电感耦合等离子体质谱法测定铁基非晶合金中痕量铝

Determination of trace aluminium in iron-based amorphous alloy by inductively coupled plasma mass spectrometry

采用盐硝混合酸（1＋1＋1）溶解样品,通过选择27 Al作为测定用同位素和设置中分辨率（R=4 000）消除质谱干扰,以标准加入法绘制校准曲线消除基体效应,避免了对样品基体进行分离的繁琐前处理过程,实现了电感耦合等离子体质谱法（ICP-MS）对铁基非晶合金中痕量铝的测定。实验表明,称取0.100 0g样品于石英三角瓶中,准确加入10.0 mL盐硝混合酸（1＋1＋1）,电热板上低温加热可将样品完全溶解;采用标准加入法建立校准曲线,相关系数为0.999 0,线性范围为0.000 1%～0.005 0%,方法的检出限为0.035μg/g。按照实验方法,对2个铁基非晶合金样品中痕量铝进行测定,测得结果的相对标准偏差（RSD,n=9）为6.1%～7.1%,回收率为96%～106%。将实验方法与电感耦合等离子体原子发射光谱法（ICP-AES）进行方法比对,两种方法对铁基非金合金实际样品中铝的测定结果基本一致。

The sample was dissolved with mixed hydrochloric acid and nitric acid（1＋1＋1）.The mass spectrometry interference was eliminated by selecting 27 Al as determination isotope and setting moderate resolution（R=4 000）.The calibration curve was prepared by standard addition method to avoid the matrix effect as well as complicated pretreatment process of matrix separation.Thus,the determiantion of trace aluminum in iron-based amorphous alloy was realized by inductively coupled plasma mass spectrometry（ICP-MS）.The results showed that 0.100 0g of sample could be fully dissolved in quartz triangular flask by low temperature heating on electric hot plate with 10.0mL of hydrochloric acid-nitric acid（1＋1＋1）as solvent.The calibration curve was established by standard addition method with correlation coefficient as 0.999 0and linear range of 0.000 1%-0.005 0%.The detection limit of method was 0.035μg/g.The experimental method was applied to the determination of trace aluminum in two iron-based amorphous alloy samples.The relative standard deviations（RSD,n=9）were between 6.1% and 7.1%,and the recoveries were between 96%and 106%.This proposed method was compared with inductively coupled plasma atomic emission spectrometry（ICP-AES）,and the determination results of trace aluminum in actual iron-based amorphous alloy sample were consisit.