电感耦合等离子体原子发射光谱法测定硅铝铁合金中多种元素的优化研究

Optimization Investigation on the Elements in Ferrum Aluminum Silicon Alloy by ICP-AES

应用电感耦合等离子体原子发射光谱 (ICP AES)法 ,对硅铝铁合金中的Al,Fe ,Ca,Cr,Mn ,Ni,Si和Ti元素进行了测定。研究了ICP AES的操作条件和溶样方法 ,确定了适宜的实验条件 ,如对仪器参数和共存元素对信号的影响进行了研究。将实验条件优化后 ,使用该方法测定硅铝铁合金中多种元素 ,标准钢样测定结果与推荐值相符。对各种元素的检出限分别为Al(0 0 2 9μg·mL- 1 ) ,Fe(0 0 0 4 μg·mL- 1 ) ,Ca(0 0 0 75 μg·mL- 1 ) ,Cr(0 0 0 15 μg·mL- 1 ) ,Mn(0 0 0 0 9μg·mL- 1 ) ,Ni(0 0 0 2 7μg·mL- 1 ) ,Si(0 0 4 5 μg·mL- 1 )和Ti(0 0 0 3μg·mL- 1 )。对所测元素 ,测定结果的相对标准偏差 (n =6 )在 0 3%～ 1 8%之间 ,加入标准溶液的回收率在96 7%～ 10 2 9%范围。测定合金样品中高含量硅的结果与标准化学 (重量 )法的结果也相符。该方法的特点是数据可靠 ,简便可行和易于推广。

A method for the determination of All Fe, Ca, Cr, Mn, Ni, Si and Ti elements in ferrum aluminum silicon alloy by inductively coupled plasma atomic emission spectrometry (ICP-AES) was described. The influence of ICP-AES operating conditions, sample dissolution methods and spectral lines were studied. The preferable experimental conditions were examined, and the influences of coexistent elements on the signals were investigated. The method was applied to the determination of elements in ferrum aluminum silicon alloy samples, and the measured results were in good agreement with the recommended. values of the standard steel. The detection limits of the method were 0.029 mug (.) mL(-1) for Al, 0.004 mug (.) mL(-1) for Fe, 0.0075 mug (.) mL(-1) for Ca, 0.0015 mug (.) mL(-1) for Cr, 0.0009 mug (.) mL(-1) for Mn, 0.002 7 mug (.) mL(-1) for Ni, 0.045 mug (.) mL(-1) for Si and 0.003 mug (.) mL(-1) for Ti. The relative standard deviation (n = 6) of this method was between 0.3%-1.8%, and the recoveries by standard addition were in the range of 96.7%-102.9%. The method was used to determine the amount of silicon in alloy samples with satisfactory results, which agreed with those by the standard gravimetry. The method is characterized by good precision, easy operation and convenience to apply.