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A catalytic method, based on the iodine–azide reaction, of the determination of sulfide in whole human blood is described. The method involves generation of hydrogen sulfide in an evolution–absorption apparatus by addition of sulfuric acid and subsequent trapping of the generated hydrogen sulfide in sodium hydroxide solution. The catalytic method allows the determination of sulfide without any interference from other sulfur compounds present in blood. A linear calibration graph was obtained over the range 1 × 10–6–5 × 10–4 mol dm–3 sulfide and the proposed method is compared with an ion-selective electrode method.
To a stirred blood sample (3-10 ml) were added 5-10 ml 14.2M-H2SO4. A N2 stream (250 ml/min) was then passed through the mixture and the H2S produced over 15 min was absorbed in 2-5 ml of 0.5M-NaOH. A portion of the alkaline sulfide solution was diluted to 50 ml with H2O, after which a known amount of 1% NaN3 and sufficient 0.1M-HCl to obtain a pH of 6.5-6.8 were added. The solution was stirred and 10 ml 0.02M-I in 1M-KI were added. After 60 s, excess I was back-titrated with 5mM-sodium arsenite using starch as indicator. The amount of I consumed was directly proportional to the sulfide concentration. The calibration graph was linear from 1-500µM-sulfide and the detection limit was 4 µg/l. The RSD (n = 6) were <2%. Recoveries were >98%. The results agreed with those obtained using an ISE.
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