“…However, our results for standards prepared from Na2S are more in agreement with Axelrod et al 6 who stated a decay rate of 3 percent in 6 hours for diluted working Na2S standards. As noted by Karush et al, 4 extremely clean glassware is necessary for optimum performance of the method.…”
Section: Stability Of Reagentssupporting
confidence: 93%
“…li5 ' 6 Additional reports describing the reactions of reduced sulfur species in aqueous solutions with either oxygen 12 or cyanide 13 also implied that these bisulfide solutions would be unstable with respect to long term storage.…”
Section: Standardizationmentioning
confidence: 99%
“…Quantification is achieved by the selective quenching effects of sulfide [S"~2] (or more correctly bisulfide [HS~] since pK2 = 19 ± 2 for H2S( aq ) 3 ) on the fluorescence of fluorescein mercuric acetate (FMA). This fluorimetric procedure was initially described by Karush et al, 4 Grunert et al, 5 and Axelrod et al 6 The work described in this paper was performed as a portion of a more comprehensive evaluation of potential analytical techniques to measure natural emissions of volatile sulfur compounds. 7 The major objectives for the specific evaluation of the AgNCVfilter/FMA fluorimetric method were to: a) compare the responses of liquid sodium sulfide standards, which are normally used to calibrate the method, with gaseous H2S standards, which better simulate actual analyte and sample matrix components; b) clarify previous conflicting reports 1 ' 2 ' 8 concerning potential positive interferences from CH3SCH3 and CH3SH; c) assess the sources and magnitudes for both indeterminate and systematic errors in the sampling and fluorimetric procedures; and d) suggest modifications to the basic method and/or operational procedures that improve both analytical ruggedness and data quality.…”
This sensitive, albeit precarious, method for measuring ppb-ppt (V/V) concentrations of H 2 S was examined for various sources of potential error within the procedure. Filter preparation, filter storage, filter extraction, fluorimetric reagent stabilities, matrix differences between standards and samples, and possible interferences from other sulfur-containing compounds were separately studied for their effects on the analytical performance of the method. The overall method showed no Interference from SO 2 , CS 2 , COS, CH 3 SH, CH3SCH3, and SO 4~2 . To minimize bias and obtain a reliable estimate of precision, the method should be calibrated with H 2 S standards rather than liquid bisulfide standards. The measurement precision is a function of the quantity of H 2 S collected as Ag 2 S and/or AgSH on the impregnated filters. Because of the method's linear dynamic range, sufficient air should be sampled to achieve filter loadings of 15 to 35 ng S/filter. A quality control method based on fluoresceln mercuric acetate (FMA) is presented that ensures data quality while reducing the otherwise frequent need for fluorimetric calibration.A sensitive method for measuring low and sub-parts-perbillion (ppb V/V) concentrations of atmospheric hydrogen sulfide has been described by Natusch et al. 1 and modified by Jaeschke et al. 2 for automated field sampling. The method employs the collection of H2S on a AgNCVimpregnated filter. The filter is then leached with a basic cyanide solution to liberate the sulfide collected as Ag2S and/or AgSH on the filter. Quantification is achieved by the selective quenching effects of sulfide [S"~2] (or more correctly bisulfide [HS~] since pK2 = 19 ± 2 for H2S( aq ) 3 ) on the fluorescence of fluorescein mercuric acetate (FMA). This fluorimetric procedure was initially described by Karush et al.,4 Grunert et al., 5 and Axelrod et al.
6The work described in this paper was performed as a portion of a more comprehensive evaluation of potential analytical techniques to measure natural emissions of volatile sulfur compounds. 7 The major objectives for the specific evaluation of the AgNCVfilter/FMA fluorimetric method were to: a) compare the responses of liquid sodium sulfide standards, which are normally used to calibrate the method, with gaseous H2S standards, which better simulate actual analyte and sample matrix components; b) clarify previous conflicting reports 1 ' 2 ' 8 concerning potential positive interferences from CH3SCH3 and CH3SH; c) assess the sources and magnitudes for both indeterminate and systematic errors in the sampling and fluorimetric procedures; and d) suggest modifications to the basic method and/or operational procedures that improve both analytical ruggedness and data quality.
Experimental Methods
ApparatusAn Aminco-Bowman spectrophotofluorometer with an analog readout was used for the fluorimetric determinations. The excitation and emission wavelengths were 499 nm and 520 nm, respectively. Conventional fused silica cuvettes were used for the fluorimetric measurements. A...
