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元素活动态提取条件和分析方法的应用研究
投稿时间:2019-07-17  修订日期:2019-09-10  点此下载全文
引用本文:
DOI:10.19762/j.cnki.dizhixuebao.2020101
摘要点击次数: 354
全文下载次数: 111
作者单位E-mail
徐进力 中国地质科学院地球物理地球化学勘查研究所 80368070@qq.com 
邢夏 中国地质科学院地球物理地球化学勘查研究所  
张鹏鹏 中国地质科学院地球物理地球化学勘查研究所  
胡梦颖 中国地质科学院地球物理地球化学勘查研究所  
白金峰 中国地质科学院地球物理地球化学勘查研究所  
张勤 中国地质科学院地球物理地球化学勘查研究所  
王学求 中国地质科学院地球物理地球化学勘查研究所  
基金项目:中国地质调查局地质调查项目(DD20190518)资助项目.
中文摘要:元素活动态作为深穿透地球化学的新方法,得到了广泛的应用。实验对水提取态、粘土吸附态、有机结合态和铁锰氧化物结合态四种元素活动态的提取条件进行了系统研究,分别考察了提取时间、液固比,离心转速、提取液放置时间对提取效果的影响,确定了元素活动态的最佳提取条件:提取时间为24h,液固比为10:1,离心转速4000rpm;提取液采用新型的高分辨率等离子体质谱法(HR-ICP-MS)测定,该仪器具有强大优势的动态线性范围(10-12~1012)和高的灵敏度,使可同时测定的元素拓展至50余种,可以大大提高工作效率。对HR-ICP-MS的主要工作条件:辅助气流量、样品气流量和采样深度等利用响应面法进行了优化。本法将传统的过滤法改为离心法,避免了滤纸或穿滤引入的误差;将新型的高分辨率等离子体质谱法(HR-ICP-MS)法应用到提取液的测定,提升了多元素同时分析能力,大大提高工作效率,同时也降低了该方法的检出限,改善了测定结果的精密度。依据实验结果,建立了HR-ICP-MS对四种元素活动态的分析方法,分别得到了四种活动态中各元素的方法检出限和方法精密度,水提取态、粘土吸附态、有机结合态和铁锰氧化物结合态中各元素的精密度范围依次为3.4%~38.1%,3.78%~35.7%,2.41%~35.9%,2.26%~32.5%;通过顺序提取,将四个相态中提取到的元素量和残渣中残留进行加和,得到50个元素的加和结果,验证了该方法的准确度(RE)为-29% ~ -1.3%,满足当前元素活动态的分析测试需求。
中文关键词:元素活动态  水提取相  粘土吸附态  有机结合态  铁锰氧化物态  高分辨率电感耦合等离子体质谱
 
Application research on extraction conditions and analysis methods of active state elements
Author NameAffiliationE-mail
XU Jinli Institute of Geophysical and Geochemical ExplorationChinese Academy of Geological Sciences 80368070@qq.com 
XING Xia Institute of Geophysical and Geochemical ExplorationChinese Academy of Geological Sciences  
ZHANG Pengpeng Institute of Geophysical and Geochemical ExplorationChinese Academy of Geological Sciences  
HU Mengying Institute of Geophysical and Geochemical ExplorationChinese Academy of Geological Sciences  
BAI Jinfeng Institute of Geophysical and Geochemical ExplorationChinese Academy of Geological Sciences  
ZHANG Qin Institute of Geophysical and Geochemical ExplorationChinese Academy of Geological Sciences  
WANG Xueqiu Institute of Geophysical and Geochemical ExplorationChinese Academy of Geological Sciences  
Abstract:As a new method of deep-penetrating geochemistry, the analytical technique of active state element has been widely used in searching for concealed ore bodies. This study systematically investigated extract condition for four types of element active states, such as Water Extractable Metals (WEM), Clay Absorption Metals (CAM), Organically Bound Metals (OBM), Occluded Metals in Iron-manganese Oxides (MM). The experiments tested effects of extraction time, liquid-solid ratio, centrifugal rotating speed and extracting solution storage time on the extraction efficiency. The extraction conditions of four types of active state elements were improved and the optimum extraction conditions were determined: the extraction time was 24 h, the liquid-solid ratio was 10:1, and the centrifugal rotating speed was 4000 rpm. The liquid was extracted using new high resolution ICP-MS, which is equipped with excellent dynamic linear range (10-12~1012) and high sensitivity and can be used to analyze more than 50 elements. This study also optimized the HR-ICP-MS working condition, including auxiliary flow, Sample gas flow and sampling depth, etc. Finally, we established the HR-ICP-MS method for the analysis of the four types of active state elements and obtained the detection limits and precision of each element in four active states respectively. The precision ranges of elements in WEM, CAM, OBM and MM are 3.4%~38.1%, 3.78%~35.7%, 2.41%~35.9%, 2.26%~32.5%, respectively. By sequential extraction, we added the amount of elements extracted from four phase states and residues in the residue, and obtained the sum results of 50 elements. The accuracy (RE) of this method is -29% ~ -1.3%, which meets the current requirements of analysis and determination of active state elements.
keywords:Active State Elements  Water extractable Metals  Clay Absorption Metals  Organically Bound Metals  Occluded Metals in Iron-manganese Oxides  High Resolution Inductively Coupled Plasma Mass Spectrometry
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