• Title/Summary/Keyword: Residual solvents

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Delignification of Lignocellulosic Biomass with High-Boiling Point Solvent and Acidic Catalyst (고비점 용제와 산 촉매에 의한 목질 바이오매스의 탈리그닌)

  • Kim, Kang-Jae;Jung, Jin-Dong;Jung, Soo-Eun;Hong, Sung-Bum;Eom, Tae-Jin
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.48 no.1
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    • pp.119-126
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    • 2016
  • In this study, we separated the lignin from the wood by using the high boiling point solvent for developing more environmental friendly pulping method. High boiling point solvents as Ethers, glycols and ketones were used to remove the lignin in the pine wood meals. The Yield and lignin content of residual wood meals was reduced according to the input of the catalyst. Me-C, E-Ca, TEG and MIBK had the best delignification rate of 9 kinds of high-boiling point solvents. At the hydrolysis ratio of the selected solvents, The TEG was highest remain ratio of carbohydrates and the E-Ca was lowest remain ratio of lignin. And the Me-C was most excellent lignin hydrolysis ratio at the low catalyst. The selectivity of delignification of Me-C, E-Ca, TEG and MIBK solvents were 49.6, 49.9, 53.8 and 53.1%, respectively, and its values were similar to those of the commercial Kraft Pulp.

Effects of Residual Solvents in the Phase Transition, Transition Enthalpy, and Transition Temperature of Phospholipid Membranes (잔류 유기 용매가 모델 세포 지질막의 상전이, 상전이 엔탈피 및 상전이 온도에 미치는 영향)

  • An, Eun Seol;Choi, Jae Sun;Lee, Dong Kuk
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.40 no.2
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    • pp.163-170
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    • 2014
  • Lipid membranes composed of phosphatidylcholine (PC) are used in biophysical study to mimic cellular membranes and interactions between the membrane and chemicals, where organics solvents are used in dissolving lipids or chemicals. Later, solvents are removed from the solution under nitrogen gas at room temperature, followed by the further removal of the solvent at vacuum condition for several hours. In this process, some solvents are easily removed under described conditions above and others are required more severe conditions. In this study, $^{31}P$ solid-state nuclear magnetic resonance (SSNMR) techniques and differential scanning calorimetry (DSC) were used to see any changes in the line shapes of $^{31}P$ NMR spectra of multilamellar vesicles (MLVs) samples of POPC and in the phase change temperature of multilamellar vesicles (MLVs) of DPPC in DSC thermogram with or without any residual solvents. The thermodynamic parameters associated with the solvents did exhibit noticeable changes depending on solvent types. Thus, it is concluded that solvents should be carefully chosen and removed completely and experimental results should also be interpreted with caution particularly for the experiments investigating lipid phase changes and related topics.

Study on the Development of Simultaneous Analytical Method for the Residual Organic Chloride Pesticides by Gas Chromatography (기체 크로마토그래피를 이용한 유기 염소계 잔류 농약 동시 분석 방법 개발에 관한 연구)

  • Kim, Woo-Seong;Lee, Bong-Hun;Park, Heung-Jai
    • Journal of Environmental Science International
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    • v.5 no.5
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    • pp.561-567
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    • 1996
  • A method for the simultaneous analysis of 31 residual organic chloride pesticides was studied using gas chromatography. Prepared analytical samples were injected to gas chromatography (HP 5890 Series II plus) on the Ultra-2 column with ECD. The packing materials for column were changed as the following reagents ; florisil and alumina N, The residual solution was loaded to column and was elected pith erection solvents ; ether : benzene (2 : 8) solution, hexane : benzene (1 : 1) solution, dichloromethane, acetone, and methanol. The analytical results showed that 6 kinds of organic chlorides were not detected when florisil (first condition) was used as the column packing material. The nondetected 6 kinds of organic chlorides in the first analytical condition were detected and the recoveries of thrin-pesticides were increased, in particular, captan and captafol, but the recoveries of benzene hexachloride compounds were decreased when dichloromethane and methanol were added as elution solvents (pac'king material was florisil as in the first condition). The recoveries of dichlornuanid, chlorofenvinfos, folpet, and dicofol were increased and that of aldrin was increased, but those of captan and captafol were not good when alumina N was used as the packing material. To detect simultaneously thrin-pesticides, captan, and captafol, florisil and alumina N were used as the packing materials. The elution result showed that captan and captafol were not detected. This was because the column was activated insufficiently. The analytical method was the best (31 kinds of organic chlorides in the residual pesticides were detected sharply and showed high sensitivity) when the column (packing materials were florisil and alumina N: together) was fuliy activated and the impurities were removed using various elution solvents.