“…However, our results for standards prepared from Na2S are more in agreement with Axelrod et al 6 who stated a decay rate of 3 percent in 6 hours for diluted working Na2S standards. As noted by Karush et al, 4 extremely clean glassware is necessary for optimum performance of the method.…”
Section: Stability Of Reagentssupporting
confidence: 93%
“…li5 ' 6 Additional reports describing the reactions of reduced sulfur species in aqueous solutions with either oxygen 12 or cyanide 13 also implied that these bisulfide solutions would be unstable with respect to long term storage.…”
Section: Standardizationmentioning
confidence: 99%
“…Quantification is achieved by the selective quenching effects of sulfide [S"~2] (or more correctly bisulfide [HS~] since pK2 = 19 ± 2 for H2S( aq ) 3 ) on the fluorescence of fluorescein mercuric acetate (FMA). This fluorimetric procedure was initially described by Karush et al, 4 Grunert et al, 5 and Axelrod et al 6 The work described in this paper was performed as a portion of a more comprehensive evaluation of potential analytical techniques to measure natural emissions of volatile sulfur compounds. 7 The major objectives for the specific evaluation of the AgNCVfilter/FMA fluorimetric method were to: a) compare the responses of liquid sodium sulfide standards, which are normally used to calibrate the method, with gaseous H2S standards, which better simulate actual analyte and sample matrix components; b) clarify previous conflicting reports 1 ' 2 ' 8 concerning potential positive interferences from CH3SCH3 and CH3SH; c) assess the sources and magnitudes for both indeterminate and systematic errors in the sampling and fluorimetric procedures; and d) suggest modifications to the basic method and/or operational procedures that improve both analytical ruggedness and data quality.…”
This sensitive, albeit precarious, method for measuring ppb-ppt (V/V) concentrations of H 2 S was examined for various sources of potential error within the procedure. Filter preparation, filter storage, filter extraction, fluorimetric reagent stabilities, matrix differences between standards and samples, and possible interferences from other sulfur-containing compounds were separately studied for their effects on the analytical performance of the method. The overall method showed no Interference from SO 2 , CS 2 , COS, CH 3 SH, CH3SCH3, and SO 4~2 . To minimize bias and obtain a reliable estimate of precision, the method should be calibrated with H 2 S standards rather than liquid bisulfide standards. The measurement precision is a function of the quantity of H 2 S collected as Ag 2 S and/or AgSH on the impregnated filters. Because of the method's linear dynamic range, sufficient air should be sampled to achieve filter loadings of 15 to 35 ng S/filter. A quality control method based on fluoresceln mercuric acetate (FMA) is presented that ensures data quality while reducing the otherwise frequent need for fluorimetric calibration.A sensitive method for measuring low and sub-parts-perbillion (ppb V/V) concentrations of atmospheric hydrogen sulfide has been described by Natusch et al. 1 and modified by Jaeschke et al. 2 for automated field sampling. The method employs the collection of H2S on a AgNCVimpregnated filter. The filter is then leached with a basic cyanide solution to liberate the sulfide collected as Ag2S and/or AgSH on the filter. Quantification is achieved by the selective quenching effects of sulfide [S"~2] (or more correctly bisulfide [HS~] since pK2 = 19 ± 2 for H2S( aq ) 3 ) on the fluorescence of fluorescein mercuric acetate (FMA). This fluorimetric procedure was initially described by Karush et al.,4 Grunert et al., 5 and Axelrod et al.
6The work described in this paper was performed as a portion of a more comprehensive evaluation of potential analytical techniques to measure natural emissions of volatile sulfur compounds. 7 The major objectives for the specific evaluation of the AgNCVfilter/FMA fluorimetric method were to: a) compare the responses of liquid sodium sulfide standards, which are normally used to calibrate the method, with gaseous H2S standards, which better simulate actual analyte and sample matrix components; b) clarify previous conflicting reports 1 ' 2 ' 8 concerning potential positive interferences from CH3SCH3 and CH3SH; c) assess the sources and magnitudes for both indeterminate and systematic errors in the sampling and fluorimetric procedures; and d) suggest modifications to the basic method and/or operational procedures that improve both analytical ruggedness and data quality.
Experimental Methods
ApparatusAn Aminco-Bowman spectrophotofluorometer with an analog readout was used for the fluorimetric determinations. The excitation and emission wavelengths were 499 nm and 520 nm, respectively. Conventional fused silica cuvettes were used for the fluorimetric measurements. A...
“…Filters were analyzed following procedures similar to those given by Natusch et al ( ), Axelrod et al (1969, and Jaeschke and Herrman (1981). Each filter was leached with an alkaline cyanide solution, and an aliquot of the resulting mixture was combined with fluorescein mercuric acetate (FMA).…”
Abstract. Emission rates of reduced sulfur gases from vegetation and soils were measured in various regions of the United States during the summer of 1985. The predominant sulfur gases emitted were hydrogen sulfide, carbonyl sulfide and dimethylsulfide. Typically, vegetative (forests, crops, etc.) emission fluxes varied between approximately 10 and 60 ng S m -2 min -1 . Biogenic sulfur fluxes from mollisol and histisol soils averaged 15 and 217 ng S m -x min -I , respectively. Salt water marsh fluxes with a geometric mean of 293 ng S m -2 min -1 were the highest measured. These biogenic sulfur fluxes are somewhat lower than those measured during the SURE study at some of the same sites. The natural sulfur emission fluxes reported herein together with those data included in the two accompanying manuscripts provide the basis for developing a national inventory of reduced sulfur emissions from soils, crops and trees. When combined these data also will provide a foundation for deriving uncertainty limits associated with these flux estimates.
“…An optical waveguide acid±vapour sensor has been shown to detect hydrogen sulphide although it is not speci®c for this gas and this is a serious drawback [12]. Fluorescence quenching has been demonstrated as a possible method for hydrogen sulphide sensing using thionine ®lms [13] and ®bre optic devices based on¯uorescein mercuric sulphate [14]. This latter method involves conversion of hydrogen sulphide gas to the hydrosulphide ion prior to reaction with the dye.…”
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