• Title/Summary/Keyword: Multi-step purification

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Influence of Functionalization on Physicochemical Properties of Multi-walled Carbon Nanotubes/Epoxy Matrix Nanocomposites

  • Seo, Min-Kang;Park, Soo-Jin
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.124-128
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    • 2009
  • In this study, the effect of multi-step purification or functionalization on physicochemical properties of multi-walled carbon nanotubes (MWNTs)/epoxy (EP) nanocomposites was investigated. The nanocomposites containing multi-step purified MWNTs showed a stronger influence on $T_g$ and increased in mechanical properties in comparison to nanocomposites containing the same amount of only purified MWNTs. Consequently, the multi-step purification of MWNTs led to an improvement of thermomechanical properties of nanocomposites, resulting from improving the intermolecular interaction of MWNTs in epoxy matrix resins.

Mineralogical Analysis and Mechano-Chemical Purification of Natural Silica Ore for High Purity Silica Powder

  • Park, Jesik;Lee, Churl Kyoung;Lee, Hyun-Kwon
    • Korean Journal of Materials Research
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    • v.26 no.6
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    • pp.306-310
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    • 2016
  • To produce 4N grade high-purity silica powder from natural ore, the mineralogical characteristics of natural silica ore were investigated and their effects on the purification process were revealed. The Chinese silica mineral ore used was composed of iron and aluminum as main impurities and calcium, magnesium, potassium, sodium, and titanium as trace impurities; these trace impurities generally exist as either single oxides or complex oxides. It was confirmed that liberation and acidic washing of the impurities were highly dependent on the particle size of the ground silica ore and on its mineralogical characteristics such as the distribution and phases of existing impurities. It is suggested that appropriate size reduction of silica ore should be realized for optimized purification according to the origin of the natural silica ore. A single step purification process, the mechano-chemical washing (MCW) process, was proposed and verified in comparison with the conventional multi step washing process.

Method for the Detection of Mutagenicity of Fried Fish (고온가열된 어류의 돌연변이성 검색을 위한 시료 추출방법)

  • 이은주;반경녀;이영근;심기환;하영래
    • Environmental Mutagens and Carcinogens
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    • v.15 no.2
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    • pp.106-114
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    • 1995
  • A method was developed to detect total mutagenicity of fried fish for S. typhimurium TA98, using Ames assay. Method described herein circumvented problems associated with the sample preparation for Ames assay, i.e., a multi-purification step of sample and interference with solvent residuals. Experiment A, the best method developed in the present study, consisted of two important steps: pH adjustment of the aqueous sample solution from fried fish samples to remove impurities, and simultaneous distillation extraction (SDE) for partially purified samples to remove volatile compounds from solvents. The procedure and results were described as below. Fillet of gizzard shad (Konosirus punctatus) fish sample fried for 10 min each side on the temperature-controlled fry-pan (210$\circ$C) was homogenized in an aqueous acidic solution (pH 2) with a homogenizer, followed by filtration through Celite. The tiltrate (pH 2), removed some impurities by extraction with chloroform:methanol (2:1, v/v) mixture, was adjusted pH to 10 and then centrifuged to remove precipitate. The ethylacetate extract from the tiltrate of pH 10 was rotoevaporated and purified by SDE apparatus for 2 hours. Experiment A revealed significantly higher revertants (1928 per 25 g fried sample) than other Experiment (B, C, or D) tested. Experiment A gave good results in the mutagenicity test of fried fish sample with few purification steps using only 25 g fried sample and 650 ml of solvents; and thus this method could be a useful tool for the screening the mutagenicity or antimutagenicity of other foods as well.

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The Vertical Alignment of CNTs and Ni-tip Removal by Etching at ICPHFCVD (ICPHFCVD에 의한 탄소나노튜브의 수직 배향과 에칭을 이용한 Ni-tip의 제거)

  • 김광식;장건익;장호정;류호진
    • Journal of the Microelectronics and Packaging Society
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    • v.9 no.4
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    • pp.55-60
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    • 2002
  • This paper presents a technique for the preparation of vertically grown CNTs by ICPHFCVD(inductively coupled plasma hot filament chemical vapor deposition) below $580^{\circ}C$. Purification of the CNTs(carbon nanotubes) using RE(radio frequency) plasma in a one step process, based on the different etching property of the Ni-tip, amorphous carbon and carbonaceous materials is also discussed. After purifying the grown materials. CNTs shown the multi walled and hollow typed structure. The typical outer and inner diameters or CNT were 50 nm and 25 nm, respectively. The graphitic wall was composed of 82 layers and the distance between wall and wall was 0.34 nm. From the results of TEM observation, the Ni catalyst at the tip of the carbon nanotubes were effectively removed by using a RF plasma etching, continuously.

