• Elastomers and Composites
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• v.55 no.4
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• pp.281-288
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• 2020

A calibration curve is needed to determine the SBR and BR blend ratio of SBR/BR blend rubber compounds using pyrolysis-gas chromatography/mass chromatography (Py-GC/MS) or Py-GC. In general, a calibration curve is obtained using reference SBR/BR vulcanizates with various blend ratios. In this study, the calibration curves were obtained using reference samples made of rubber solutions and were compared to those plotted using the reference SBR/BR vulcanizates. Calibration curves using variations of 1,3-butadiene/styrene, 4-vinylcyclohexene (VCH)/styrene, 2-phenylpropene (PhP)/butadiene, PhP/VCH, 4-phenylcyclohexene (PhCH)/butadiene, and PhCH/VCH ratios with the BR content were examined for the suitability. We found that the calibration curves obtained using the mixed rubber solution references (1,3-butadiene/styrene and PhP/butadiene) could replace those constructed using the reference SBR/BR vulcanizates. The calibration curves of 1,3-butadiene/styrene and PhP/butadiene obtained using the raw references can be used for the determination of the SBR/BR blend ratios by applying some correction factors.

• Journal of the Korean Society of Clothing and Textiles
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• v.33 no.12
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• pp.2002-2010
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• 2009

The degradation behavior of berberine is examined using GC-MS to select the fingerprint products that can be used to identify berberine dye in badly faded archaeological textiles. A total of $100^{\circ}C$ thermal and $H_2O_2/UV/O_2$ degradation systems were used to degrade berberine chloride 0.1% solution up to 408 hours. The samples were analyzed using the GC-MS. Dihydroberberine, 2-pteridinamine, 6,7-dimethyl-N-[(trimethylsilyl) oxy]-, and 8-methoxy-11-[3-methylbutyl]-11H-indolo[3,2-c]-quinoline, 5-oxide were detected as the major products of thermal degradation and identified as the fingerprint products for berberine dye at the early stage of degradation. Isobenzofuran-1,3-dione,4,5-dimethoxy-, 9H-fluorene,3,6-bis(2-hydroxyethyl)-,1,3-dioxolo[4,5-g]isoquinolin-5(6H)-one,7,8-dihydro-, and 3-tert-butyl-4-hydroxyanisole were detected as the major products generated by the $H_2O_2/UV/O_2$ degradation and identified as the fingerprint products for berberine dye under severe degradation conditions.

• Analytical Science and Technology
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• v.24 no.5
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• pp.352-359
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• 2011

An analytical method for solvent-free determination of benzene, toluene, ethylbenzene, and xylenes (BTEX) in water using repetitive membrane extractions coupled to cryofocusing and GC-MS was derived. BTEX compounds that permeated through a nonporous silicone membrane from the aqueous phase and evaporated into the acceptor phase were purged into a cryofocusing trap ($-100^{\circ}C$) with helium gas. The BTEX compounds, thus enriched in the trap, were thermally desorbed into a capillary column GC and detected using an MS. The flow rate of the donor phase (30 mL water) was set at 10 mL/min, and membrane extractions, accomplished by returning the water drained from the extraction module to the sample container, were repeated three times at $20{\pm}2^{\circ}C$. Although recoveries (%) were variable, from the highest for benzene (approximately 80%) to the lowest for ethylbenzene and xylenes (3.5-10%), the method showed satisfactory precision (RSD 2.2-10%) with good-linearity calibration curves ($r^2$ 0.9976-0.9997 in 1-100 ${\mu}g$/L range) for all of the compounds. The method detection limits (MDLs) ranged from 0.16 to 1.8 ${\mu}g$/L. The results showed the method's advantages such as short analysis time and overall simplicity without solvent compared to the conventional techniques.

• Analytical Science and Technology
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• v.27 no.2
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• pp.100-107
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• 2014

Plastic has been widely used in modern artworks' materials due to its merits of process ability and mass production. In the country, value of plastic artifact is increasing but the field of plastic study is limited to industrial purpose. In this study, Identification methods of plastic were performed by SPME-GC/MS and pyrolysis-GC/MS using trace of samples. As a result of identification using SPME-GC/MS, aromatic compounds were identified from polyvinyl chloride. And alkane compounds were identified from polyethylene, and polypropylene. Aromatic compounds were identified from polystyrene, and diethylene glycol appeared in polyurethane based on polyester was identified from polyurethane. As a result of identification using pyrolysis- GC/MS, aliphatic alkenes compounds and phthalate(DEHP) were identified from polyvinyl chloride. Aliphatic alkenes compounds and phthalate(DIBP) were detected from polyethylene. 1-hexene, etc., were detected from polypropylene, aromatic compounds were identified from polystyrene, and methylene diphenyl diisocyanate which is polyurethane basic material was confirmed from polyurethane. This study suggested that non-destructive SPME and pyrolysis-GC/MS are useful to identify compounds particularly polystyrene and polyurethane. These two analytical methods were expected to be applied for identification of unidentified plastic artworks before conservation treatment.

• Analytical Science and Technology
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• v.18 no.4
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• pp.320-328
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• 2005

The most common five chlorophenols (4-chloro-3-methylphenol, 2,4,5-trichlorophenol, 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol, pentachlorophenol) were determined from the industrial wastewater by GC/MS. The samples were collected from the petrochemical company, textile company and leather making company. The developed analytical method was modified by USEPA Method 3510. The samples were extracted with dichloromethane under pH 2 and pH 5-6, and determined by the GC/MS with SIM mode. There were good linearities (above $R^2=0.9943$) on e ranges of the 0.1 ng/mL~10 ng/mL and 0.5 ng/mL~10 ng/mL, and the limit of detection were between 0.1 ng/mL and 0.5 ng/mL. The absolute recoveries were measured at the concentration of 1, 5, and 10 ng/mL, and the recovery was 71.6~98.9% except for PCP. The relative standard deviation (RSD) was 1.2~14.3% and it gave a good reproducibility for the assay. The bias, which shows the accuracy, was a good although it was a little high values (11.3~22.1%) at the low concentration (1 ng/mL).

