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三维打印双模式化学蒸气发生点放电光发射光谱仪用于汞和无机硒的现场形态分析。

Three-Dimensional Printed Dual-Mode Chemical Vapor Generation Point Discharge Optical Emission Spectrometer for Field Speciation Analyses of Mercury and Inorganic Selenium.

机构信息

Key Laboratory of Green Chemistry and Technology of MOE, College of Chemistry, Sichuan University, Chengdu, Sichuan 610064, China.

West China School of Basic Medical Sciences and Forensic Medicine, Sichuan University, Chengdu, Sichuan 610064, China.

出版信息

Anal Chem. 2021 Nov 16;93(45):14923-14928. doi: 10.1021/acs.analchem.1c02023. Epub 2021 Nov 2.

DOI:10.1021/acs.analchem.1c02023
PMID:34726372
Abstract

Due to the large size and high energy consumption of instruments, field elemental speciation analysis is still challenging so far. In this work, a portable and compact system device (230 mm length × 38 mm width × 84 mm height) was fabricated by using three-dimensional (3D) printing technology for the field speciation analyses of mercury and inorganic selenium. The device comprises a cold vapor generator, photochemical vapor generator, and miniaturized point discharge optical emission spectrometer (μPD-OES). For mercury, inorganic mercury (IHg) was selectively reduced to Hg by cold vapor generation, whereas the reductions of both IHg and methylmercury (MeHg) were obtained by photochemical vapor generation (PVG) in the presence of formic acid. For selenium, Se(IV) and total inorganic selenium were converted to their volatile species by PVG in the presence and the absence of nano-TiO, respectively. The generated volatile species were consequently detected by μPD-OES. Limits of detection of MeHg, IHg, Se(IV), and Se(VI) were 0.1, 0.1, 5.2, and 3.5 μg L, respectively. Precision expressed as the relative standard deviations ( = 11) were better than 4.5%. The accuracy and practicality of the proposed method were evaluated by the analyses of Certified Reference Materials (DORM-4, DOLT-5, and GBW(E)080395) and several environmental water samples with satisfactory recoveries (95-103%). This work confirms that 3D printing has great potential to fabricate a simple, miniaturized, easy-to-operate, and low gas and power consuming atomic spectrometer for field elemental speciation analysis.

摘要

由于仪器体积大、能耗高,因此目前现场元素形态分析仍然具有挑战性。在这项工作中,采用三维(3D)打印技术制造了一种便携式紧凑型系统设备(230 毫米长×38 毫米宽×84 毫米高),用于汞和无机硒的现场形态分析。该设备包括冷蒸气发生器、光化学蒸气发生器和微型放电光学发射光谱仪(μPD-OES)。对于汞,通过冷蒸气发生将无机汞(IHg)选择性还原为 Hg,而在存在甲酸的情况下,通过光化学蒸气发生(PVG)可以同时还原 IHg 和甲基汞(MeHg)。对于硒,通过 PVG 在存在和不存在纳米 TiO 的情况下分别将 Se(IV)和总无机硒转化为其挥发性物质。生成的挥发性物质随后由 μPD-OES 检测。MeHg、IHg、Se(IV)和 Se(VI)的检出限分别为 0.1、0.1、5.2 和 3.5 μg L。相对标准偏差(n = 11)表示的精密度优于 4.5%。通过对认证参考材料(DORM-4、DOLT-5 和 GBW(E)080395)以及几个环境水样的分析,评估了该方法的准确性和实用性,回收率令人满意(95-103%)。这项工作证实,3D 打印在制造用于现场元素形态分析的简单、小型化、易于操作且耗气量和功耗低的原子光谱仪方面具有巨大潜力。

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