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In-Vitro Refolding of PEGylated Lipase (PEGylation된 Lipase의 In-Vitro 재접힘)

  • Kim, Min-Young;Kwon, Jin-Sook;Lee, Eun-Kyu
    • KSBB Journal
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    • v.20 no.5 s.94
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    • pp.338-340
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    • 2005
  • Covalent modification of a protein with polyethylene glycol (PEG) has become one of the most widely used and well established drug enhancement strategies in the biopharmaceutical industry. The general benefits enjoyed by PEGylation, such as prolonged serum half-lives or reduced immunogenicity in vivo, are well known. By now the PEGylation process has been performed with purified proteins, and it is required to recover the desired PEGylate by a multi-step purification process. The ultimate aim of our research is to develop an integrated process of PEGylation and in vitro refolding starting with inclusion body material. For this, we investigated the feasibility that a protein could be PEGylated under a denaturing condition and also the PEGylated proteins could be refolded correctly. Using lipase as a model protein, we found that it was PEGylated in the presence of 8M urea and that the PEG molecules covalently attached to lipase did not appear to hinder its refolding.

Solid-phase PEGylation for Site-Specific Modification of Recombinant Interferon ${\alpha}$-2a : Process Performance, Characterization, and In-vitro Bioactivity (재조합 인터페론 알파-2a의 부위 특이적 수식을 위한 고체상 PEGylation : 공정 성능, 특성화 및 생물학적 활성)

  • Lee, Byung-Kook;Kwon, Jin-Sook;Lee, E.K.
    • KSBB Journal
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    • v.21 no.2
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    • pp.133-139
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    • 2006
  • In 'solid-phase' PEGylation, the conjugation reaction occurs as the proteins are attached to a solid matrix, and thus it can have distinct advantages over the conventional, solution-phase process. We report a case study: rhIFN-${\alpha}$-2a was first adsorbed to cation exchange resin and then N-terminally PEGylated by aldehyde mPEG of 5, 10, and 20 kD through reductive alkylation. After the PEGylation, salt gradient elution efficiently recovered the mono-PEGylate in a purified form from the unwanted species such as unmodified IFN, unreacted PEG, and others. The mono-PEGylation and its purification were integrated in a single chromatographic step. Depending on the molecular weight of the mPEG aldehyde used, the mono-PEGylation yield ranged 50-64%. We could overcome the major problems of random, or uncontrollable, multi-PEGylation and the post-PEGylation purification difficulties associated with the solution-phase process. N-terminal sequencing and MALDI-TOF MS confirmed that a PEG molecule was conjugated only to the N-terminus. Compared with the unmodified IFN, the mono-PEGylate showed the reduced anti-viral activity as measured by the cell proliferation assay. The bioactivity was reduced more as the higher molecular weight PEG was conjugated. Immunoreactivity, evaluated indirectly by antibody binding activity using a surface plasmon resonance biosensor, also decreased. Nevertheless, trypsin resistance as well as thermal stability was considerably improved.

Evaluation of accuracy for measurement of Dioxins (PCDDs/PCDFs) by using certified reference material (CRM) (인증표준물질(Certified reference materials, CRM)을 이용한 이옥신류(PCDDs/PCDFs) 측정의 정확도 평가)

  • Youn, Yeu Young;Park, Deok Hie;Lim, Young Hee;Cho, Hye Sung
    • Analytical Science and Technology
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    • v.22 no.5
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    • pp.376-385
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    • 2009
  • In our study, the accuracy for measurement of seventeen 2,3,7,8-substituted PCDDs/PCDFs in certified reference material (CRM) which is the sample of homogeneous sediment matrix taken from an area known to have significant chemical contamination, particularly PCBs (polychlorinated biphenyls), was evaluated. Though the methodology in this study followed the official method of unintentionally produced persistent organic pollutants (UPOPs) announced by the Ministry of Environment of the Republic of Korea in 2007, there were slight changes using additional purification step by activated carbon column because the interferences of sample were not sufficiently removed when only multi-silica column and alumina column have been used for purification. The |En| number proposed by the Korea Research Institute of Standards and Science was used for a valuation basis of the accuracy. The |En| numbers of seventeen 2,3,7,8-substituted PCDDs/PCDFs have been indicated as 1 and below, they were decided "Pass" in this test, when DB-5MS column and SP-2331 column were used together. Because 1,2,3,7,8-PeCDD and #169-HxCB were not separated on DB-5MS column, the ions of 1,2,3,7,8-PeCDD were selected at M/M+2 instead of M+2/M+4 suggested by EPA 1613. It is possible to distinguish them in HRGC/HRMS analysis.

