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Assessment of the equivalence and correlation between total sulfur determination methods in biodiesel: An use of isotope dilution inductively coupled plasma mass spectrometry

机译：生物柴油中总硫测定方法之间的当量和相关性评估：同位素稀释电感耦合等离子体质谱法的应用

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摘要

This paper describes an evaluation of current test methods for total sulfur determination in biodiesel, according to international specifications requirements, which was carried out using isotope dilution and inductively coupled plasma mass spectrometry (ID-ICP-MS) as a metrological tool. Closed vessel microwave-assisted digestion was employed using nitric acid and hydrogen peroxide as the decomposition medium, followed by isotope spike with S-34 dissolved in n-propanol. In order to overcome the spectral interference due to the presence of diatomic oxygen molecules in the ion beam, a reaction cell was used. Under optimized operating conditions, the determination of sulfur could be carried out at m/z + 16, i.e., monitoring SO+ signal for both sulfur isotopes. The ID-ICP-MS method was able to provide reference values for a series of commercial samples, which resulted in the evaluation of an extended concentration range. Sample sets including commercial biodiesel and inorganic sulfur-enriched biodiesel were employed as a means to evaluate the accuracy of routine methods for possible different sulfur species. No statistically significant difference was observed among the values measured with the proposed method and with the standard methods by UV fluorescence spectrometry and inductively coupled plasma optical emission spectrometry. (C) 2017 Elsevier Ltd. All rights reserved.
机译：本文描述了根据国际规格要求对生物柴油中总硫含量测定的当前测试方法的评估，该评估方法是使用同位素稀释和电感耦合等离子体质谱法（ID-ICP-MS）作为计量工具进行的。使用硝酸和过氧化氢作为分解介质的密闭容器微波辅助消解，然后使用溶解在正丙醇中的S-34进行同位素加标。为了克服由于离子束中双原子氧分子的存在而引起的光谱干扰，使用了反应池。在优化的操作条件下，硫的测定可以在m / z + 16下进行，即监视两种硫同位素的SO +信号。 ID-ICP-MS方法能够为一系列商业样品提供参考值，从而可以评估更大的浓度范围。包括商业生物柴油和富含无机硫的生物柴油在内的样品组被用作评估可能的不同硫物种常规方法准确性的方法。在通过提议的方法和通过紫外线荧光光谱法和感应耦合等离子体光发射光谱法的标准方法测量的值之间没有观察到统计学上的显着差异。 （C）2017 Elsevier Ltd.保留所有权利。

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