RationaleSulfur isotopes have been widely used to solve some key scientific questions, especially in the last two decades with advanced instruments and analytical schemes. Different sulfur speciation and multiple isotopes analyzed in laboratories worldwide and in situ microanalysis have also been reported in many articles. However, methods of sampling to measurements are multifarious, and occasionally some inaccuracies are present in published papers. Vague methods may mislead newcomers to the field, puzzle readers, or lead to incorrect data‐based correlations.MethodsWe have reviewed multiple methods on sulfur isotopic analyses from the perspectives of sampling, laboratory work, and instrumental analysis in order to help reduce operational inhomogeneity and ensure the fidelity of sulfur isotopic data. We do not deem our proposed solutions as the ultimate standard methods but as a lead‐in to the overall introduction and summary of the current methods used.ResultsIt has been shown that external contamination and transformation of different sulfur species should be avoided during the sampling, pretreatment, storage, and chemical treatment processes. Conversion rates and sulfur isotopic fractionations during sulfur extraction, purification, and conversion processes must be verified by researchers using standard or known samples. The unification of absence of isotopic fractionation is needed during all steps, and long‐term monitoring of standard samples is recommended.ConclusionThis review compiles more details on different methods in sampling, laboratory operation, and measurement of sulfur isotopes, which is beneficial for researchers' better practice in laboratories. Microanalyses and molecular studies are the frontier techniques that compare the bulk sample with the elemental analysis/continuous flow–gas source stable isotope ratio mass spectrometry method, but the latter is widely used. The development of sulfur isotopic measurements will lead to the innovation in scientific issues with sulfur proxies.

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从样品到硫同位素数据的程序：回顾

基本原理硫同位素已被广泛用于解决一些关键的科学问题，特别是在过去二十年中，凭借先进的仪器和分析方案。在世界各地的实验室中分析了不同的硫形态和多种同位素就地许多文章也报道了微量分析。然而，采样测量的方法多种多样，发表的论文中偶尔会出现一些不准确的情况。模糊的方法可能会误导该领域的新手、使读者困惑，或导致基于数据的错误相关性。方法我们从采样、实验室工作和仪器分析的角度回顾了硫同位素分析的多种方法，以帮助减少操作的不均匀性和确保硫同位素数据的保真度。我们并不认为我们提出的解决方案是最终的标准方法，而是作为对当前所用方法的整体介绍和总结的引导。结果表明，在采样过程中应避免外部污染和不同硫物质的转化，预处理、储存和化学处理过程。研究人员必须使用标准或已知样品来验证硫提取、纯化和转化过程中的转化率和硫同位素分馏。所有步骤均需要统一，不进行同位素分馏，建议对标准样品进行长期监测。结论本综述对硫同位素的取样、实验室操作和测量中的不同方法进行了更多详细介绍，有利于研究人员更好的实验室实践。微量分析和分子研究是将大体积样品与元素分析/连续流-气源稳定同位素比质谱法进行比较的前沿技术，但后者应用广泛。硫同位素测量的发展将导致硫代用科学问题的创新。