• Analytical Science and Technology
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• v.18 no.1
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• pp.66-73
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• 2005

In this study, we investigated the gas chromatography (GC) and pulsed flame photometric detection (PFPD) system for the analysis of four major reduced S compounds including hydrogen sulfide ($H_2S$); methyl mercaptan ($CH_3SH$); dimethyl sulfide (DMS); and dimethyl disulfide (DMDS) contained in environmental samples. To analyze these compounds in high concentration range (above ppb level), we developed a high mode analytical setting with the loop-injection system. By contrast, we also established a low mode setting for the analysis of low concentration samples (ppt-level samples from ambient air) by the combination with thermal desorption unit (TDU). Comparative analysis of both settings revealed that relative detection properties of four S compounds are systematic enough. The results of high mode analysis indicated that the patterns were systematic among S compounds: $H_2S$ exhibited the lowest sensitivity, while DMDS showed the strongest one. The results were also compared in terms of sensitivity reductions for all compounds by dividing slope ratios between low and high mode system. Although low mode system exhibited significant reductions on the order of a few tens times, their detection characteristics were highly consistent as it was shown in the high mode setting. To learn more about absolute and relative relations between two different modes of S analysis, future studies may have to be directed to cover more complicated nature of GC/PFPD performance.

• Proceedings of the Korean Environmental Health Society Conference
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• 2005.06a
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• pp.399-405
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• 2005

In this study, we investigated the gas chromatography (GC) and pulsed flame photometric detection (PFPD) system for the analysis of four major reduced S compounds including hydrogen sulfide ($H_2S)$; methyl mercaptan ($CH_3SH$); dimethyl sulfide (DMS); and dimethyl disulfide(DMDS) contained in environmental samples. To analyze these compounds in high concentration range (above ppb level), we developed a high mode analytical setting with the loop-injection system. By contrast, we also established a low mode setting for the analysis of low concentration samples (ppt-level samples from ambient air) by the combination with thermal desorption unit(TDU). Comparative analysis of both settings revealed that relative detection properties of four S compounds are systematic enough. The results of high mode analysis indicated that the patterns were systematic among compounds: H2S exhibited the lowest sensitivity, while DMBS showed the strongest one. The results were also compared in terms of sensitivity reductions for all compounds by dividing slope ratios between low and high mode system. Although low mode system exhibited significant reductions on the order of a few tens times, their detection characteristics were highly consistent as it was shown in the high mode setting. To learn more about absolute and relative relations between two different modes of S analysis, future studies may have to be directed to cover more complicated nature of GC/PFPD performance. Hydrogen sulfide($H_2S$) was over in summer about low level of olfactory sense 410 ppt, Methyl mercaptan(C$H_3SH$) was over in apring and summer about low level of olfactory sense 70, Dimethyl sulfide(DMS) was not over in four season about low level of olfactory sense 2,200 ppt. Carbon disulfide($CS_2$) was not over in four deason about Tow level of olfactory sense 210,000, Dimethyl disulfide(DMDS) was not over in summer about low level of olfactory sense2,000.

• Journal of Korean Society for Atmospheric Environment
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• v.21 no.2
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• pp.269-274
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• 2005

In this work, analytical bias arising from the gas chromatographic determination of sulfur compounds was evaluated by the application of direct loop injection method to the GC/PFPD detection of four sulfur compounds including H$_{2}$S, CH$_{3}$SH, DMS, and DMDS. For the proper evaluation of analytical uncertainties involved in GC calibration, we employed two comparative techniques of calibration at fxed concentration injection (CFCI) vs calibration at fixed volume injection (CFVI) method. The results of our study indicate that CFCI method exhibits very poor sensitivity due to the matrix effect with varying injection volumes. On the other hand, as CFVI method overcomes such limitation, it can be used to obtain very accurate quantification of S compounds at their high concentration levels above a few to a few tens ppb.

• Korean Journal of Food Science and Technology
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• v.37 no.5
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• pp.695-701
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• 2005

Efficient method was established for analysis of sulfur-containing compounds, including dimethyl disulfide, dimethyl trisulfide, 3-methyl thiophene, allyl mercaptan, 2-methyl-3-furanthiol, and methional. Sulfur-containing compounds were extracted through solid phase microextraction (SPME) or static headspace extraction (SH), and quantified using gas chromatograph equipped with pulsed flame photometric detector. All sulfur compounds, except ally mercaptan, showed higher detection response when dissolved in hexane than in dichloromethane. Linear range was $10^2-10^4$. Dimethyl trisulfide showed lowest limit of detection (LOD) value of 15.2 ppt, and methional highest of 70.5 ppb. Highest extraction efficiency for sulfur-containing compounds, particularly polar and small molecular weight compounds, was observed in 75mm carboxen/polydimethylsiloxane fiber, followed by 65mm polydimethylsiloxane/divinylbenzene and 100mm polydimethylsiloxane. Compared to SPME, less sulfur-containing compounds could be analyzed by SH, mainly due to its low extraction efficiency, although lower amount of artifacts were formed during sample preparation.

• Analytical Science and Technology
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• v.17 no.2
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• pp.145-152
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• 2004

In this study, analytical characteristics of S gas detection technique were investigated against four major reduced S compounds (including hydrogen sulfide; methyl mercaptan; dimethyl sulfide (DMS); and dimethyl disulfide (DMDS)). To analyze such properties, an analytical system was constructed by combining the GC/PFPD system with the loop injection method. The results of our analysis indicated that response behavior of S gases differs greatly between compounds; H2S exhibited the weakest sensitivity of all compounds, while DMDS with two S-atom compounds the strongest sensitivity. To learn more about their response behavior on GC/PFPD method, their calibration patterns were compared using the three arbitrarily set concentration ranges of low, intermediate, and high. The results showed that calibration patterns of each compound are distinguished because of different factors. There was a line of evidence that calibration of $H_2S$ was affected noticeably by adsorptive loss within the system, whereas those of DMS and DMDS were influenced most sensitively by such factor as the linearity response at a given PMT voltage setting. The overall results of our study suggest that quantification of malordorous S compounds require a better knowledge of compound-specific response behavior against GC detection.

