Yang X J, Pin C
Département de Géologie, UMR 6524 [Formula: see text] CNRS, Université Blaise Pascal, 5, rue Kessler, 63038, Clermont-Ferrand, France, and Department of Chemical Engineering, The University of New South Wales, Sydney 2052, Australia.
Anal Chem. 1999 May 1;71(9):1706-11. doi: 10.1021/ac980833w.
This paper presents a new chemical separation method for Hf and Zr from rocks using extraction chromatographic resins prepared from inert polymeric supports and the liquid anionic exchangers tri-n-octylamine or trioctylmethylammonium chloride (Aliquat 336). The method was developed using basaltic and trachyandesitic rocks with high contents of Al, Fe, and Ti. A 100-mg rock sample was decomposed with HF-HNO(3)-HClO(4) and fumed with HClO(4). The residue of this process was dissolved in 10 M HCl and then loaded on the column (6 mm i.d. × 75 mm). The major elements (Al, Ca, Mg, Ti, etc.) were eluted with 10 mL of 10 M HCl, and then Hf, Zr, and Fe were eluted sequentially using 20 mL of 8 M HCl, 20 mL of 2 M HCl, and 5 mL of 1 M HNO(3). The removal efficiency of major elements (Al, Fe, Ca, Mg) was greater than 99% and that of Ti was greater than 95%. The recoveries of Hf and Zr were better than 90% and the Zr/Hf ratio decreased from the natural ratio of 45 in the rock sample to 0.3 in the Hf fraction. This method provides an alternative to the less straightforward procedures based on several stages of ion-exchange separation and might be used for sample preparation prior to (176)Hf/(177)Hf determinations by magnetic sector multicollection ICPMS.
本文介绍了一种新的从岩石中分离铪和锆的化学方法，该方法使用由惰性聚合物载体和液态阴离子交换剂三正辛胺或氯化三辛基甲基铵（Aliquat 336）制备的萃取色谱树脂。该方法是针对铝、铁和钛含量高的玄武岩和粗安岩开发的。将100毫克岩石样品用氢氟酸 - 硝酸 - 高氯酸分解，并用高氯酸冒烟。该过程的残渣溶解在10 M盐酸中，然后加载到柱（内径6毫米×75毫米）上。用10毫升10 M盐酸洗脱主要元素（铝、钙、镁、钛等），然后依次用20毫升8 M盐酸、20毫升2 M盐酸和5毫升1 M硝酸洗脱铪、锆和铁。主要元素（铝、铁、钙、镁）的去除效率大于99%，钛的去除效率大于95%。铪和锆的回收率优于90%，锆/铪比值从岩石样品中的天然比值45降至铪馏分中的0.3。该方法为基于几个离子交换分离阶段的不太直接的程序提供了一种替代方法，可用于通过磁扇形多接收电感耦合等离子体质谱法进行（176）铪/（177）铪测定之前的样品制备。
