• Title/Summary/Keyword: reference compounds

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Development of primary reference gas mixtures of 18 volatile organic compounds in hazardous air pollutants (5 nmol/mol level) and their analytical methods

  • Kang, Ji Hwan;Kim, Yong Doo;Lee, Jinhong;Lee, Sangil
    • Analytical Science and Technology
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    • v.34 no.5
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    • pp.202-211
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    • 2021
  • Volatile organic compounds (VOCs) in hazardous air pollutants (HAPs) have been regulated by the Air Pollution Control Act (1978) and their atmospheric concentrations have been monitored in 39 monitor sites in Korea. However, measurement standards of volatile organic compounds (VOCs) in HAPs at ambient levels have not been established in Korea. Primary reference gas mixtures (measurement standards) at ambient levels are required for accurately monitoring atmospheric VOCs in HAPs and managing their emissions. In this study, primary reference gas mixtures (PRMs) at 5 nmol/mol were developed in order to establish primary national standards of VOCs in HAPs at ambient levels. Primary reference gas mixtures (PRMs) were prepared in pressurized aluminum cylinders with special internal surface treatment using gravimetric method. Analytical methods using gas chromatography-flame ionization detector (GC-FID) coupled with a cryogenic preconcentrator were also developed to verify the consistency of gravimetrically prepared HAP VOCs PRMs. Three different columns installed in the GC-FID were evaluated and compared for the retention times and separation of eighteen target components in a chromatogram. Results show that the HAP VOCs PRMs at 5 nmol/mol were consistent within a relative expanded uncertainty (k=2) of less than 3 % except acrylonitrile (less than 6 %) and the 18 VOCs were stable for 1 year within their associated uncertainties.

Simultaneous Determination of (-)-Menthone and (-)-Menthol in Menthae Herba by Gas Chromatography and Principal Component Analysis

  • Kim, Jung-Hoon;Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Natural Product Sciences
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    • v.16 no.3
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    • pp.180-184
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    • 2010
  • The simple and accurate method was established for the simultaneous determination of (-)-menthone and (-)-menthol in Menthae herba obtained from Korea and China. A quantitative analysis was performed with a gas chromatography-flame ionization detector and reference compounds were separated on a capillary HP-Innowax column (30 m $\times$ 0.23 mm, 0.50 ${\mu}m$, Agilent, MA, USA). The correlation coefficients of the compounds showed good linearity ($r^2$ > 0.9997) over the linear range. The precision, repeatability and stability showed less than 1.7% of relative standard deviation (RSD) values for two compounds. Recovery rates were within the range of 95.72 - 103.76%. The method was applied successfully to analyze 15 samples of Menthae herba and achieved sufficient and specific separation of reference compounds. The principal component analysis (PCA) exhibited the classification of 15 samples according to their locations of origin.

Building Calibration Curve for Py-GC/MS Analysis of SBR/BR Blend Rubber Compounds

  • Chae, Eunji;Choi, Sung-Seen
    • 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.

Compositional differences of Bojungikgi-tang decoctions using pressurized or non-pressurized extraction methods with variable extraction times

  • Kim, Jung-Hoon;Seo, Chang-Seob;Kim, Seong-Sil;Shin, Hyeun-Kyoo
    • The Korea Journal of Herbology
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    • v.28 no.4
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    • pp.1-6
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    • 2013
  • Objectives : In other to determine the optimal extraction conditions, the various Bojungikgi-tang (BJIGT) decoctions prepared by different pressure levels and different extraction times were compared and evaluated in terms of the extract yield and the total soluble solid content. Methods : Decoctions were prepared by the pressure levels of 0 (non-pressurized) and 1 $kgf/cm^2$ (pressurized) for 60, 120 and 180 min. The extract yield and the total soluble solids content of decoctions were measured, and the amounts of the reference compounds in decoctions were investigated by the analysis using high performance liquid chromatography. Results : The extract yield and the total soluble solid content were higher in decoctions extracted by the pressurized method than those from decoction with non-pressurized method. The patterns of yield and contents showed a proportional increase to the extraction time. In analysis of the linear regression for four reference compounds such as liquiritin, nodakenin, hesperidin, and glycyrrhizin, the good linearity with the correlation coefficient more than 0.9999 was observed. The highest contents for four reference compounds were observed at 180 min of both the pressurized method and the non-pressurized method. Conclusions : This study suggests that the pressure in extraction method and the extraction time affect the compositional constituents in BJIGT decoctions. The extraction time of 180 min could be chosen in both pressurized and non-pressurized method as optimal extraction condition.

