• 한국식품과학회지
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• 제37권5호
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• pp.695-701
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• 2005

각각의 황 함유 화합물의 표준곡선을 그렸을 때, linear range의 범위는 $10^2$부터 $10^4$까지의 범위를 보였다. Dimethyl trisulfide가 가장 작은 limit of detection(LOD) 값과 가장 넓은 linear range $(10^4)$를 보이는 반면, methional은 가장 큰 LOD 값과 가장 좁은 linear range$(10^2)$를 가졌다. 각 황 함유 화학물의 분자구조와 PFPD의 황 함유 화합물 분석 원칙에 영향을 받는 것으로 사료된다. 서로 다른 세 종류의 fiber를 사용시, 미세 고체상 추출법(SPME)을 사용했을 때, CAR/PDMS fiber는 가장 좋은 추출 효율을 보였고, 반대로 PDMS/DVB fiber는 가장 낮은 효율을 나타내었다. SPME 방법을 사용하면, 시료에 포함되어 있는 6개의 황 함유 화합물들 중, 최대 5개까지 분석이 가능하였다. 그러나 본 실험에서 사용하지 않은 황 함유 화합물들도 다수 동정 되었는데, 이렇게 추출과정 중 artifacts로 생성된 황 함유 화합물들은 분석 시 오차를 작용할 수 있다. 고정상 기체추출법(SH)은 SPME와 비교했을 때 더 적은 수의 황 함유 화합물을 감지해냈다. SPME와 비교 시 SH의 추출 효율은 낮았지만, artifact로 생성되는 화합물의 수는 적었다.

• 통합자연과학논문집
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• 제8권2호
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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.

• 한국대기환경학회지
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• 제19권6호
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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.

• 분석과학
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• 제23권1호
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• pp.24-35
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• 2010

본 연구에서는 GC-PFPD와 열탈착 분석기법을 이용한 환원 황화합물(reduced sulfur compounds: RSC)에 대한 열탈착 검량방식의 시간적 재현성을 기존의 외부 검량기법에 덧붙여, 내부표준시료 기법을 연계하여 평가하고자 하였다. 이를 위하여, 4종류의 악취성 황화합물질($H_2S$, $CH_3SH$, DMS, DMDS)과 이들에 대한 내부 표준시료로 CS2를 준비하였다. 이들 표준시료는 저농도(10, 20, 50, 100 ppb)와 고농도 그룹(100, 200, 500, 1000 ppb)을 대표할 수 있게 넓은 범위로 준비하였다. 그리고 외부검량(external calibration)방식의 분석 결과를 부피고정방식(fixed standard volume: FSV)과 농도고정방식(fixed standard concentration: FSC)로 비교하였다. 또한, 2차적으로 FSV 방식의 결과에 외부 및 내부 검량기법을 동시에 적용하여 검량방식의 경시변화(안정도)를 평가하였다. 본 실험의 결과, 감도에 대한 경시변화는 FSC 방식에 비해 FSV 방식에서 작게 나타났다. 따라서 RSC 분석에서 FSV방식이 경시변화를 줄여주는데 상대적으로 효과적이라는 것을 알 수 있었다. 2차적으로 FSV 방식의 결과에 대해 외부 및 내부방식의 감도(기울기 값)를 비교하였다. 이러한 비교를 상대표준편차(RSD)값으로 평가하면, GC-PFPD-TD 시스템의 감도가 비교적 강한 경시변화를 보인다는 것을 알 수 있다. 따라서 이러한 분석기법의 시간적 재현성을 확보하기 위해서는 여러 가지 검정노력이 필요한 것으로 사료된다.

