acid.P 178.221 nm,Fe 239.562 nm and Hf 277.336 nm were selected as the analytical line.The background was deducted by two-point correction method.The determination method of phosphorus,iron and hafnium in zirconium-hafnium alloy by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.The calibration curves of elements had good linearity and the correlation coefficients were all higher than 0.999.The determination range of the method was 0.002%-0.036%for phosphorus,0.01%-0.36%for iron and 1.00%-5.00%for hafnium,respectively.The limit of detection of elements were in range of 0.000032%-0.0019%(mass fraction).The contents of phosphorus,iron and hafnium in one zirconium-hafnium alloy sample were determined according to the experimental method.The relative standard deviations(RSD,n=10)of determination results were less than 3%,and the recoveries were between 94%and 107%.