Synthesis and Biological Activities of Some New 3,6-Disubstituted 1,2,4-Triazolo[3,4-b]1,3,4-thiadiazole Derivatives

  • Rafiq, Muhammad;Saleem, Muhammad;Hanif, Muhammad;Maqsood, Muhammad Rizwan;Rama, Nasim Hasan;Lee, Ki-Hwan;Seo, Sung-Yum
    • Bulletin of the Korean Chemical Society
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    • v.33 no.12
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    • pp.3943-3949
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    • 2012
  • A series of aromatic hydrazides 3a-j were prepared by refluxing esters 2a-j with hydrazine hydrate in methanol, which were prepared by the esterification of 1a-j. Acetohydrazides 3a-j upon treatment with carbon disulfide and methanolic potassium hydroxide yielded potassium dithiocarbazate salts 4a-j, which on refluxing with hydrazine hydrate yielded substituted 4-amino-5-aryl-3H-1,2,4-triazole-3-thiones 5a-j. The target compounds 6a-j were synthesized by condensing furan-3-carboxylic acid in the presence of polyphosphoric acid under reflux. The structures of newly synthesized compounds were characterized by IR, $^1H$ NMR, $^{13}C$ NMR, elemental analysis and mass spectrometric studies. All the synthesized compounds were screened for their urease, acetylcholine esterase inhibition, antioxidant and alkaline phosphatase inhibition activity. Almost all of the compounds 6a-j showed good to excellent activities against urease and acetylcholine esterase more than the reference drugs. Compounds 6f and 6g were more potent scavenger of free radicals than the reference n-propyl gallate. Compound 6b and 6h showed excellent activities of alkaline phosphatase as compare to the reference $KH_2PO_4$.

Development of a Chloroform Reference Material for the Proficiency Testing of Hazardous Compounds in Commercial Consumer Chemical Products Under the Consumer Chemical Products and Biocide Safety Management Act (K-BPR)

  • Lee, Sang Tak;Lee, Jae-ung;Kim, Joo-Hyon;Oh, Han Bin
    • Mass Spectrometry Letters
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    • v.10 no.4
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    • pp.112-116
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    • 2019
  • In this study, a chloroform consumer chemical product (CCP) reference material (RM) is successfully developed, with potential to be used in the proficiency testing of hazardous compounds in CCPs for analysis and testing agencies. Validation experiments are rigorously conducted to evaluate whether the RM meets the requirements set by the ISO 13528 and ISO Guide 35, using a reliable GC/MS method for the analysis of chloroform. The obtained calibration plot linearity, limit of detection (LOD), and limit of quantitation (LOQ) are excellent. The developed RM meets the homogeneity and stability requirements; the between-unit (sbb) and within-unit (swb) standard deviations are less than 2.5%, and the stability is found to be guaranteed for 50 days.

Synthesis and Antimicrobial Activity of Some New 1-Alkyl-2-alkylthio-1,2,4-triazolobenzimidazole Derivatives

  • Mohamed, Bahaa Gamal;Hussein, Mostafa Ahmed;Abdel-Alim, Abdel-Alim Mohamed;Hashem, Mohammed
    • Archives of Pharmacal Research
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    • v.29 no.1
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    • pp.26-33
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    • 2006
  • Some new derivatives of 1,2,4-triazolo[2,3-a]benzimidazoles were synthesized through the reaction of 1,2-diaminobenzimidazole with carbon disulfide. The resulting 1,2,4-triazolo-[2,3a]benzimidazole-2-thione intermediate was reacted with one equivalent of alkyl halides to give the corresponding 2-alkylthio derivatives, which were further alkylated through the reaction with another one equivalent of different alkyl halides to afford the target compounds; 1-alkyl-2alkylthio-1,2,4-traizolo[2,3-a]benzimidazoles. On the other hand, the 1,2-disubstituted derivatives with two identical alkyl substituents were prepared by the reaction of 1,2,4-triazolo[2,3-a]benzimidazole-2-thione with two equivalents of the alkyl halides. The structures of the new compounds were assigned by spectral and elemental methods of analyses. The synthesized compounds were tested for their antibacterial and antifungal activities. Most of the tested compounds proved comparable results with those of ampicillin and fluconazole reference drugs. The study indicated that, the antibacterial as well as the antifungal activities of the test compounds were improved with increase in the bulkiness of the introduced alkyl groups. Also, some active antibacterial compounds were tested for their antimycobacterial activity. All the test compounds showed equipotent antitubercular activity as that of INH as a reference drug.

