• Analytical Science and Technology
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• v.8 no.4
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• pp.739-744
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• 1995

The two main methods to prepare water samples for analyzing volatile organic compounds(VOC's) were investigated. One is the purge and trap(PT) method and another is the head space(HS) sampling method. Both methods were effective to transfer the low boiling point components from the water sample onto the capillary column. The cryo-focusing at the top of the main capillary column was an effective way to obtain the sharpness of the chromatographic peaks but could be avoided when a semi-wide bore column was used. The recovery from the same amount of the sample was better in PT than in HS but a larger sample volume in HS method could compensate the lower efficiency. Therefore PT is suitable to the analysis of drinking water where the very low concentration must be determined. HS is suitable to waste water analysis because of the easiness of the operation. The repeatability was good and similar in both methods. For the contamination of the former sample, both methods were tough and could be used without any problems. The matrix effect which could change the equilibrium parameters in HS method was find negligible in many components. The actual samples such as tap water and river water were analyzed with both methods concerning 16 components regulated in Korea.

• Korean Journal of Food Science and Technology
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• v.30 no.2
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• pp.260-265
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• 1998

In this study, volatile flavor compounds in sesame oils were analyzed by using pure-and-trap method and a gas chromatography. 2-ethoxy-3-ethylpyrazine was used as an internal standard and retention index (Kovat's number) for the volatiles were determined through the use of a n-paraffin $(C_5-C_{25})$ standards. A total of 33 volatile compounds including 14 pyrazines, 7 thiazoles, 4 pyridines, 2 oxazoles and 6 others were identified in the sesame oils. By comparing the total yields of volatile flavor compounds, the pyrazines are the most abundant compounds all of the oil samples and considered as good contributor to characteristic flavor of sesame oil. The oil from the seeds roasted in the electric pan at $200^{\circ}C$ and $230^{\circ}C$ for 10 minutes generated 277.06 ppm, 264.81 ppm in pyrazine and 15.16 ppm, 13.19 ppm in thiazole, respectively. The sensory evaluation of oil samples was also investigated. The sesame oil obtained from the sesame seeds roasted at $200^{\circ}C$ for 10 minutes with electric pan showed good flavor scores and quality among the all of samples.

• Proceedings of the Korean Society of Food Hygiene and Safety Conference
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• 2001.10a
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• pp.140-140
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• 2001

A sensitive analytical method based on gas chromatograpy-mass spectrometry with a selected ion monitoring (GC/MS-SIM) with the purge-and-trap concentration and with headspace method (in limited applications) was developed for determining of epichlorohydrin in canned beverages coated with epoxy resin. The calibration curve in the range of $0.5\sim50ng$ had correlation coefficient greater than 0.998 and a detection limit of $0.l\mug/L$ was obtained using a sample volume of 20ml. The predominant ions of epichlorohydrin produced in MSD using electron ionization(EI) were m/z 57 ([M-CI]+) and 62/64 $([M-CH_2O]+)$. In survey of epichlorohydrin in thirty commercial canned beverage samples, none of them was detected.

• Analytical Science and Technology
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• v.22 no.1
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• pp.44-50
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• 2009

In this study, the use of purge & trap GC-MS technique for determination of methylmercury in sediment samples was described. The method detection limit of the method was determined as 0.06 ng/g and the recovery of the method was $102{\pm}11.4%$, with precisions better than 11.2%. The method was validated by analysis of CRMs such as ERM CC580 (estuarine sediment) and IAEA 405 (sediment). Additionally, the performance of the method was tested on river sediment samples and the analytical results were compared with those of the GC-CVAFS, which has been widely used for methylmercury analysis.

• Analytical Science and Technology
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• v.34 no.1
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• pp.23-35
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• 2021

In order to measure the volatile organic compounds (VOCs) of a sample which is too large to use commercially available chamber, a stainless steel vacuum chamber (VC) (with an internal diameter of 205 mm and a height of 50 mm) was manufactured and the temperature of the chamber was controlled using an oven. After concentrating the volatiles of the sample in the chamber by helium gas, it was made possible to remove residual volatile substances present in the chamber under reduced pressure ((2 ± 1) × 10-2 mmHg). The chamber was connected to a purge & trap (P&T) using a 6 port valve to concentrate the VOCs, which were analyzed by gas chromatography-mass spectrometry (GC-MS) after thermal desorption (VC-P&T-GC-MS). Using toluene, the toluene recovery rate of this device was 85 ± 2 %, reproducibility was 5 ± 2 %, and the detection limit was 0.01 ng L-1. The method of removing VOCs remaining in the chamber with helium and the method of removing those with reduced pressure was compared using Korean drinking water regulation (KDWR) VOC Mix A (5 μL of 100 ㎍ mL-1) and butylated hydroxytoluene (BHT, 2 μL of 500 ㎍ mL-1). In case of using helium, which requires a large amount of gas and time, reduced pressure ((2 ± 1) × 10-2 mmHg) only during the GC-MS running time, could remove VOCs and BHT to less than 0.1 % of the original injection concentration. As a result of analyzing volatile substances using VC-P&T-GC-MS of six types of cell phone case, BHT was detected in four types and quantitatively analyzed. Maintaining the chamber at reduced pressure during the GC-MS analysis time eliminated memory effect and did not affect the next sample analysis. The volatile substances in a cell phone case were also analyzed by dynamic headspace (HT3) and GC-MS, and the results of the analysis were compared with those of VC-P&T-GC-MS. Considering the chamber volume and sample weight, the VC-P&T configuration was able to collect volatile substances more efficiently than the HT3. The VC-P&T-GC-MS system is believed to be useful for VOCs measurement of inhomogeneous large sample or devices used inside clean rooms.

