Article: Ion chromatographic determination of sulfide and cyanide in real matrices by using pulsed amperometric detection on a silver electrode.
2004 Volume 1023, Issue 1, Page(s) 105–112
Abstract: The determination of free sulfide and cyanide by pulsed amperometric detection (PAD) at a silver-working electrode was improved through a deep de-oxygenation (at least 10 min) of both standard and real solutions containing the two analytes and adopting a ...
| Abstract | The determination of free sulfide and cyanide by pulsed amperometric detection (PAD) at a silver-working electrode was improved through a deep de-oxygenation (at least 10 min) of both standard and real solutions containing the two analytes and adopting a two-potential waveform able to eliminate Ag working electrode fouling. The waveform stepped around the oxidation of Ag in the presence of 0.1-0.4 M hydroxyl ion, from -0.1 to 0.1 V versus saturated calomel electrode (SCE). The eluent composition (0.4 M NaOH plus 7.5 mM oxalate solution) allowed a very good column efficiency and selectivity. The presence of a polysulfide species was hypothesized in sulfide solutions that had not been de-oxygenated and aged. The polysulfide eluted just before sulfide and was confirmed by a chemical test with SO3(2-) producing the elimination of the polysulfide peak. Detection limits, according to the Hubaux-Vos method, were 1.0 and 2.0 microg/l for S2- and CN , respectively. We demonstrated good performance of the optimized method by repeatedly injecting standard solutions and by analyzing different real matrices. The method exhibited very good accuracy and repeatability (10 microg/l and a 500 microl injection loop, had a repeatability better than 3% for sulfide and 100 microg/l had a repeatability better than 1% for cyanide). The two-potential waveform ensured long-term stability of the electrode surface that required no manual polishing procedure for at least 1 month (20 analysis per day). |
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| MeSH term(s) | Chromatography, Liquid/methods ; Cyanides/analysis ; Electrochemistry/methods ; Electrodes ; Silver ; Sulfides/analysis |
| Chemical Substances | Cyanides ; Sulfides ; Silver (3M4G523W1G) |
| Language | English |
| Publishing date | 2004-01-09 |
| Publishing country | Netherlands |
| Document type | Journal Article ; Research Support, Non-U.S. Gov't |
| ZDB-ID | 1171488-8 |
| ISSN | 1873-3778 ; 0021-9673 |
| ISSN (online) | 1873-3778 |
| ISSN | 0021-9673 |
| DOI | 10.1016/j.chroma.2003.10.001 |
| Database | MEDical Literature Analysis and Retrieval System OnLINE |
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