材料期刊网

纯金属分析时为了消除基体效应的影响,通常需要先分离基体,再对其痕量元素进行测定,这不仅前处理过程较为复杂,还易造成样品污染.实验以硝酸(1+1)溶解样品,采用基体匹配法配制标准溶液系列以绘制校准曲线,最终实现了电感耦合等离子体质谱法(ICP-MS)对纯铟中镁、铬、锰、钴、镍、锆、钼、锑8种元素的测定.通过选择合适的同位素消除了质谱干扰;采用10 ng/mL钪对元素镁、铬、锰和镍进行校正,采用10 ng/mL铑对钴、钼、锑和锆进行校正,克服了基体效应和信号漂移的影响.实验表明,各元素的质量浓度在1.00~50.0 ng/mL范围内与其信号强度呈一定的线性关系,相关系数均大于0.999.方法的检出限为0.09~0.78 ng/mL.将实验方法应用于纯铟实际样品中镁、铬、锰、钴、镍、锆、钼、锑8种元素的测定,相对标准偏差(RSD,n=7)不大于10.2%,加标回收率为88%~114%.

Before the analysis of trace elements in pure metals, the matrix effect should be eliminated by matrix re-separation.While, the pretreatment process was complicated, and the sample was easily polluted.The sample was dissolved with nitric acid (1+1).The standard solution series were prepared by matrix matching method to plot the calibration curve.Finally, the content of eight elements including magnesium, chromium, manganese, cobalt, nickel, zirconium, molybdenum and antimony in pure indium was determined by inductively coupled plasma mass spectrometry (ICP-MS).The mass spectral interference was eliminated by selecting proper isotopes.The influence of matrix effect and signal drift was eliminated when magnesium, chromium, manganese and nickel were corrected with 10 ng/mL of scandium, cobalt, molybdenum, antimony and zirconium were corrected with 10 ng/mL rhodium.The experimental results indicated that the mass fraction of elements in range of 1.00-50.0 ng/mL were linear to their corresponding signal intensity, respectively.The linear correlation coefficients were higher than 0.999.The detection limits were between 0.09 ng/mL and 0.78 ng/mL.The proposed method was applied to the determination of magnesium, chromium, manganese, cobalt, nickel, zirconium, molybdenum and antimony in pure indium actual samples.The relative standard deviations (RSD, n=7) were not higher than 10.2%.The recoveries were between 88% and 114%.