• Title/Summary/Keyword: In-fiber derivatization

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Analysis of Haloacetic Acids in Drinking Water by Direct Derivatization and Headspace-SPME Technique with GC-MS (Handspace Solid Phase Microextraction 방법에 의한 HAAs 분석에 관한 연구)

  • Cho, Deok-Hee
    • Journal of Korean Society of Water and Wastewater
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    • v.18 no.5
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    • pp.638-648
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    • 2004
  • In many drinking water treatment plants, chlorination process is one of the main techniques used for the disinfection of water. This disinfecting treatment leads to the formation of haloacetic acid (HAAs). In this study, headspace solid-phase microextraction (HS-SPME) was studied as a possible alternative to liquid-liquid extraction for the analysis of HAAs in drinking water. The method involves direct derivatization of the acids to their methyl esters without methyl tert-butyl ether (MTBE) extraction, followed by HS-SPME with a $2cm-50/30{\mu}m$ divinylbenzene/carboxen/polydimethylsiloxane fiber. The effects of experimental parameters such as selection of SPME fiber, the volume of sulphuric acid and methanol, derivatization temperature and time, the addition of salts, extraction temperature and time, and desorption time on the analysis were investigated. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The $2cm-50/30{\mu}m$-divinylbenzene/carboxen/polydimethylsiloxane fiber, sulphuric acid of 1ml, methanol of 3ml, derivatization temperature of $50^{\circ}C$ derivatization time of 2hrs, sodium chloride salt of 10g, extraction time of 30 minutes, extraction temperature of $20^{\circ}C$ and desorption time of 1 minute at $260^{\circ}C$ were selected as the optimal experimental conditions for the analysis of HAAs. The linearities ($r^2$), relative standard deviations (%RSD) and limits of detection (LOD) for HAAs were 0.9978~0.9991, 1.1~9.8% and $0.05{\sim}0.2{\mu}g/l$, respectively.

Determination of Volatile Fatty Acids in Aqueous Samples by HS-SPME with In-Fiber Derivatization (Fiber내 유도체화/HS-SPME를 이용한 수용액 시료 중 휘발성 지방산의 분석)

  • Ahn, Yun Gyong;Lee, Jee Yeon;Kim, Jeehyeong;Hong, Jongki
    • Analytical Science and Technology
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    • v.16 no.6
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    • pp.458-465
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    • 2003
  • The HS (headspace)-SPME (Solid phase microextraction) as rapid and simple method was performed for the determination of volatile fatty acids (VFAs) from the aqueous samples. In-fiber derivatization of VFAs with 1-Pyrenyldiazomethane (PDAM) was applied to improve their sensitivity of detection. In SPME procedure, typical parameters such as effects of solution pH, and salting out reagent and ultrasonication were investigated to improve the extraction efficiency. Based on the developed method, VFAs in wastewater samples were determined by gas chromatography / mass spectrometry-selected ion monitoring (GC/MS-SIM) mode.

Determination of ethylene glycol in alkali wastewater by gas chromatography/mass spectrometry (GC/MS를 이용한 알칼리 폐수 중 ethylene glycol 정량)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.527-531
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    • 2004
  • Treatment with aqueous sodium hydroxide solution plays an important role to impart certain desirable properties - feel and luster on the surface of polyester fiber. In this process alkali wastewater contains disodium terephthalate, ethylene glycol (EG) and residual sodium hydroxide. In this paper we report a new method containing the pretreatments of derivatization with benzoyl chloride and solvent extraction using pentane. The calibration curve of EG determined by GC/MS-SIM shows a good linearity in the range of 0.1 to $25{\mu}g/mL$ having the standard deviation of ${\leq}8.7%$. The recovery and the detection limit of this method are 91.9-93.7% and $0.05{\mu}g/mL$ respectively.

A Study on the Chromatographic Separation of Proteins Using Fibrous Beds(I) -Adsorbent Fiber Manufactures and Data Handling- (섬유층을 이용한 단백질의 크로마토그래피적 분리에 관한 연구(I) -흡착성 섬유제조 및 자료처리-)

  • 박돈희;박주정
    • KSBB Journal
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    • v.9 no.2
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    • pp.98-103
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    • 1994
  • A bed configuration wherein sheets of modified fibrous polyethylene are potted within a Millipore Filter Cartridge matrix has been developed. Polyethylene fibers form sturdy beds but the native hydrophobicity and inertness of polyethylene have precluded their use in protein chromatography The polyethylene fibers used in this system were modified by plasma oxidation and further derivatization. The resulting fibers are hydrophilic, bind protein reversibly and serve as an anion-exchange stationary phase. Separation of Bovine Serum Albumin on this bed, as well as results of basic studies on capacity and reversibility of binding within a fibrous bed and experimental data handling system are shown.

