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[J]. Chinese Journal of Analytical Chemistry, ;2018, 46(9): 1386-1392. doi: 10.11895/j.issn.0253-3820.181285 shu

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

1.
State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China;
2.
China National Environmental Monitoring Centre, Beijing 100012, China

Received Date: 27 April 2018
Revised Date: 5 July 2018

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

X-ray fluorescence (XRF) spectrometry has been widely used for elemental analysis of a wide variety of samples due to its important features such as acceptable speed, economy and nondestructive for samples. Portable energy dispersive X-ray fluorescence spectrometry (EDXRF) is a key technology for on-site determination. However, the poor detection limits make the conventional XRF direct analysis unsatisfactory for liquid samples. Therefore, a proper pre-concentration procedure is needed to decrease the detection limit. In this study, we prepared a kind of three-dimensional flower-shaped magnesium silicate (3DFMS). Due to the high surface area, large pore size and hierarchical nanostructures, 3DFMS was employed as a solid sorbent for selective pre-concentration of Pb²⁺, Zn²⁺ and Cu²⁺. And then portable EDXRF was applied to directly quantify. The structure and morphology of 3DFMS were characterized by X-ray diffraction, scanning and transmission electron microscopes. The related adsorption and detect conditions have been optimized. Under the optimal conditions (100 mg of adsorbent dose, 150 mL of water, pH 4 and 10 min of sorption time), the detection limits (S/N=3) for Pb²⁺, Zn²⁺ and Cu²⁺ were 0.57, 0.69 and 0.76 μg/L, respectively. The linear range was 2.0-240 μg/L for three elements. Furthermore, the recovery of metal ions in the actual water sample was 88.0%-118.0%. The relative standard deviations for five successive measurements were 3.8%-5.0% for 100 μg/L metal ions. The actual water sample was also determined by the proposed method. This present method is rapid, simple, free of organic reagent pollution and low in cost, which is suitable for the rapid determination of trace lead, zinc and copper ions in water.
- Three-dimensional flower-shaped magnesium silicate,
- Solid phase extraction,
- X-ray fluorescence spectrometry,
- Metal ions,
- Field test
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沈阳化工大学材料科学与工程学院沈阳 110142