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使用阀上实验室系统,通过固相萃取与能量色散X射线荧光检测相结合的方法自动测定古代纸张提取物中的汞和砷。

Automated determination of mercury and arsenic in extracts from ancient papers by integration of solid-phase extraction and energy dispersive X-ray fluorescence detection using a lab-on-valve system.

作者信息

Alcalde-Molina M, Ruiz-Jiménez J, Luque de Castro M D

机构信息

Department of Analytical Chemistry, Annex Marie Curie, Campus of Rabanales, University of Córdoba, E-14071, Córdoba, Spain.

出版信息

Anal Chim Acta. 2009 Oct 12;652(1-2):148-53. doi: 10.1016/j.aca.2009.05.034. Epub 2009 May 27.

Abstract

A method to detect the presence and determine the concentration of mercury and arsenic in extracts of ancient papers, based on an approach which allows integration of solid-phase concentration of the target analytes and their detection, is proposed. Automation of the overall process (viz. swelling and conditioning of the sorbent, sample introduction for analytes retention, drying of the sorbent by air for proper measurement, elution and conditioning of the sorbent prior to introduction of the next sample) is achieved by on-line connection of a lab-on-valve system to a laboratory-made methacrylate cell for concentration-measurement. After optimization of the variables influencing the method, characterization of the method provided LODs and LOQs of 0.006 and 0.02microgg(-1) of paper, respectively, for Hg; and 0.007 and 0.027microgg(-1), respectively, for As, with repeatability of 6.37% for Hg and 5.62% for As, and reproducibility of 8.13% and 7.46% for Hg and As, respectively.

摘要

本文提出了一种检测古代纸张提取物中汞和砷的存在并测定其浓度的方法,该方法基于一种能够将目标分析物的固相富集及其检测相结合的方法。通过将阀上实验室系统在线连接到实验室自制的用于浓度测量的甲基丙烯酸酯池,实现了整个过程的自动化(即吸附剂的溶胀和预处理、引入样品以保留分析物、通过空气干燥吸附剂以进行准确测量、在下一个样品引入之前对吸附剂进行洗脱和预处理)。在对影响该方法的变量进行优化后,该方法的表征结果表明,对于汞,纸张的检测限和定量限分别为0.006和0.02μg g⁻¹;对于砷,分别为0.007和0.027μg g⁻¹,汞的重复性为6.37%,砷的重复性为5.62%,汞和砷的重现性分别为8.13%和7.46%。

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