• Analytical Science and Technology
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• v.13 no.3
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• pp.277-281
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• 2000

The solid phase microextrction (SPME) fiber which contains $100{\mu}m$ polydimethyl siloxane of a stationary phase was used for the analysis of volatile organic compounds contained in aqueous solution. sixteen volatile organic compounds, which were spiked in blank water and extracted by the headspace SPME techique, were analyzed by gas chromatography/mass spectrometry (GC/MS). Analytical results showed that the percent of average recoveries and relative standard deviations were 97% and 4.7%, respectively. The value of detection limit was ranged from 0.01 to $0.5{\mu}g/l$. These results are more accurate than those obtained by the other methods such as purge and trap and headspace methods.

• Analytical Science and Technology
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• v.14 no.3
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• pp.274-285
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• 2001

In this study, the thermal desorption-cryofocusing-gas chromatographic(TD-C-GC) method was developed for determination of volatile organic compounds(VOCs) in ambient air and was applied at the municipal solid waste landfill sites. On-column cryofocusing was possible only with a 100 ml dewars bottle in TD-C-GC method with a stainless steel column. However, high operating pressure was needed for purging VOCs from the absorbent trap, which was able to solve by pressure programming with a electric pressure controller. By using both pressure and temperature programming brought increasing of resolution power in on-column cryofocusing method, but the high pressure caused a leakage of sample tube with repeated use. A loop cryofocusing devise was also developed and compared with the direct on-column method. In loop cryofocusing method, VOCs were concentrated on a 0.8mm i.d. loop which is located between the injector and separation column by using liquid nitrogen. In order to purge VOCs from the absorbent trap, only 0.4 psi of pressure was need in the loop cryofocusing method. Dual detection system was applied for the analysis of VOCs; a FID was used for hydrocarbons and a FPD was used for sulfur-containing compounds. Qualitative analysis was done by on-column cryofocusing GC-MS system. Among the large number of VOCs, toluene was the most abundant. Hydrogen sulfide, dimethyl sulfide, carbon disulfide, dimethyl disulfide and methyl propyl disulfide were detected at landfill site by FPD.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2009.11a
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• pp.13-13
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• 2009

본 연구는 MLCC 구성성분의 증발/비등에 의한 저분자물질의 제거가 bar 수축에 미치는 영향도를 평가하기 위해, 압착 bar에서 발생하는 고농도의 out gas를 정량하기 위한 최적 system을 구축하고자 하였다. gas 포집에 범용적으로 사용하는 Purge & Trap sampler 대신 Heating block를 사용하여 gas를 발생시키고 동시에 solvent에 용해시킴으로써 고농도의 시료가 희석될 수 있는 전처리 장치를 디자인하였다. 그 결과 고농도 gas 주입에 의한 장비오염과 peak saturation 문제가 해결되었고, gas phase의 시료를 liquid phase로 상전이 시켜 autosampler를 이용한 정확한 량의 시료 주입이 가능하였다. System의 Gage Linearity와 Bias는 각각 1.7%와 1.3%로 개선이 필요없는 수준의 정확도를 가졌다.

• Preventive Nutrition and Food Science
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• v.3 no.2
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• pp.119-122
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• 1998

Pumpkin venegar was produced using autoclaved pumpkin juice by fermenting with cetobacter starter and ethanol at the ratio of 4 % and 10% to the volume of pumpkin juice, respectivley. Fermentation was carried out at 2$0^{\circ}C$ for 14 days followed by aging at 1$0^{\circ}C$ for 14 days. Flavor components of pumpkin vinegar was determined using GC/MS. Identified components, were 2 aldehydes (4.74%), 5 acohols (30.06%), 4 ketones (8.99%), 4 acids (16.39%), 5 alkanes (11.10%), 11 miscellaneous compounds (27.01%) and 9 unknown compounds (1.71%). Pumpkin vinegar showed very similar flavor characteristics to those of conventional wien vinegar and sherry wine vinegar in particular , acetioin, methyl acetate, and butanoic acid were typical volatile components of these three kinds of vinegar. Pumpkin vinegar showed possiblity to compete with European wine vinegar.

• Microbiology and Biotechnology Letters
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• v.27 no.3
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• pp.236-245
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• 1999

Andong Soju is a Korean traditional distilled liquor brewed with Nuruk which is cultured with wild microorganisms. To provide useful information for scientific production and systematic quality control of traditional distilled liquor, the effects of mixed culture of the alcoholic yeasts and saccharifying molds isolated from the Nuruk, and mashes on the flavor and sensory characteristics were investigated. Distillate from mashes cocultured with Saccharomyces cerevisiae and Hansenula anomala using Mucor Nuruk was compared with distillate from mashes brewed with Andong Nuruk and with distillate from plant fermented mashes to analyze their flavor characteristics. The volatile flavor compounds in distillates were analyzed by GC and GC-MS using direct injection, solvent extraction, and purge & trap methods. Alcohols such as 3-methyl-1-butanol, 2-methyl-1-propanol, 1-propanol, and 2-phenyl ethanol; aldehydes such as acetaldehyde and 2-furancar-boxaldehyde; esters such as ethyl ester of acetic acid, hexanoic acid, octanoic acid, decanoic acid; alkanes, alkenes, ketone, sulfur, and pyrone compounds were detected. Alcohols were chief components of flavor compounds. No significant difference in overall acceptability test was shown among three experimental groups(p<0.05), but Nuruk-like aroma, Kaoliangchiew-like aroma, sweet taste, and well rounded mouthfeel showed significant differences among them(p<0.05).