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通过流动注射分析和使用毛细管除雾管进行在线预富集同时测定纳摩尔量的二氧化硫和硫化氢。

Simultaneous determination of nanomole amounts of sulphur dioxide and hydrogen sulphide by flow injection analysis with on-line preconcentration by means of capillary denuder tubes.

作者信息

Achilli Marco, Gács Istvan

机构信息

CESI SpA, Via Reggio Emilia 39, 20090 Segrate, MI, Italy.

出版信息

Ann Chim. 2002 May-Jun;92(5-6):563-74.

Abstract

A simple and rapid method for trace determination of SO2 and H2S in gaseous samples by using a flow injection system with on line preconcentration on capillary denuder is described. The gaseous samples are led through a 0.4 M sulphamic acid solution, retaining nitrogen dioxide, ammonia and hydrogen chloride. The sulphur dioxide is collected from the carrier gas stream (250 cm3 min-1) as sulphuric acid in a capillary denuder tube coated with a thin layer of 0.01-0.03 M hydrogen peroxide solution of 0.05 mM sulphuric acid; hydrogen sulphide passes into a second tube coated with 0.075 mM sodium sulphide solution of 0.1 M aqueous sodium hydroxide. The films containing the sulphuric acid and the sodium sulphide, respectively, are eluted with the corresponding circulating absorbent streams and pass through the detectors. Sulphuric acid is detected by conductimetry and sulphide is determined spectrophotometrically at 230 nm. If nanoequivalent amounts of H2S are present in the sample containing a large concentration of SO2 (SO2/H2S concentration ratio > 20), the sulphur dioxide is filtered out of the sample gas stream by solid sodium hydrogen carbonate. A limit of detection of 3.5 micrograms m-3 is obtained.

摘要

描述了一种使用流动注射系统并在毛细管除雾器上进行在线预富集来痕量测定气态样品中二氧化硫和硫化氢的简单快速方法。气态样品通过0.4M氨基磺酸溶液,以保留二氧化氮、氨和氯化氢。二氧化硫作为硫酸从载气流(250cm³ min⁻¹)中收集在涂有0.01 - 0.03M过氧化氢溶液和0.05mM硫酸的毛细管除雾器管中;硫化氢进入涂有0.075mM硫化钠溶液和0.1M氢氧化钠水溶液的第二个管中。分别含有硫酸和硫化钠的膜用相应的循环吸收剂流洗脱并通过检测器。硫酸通过电导法检测,硫化物在23℃下用分光光度法测定。如果在含有高浓度二氧化硫(二氧化硫/硫化氢浓度比>20)的样品中存在纳摩尔量的硫化氢,则通过固体碳酸氢钠从样品气流中滤出二氧化硫。检测限为3.5微克 m⁻³。

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