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Analysis of Residual Solvents of [F-18]FDG Using Gas Chromatography (기체크로마토그래프법을 이용한 [F-18]FDG의 잔류용매 분석)

  • Kim, Dong-Il;Lee, Il-Jung;Kim, Shi-Hwal;Chi, Yong-Gi;Seok, Jae-Dong
    • The Korean Journal of Nuclear Medicine Technology
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    • v.15 no.2
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    • pp.26-29
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    • 2011
  • Purpose: The general test method of the Korean Pharmacopeia specifies the test method on the clauses of quality control after manufacturing. According to KFDA Guidance for Medicines, standards of residual solvents regulates the maximum permissible dose of acetonitrile as 400 ppm, ethanol as 5,000 ppm, and acetic acid as 5,000 ppm. This study aims at identifying the type of resiual solvents in the final [F-18]FDG vial of an automatic synthesizer and measure its residual quantity. Materials and Methods: The center carried out residual solvents test of [F-18]FDG injection using Agilent Technologies 7890A with a Flame Ionization Detector. The column of Agilent Technologies 7890A used in measuring of residual solvents was CP WAX column ($30m{\times}0.53mm{\times}1.0{\mu}m$) and analysis condition was split mode 1:1 at the initial temperature $70^{\circ}C$ which was increased $20^{\circ}C/minute$ after two minutes and maintained at the final $140^{\circ}C$ for two minutes. The analysis method was as following: Firstly, ethanol-acetonitrile-acetic acid mixture was classified into four types of concentration (250-25-250 ppm, 1,000-100-1,000 ppm, 3,000-300-3,000 ppm, and 6,000-600-6,000 ppm), and $1.0{\mu}L$ of each type of concentration was injected into gas chromatography followed by an analysis of its peak domain. Then, a calibration-curve by the external standard method was drawn based on the analysis result. Results: While ethanol and acetonitrile were detected in TRACERlab MX, FASTlab had additional acetic acid. The residual quantity of the ethanol-acetonitrile-acetic acid mixture evaluated using the calibration-curve was average 72 ppm ethanol, 54 ppm acetonitrile, and 1030 ppm acetic acid for FASTlab, whereas average 439 ppm ethanol and 79 ppm acetonitrile for TRACERlab MX. This indicated that both of them were within the maximum permissible dose. Conclusion: Solvent residues in the [F-18]FDG injection were all within maximum permissible doses and proper to be used to examine a patient. The result indicated that types and quantities of solvent resides of radioactive pharmaceuticals vary depending on the automatic synthesizer.

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Purity assignment of 17α-hydroxyprogesterone by mass balance method to establish traceability in measurement

  • Lee, Hwa Shim;Park, Su Jin
    • Analytical Science and Technology
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    • v.32 no.6
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    • pp.225-232
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    • 2019
  • Traceability establishment in chemical measurements is a like a linkage established through an unbroken chain from the measured results to the international system (SI) of units. The primary process for traceability establishment is the purity assignment of a target material to be measured. In this study, we studied the purity assignment of 17α-hydroxyprogesterone (17-OHP). The presence of 17-OHP is indicative of congenital adrenal hyperplasia (CAH) and it builds up due to the deficiency of 21-hydroxylase and 11β-hydroxylase enzyme in the human blood. The purity assignment of 17-OHP was performed by the mass balance method, in which the impurities are categorized into four classes: total related structural impurities, water, residual organic solvents, and nonvolatiles/inorganics. The total related structural impurities were characterized by HPLC-UV; water content was determined by Karl-Fisher coulometer; and the total residual solvents and nonvolatiles/inorganics were determined by TGA. The purity of 17-OHP from a commercial manufacturer was calculated as 993.30 mg/g, and the expanded uncertainty was 0.58 mg/g. The proposed method was validated by uncertainty evaluation and comparing with the actual value of purity.