• Journal of Integrative Natural Science
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• v.8 no.2
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• pp.128-134
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• 2015

This paper focuses on the applicability of a continuous monitoring method on trace sulfur compounds in the ambient air by TD and GC/PFPD. The target compounds for monitoring include H2S(hydrogen sulfide), Methyl mercaptan, Dimethyl Sulfide, and Dimethyl disulfide. The result of QA/QC on monitoring instruments satisfies all the standards of Odor Measurement and Analysis Method, showing that the reproductivity of the compounds by concentration is within 10%, linearity is above 0.98 of a correlation efficient, method detection limit is 0.16 ppb by MM standard, and recovery rate is over 70%. Monitoring was conducted for two years from March 2006 to February 2008. As a result of the monitoring, the average concentration of H2S was 0.08 ppb, with the maximum concentration at 16.15 ppb. The result indicates that it is reasonable to do continuous monitoring as there appears a spontaneous event of high concentration by the condition of the site during monitoring odor-causing substances. Therefore, it is suggested that the continuous monitoring method used in this paper is appropriate to identify the characteristics of sudden occurrence and concentration variations of sulfur compounds.

• Journal of Korean Society for Atmospheric Environment
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• v.27 no.2
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• pp.133-141
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• 2011

In this study, different calibration approaches for reduced sulfur compounds (RSCs) were investigated by using thermal desorption coupled with gas chromatography (GC) and pulsed flame photometric detection (PFPD). To evaluate the effects of calibration procedures, gaseous standards of 4 RSCs ($H_2S$, $CH_3SH$, DMS, and DMDS) prepared at 10 ppm level were analyzed at 7 loading injection volumes (40, 60, 80, 100, 160, 240, and 320 ${\mu}L$). The results were then compared with calibration curves made with the Z (zero offset) and N (non-zero offset) method. The concentrations of unknown samples were then quantified by using R (ratio) method in which the slope values are compared between standards and samples. Secondly, in A (average) method, results obtained from a multi-point analysis of unknown samples were also averaged to extract representative values for each sample. Results of both experiments showed that analytical error of low molecular weight components (such as $H_2S$ and $CH_3SH$) was greatly expanded with the Z method. In conclusion, the combined application of N-A method was the more realistic approach to reduce biases in the quantification of RSCs.

• Journal of Korean Society for Atmospheric Environment
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• v.19 no.6
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• pp.679-687
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• 2003

In this study, we investigated the analytical techniques to quantify the ambient concentration of hydrogen sulfide (H$_2$S) in air at ppt concentration level. For this purpose, an on-line GC analytical system equipped with both pulsed-flame photometric detector (PFPD) and thermal desorption unit (TDU) was investigated by collecting ambient air samples. The results of our study generally indicated that calibration conditions of GC system is highly sensitive to affect the accuracy of the analytical technique. Most importantly. we found that the use of different matrices in the the preparation stage of working standards was sensitive to control the overall performance of this technique. The calibration of our analytical system was tested by the two types of working standard (prepared by mixing either with high purity $N_2$ or with the ambient air). According to this test, the latter represented more efficiently the detecting conditions of actual air samples. The peak occurrence patterns of both air samples and standards (prepared by mixing with ambient air) were altered in a similar manner as the function of the loaded volume; however, it was not the case for the $N_2$-mixed standards. Results of our study suggest that detection of H$_2$S is highly different from other sulfides and that its quantification requires minimiaing interfering effects of non -pure substance (like water vapor) and (either sorptive or destructive) loss effects.

• Journal of Korean Society for Atmospheric Environment
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• v.22 no.2
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• pp.249-257
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• 2006

In this work, the adsorptive and desorptive behavior of reduced sulfur compounds (RSC) was investigated using the combination of the Peltier cooling (PC)/thermal desorption (TD) unit with the gas chromatographic (GC) detection technique. To examine the adsorptive characteristics of RSC on clothing materials, a total of nine experiments were conducted in a stepwise manner. Once small towel pieces are exposed to significant quantities of RSC standards with high concentrations (10 ppm), the desoprtion stage was then induced by deloading RSC with ultrapure $N_2$ at three different flow rates (FR) of 20, 40, and 60 mL/min. At each FR, the total deloading volume of 400, 800, and 1,600 mL were maintained. These results were then compared in terms of odoring efficiency by dividing the total amount of desorption with the total amount used for exposition or RSC loading. The results indicated that desorption reaction of certain compounds ($CH_3SH$ and DMS) can be influenced significantly with the reducing FR, while they are not affected directly by the total deloading volume. In addition, when the extent of adsorption was compared for most S compounds by the odoring efficiency term, the extent of absorption generally occurred at approximately 1/1000 level of original exposition.

• Analytical Science and Technology
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• v.18 no.4
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• pp.338-343
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• 2005

In this work, sample loss of reduced sulfur compounds (RSC) was investigated with respect to bag sampling techniques. For comparison purpose, calibration slopes were obtained by analyzing standards prepared by 'within syringe dilution' (WSD) method against those made either by 'Tedlar bag dilution' (TBD) or by 'polyester aluminum bag dilution' (PBD) method. The results indicated that the recovery rate of TBD showed the mean values of about 87%, while those of PBD about 77%. Despite the fact that sample loss is inevitable, precise sampling of reduced sulfur compounds may still be possible, if one acknowledges and be prepared for such loss rates of bag sampling methods.