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Determination of Cu, Zn, As, Cd, In, Sn, Pb, and Bi in nickel-based superalloys after multi-matrix separation

机译:多基体分离后测定镍基高温合金中的铜,锌,砷,镉,铟,锡,铅和铋

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摘要

A procedure has been developed for the determination of critical elements such as Cu, Zn, As, Cd, In, Sn, Pb, and Bi present at trace/ultra-trace levels in different types of Ni-based superalloys. These elements were quantitatively separated from a multicomponent superalloy (nearly 10 major constituents) by a solvent extraction method using 1M KI + 2M H2SO4 medium, then extracted into MIBK (Methyl Isobutyl Ketone), and determined by Inductively Coupled Plasma Quadrupole Mass Spectrometry (ICP-QMS). Significant separation of all the major matrix elements (Al, Ti, V, Cr, Co, Nb, Mo, Hf, Ta, W, Ni, and Re) has been achieved. Recoveries of > 95% were achieved for the elements Cu, Zn, Cd, In, Sn, Pb, and Bi, and 85% for As. Good agreement was observed for these results with the certified values of British Chemical Standard (BCS 346) and with the values obtained from the direct analysis by Glow Discharge Quadrupole Mass Spectrometry (GD-QMS). Reproducibility of the procedure is 20% RSD and the accuracy is within +/- 25% for the elements at trace levels. The procedure provides detection limits of 0.7 mu g kg(-1) (Bi) and 0.07 mg kg(-1) (Zn).
机译:已经开发出一种用于确定不同类型的镍基高温合金中痕量/超痕量水平的关键元素(例如,铜,锌,砷,镉,铟,锡,铅和铋)的测定方法。通过使用1M KI + 2M H2SO4介质的溶剂萃取法将这些元素从多组分高温合金(将近10种主要成分)中进行定量分离,然后萃取到MIBK(甲基异丁基酮)中,并通过电感耦合等离子体四极质谱(ICP-MS)测定QMS)。已实现所有主要基质元素(Al,Ti,V,Cr,Co,Nb,Mo,Hf,Ta,W,Ni和Re)的显着分离。 Cu,Zn,Cd,In,Sn,Pb和Bi的回收率> 95%,而As的回收率> 85%。这些结果与英国化学标准(BCS 346)的认证值以及通过辉光放电四极杆质谱(GD-QMS)直接分析获得的值一致。该方法的重现性为RSD的20%,而痕量元素的准确度在+/- 25%之内。该程序提供了0.7μg kg(-1)(Bi)和0.07 mg kg(-1)(Zn)的检出限。

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