【引用本文】 王娜, 徐铁民, 魏双, 等. 微波消解-电感耦合等离子体质谱法测定超细粒度岩石和土壤样品中的稀土元素[J]. 岩矿测试, 2020, 39(1): 68-76. doi: 10.15898/j.cnki.11-2131/td.201904010043
WANG Na , XU Tie-min , WEI Shuang , et al. Determination of Rare Earth Elements in Ultra-fine Rock and Soil Samples by ICP-MS Using Microwave Digestion[J]. Rock and Mineral Analysis, 2020, 39(1): 68-76. doi: 10.15898/j.cnki.11-2131/td.201904010043

微波消解-电感耦合等离子体质谱法测定超细粒度岩石和土壤样品中的稀土元素

1. 中国地质调查局天津地质调查中心, 天津 300170;

2. 中国地质调查局泥质海岸带地质环境重点实验室, 天津 300170

收稿日期: 2019-04-01  修回日期: 2019-05-28 

基金项目: 中国地质调查局地质调查项目"地质调查标准化与标准制修订"(DD20190472)和"地质调查标准制修订与升级推广"(DD20160094)

作者简介: 王娜,硕士,工程师,主要从事岩石矿物分析研究。E-mail:hmilywna@163.com。。

Determination of Rare Earth Elements in Ultra-fine Rock and Soil Samples by ICP-MS Using Microwave Digestion

1. Tianjin Center of Geological Survey, China Geological Survey, Tianjin 300170, China;

2. Key Laboratory of Muddy Coast Geo-Environment, China Geological Survey, Tianjin 300170, China

Received Date: 2019-04-01
Revised Date: 2019-05-28

摘要:ICP-MS分析岩石和土壤样品中稀土元素的含量,取样量可低至数毫克级,但200目样品粒度要求分析取样100mg才能保证代表性,导致ICP-MS灵敏度高、取样量小的优势难以得到充分发挥。本文研究了研磨方式、研磨时间、物料比对超细粒度土壤和岩石样品制备的影响,结果表明采用乙醇作为分散剂进行湿法球磨,200粒度的土壤、岩石样品分别研磨10min和15min,土壤样品的物料比采用物料7g、研磨球500个、分散剂45mL,岩石样品的物料比选取物料5g、研磨球500个、分散剂45mL,细化程度最佳。在此条件下制备的超细粒度土壤标准物质GBW07404、GBW07447的粒径分布D95可低至7.51μm、7.05μm,超细粒度岩石标准物质GBW07104、GBW07121的D95可低至8.42μm、8.30μm。在硝酸-氢氟酸-过氧化氢酸溶体系中微波消解处理超细粒度岩石样品GBW07104,取样量减少至5mg,总用酸量减至0.25mL,消解时间降低为25min,稀土元素的测定值与认定值基本一致,相对标准偏差在1.64%~5.21%之间。该方法用于分析其他超细粒度标准物质(GBW07404、GBW07447和GBW07121)中的稀土元素,相对误差为0.17%~6.60%,满足《地质矿产实验室测试质量管理规范》的一级标准。

关键词: 岩石, 土壤, 稀土元素, 超细样品制备, 湿法球磨, 乙醇, 微波消解, 电感耦合等离子体质谱法

Determination of Rare Earth Elements in Ultra-fine Rock and Soil Samples by ICP-MS Using Microwave Digestion

KEY WORDS: rock, soil, rare earth elements, ultra-fine sample preparation, wet-milling, ethanol, microwave digestion, inductively coupled plasma-mass spectrometry

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微波消解-电感耦合等离子体质谱法测定超细粒度岩石和土壤样品中的稀土元素

王娜, 徐铁民, 魏双, 王家松, 曾江萍, 张楠