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A fast and robust direct solid sampling method for the determination of 27 trace, main and minor elements in soda-lime glass based on ETV-ICP OES and using a gaseous halogenating modifier
Journal of Analytical Atomic Spectrometry ( IF 3.4 ) Pub Date : 2021-6-8 , DOI: 10.1039/d1ja00081k
C. Hommel 1, 2, 3 , J. Hassler 1, 3, 4 , R. Matschat 1, 3, 5, 6, 7 , T. Vogt 1, 3, 4 , A. K. Detcheva 8, 9, 10 , S. Recknagel 3, 5, 6, 7
Affiliation  

A method, based on electrothermal vaporization (ETV) coupled to inductively coupled plasma optical emission spectrometry (ICP OES), has been optimized for direct solid sampling analysis of soda-lime glass—the most common type of industrially manufactured glass. This method allows fast and reliable quantification of the main elements—Al, Ca, K, Mg, Na, and Si—and trace elements—As, Ba, Cd, Ce, Co, Cr, Cu, Fe, Mn, Mo, Ni, (P), Pb, Sb, (Se), Sn, Sr, Ti, V, Zn, and Zr. In the presented ETV-ICP OES method, calibration is performed predominantly with matrix-free synthetic samples. This metrological advantage is normally not achieved with direct solid sampling methods and is one of the goals of the present study. In a certification interlaboratory comparison for the soda-lime glass CRM BAM-S005c, 2 out of 16 laboratories employed the ETV-ICP OES method. An improved analytical performance was obtained compared with the results of laboratories that used conventional liquid ICP OES. For both methods, the average relative deviations between the laboratory results and certified values as well as the average values of relative standard deviation were with a few exceptions <10%, in most cases even <5%, which indicated high trueness and precision. The limits of quantification of the trace elements by ETV-ICP OES were mostly <3 mg kg−1. Low subsample masses of 0.2–0.6 mg were used to avoid matrix effects. The optimized conditions consist of using CHF3 as a modifier gas at a flow rate of 2.3 mL min−1, an ETV temperature program with a final temperature of 2530 °C, and use of graphite grit material in combination with a sample boat with a hemispherical cavity for the optimal release of the analytes.

中文翻译:

基于 ETV-ICP OES 并使用气态卤化改性剂测定钠钙玻璃中 27 种痕量元素、主要元素和微量元素的快速、稳健的直接固体采样方法

一种基于电热蒸发 (ETV) 与电感耦合等离子体发射光谱法 (ICP OES) 相结合的方法,已针对钠钙玻璃(最常见的工业制造玻璃类型)的直接固体采样分析进行了优化。该方法可以快速可靠地定量分析主要元素——Al、Ca、K、Mg、Na 和 Si——以及痕量元素——As、Ba、Cd、Ce、Co、Cr、Cu、Fe、Mn、Mo、Ni 、(P)、Pb、Sb、(Se)、Sn、Sr、Ti、V、Zn 和 Zr。在介绍的 ETV-ICP OES 方法中,主要使用无基质合成样品进行校准。这种计量优势通常无法通过直接固体采样方法实现,并且是本研究的目标之一。在钠钙玻璃 CRM BAM-S005c 的认证实验室间比较中,16 个实验室中有 2 个采用了 ETV-ICP OES 方法。与使用传统液体 ICP OES 的实验室的结果相比,获得了改进的分析性能。对于这两种方法,实验室结果与标准值的平均相对偏差以及相对标准偏差的平均值除少数例外<10%,大多数情况下甚至<5%,表明正确性和精密度较高。ETV-ICP OES 对痕量元素的定量限大多<3 mg kg 这表明高真实性和精确度。ETV-ICP OES 对痕量元素的定量限大多<3 mg kg 这表明高真实性和精确度。ETV-ICP OES 对痕量元素的定量限大多<3 mg kg-1。使用 0.2–0.6 mg 的低子样品质量来避免基质效应。优化条件包括使用 CHF 3作为改性剂气体,流速为 2.3 mL min -1,最终温度为 2530 °C 的 ETV 温度程序,以及使用石墨砂材料与带有半球形腔体,可实现分析物的最佳释放。
更新日期:2021-06-23
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