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引用本文:   朱万军, 翟晓颖, 黄人瑶, 冯拥军, 袁懋, 陈旭, 杨文胜. 三维花状硅酸镁富集-X-射线荧光光谱法测定水中痕量铅锌铜. 分析化学, 2018, 46(9): 1386-1392. doi:  10.11895/j.issn.0253-3820.181285 [复制]

Citation:   ZHU Wan-Jun, ZHAI Xiao-Ying, HUANG Ren-Yao, FENG Yong-Jun, YUAN Mao, CHEN Xu, YANG Wen-Sheng. Analysis of Trace Pb, Zn and Cu in Water Samples Based on Three-dimensional Flower-Shaped Magnesium Silicate as A Solid Sorbent and X-ray Fluorescence Spectrometry. Chinese Journal of Analytical Chemistry, 2018, 46(9): 1386-1392. doi: 10.11895/j.issn.0253-3820.181285 [复制]

三维花状硅酸镁富集-X-射线荧光光谱法测定水中痕量铅锌铜

通讯作者:  冯拥军, yifeng@mail.buct.edu.cn; 陈旭, chenxu@mail.buct.edu.cn

收稿日期: 2018-04-27

接受日期: 2018-07-05

出版日期: 2018-09-01

基金项目: 本文系国家自然科学基金项目(No.21521005)资助

Analysis of Trace Pb, Zn and Cu in Water Samples Based on Three-dimensional Flower-Shaped Magnesium Silicate as A Solid Sorbent and X-ray Fluorescence Spectrometry

Corresponding author:  FENG Yong-Jun, yifeng@mail.buct.edu.cn; CHEN Xu, chenxu@mail.buct.edu.cn

Received Date:  2018-04-27

Accepted Date:  2018-07-05

Published Date:  2018-09-01

Fund Project:  This work was supported by the National Natural Science Foundation of China (No. 21521005)

X-射线荧光光谱(XRF)分析技术在自动化程度、分析成本和对环境的影响等方面具有明显优势,已被应用于现场快速检测中。但其用于直接测定水体中金属元素时,检出限过高,不能满足检测要求。本研究采用一步混合溶剂热法合成了三维花状结构硅酸镁(Three-dimensional flower-shaped magnesium silicate,3DFMS)纳米材料,以此材料作为吸附剂,选择性富集水中的Pb2+、Zn2+和Cu2+,使用便携式能量色散X射线荧光光谱(EDXRF)仪直接分析测定。通过电子显微镜、氮气吸-脱附等对3DFMS的形貌和结构进行表征,并对富集-EDXRF检测中的实验条件进行了优化。优化后的条件为:吸附剂用量为100 mg,水样体积150 mL,pH=4,吸附时间为10 min。在优化条件下,测定Pb2+、Zn2+和Cu2+的线性范围为2.0~240 μg/L,检出限分别为0.57、0.69和0.76 μg/L。对各金属离子浓度为100 μg/L的试样连续测定5次,相对标准偏差为3.8%~5.0%,用于测定实际水样中金属离子的回收率为88.0%~118.0%。本研究建立的3DFMS富集-便携式EDXRF法快速简便,无有机试剂污染,成本低,适用于水体中痕量Pb2+、Zn2+和Cu2+的现场快速检测。

关键词:   三维花状硅酸镁, 固相萃取, X-射线荧光光谱法, 金属离子, 现场检测
Key words:   Three-dimensional flower-shaped magnesium silicate, Solid phase extraction, X-ray fluorescence spectrometry, Metal ions, Field test
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目录

三维花状硅酸镁富集-X-射线荧光光谱法测定水中痕量铅锌铜

朱万军, 翟晓颖, 黄人瑶, 冯拥军, 袁懋, 陈旭, 杨文胜

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