• 한국대기환경학회지
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• 제28권3호
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• pp.306-315
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• 2012

In this study, storage stability of reduced sulfur compounds ($H_2S$, $CH_3SH$, DMS, $CS_2$, and DMDS) and $SO_2$ in sampling bags was investigated in terms of two contrasting storage approaches between forward (F) and reverse (R) direction. The samples for the F method were prepared at the same time and analyzed sequentially through time. In contrast, those of reverse (R) method were prepared sequentially in advance and analyzed all at once upon the preparation of the last sample. In addition, relative performance between two different bag materials (PVF and PEA) was also assessed by using 100 ppb standard. The response factors (RF) of gaseous RSC samples were determined by gas chromatography/pulsed flame photometric detector (GC/PFPD) combined with air server (AS)/thermal desorber (TD) system at storage intervals of 0, 1, and 3 days. There is no statistical difference in all RSCs between two storage methods. However, the results of relative recovery indicated 2.58~12.8% differences in compound type between the two storage methods. Moreover, loss rates and storage stability of $H_2S$ and $SO_2$ were considerably affected by bag materials than any other variables. Therefore, some considerations about storage methods (or bag material types) for sulfur compounds are needed if stored by sampling bag method.

• Bulletin of the Korean Chemical Society
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• 제35권7호
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• pp.2057-2064
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• 2014

Thermochemical sulfate reduction (TSR) was conducted in autoclave on the system of crude oil and $MgSO_4$ at different temperatures. Gas chromatography pulsed flame photometric detector (GC-PFPD) was used to detected the composition of organic sulfur compounds in oil phase products. The results of the analysis indicate that with increased temperature, the contents of organic sulfur compounds with high molecular weight and thermal stability, such as benzothiophenes and dibenzothiophenes, gradually became dominated. In order to gain greater insight into the formation and distribution of organic sulphur compounds from TSR, positive ion electrospray Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) was used in detecting the detailed elemental composition and distribution of them. The mass spectra showed that the mass range of sulfur compounds was 200-550 Da. Four sulfur class species, $S_1$, $N_1S_1$, $O_1S_1$ and $O_2S_1$, were assigned in the positive-ion spectrum. Among the identified sulfur compounds, the $S_1$ class species was dominant. The most abundant $S_1$ class species increase associated with the DBE value and carbon number increasing which also indicates the evolution of organic sulfur compounds in TSR is from the labile series to the stable one. In pure blank pyrolysis experiments with crude oil cracking without TSR, different composition and distribution of organic sulfur compounds in oil phase products were seen from mass spectra in order to evaluate their pyrolysis behaviors without $MgSO_4$. FT-IR and XRD were used in analyzing the products of solid phases. Two distinct crystallographic phases MgO and $MgSO_4$ are found to coexist in the products which demonstrated the transformation of inorganic sulfur compounds into organosulfur compounds exist in TSR.

• 한국대기환경학회지
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• 제27권4호
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• pp.454-459
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• 2011

In this study, the recovery rate of Tedlar bag (T) sampler was investigated in comparison to polyester aluminum bag (P) sampler. To derive the comparative data sets for the relative performance between different samplers, a series of calibration experiments were performed by using 1 ppb standard of four offensive reduced sulfur compounds (RSC) odorants ($H_2S$, $CH_3SH$, DMS, and DMDS) along with $SO_2$ and $CS_2$. All the analysis was made by gas chromatography/pulsed flame photometric detector (GC/PFPD) combined with air server/thermal desorber (AS/TD). The measurement data were obtained by loading gaseous standards (1 ppb) at 3 injection volumes (250, 500 and 1,000 mL) at three intervals (0, 24 and 72 hrs). The recovery rates (RR) of P sampler were computed against the slope values of T sampler. According to our analysis, P sampler exhibits slightly enhanced loss relative to T, especially with light RSCs ($H_2S$ and $CH_3SH$). At day 0, RR for the two were 88 and 85%, respectively. Such reduction proceeded rather rapidly in the case of $H_2S$ through time. However, P sampler was more stable to store $SO_2$ unlike others. Despite slightly reduced recovery, P sampler appears as a good replacement of T sampler.

