Analysis of deliquescent chloride salt by laser-induced breakdown spectroscopy with controlled uniform precipitation

IF 5.7 2区化学 Q1 CHEMISTRY, ANALYTICAL

Analytica Chimica Acta Pub Date : 2024-10-09 DOI:10.1016/j.aca.2024.343315

Lizhu Kang , Ji Chen , Zhijie Huang , Zhanjian Lin , Rui Zhang , Bing Lu , Xiangyou Li

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引用次数: 0

Abstract

Background

The electrolytic efficiency in magnesium (Mg) production by molten salt electrolysis is mainly affected by the chloride content, which is determined by the metal content in the cooled molten salt. Laser-induced breakdown spectroscopy (LIBS) is a potential element detection method in cooled molten salt element detection. However, the cooled molten chloride salt is easily deliquescent, which greatly affects the LIBS detection results.

Results

To solve the problem, a liquid-phase precipitation method based on the addition of a dispersant named as controlled uniform precipitation (CUP) method was proposed to pretreat the samples. Compared with the conventional powder compacting method and precipitation method, the CUP obtained the highest spectral stability and detection accuracy. The average relative standard deviation (ARSD) of Mg, Ca, and Na decreased from the 51.80%, 77.04%, and 44.01% to 6.77%, 6.27%, and 29.97%, the determination coefficient of the calibration curve (R²) increased from 0.044, 0.084, and -0.109 to 0.974, 0.954, and 0.802, and the average relative error (ARE) decreased from 58.49%, 52.46%, and 99.78% to 8.58%, 11.28%, and 29.38%, respectively, compared with the powder compacting method. Further investigation showed that the CUP method suppressed the sample deliquescence and the coffee ring effect, leading to the performance improvement of LIBS quantitative detection.

Significance

The CUP provided an effective method of detecting metal elements for deliquescent samples and showed applied potential for other precipitable elements detection.

Abstract Image

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用激光诱导击穿光谱法分析受控均匀沉淀的潮解氯化盐

背景熔盐电解法生产镁（Mg）的电解效率主要受氯化物含量的影响，而氯化物含量则由冷却熔盐中的金属含量决定。激光诱导击穿光谱（LIBS）是一种潜在的冷却熔盐元素检测方法。为了解决这个问题，我们提出了一种基于添加分散剂的液相沉淀方法，即受控均匀沉淀法（CUP）来预处理样品。与传统的粉末压制法和沉淀法相比，CUP 法获得了最高的光谱稳定性和检测准确度。Mg、Ca和Na的平均相对标准偏差（ARSD）从51.80%、77.04%和44.01%下降到6.77%、6.27%和29.97%，校正曲线的确定系数（R2）从0.与粉末压实法相比，平均相对误差（ARE）分别从 58.49%、52.46% 和 99.78%下降到 8.58%、11.28% 和 29.38%。进一步的研究表明，CUP 方法抑制了样品潮解和咖啡环效应，从而提高了 LIBS 定量检测的性能。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Analytica Chimica Acta 化学-分析化学

CiteScore

10.40

自引率

6.50%

发文量

1081

审稿时长

38 days

期刊介绍： Analytica Chimica Acta has an open access mirror journal Analytica Chimica Acta: X, sharing the same aims and scope, editorial team, submission system and rigorous peer review. Analytica Chimica Acta provides a forum for the rapid publication of original research, and critical, comprehensive reviews dealing with all aspects of fundamental and applied modern analytical chemistry. The journal welcomes the submission of research papers which report studies concerning the development of new and significant analytical methodologies. In determining the suitability of submitted articles for publication, particular scrutiny will be placed on the degree of novelty and impact of the research and the extent to which it adds to the existing body of knowledge in analytical chemistry.