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Prediction of Chemical Composition and Fermentation Parameters in Forage Sorghum and Sudangrass Silage using Near Infrared Spectroscopy

  • Park, Hyung-Soo;Lee, Sang-Hoon;Choi, Ki-Choon;Kim, Ji-Hye;So, Min-Jeong;Kim, Hyeon-Seop
    • Journal of The Korean Society of Grassland and Forage Science
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    • v.35 no.3
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    • pp.257-263
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    • 2015
  • This study was conducted to assess the potential of using NIRS to accurately determine the chemical composition and fermentation parameters in fresh coarse sorghum and sudangrass silage. Near Infrared Spectroscopy (NIRS) has been increasingly used as a rapid and accurate method to analyze the quality of cereals and dried animal forage. However, silage analysis by NIRS has a limitation in analyzing dried and ground samples in farm-scale applications because the fermentative products are lost during the drying process. Fresh coarse silage samples were scanned at 1 nm intervals over the wavelength range of 680~2500 nm, and the optical data were obtained as log 1/Reflectance (log 1/R). The spectral data were regressed, using partial least squares (PLS) multivariate analysis in conjunction with first and second order derivatization, with a scatter correction procedure (standard normal variate and detrend (SNV&D)) to reduce the effect of extraneous noise. The optimum calibrations were selected on the basis of minimizing the standard error of cross validation (SECV). The results of this study showed that NIRS predicted the chemical constituents with a high degree of accuracy (i.e. the correlation coefficient of cross validation ($R^2{_{cv}}$) ranged from 0.86~0.96), except for crude ash which had an $R^2{_{cv}}$ of 0.68. Comparison of the mathematical treatments for raw spectra showed that the second-order derivatization procedure produced the best result for all the treatments, except for neutral detergent fiber (NDF). The best mathematical treatment for moisture, acid detergent fiber (ADF), crude protein (CP) and pH was 2,16,16 respectively while the best mathematical treatment for crude ash, lactic acid and total acid was 2,8,8 respectively. The calibrations of fermentation products produced poorer calibrations (RPD < 2.5) with acetic and butyric acid. The pH, lactic acid and total acids were predicted with considerable accuracy at $R^2{_{cv}}$ 0.72~0.77. This study indicated that NIRS calibrations based on fresh coarse sorghum and sudangrass silage spectra have the capability of assessing the forage quality control

The Study on the Rapid Screening of Schedule Chemicals in Aqueous Solution Using SPE-ACF (수용액에서 SPE-ACF를 이용한 특정화학물질의 신속 스크리닝 기법 연구)

  • Park, Hoon;Jung, Chang-Hee;Lee, Yong-Han;Hong, Dea-Sik
    • Journal of the Korean Chemical Society
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    • v.52 no.3
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    • pp.239-248
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    • 2008
  • study of the solid phase extraction (SPE) technique using activated carbon fiber (ACF) as a sorbent was carried out on the schedule chemicals in water. 14 different schedule chemicals, which are the hydrolysis products and simulants of chemical agents such as alkylphosphonate, thiodiglycol etc. were selected for the study. Pyridine was used as a promoter to increase the derivatization efficiency, especially to improve silylation of 3-quinuclidinol. To improve the recovery efficiency of amines in the water solution, 1 mL of 5% Et3N/MeOH was introduced into SPE-ACF before the water sample loading. Throughout this study, the optimum condition was established to detect rapidly above chemicals in water.

An Integrated Air Monitoring Approach for Assessment of Formaldehyde in the Workplace

  • Dugheri, Stefano;Bonari, Alessandro;Pompilio, Ilenia;Colpo, Marco;Mucci, Nicola;Arcangeli, Giulio
    • Safety and Health at Work
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    • v.9 no.4
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    • pp.479-485
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    • 2018
  • The aim of this study is to validate an integrated air monitoring approach for assessing airborne formaldehyde (FA) in the workplace. An active sampling by silica gel impregnated with 2,4-dinitrophenylhydrazine, a passive solid phase microextraction technique using O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine as on-fiber derivatization reagent, an electrochemical direct-reading monitor, and an enzyme-based badge were evaluated and tested over a range of 0.020-5.12 ppm, using dynamically generated FA air concentrations. Simple linear regression analysis showed the four methods were suitable for evaluating airborne FA. Personal and area samplings in 12 anatomy pathology departments showed that the international occupational exposure limits in the GESTIS database were frequently exceeded. This monitoring approach would allow a fast, easy-to-use, and economical evaluation of both current work practices and eventual changes made to reduce FA vapor concentrations.