Design, Synthesis, and Antimicrobial Activity, of New 1,4-disubstituted Octahydroquinoxaline-2,3-dione Derivatives

  • Hussein, Mostafa A.
    • Bulletin of the Korean Chemical Society
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    • v.32 no.5
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    • pp.1511-1518
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    • 2011
  • A series of 1,4-disubstituted octahydroquinoxaline-2,3-dione derivatives was prepared through two steps reaction. The latter involves the formation of N,N-disubstituted cyclohexane-1,2-diamine derivatives (la-j) through reductive alkylation of 1,2-cyclohexanediamine with different aldehydes in presence of sodium cyanoborohydride. Fusion of compounds (1a-j) with diethyl oxalate affording the target compounds (2a-j). Elucidation of structures of compounds (2a-j) was based upon different spectral data as well as the elemental methods of analyses. In addition, mass spectrometry and X-ray diffraction analyses were carried out. Moreover, the lipophilicity of the target compounds as expressed from the Clog P. Most of the test compounds (2a-j) showed weak to moderate antibacterial and antifungal activities against most of the used bacterial and fungal strains in comparison to chloramphenicol and clotrimazole as reference drugs respectively.

The Effect of Solvent Trap Apparatus on the Analysis of Carbonyl Compounds in Cigarette Smoke (용매 포집장치가 연기 중 Carbonyl 화합물의 분석에 미치는 영향)

  • 김효근;이존태;윤오섭;이문수
    • Journal of the Korean Society of Tobacco Science
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    • v.25 no.2
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    • pp.137-143
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    • 2003
  • Among the most popular means of mainstream smoke collection for specific analysis are solvent traps. Determination of the carbonyl compounds as their 2,4-dinitrophenylhydrazones(DNPHs) by HPLC offers increased sensitivity and reproducibility in the analysis of mainstream cigarette smoke. In this work, the mainstream smoke of a reference cigarette(lR4F) was collected in four kinds of gas washing bottles and their effects on the analysis of carbonyl compounds were investigated. The results show that the porosity of fritted glass filter in gas washing bottles exerted profound effect on the composition of the carbonyl compounds in mainstream smoke.

Characterization of Volatile Organic Compounds associated with Environmental Tobacco Smoke

  • Baek, Sung-Ok;Roger A. Jenkins
    • Journal of Korean Society for Atmospheric Environment
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    • v.14 no.E
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    • pp.41-58
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    • 1998
  • In this study, a wide range of volatile organic constituents of environmental tobacco smoke (ETS) were determined using an environmental chamber, where ETS is the sole source of target compounds. ETS was generated in an environmental chamber by a number of different cigarettes, including the Kentucky reference cigarette and eight different commercial brands. More than 30 compounds were measured simultaneously for a total of twelve experimental runs. The target compounds are classified into three major classes, i.e. vapor phase ETS markers including 3-ethnylpyridine (3-EP) and nicotine, carbonyl compounds including formaldehyde, and volatile organic compounds (VOCs). The results from the chamber study were used to generate characterized ratios of selected VOCs to 3-EP, a vapor phase ETS marker. Emission factors for VOCs associated with ETS were also estimated. The characteristic ratios appeared to be generally in good agreement with published data obtained by environmental chamber studies similar to this study. This implies that the ratios may be useful for identifying and quantifying the impact of ETS as a source of target compounds in 'real world' indoor environments, which is affected by a complex mixture of multi-sources. The environmental chamber method described here provides a direct and reliable method to compare the ETS generated by different cigarettes. The method can also be applied to the simultaneous determination of many different ETS components.

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