阴离子树脂Bio-RadAG1-X8对黑色页岩中的Mo有很好的分离纯化效果。该方法可以有效去除Mo同位素分析过程中可能存在的同质异位素干扰(如Zr、Sr等),对其他金属元素的去除效果也比较理想。大部分基体元素如Fe、Ca、Na、Mn、Mg、Sr、Al、Cu、K等可以使用1mol/LHF+0.5mol/LHCl洗脱,随后使用4mol/LHCl洗脱Ti和Zr,最后使用3mol/LHNO3洗脱Mo。在用单元素标准溶液过柱的过程中发现,样品中的Mo主要在前5mL3mol/LHNO3的淋洗液中洗脱,先淋洗出的溶液富集Mo的重同位素,后淋洗出的溶液富集Mo的轻同位素。当上柱的样品量较大时(Mo≥50μg),"柱基体效应"可以忽略不计,该化学纯化法适用于样品-标样交叉法和双稀释剂法;当样品量较小时(Mo〈50μg),该化学分离方法只适用于双稀释剂法。
The anion exchange resin Bio-Rad AG1-X8 can be used to separate Mo from matrix elements in black shale and other geological samples.Most matrix elements,such as Fe,Ca,Na,Mn,Mg,Sr,Al,Cu and K,were eluted firstly by 1 mol/L HF+0.5 mol/L HCl;then Ti and Zr were eluted by 4 mol/L HCl;and Mo was eluted lastly by 3 mol/L HNO3.Sr,which leads Mo isotope fractionation when Mo isotopic composition is analyzed by MC-ICP-MS,can be separated completely from Mo.During the eluting,most Mo was eluted within the first 5 mL HNO3;the heavier Mo isotopes were collected first,then the lighter ones,so the eluant must be collected completely to avoid Mo isotope fractionation.When the amount of Mo in sample is large enough(≥50 μg),"column matrix effects" can be neglected and the Mo isotopic composition is unchanged after ion exchange separation,so the separation method is suitable for both sample-standard bracketing and double spiking techniques to calibrate the instrumental mass bias;nevertheless,due to "column matrix effects",this method is suitable for double spiking only when the amount of Mo is small(〈50 μg).