Ruminant Feed Production from Wood by Steaming-Extraction Method (I) -Effect of Solvent Extraction on Asplund Pulp and Steam Exploded Wood- (증기(蒸氣)-추출(抽出) 방법(方法)에 의한 목질계(木質系)로부터의 조사료(粗飼料) 생산(生産) (I) -용매(溶媒) 추출(抽出)이 폭쇄재(爆碎材) 및 열해섬(熱解纖) 펄프에 미치는 영향(影響)-)

  • Paik, Ki-Hyon;Kang, Chin-Ha;Kim, Dong-Ho
    • Journal of the Korean Wood Science and Technology
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    • v.20 no.4
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    • pp.65-72
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    • 1992
  • Steam defiberated pulp and steam exploded wood(birch chip) were extracted with solvents (hot-water, 1% NaOH, MeOH, hot water, 1% NaOH). The properties of residual fiber were examined for the utilization as ruminants feed. The digestibility is 38% in steam defiberated pulp(10kg /$cm^2$-15min) and 62-77% in exploded wood(17-18kg/$cm^2$-2~10min), respectively. The more steam pressure and time increase, the more the digestibility increase. The sugars obtained from extractives is amount from 7% to 13% in asplund pulp and from 7% to 10% in exploded pulp. The sugars was mainly composed of 70-80% xylose. The digestibility of residual fiber which is extracted with solvents is low than these of original fibers. Considering the yield and digestibility as ruminant feed, exploded pulp under 17kg /$cm^2$ for 10min has the best efficiency. The exploded wood gives 75.3% on yield(O. D. chip) and 48% on the digestibility.

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Analysis of Residual Organic Solvent in Environmentally-friendly Farming Materials with Headspace Method (Headspace 법을 사용한 유기농업자재 중 잔류 유기용매 분석)

  • Choi, Geun Hyoung;Kong, Seung-Heon;Park, Byung-Jun;Moon, Byeong-Cheol;Kim, Jin-Hyo
    • The Korean Journal of Pesticide Science
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    • v.20 no.2
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    • pp.128-132
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    • 2016
  • Volatile organic solvents are used to extract the bioactive materials from raw materials for environmentally-friendly farming materials (EFFM), but the solvent should not remain in EFFM for the safety reasons. Thus qualitative and quantitative analysis method for the solvents using Headspace-GC were evaluated. Water content depleted the detection ratio of hydrophilic solvents and disturbing the hydrophilic interaction with solvents by DMSO might be helped to increase the detection ratio (up to 715%). Surfactant concentration affected to the detection ratio (68.5-179.1%) while surfactant type was not deeply involved the solvent detection. On the other hand, matrix-matched calibration method was accepted the minimum requirements for the quantitative analysis of the solvents in EFFM.

Preparation of New Polyenaminonitriles Containing Cyclic and Methylene Units and Their Thermal Properties

  • Cho, Jeong-Hyun;Gong, Myoung-Seon
    • Macromolecular Research
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    • v.8 no.5
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    • pp.209-214
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    • 2000
  • Polyenaminonitriles containing cycloaliphatic and aliphatic units were prepared by interfacial or solution polymerization reaction of p-bis(1-chloro-2,2-dicyanovinyl) benzene (1) with 4-aminobenzyl-amine, 1-(2-aminoethyl)piperazine, 2-(aminomethyl)pyrrolidine and 4-(aminomethyl)piperidine. The chemical structure of the polymers was confirmed through a syntheses of the model compound. The resulting polymers possessed inherent viscosities of 0.29∼0.62 dL/g and they were easily soluble in polar aprotic solvents and common organic solvents. Thermal properties of the polymers such as curability and stability were studied by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and infrared spectroscopy. The polymers exhibited a large exotherm in DSC analyses and underwent a curing reaction around 340-370$\^{C}$ to form insoluble materials. The polymers showed 70-80% residual weight at 600 $\^{C}$ under nitrogen.

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Preparation of Polyesters Containing Enaryloxynitrile Moiety and Their Thermal Properties

  • Moon Sung-Hee;Lee Seung-Jae;Kim Jin-Bong;Gong Myoung-Seon
    • Bulletin of the Korean Chemical Society
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    • v.15 no.12
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    • pp.1089-1093
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    • 1994
  • Polyesters containing enaryloxynitriles moiety have been newly prepared from p-bis[1-[4-(3-hydroxypropyl)phenoxy]-2,2-dicyano vinyl]benzene (3) and common diols with terephthaloyl chloride. The copolyesters have a good solubility in common organic solvents as well as polar aprotic solvents. They undergo a curing reaction at around 350 $^{circ}C$ and show a 50-60${\%}$ of residual weight at 500 $^{circ}C$. The enhanced thermal stabilities were due to the intramolecular cyclization or intermolecular cross-linking reaction of the dicyanovinyl group incorporated into polyester by copolymerization.