• Analytical Science and Technology
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• v.23 no.2
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• pp.179-186
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• 2010

The oxidative metabolism of ibuprofen in healthy male urine collected at 3, 6, 9, 12 and 15 h after oral administration of ibuprofen was studied by GC/MS assay. To detect conjugated metabolites of ibuprofen, urine sample was acid-hydrolyzed with 6 M HCl at $100^{\circ}C$ for 30 min. To effectively extract ibuprofen and its metabolites, liquid-liquid extraction (LLE) was conducted at pH 3, 5, and 7, respectively. As a result, LLE at pH 3 was shown to be the best extraction condition. For the determination of trace amounts of ibuprofen and its metabolites in extract, trimethylsilylation (TMS) with BSTFA was applied and followed by GC/MS analysis. In this study, main 5 metabolites including parent drug were detected and these metabolites were assigned as three hydroxylated forms and one carboxylated form. Each metabolite was tentatively identified by both interpretation of mass spectrum and comparison with previously reported results. In addition, time profile of urinary excretion rate for parent drugs and metabolites was studied. Finally, the metabolic pathways of ibuprofen were suggested on the basis of the structural elucidation of its metabolites and excretion profiles.

• Analytical Science and Technology
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• v.23 no.2
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• pp.128-137
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• 2010

The purpose of this study is to set up the analytical method of new persistent organic pollutants (POPs) such as chlordecone, endosulfan, ${\alpha}$-HCH, ${\beta}$-HCH, ${\gamma}$-HCH. The analytical methods for these compounds listed as new POPs by the Stockholm Convention need to be newly established. Therefore, we proposed the analytical method for 5 organic chlorinated pesticides (OCPs) and then applied the analytical method to environmental samples. To do this, the pre-treatment such as florisil and activated carbon cleanup process in the Korean official method for classic POPs had been reviewed. All of compounds except chlordecone were pre-treated simultaneously with reviewed cleanup process and detected by GC/MS and HRGC/HRMS respectively. There is a problem that chlordecone could not get a high sensitivity by GC analysis, but in this study GC/MS method was proposed.

• Journal of the Society of Disaster Information
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• v.9 no.3
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• pp.249-258
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• 2013

Recieved Mar. 06, 2013 Revised Mar. 29, 2013 Accepted Sep. 11, 2013In this study, we evaluated the method performance and the optimum sample injection method of the portable GC/MS(HAPSITE) which were designed to operate on scene of chemical accidents. Chemicals used for performance test were vinyl chloride(VC), methyl chloride(MC), benzene(Bz), toluene(Tol). CRM(Certified Reference Material) Manufactured by KRISS(Korea Research Institute of Standards and Science) was used as the standard gas. The results showed that 1) Among three sample injection methods(Cylinder, Silico canister, and Bag), bag was identified as the most appropriate sample injection method. Bag material and capacity did not significantly affect the results. The most ideal reproducibility occurred at the 2-minute point of the purge time in the loop and tenax methods. 2) Performance evaluation of HAPSITE was conducted. Evaluation items were reproducibility, linearity, method detection limit, etc. Tenax concentration method was appropriate for larger molecules and Carbopack concentration method was suitable for smaller molecules.

• Analytical Science and Technology
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• v.15 no.6
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• pp.534-539
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• 2002

We established an analytical method for the measurement of trace amounts of earthy/musty odorous geosmin (GSM) and 2-methylisoborneol (2-MIB) in water using GC/MS. Water samples were extracted with n-hexane (liquid-liquid extraction, LLE) and the extracts were measured by GC/MS. The extraction yields of the two compounds were tested to be ($87{\pm}8$)% and ($78{\pm}8$)%, respectively. The limits of quantitation (LOQs) of the two compounds by this method were greatly improved to ~0.3 ng/L. The analytical methods were applied to analyze water samples from several rivers in Korea and waters after water treatment processes. The highest levels of geosmin and 2-methylisoborneol in raw water from a river were measured to be ($4.2{\pm}0.4$) ng/L and ($44{\pm}4$) ng/L, respectively. The levels only slightly decreased to ($1.3{\pm}0.1$) ng/L and ($18{\pm}2$) ng/L even after water treatment, indicating that the odorous compounds were not properly removed by the treatment processes.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.67 no.4
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• pp.335-341
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• 2022

Proso millet (Pacnicum miliaceum L.) has a various of functional substances, so the demand is increasing as interest in human health benefits. In particular, miliacin, a triterpenoid in proso millet, is known to be effective in hair loss due to its promoting metabolism and proliferation of keratinocytes and showing protective effects from apoptosis. In this study, proso millet oil was extracted and analyzed by GC/MS using the extraction method of unsaponifiable substances after saponification reaction. The components of proso millet oil were confirmed through qualitative analysis by GC/MS. The miliacin content of 5 varieties of proso millet and 2 varieties of foxtail for comparison was analyzed. In the result, components of pentacyclic triterpenes such as β-amyrine and lupeol were detected in proso millet, and the content of miliacin was highest in Hallachal at 370.38±0.04 ㎍/100 mg oil. In addition, the content of miliacin was not detected in Samdachal and Samdamae, which are varieties of foxtail millet.