电感耦合等离子体原子发射光谱法测定铌锰铁中铌和锰

铌锰铁是炼钢过程中的一种重要原料,建立测定铌和锰的方法尤为重要。铌锰铁中铌和锰为主元素,含量高,运用化学湿法分析时主元素之间会相互干扰,影响测定的准确性。实验采用盐酸、硝酸、氢氟酸溶解样品,选择Nb 269.706nm为分析线、Mo 281.618nm为内标线;选择Mn 293.305nm为分析线、V 292.401nm为内标线,建立了采用电感耦合等离子体原子发射光谱法(ICP-AES)测定铌锰铁中铌和锰的方法。共存元素的干扰校正试验表明,样品中共存元素对待测元素无干扰。各待测元素的校准曲线线性相关系数均大于0.999 5。实验方法用于铌锰铁实际样品中铌和锰的测定,铌测定结果的相对标准偏差(RSD,n=11)为0.26%～0.28%;锰测定结果的相对标准偏差(RSD,n=11)为0.29%～0.33%。采用实验方法对铌锰铁实际样品中铌和锰进行测定,测得结果分别与日本标准JIS G 1328—1982中丹宁酸水解重量法测定铌和国标GB/T 5686.1—2008中高氯酸氧化滴定法测定锰的结果基本一致。

Determination of niobium and manganese in niobium-manganese-iron alloy by inductively coupled plasma atomic emission spectrometry

Niobium-manganese-iron alloy is important raw material in steel making process, so it is necessary to establish the method for the determination of niobium and manganese. Niobium and manganese are the major elements in niobium-manganese-iron alloy and their contents are high. The mutual interference of major elements exists in the chemical wet analysis of niobium-manganese-iron, which influences on the accuracy of determination. The sample was dissolved with hydrochloric acid, nitric acid and hydrofluoric acid. Nb 269.706nm was selected as the analytical line for niobium and Mo 281.618nm was used as the internal standard line. Mn 293.305nm was selected as the analytical line for manganese and V 292.401nm was used as the internal standard line. The determination method of niobium and manganese in niobium-manganese-iron alloy by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The interference correction tests of coexisting elements showed that the coexisting elements in sample had no influence on the testing elements. The linear correlation coefficients of calibration curves for testing elements were all higher than 0.9995. The experimental method was applied for the determination of niobium and manganese in actual niobium-manganese-iron alloy sample. The relative standard deviation (RSD, n=11) of determination results for niobium was 0.26%-0.28%, and the RSD for manganese was 0.29%-0.33%. The contents of niobium and manganese in actual niobium-manganese-iron alloy sample were determined according to the experimental method. The found results were basically consistent with those obtained by JIS G 1328-1982 Determination of niobium content by tannic acid hydrolysis gravimetric method and GB/T 5686.1-2008 Determination of manganese content by perchloric acid oxidation titration method.