Sulfide and sulfate determination in water samples by means of hydrogen sulfide generation-inductively coupled plasma-atomic emission spectrometry (original) (raw)
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Analytica Chimica Acta, 2008
Inductively coupled plasma-atomic emission spectroscopy Vapor generator Water analysis a b s t r a c t Two new, simple and accurate methods for the determination of sulfide (S 2− ) at low levels (g L −1 ) in aqueous samples were developed. The generation of hydrogen sulfide (H 2 S) took place in a coil where sulfide reacted with hydrochloric acid. The resulting H 2 S was then introduced as a vapor into an inductively coupled plasma-atomic emission spectrometer (ICP-AES) and sulfur emission intensity was measured at 180.669 nm. In comparison to when aqueous sulfide was introduced, the introduction of sulfur as H 2 S enhanced the sulfur signal emission. By setting a gas separator at the end of the reaction coil, reduced sulfur species in the form of H 2 S were removed from the water matrix, thus, interferences could be avoided.
Kinetic Spectrophotometric Determination of Trace Amounts of Sulfide
A method for the determination of trace amount of sulfide based on the addition reaction of sulfide with methyl green at pH 7.5 and 25 o C is described. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of the dyestuff at 637 nm by the initial rate and fixed time method. The calibration graph is linear in the range 30-1200 ppb. The theoretical limit of detection was 0.014 ppm. Seven replicate analysis of a sample solution containing 0.70 ppm sulfide gave a relative standard deviation of 1.5%. The interfering effects of various ions on sulfide determination have been reported and procedures for removal of interference have been described. The proposed method was applied successfully to the determination of sulfide in tap and wastewater samples.
Determination of sulfide in waters by flow-injection solid phase spectrophotometry
The Analyst, 2000
A highly sensitive flow injection solid-phase spectrophotometric method was developed for the determination of sulfide in waters. The method is based on the formation of Methylene Blue (MB) by reaction between sulfide and N,N-dimethyl-p-phenylenediamine chloride in presence of Fe(III) in acidic medium. The MB formed was adsorbed on C 18 bonded silica, located inside a laboratory-made flow cell, which was placed in the optical path of the spectrophotometer. Analyte retention and detection at 666 nm were performed simultaneously, followed by elution with a mixture of methanol and hydrochloric acid. Several variables of the system, such as amine concentration, acidity of the reaction medium, reactor coil volume, sample volume and flow rate of the cleaning solution, were studied in order to achieve the best performance in the analysis of natural samples. This procedure provides an alternative for the determination of sulfide in the range 5-50 g L 21 with a relative standard deviation of 4.0% for 10 independent determinations at a concentration level of 50 g L 21 . A detection limit of 1.7 g L 21 , for a confidence level of 99.7%, was found. The system presented an analytical throughput of 12 h 21 .
Kinetic spectrophotometric determination of traces of sulfide
Talanta, 1997
A method for the determination of trace amount of sulfide based on the addition reaction of sulfide with methyl green at pH 7.5 and 25 o C is described. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of the dyestuff at 637 nm by the initial rate and fixed time method. The calibration graph is linear in the range 30-1200 ppb. The theoretical limit of detection was 0.014 ppm. Seven replicate analysis of a sample solution containing 0.70 ppm sulfide gave a relative standard deviation of 1.5%. The interfering effects of various ions on sulfide determination have been reported and procedures for removal of interference have been described. The proposed method was applied successfully to the determination of sulfide in tap and wastewater samples.
Analytica Chimica Acta, 2000
Dissolved sulfide ions are separated and detected by using ion chromatography (IC) and electrochemical detection with a glassy carbon electrode modified by electrochemical deposition of palladium particles. The influence of various experimental factors such as pH, loading of palladium, applied potential and flow rate of mobile phase is evaluated. The effect of some common organic and inorganic compounds on the amperometric signal is also evaluated. Under optimal chromatographic conditions, the detection limit for sulfide (S/N = 3) was 0.3 M (15 pmol injected) and the calibration plot was linear for 0.5-350 M sulfide (r = 0.9964, n = 16). The separation and detection of sulfides in human blood serum is presented as an example of an application to real specimens.
Novel methods to determine sulfide in aqueous samples by quantification of lead sulfide spots
Journal of Sulfur Chemistry, 2011
Two new, simple, accurate, and economical methods to find out sulfide (S2−) at low levels (10−9 g) in aqueous samples have been proposed. The first method involved the generation of hydrogen sulfide (H2S) in a specially designed small cell by interacting sulfide solution with hydrochloric acid. The resulting H2S is passed through a filter paper pre-dipped in lead acetate solution that made dark brown lead sulfide spots on the paper. In the second method, micro-liter drops of sulfide solution are applied on silica gel TLC pre-moistened with the lead acetate solution that developed lead sulfide spots. The color densities of the spots were calculated by scanning the spotted paper and TLC and analyzing the image using a specially developed software. The TLC method was more effective at trace levels having a linear response in the range 5–100 ng in comparison to 100–900 ng of the H2S method. Statistical examination of the calibration line validated the pertinence of these methods for the analysis of reduced form of sulfur in aqueous samples, particularly when dealing with small sample volumes.
2017
Sulfides and sulfur oxyanions, including thiosulfate, sulfate, and polythionates, can impact environmental quality and have negative economic consequences for industrial processes. For example, anaerobic reduction can produce toxic corrosive hydrogen sulfide, and oxidation can lead to environmental acidification accompanied with mobilization of toxic metals. Understanding the chemistry of various systems so that the reductive or oxidative processes can be curtailed requires methods to quantify key sulfur species. Accurate quantitation requires baseline separation and accommodation for co-migrating interferents, such as thiosulfate which co-migrates with chloride, found in abundance in briny waters. A strategy was developed using two capillary zone electrophoresis (CZE) methods, one with direct detection and the other with indirect detection, for speciation analysis of charged sulfur species (sulfate (SO42-), thiosulfate (S2O32-), tetrathionate (S4O62-), sulfite (SO32-), and sulfide ...