强热压处理结合液膜富集-电感耦合等离子体质谱法测定煤矸石中再利用铅含量  

Determination of reusable lead content in coal gangue by strong heat pressing combined with liquid membrane enrichment-inductively coupled plasma mass spectrometry

作　　者：张歌[1] 文玉成[1] 狄雅肖 庞博 王丽芳 刘菁钧[1] 李晓星[1] 刘亮 傅尧[1] ZHANG Ge;WEN Yucheng;DI Yaxiao;PANG Bo;WANG Lifang;LIU Jingjun;LI Xiaoxing;LIU Liang;FU Yao(Chinese Research Academy of Environmental Sciences Center of Cleaner Production and Circular Economy Research,Beijing 100012,China)

机构地区：[1]中国环境科学研究院清洁生产与循环经济研究中心,北京100012

出　　处：《分析试验室》2024年第11期1521-1528,共8页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(52174385)资助。

摘　　要：本研究利用强热压处理、液膜富集和电感耦合等离子体质谱(ICP-MS)技术测定煤矸石中可再利用铅含量。通过强热压处理,提高了铅的释放效率和样品的溶解性。采用HF∶HNO_(3)∶HClO_(4)混酸体系液膜富集处理下的ICP-MS方法测定煤矸石中再利用铅含量,采用^(208)Pb同位素并使用内标校正方法消除基体效应、物理效应和仪器漂移等干扰。通过分析4种代表性土壤标准样品和铅同位素标准物质进行方法准确性验证。在0.05~100 ng/mL浓度范围内,校准曲线的线性相关系数均大于0.9999,方法检出限均小于0.021 ng/mL。实际样品分析结果表明,本方法结果与原子吸收光谱法基本一致。本方法浓度对数偏差(△lg C)范围为0.30%~3.66%,相对标准偏差(RSDs)范围为0.11%~1.7%,加标回收率在98.6%~101.1%范围内。强热压处理结合液膜富集-ICP-MS技术可用于测定煤矸石中的铅含量,为煤矸石的再利用和环境保护提供了重要的参考依据。A method utilizing the strong heat pressing,liquid membrane enrichment and inductively coupled plasma mass spectrometry(ICP-MS) techniques was developed to determine the reusable lead content in coal gangue.The strong heat pressing technique was employed to enhance the release efficiency of lead and improve the solubility of the samples.The ICP-MS method,using a mixed acid system of HF∶HNO_(3)∶HClO_(4) for liquid membrane enrichment,was utilized to measure the reusable lead content in coal gangue.The ^(208)Pb isotope was used for analysis,and interference from matrix effects,physical effects,and instrumental drift was eliminated by employing an internal standard correction method.The accuracy of the method was validated by analyzing four representative soil standard samples and lead isotope standards.The calibration curves showed linear correlation coefficients greater than 0.9999 within the concentration range of 0.05-100 ng/mL,and the method detection limits were all below 0.021 ng/mL.The analysis of real samples demonstrated that the results were in good agreement with those obtained by atomic absorption spectroscopy.The concentration logarithmic deviation (△lg C) ranged from 0.30% to 3.66%,the relative standard deviations(RSDs) ranged from 0.11% to 1.7%,and the spiked recoveries ranged from 98.6% to 101.1%.The results of this study indicate that the combination of strong heat pressing,liquid membrane enrichment,and ICP-MS technique is an effective,rapid,and reliable method for determining the lead content in coal gangue.It provides an important reference for the reutilization of coal gangue and environmental protection.

关 键 词：电感耦合等离子体质谱(ICP-MS) 强热压处理 煤矸石 再利用 铅 

分 类 号：O657.39[理学—分析化学] X833[理学—化学]