Development of Miniaturized Automatic Chromatography System for validation Study of Chromatographic Resin lifetime (크로마토그래피 담체의 수멍을 검증하기 위한 자동화 미니 크로마토그래피 시스템 개발)

  • 박재하;서창우
    • KSBB Journal
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    • v.17 no.4
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    • pp.326-332
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    • 2002
  • The quality of biopharmaceutical proteins is strongly affected by a manufacturing process employed to produce Et, and thus validation of the manufacturing bioprocess is a very important issue. Chromatography is probably the most widely used bioprocess unit operation for protein purification. In this study, a miniaturized automatic chromatography system was designed and constructed for scale-down studies for process chromatography validation. This system, named MiniValChrom, has the following features: automatic and repeated operation, flexible sequences and intervals among the steps, on-line and real-time monitoring and control, method files savings, etc. Using the MiniValChrom, we peformed a case study of an abbreviated experiment to estimate chromatographic resin lifetime. BSA (bovine serum albumin) and Cibacron Blue 3G-A were used as the model protein and the resin, respectively. The resin deterioration was evaluated by determining and monitoring the HETP and NTP values from the chromatograms every 5 cycles. It was observed that the HETP and the NTP values were changed by 9% after 15 cycles. The resin lifetime validation could be completed by repeating this experiment until the HETP value reached a predetermined value. The MiniValChrom's concept and the protocol suggested in this study can serve as a rapid and economical tool for the validation studies of bioprocess chromatography system.

A Study on the Applicability of Soilremediation Technology for Contaminated Sediment in Agro-livestock Reservoir (농축산저수지 오염퇴적토의 토양정화기술에 대한 적용성 연구)

  • Jung, Jaeyun;Chang, Yoonyoung
    • Journal of Environmental Impact Assessment
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    • v.29 no.3
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    • pp.157-181
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    • 2020
  • Sediments from rivers, lakes and marine ports serve as end points for pollutants discharged into the water, and at the same time serve as sources of pollutants that are continuously released into the water. Until now, the contaminated sediments have been landfilled or dumped at sea. Landfilling, however, was expensive and dumping at sea was completely banned due to the London Convention. Therefore, this study applied contaminated sedimentation soil of 'Royal Palace Livestock Complex' as soil purification method. Soil remediation methods were applied to pretreatment, composting, soil washing, electrokinetics, and thermal desorption by selecting overseas application cases and domestically applicable application technologies. As a result of surveying the site for pollutant characteristics, Disolved Oxigen (DO), Suspended Solid (SS), Chemical Oxygen Demand (COD), Total Nitrogen (TN), and Total Phosphorus (TP) exceeded the discharged water quality standard, and especially SS, COD, TN, and TP exceeded the standard several tens to several hundred times. Soil showed high concentrations of copper and zinc, which promote the growth of pig feed, and cadmium exceeded 1 standard of Soil Environment Conservation Act. In the pretreatment technology, hydrocyclone was used for particle size separation, and the fine soil was separated by more than 80%. Composting was performed on organic and Total Petroleum Hydrocarbon (TPH) contaminated soils. TPH was treated within the standard of concern, and E. coli was analyzed to be high in organic matter, and the fertilizer specification was satisfied by applying the optimum composting conditions at 70℃, but the organic matter content was lower than the fertilizer specification. As a result of continuous washing test, Cd has 5 levels of residual material in fine soil. Cu and Zn were mostly composed of ion exchange properties (stage 1), carbonates (stage 2), and iron / manganese oxides (stage 3), which facilitate easy separation of contamination. As a result of applying acid dissolution and multi-stage washing step by step, hydrochloric acid, 1.0M, 1: 3, 200rpm, 60min was analyzed as the optimal washing factor. Most of the contaminated sediments were found to satisfy the Soil Environmental Conservation Act's standards. Therefore, as a result of the applicability test of this study, soil with high heavy metal contamination was used as aggregate by applying soil cleaning after pre-treatment. It was possible to verify that it was efficient to use organic and oil-contaminated soil as compost Maturity after exterminating contaminants and E. coli by applying composting.