Protocol for Quantitative Detection of Elemental Sulfur and Polysulfide Zero-Valent Sulfur Distribution in Natural Aquatic Samples
Protocol for Quantitative Detection of Elemental Sulfur and Polysulfide Zero-Valent Sulfur Distribution in Natural Aquatic Samples
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DOI：
10.1111/j.1751-908x.2009.00907.x
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发表时间：
2009-09-01
影响因子：
3.8
通讯作者：
Ferdelman, Timothy G.
中科院分区：
文献类型：
--
作者：
Kamyshny, Alexey, Jr.;Borkenstein, Clemens G.;Ferdelman, Timothy G.
已开发出一种基于 HPLC 的方案，用于测定零价硫 (ZVS) 形态，包括天然水生样品中的固体、胶体元素硫和单个无机多硫化物。该方案包括四个实验程序：（1）通过三氟甲磺酸甲酯快速单相衍生化测定多硫化物形态； (2)通过与氰化氢反应(氰解)测定多硫化物和胶体硫的总量； (3)氯化锌处理后氯仿萃取测定总零价硫； (4) 色谱法测定连多硫酸盐，无需样品前处理。通过在现场或船上采用适当的采样和保存技术，这种方法组合可以定量测定： (a) 单个多硫化物种类； (b)分散的胶体硫； (c)分散的固体元素硫； (d) 四硫酸盐、五硫酸盐和六硫酸盐。经过较小的修改，该方法可以扩展到包括其他连多硫酸盐。对 9 种合成参考样品（包括固体元素硫、胶体元素硫、无机多硫化物和连多硫酸盐）测试了 16 种不同的湿化学和液相色谱方法，以建立最佳方案。通过分析微生物产生的硫和来自瓦登海（德国）潮滩池的富含硫化物的海水的两个天然样品中的硫的零价硫含量，进一步评估了该方案。
A HPLC-based protocol has been developed for the determination of zero-valent sulfur (ZVS) speciation, including solid, colloidal elemental sulfur and individual inorganic polysulfides in natural aquatic samples. The protocol includes four experimental procedures: (1) determination of polysulfide speciation by rapid single-phase derivatisation with methyl trifluoromethanesulfonate; (2) determination of the sum of polysulfide and colloidal sulfur by reaction with hydrogen cyanide (cyanolysis); (3) determination of total zero-valent sulfur by treatment with zinc chloride followed by extraction with chloroform; and (4) chromatographic determination of polythionates without sample pre-treatment. With proper sampling and preservation techniques in the field or on board ship, this combination of methods allowed the quantitative determination of: (a) individual polysulfide species; (b) dispersed colloidal sulfur; (c) dispersed solid elemental sulfur; and (d) tetra-, penta- and hexathionates. With minor modification, the method could be expanded to include other polythionates. Sixteen various wet chemical and liquid chromatographic methods were tested on nine synthetic reference samples (including solid elemental sulfur, colloidal elemental sulfur, inorganic polysulfides and polythionates) to establish the optimal protocol. The protocol was further evaluated by analysing the zero-valent sulfur content in microbially-produced sulfur and in sulfur from two natural samples of sulfide-rich seawater from tidal flats pools of the Wadden Sea (Germany).