A minimal sample preparation for the determination of Ni and V in crude oil samples by LA-ICP-MS

IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Microchemical Journal Pub Date : 2025-03-01 Epub Date: 2025-02-07 DOI:10.1016/j.microc.2025.112988
Eduarda Q. Machado , Danielle da S. Francischini , Rodrigo M. Galazzi , Cleverson J.F. de Oliveira , Marco A.Z. Arruda
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Abstract

This work demonstrates the feasibility of using minimalist strategies for crude oil analysis using filter paper as a solid support for performing the analytical curves to determine Ni and V in such samples by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) using aqueous standards with a minimal sample preparation. Aliquots (4 µL) of the standards and samples were added directly to the surface of the filter paper and dried at 37 °C. Three calibration curves in the range 0.5–30 mg kg−1 were evaluated using oil-based standards, aqueous standards and with or without 13C as an internal standard for both curves to normalize the Ni and V results. Better results were obtained with an aqueous curve without normalization. The accuracy of this method was checked against microwave system decomposition and determination by inductively coupled plasma mass spectrometry (ICP-MS). For analysis, were used 110 µm spot size, 110 µm s−1 scan speed and 60 % (6.99 J cm−2 of fluency) laser intensity for ablation conditions and 1.2 L min−1 nebulizer gas, 1.6 L min−1 auxiliary gas and 1200 W for ICP-MS conditions. All the results are in accordance with the microwave digestion method, and are in the range 80–120 %.

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LA-ICP-MS测定原油样品中镍和钒的最小样品制备
这项工作证明了使用极简策略进行原油分析的可行性,使用滤纸作为执行分析曲线的坚实支撑,通过激光烧蚀电感耦合等离子体质谱(LA-ICP-MS)使用最小样品制备的水标准来测定样品中的Ni和V。将等份(4µL)标准品和样品直接加入滤纸表面,37℃干燥。在0.5 - 30mg kg−1范围内的三条校准曲线分别使用油基标准品、水溶液标准品和用或不用13C作为两条曲线的内标品,对Ni和V的结果进行归一化。用不归一化的水溶液曲线得到较好的结果。通过微波系统分解和电感耦合等离子体质谱(ICP-MS)测定验证了该方法的准确性。为了进行分析,在烧蚀条件下使用110µm光斑尺寸,110µm s−1扫描速度和60% (6.99 J cm−2流畅度)激光强度,在ICP-MS条件下使用1.2 L min−1雾化器气体,1.6 L min−1辅助气体和1200 W。结果符合微波消解法,在80 ~ 120%范围内。
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来源期刊
Microchemical Journal
Microchemical Journal 化学-分析化学
CiteScore
8.70
自引率
8.30%
发文量
1131
审稿时长
1.9 months
期刊介绍: The Microchemical Journal is a peer reviewed journal devoted to all aspects and phases of analytical chemistry and chemical analysis. The Microchemical Journal publishes articles which are at the forefront of modern analytical chemistry and cover innovations in the techniques to the finest possible limits. This includes fundamental aspects, instrumentation, new developments, innovative and novel methods and applications including environmental and clinical field. Traditional classical analytical methods such as spectrophotometry and titrimetry as well as established instrumentation methods such as flame and graphite furnace atomic absorption spectrometry, gas chromatography, and modified glassy or carbon electrode electrochemical methods will be considered, provided they show significant improvements and novelty compared to the established methods.
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