五酸溶样-电感耦合等离子体质谱法同时测定地质样品中的稀土等28种金属元素

龚仓; 丁洋; 陆海川; 卜道露; 王立华; 熊韬; 张志翔

doi:10.15898/j.cnki.11-2131/td.202011030136

五酸溶样-电感耦合等离子体质谱法同时测定地质样品中的稀土等28种金属元素

Simultaneous Determination of 28 Elements including Rare Earth Elements by ICP-MS with Five-Acid Dissolution

摘要

摘要: 电感耦合等离子体质谱法（ICP-MS）测定大批量地质样品中的稀土和钴铪铟锰铌钽铊铬镉镓锗钒锡等金属元素，主要采用三酸或四酸溶解样品。由于地质样品组分复杂，稀土等金属元素含量低，各元素性质差异大，三酸或四酸溶样经常出现易挥发元素如钒铬镉镓锡的测定结果不稳定、镧铈镨钕等稀土元素溶解不完全的问题。本文在盐酸-硝酸-氢氟酸-高氯酸四酸基础上引入硫酸，形成盐酸-硝酸-氢氟酸-高氯酸-硫酸五酸溶样体系，用于水系沉积物、土壤和岩石等不同类型地质样品的一次敞口溶解，采用在线加入¹⁸⁵Re和¹⁰³Rh内标方式，建立了应用ICP-MS同时测定稀土等28种金属元素的方法。钒铬镉镓锡元素的准确度提高了1.4%~14.6%，镧和铈元素的准确度提高了0.2%~8.9%。该方法应用于分析水系沉积物、土壤、岩石标准物质（分别为GBW07301a、GBW07408、GBW07107），其测定值与认定值相一致，相对标准偏差（RSD）为1.14%~9.84%，准确度（△lgC）均≤0.1。该方法分析过程较简单，结果准确可靠，可满足测定大批量地质样品中稀土和钴铪铟锰铌钽等金属元素含量的要求。

Abstract:
BACKGROUNDThree acids and four acids dissolution methods are the two main dissolution methods for determination of rare earth, cobalt, hafnium, indium, manganese, niobium, tantalum, thallium, chromium, cadmium, gallium, germanium, vanadium and tin in geological samples by inductively coupled plasma-mass spectrometry (ICP-MS). However, the composition of geological samples is complex, the content of rare earth and other metal elements is low, and the properties of each element are different, which makes the measurement results of volatile elements such as vanadium, chromium, cadmium, gallium and tin unstable, and rare earth elements such as lanthanum, cerium, praseodymium and neodymium are not completely dissolved by three acids or four acids.
OBJECTIVESTo improve the four acids dissolution system for the determination of 28 elements including rare earth elements and rare metal elements.
METHODSThe method of HCl-HNO₃-HF-HClO₄-H₂SO₄ was developed by addition of H₂SO₄ in the dissolution system of HCl-HNO₃-HF-HClO₄. A new analysis method has been developed for the certified reference material of stream sediment, soil and rock, and 28 elements including rare earth elements in samples were determined simultaneously by ICP-MS with 10ng/mL ¹⁰³Rh and ¹⁸⁵Re as the internal standard by on-line injections.
RESULTSThe accuracy of volatile elements such as vanadium, chromium, cadmium, gallium and tin was improved by 1.4%-14.6%, and that of rare earth elements such as lanthanum and cerium was improved by 0.2%-8.9%. The certified reference materials of stream sediment (GBW07301a), soil (GBW07408) and rock (GBW07107) were analyzed to test the method. The determined values were in good agreement with the certified values. The standard deviations (RSD) of the method were 1.14%-9.84% and accuracy (△lgC) was not higher than 0.1.
CONCLUSIONSThis method is rapid, simple, and accurate and can meet the requirements for determining the content of rare earth, cobalt, hafnium, indium, manganese, niobium, tantalum and other metal elements in large quantities of geological samples.

HTML全文

参考文献(30)

施引文献

资源附件(0)