• 한국산업보건학회지
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• 제17권2호
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• pp.81-88
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• 2007

The aim of this study was to investigate whether the exposure to vinyl chloride monomer(VCM) induces lipid peroxidation in workers by evaluating the concentration of malondialdehyde(MDA) in the urine in order to assess worker's oxidative stress due to exposure of vinyl chloride monomer. The subjects investigated in the study were divided into the experimental group; 18 workers exposed to VCM, and the control group; 19 workers unexposed to VCM. A gas chromatography/pulsed flame photometric detector(GC/PFPD) was utilized to analyze thiodiglycolic acid(TDGA), which was methylated with trimethylsilyldiazomethane (2.0M in diethyl ether) in urine and the urinary MDA, the product of lipid peroxidation, was determined by high-performance liquid chromatography/ultraviolet-visible detector after derivatized with 2,4-dinitrophenylhydrazine(DNPH). The concentrations of urinary TDGA in controls and VCM exposure workers were 0.13(2.01)mg/g Cr. GM(GSD) and 0.35(1.96)mg/gCr. GM(GSD), respectively. The concentrations of urinary MDA were $0.12(2.21){\mu}mol/gCr$. GM(GSD) in controls and $1.35(1.79){\mu}mol/gCr$. GM(GSD) in VCM exposure workers. As a result of simple regressions analysis between urinary concentration of TDGA and MDA in VCM exposure workers, it was found that the $R^2$ value was 0.261 (p=0.03) and the drinking and smoking did not affect their level. In conclusion, the workers exposed to VCM have a potentially to suffered by oxidative stress due to VCM exposure and the urinary MDA can be applicable to the marker of effect to assess the level of worker's VCM exposure.

• Journal of Animal Science and Technology
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• 제48권3호
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• pp.453-466
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• 2006

효율적인 악취방지책을 수립하고 시행하는 것은 지속가능한 축산 뿐만 아니라 증가되는 악취 민원과 더욱 엄격해지는 법규에 대응하기 위해 필수적이다. 본 연구는 돈분뇨의 처리방법에 따른 액상분뇨 유래 악취 및 처리방법이 다른 액상분뇨를 토양에 살포시 발생하는 악취 및 악취물질을 평가하기 위하여 수행되었다. 시험에 사용된 액상분뇨는 신선 분뇨, 혐기성 소화 액상분뇨 및 고온 호기성 소화 액상분뇨를 이용하였고, 토양 특성이 다른 논/밭 토양을대상으로 총 6처리 5반복 설계 배치하였다. 시료 포집은 관능법과 기기분석법에 사용될 시료를 각각 주사기와 테들러 백을 이용하여 액상분뇨와 액상분뇨를 살포한 토양의 상부공간에서 채취하였다. 악취 분석은 관능법을 이용하여 악취강도 및 불쾌도를 평가하였고, 기기분석법으로는 질소화합물 악취물질인 암모니아를 흡광광도법, 황화합물 악취물질인 황화수소, 메틸머캅탄, 다이메틸설파이드 및 다이메틸다이설파이드를 GC-PFPD를 이용하여 분석하였다. 처리과정이 다른 액상분뇨의 악취 및 악취물질 발생 평가에서 고온 호기성 소화 액상분뇨가 신선 분뇨 및 혐기성 소화 액상분뇨에 비해 악취강도, 불쾌도 및 악취농도 저감 효과가 매우 두드러지게 나타났으며 통계적으로도 유의적인 차이가 인정되었다. 혐기성 소화 액상분뇨와 고온 호기성 소화 액상분뇨에서 발생되는 황화수소, 메틸머캅탄, 다이메틸설파이드, 다이메틸다이설파이드 및 암모니아의 평균농도는 각각 65.93 : 5.15 ppb, 18.55 : 0.97ppb, 5.26 : 0.80ppb, 0.33 : 0.56ppb 및 10.57 : 1.34ppm으로 분석되었다. 액상분뇨를 밭과 논 토양에 살포시 혐기성 소화 액상분뇨와 고온 호기성 소화 액상분뇨가 각각 51～94% 및 22～91%의 암모니아 저감 효율을 나타내었다. 본 시험의 결과를 종합할 때 고온 호기성 소화 액상분뇨가 악취 저감이라는 측면에서 다른 처리방법에 비해 우수한 것으로 나타났으며, 액상분뇨의 토양환원에서 발생되는 악취문제는 액상분뇨의 처리방법에 따른 악취발생 정도와 직접적인 연관이 있다고 사료된다.