• Title/Summary/Keyword: Particle separation process

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Full validation of high-throughput bioanalytical method for the new drug in plasma by LC-MS/MS and its applicability to toxicokinetic analysis

  • Han, Sang-Beom
    • Proceedings of the Korean Society of Toxicology Conference
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    • 2006.11a
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    • pp.65-74
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    • 2006
  • Modem drug discovery requires rapid pharmacokinetic evaluation of chemically diverse compounds for early candidate selection. This demands the development of analytical methods that offer high-throughput of samples. Naturally, liquid chromatography / tandem mass spectrometry (LC-MS/MS) is choice of the analytical method because of its superior sensitivity and selectivity. As a result of the short analysis time(typically 3-5min) by LC-MS/MS, sample preparation has become the rate- determining step in the whole analytical cycle. Consequently tremendous efforts are being made to speed up and automate this step. In a typical automated 96-well SPE(solid-phase extraction) procedure, plasma samples are transferred to the 96-well SPE plate, internal standard and aqueous buffer solutions are added and then vacuum is applied using the robotic liquid handling system. It takes only 20-90 min to process 96 samples by automated SPE and the analyst is physically occupied for only approximately 10 min. Recently, the ultra-high flow rate liquid chromatography (turbulent-flow chromatography)has sparked a huge interest for rapid and direct quantitation of drugs in plasma. There is no sample preparation except for sample aliquotting, internal standard addition and centrifugation. This type of analysis is achieved by using a small diameter column with a large particle size(30-5O ${\mu}$m) and a high flow rate, typically between 3-5 ml/min. Silica-based monolithic HPLC columns contain a novel chromatographic support in which the traditional particulate packing has been replaced with a single, continuous network (monolith) of pcrous silica. The main advantage of such a network is decreased backpressure due to macropores (2 ${\mu}$m) throughout the network. This allows high flow rates, and hence fast analyses that are unattainable with traditional particulate columns. The reduction of particle diameter in HPLC results in increased column efficiency. use of small particles (<2 urn), however, requires p.essu.es beyond the traditional 6,000 psi of conventional pumping devices. Instrumental development in recent years has resulted in pumping devices capable of handling the requirements of columns packed with small particles. The staggered parallel HPLC system consists of four fully independent binary HPLC pumps, a modified auto sampler, and a series of switching and selector valves all controlled by a single computer program. The system improves sample throughput without sacrificing chromatographic separation or data quality. Sample throughput can be increased nearly four-fold without requiring significant changes in current analytical procedures. The process of Bioanalytical Method Validation is required by the FDA to assess and verify the performance of a chronlatographic method prior to its application in sample analysis. The validation should address the selectivity, linearity, accuracy, precision and stability of the method. This presentation will provide all overview of the work required to accomplish a full validation and show how a chromatographic method is suitable for toxirokinetic sample analysis. A liquid chromatography/tandem mass spectrometry (LC-MS/MS) method developed to quantitate drug levels in dog plasma will be used as an example of tile process.

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A Feasibility Study on the Utilization of by-Product Sludge Generated from Waste Concrete Recycling Process (폐 콘크리트 재생순환자원 부산물 슬러지의 활용 기초연구)

  • Shin, Hee-young;Ji, Sangwoo;Woo, Jeong-youn;Ahn, Gi-oh;An, Sang-ho
    • Resources Recycling
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    • v.25 no.3
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    • pp.29-36
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    • 2016
  • The characteristics analysis and pH neutralization test were carried out to use of slurry generated from recycling processes of construction wastes. D (5.0) of raw sludge was $42.4{\mu}m$ and over 60 % of sludge distribute under 45 um (-325 mesh). Muscovite and carbonate minerals were main minerals of fine particles, and the portion of carbonate minerals increased as particle size decreased. Although the more heavy metals were observed in the finer particle size, the contents was found to be less than Korean contaminated soil regulation (area 2). The effects of flocculants addition for accelerating solid-liquid separation were negligible because the slurry already contains excess of coagulant added in the waste concrete recycling process. It was difficult to neutralize the sludge supernatant due to high pH (about 12) by adding acids, but the introduction of $CO_2$ decreased the pH to 8.5, The precipitate recovered during $CO_2$ introduction was determined to be $CaCO_3$ with XRD, and it indicates that high pure $CaCO_3$ could be obtained during the process.

Breakage and Surface Oxidation Characteristics of Waste NdFeB Magnet for Recycling (NdFeB 자석 재활용을 위한 파분쇄 및 그에 따른 표면 산화 특성 연구)

  • Kim, Kwanho;Kim, Gahee;Lee, Hoon;Kang, Jungshin
    • Resources Recycling
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    • v.28 no.3
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    • pp.26-34
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    • 2019
  • Due to the increasing demand of rare earth magnet for various application, it is predicted that the amount of waste rare earth magnet will increase sharply. The process of waste rare earth magnet recycling is mainly consisted of leaching and separation of rare earth element contained in the magnet. However, there is no study on the breakage characteristics of the waste rare earth magnet for production of magnet powder. Therefore, in this study, effective crushing/grinding process and breakage characteristics were investigated for waste rare earth magnet. In the case of jaw crusher, the particle size of magnet was effectively reduced without rapid oxidation. In ball mill grinding test, it was found that the grinding process was not performed properly at the early stage of grinding. Moreover, waste rare earth magnet showed very low specific rate of breakage(S) and high fraction of fine particle breakage distribution(B) compared to ordinary minerals. These results can be used as a basic data for developing crushing/grinding circuit of waste rare earth magnet.

Characteristics of Filtration Treatment Using Diatomite Filter Aids for Sewage Water Reuse (하수처리수 재이용을 위한 가압식 규조토 여과의 처리성능평가)

  • Lim, Byung Ran;Kim, Hee Seo;Go, Yeon Sil;Kim, Hyun Kab;Kim, Jong Hak;Lee, Tae Jin
    • Journal of Korean Society on Water Environment
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    • v.35 no.2
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    • pp.145-151
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    • 2019
  • The purpose of this study was to investigate treatment characteristics of diatomite filtration, that would allow water recovery from biologically-treated effluent for reuse. Diatomite, Celpure 100, and acid clay were used as filter-aids, with a support filter manufactured from polyethylene (PE), and polypropylene (PP). This pre-coating process using diatomite filter-aids, is used in the filtration range of pressure filters, and has consistently provided high-quality separation. The results showed that variations in average removal efficiency of SS, and T-P from biologically treated effluent by the diatomite-coated PE filter, were approximately 82.2 ~ 88.9 % and 4.8 ~ 21.1 %, respectively. T-P treatment efficiency of the PP filter pre-coated with diatomite and $Celpure^{(R)}100$ at $57.64g/m^2$, was approximately $24{\pm}10%$ and $40{\pm}15%$ on average, respectively. Particle size distribution of secondary effluent varied from 0.05 to $200{\mu}m$, and $d_{50}$ value was $20.76{\mu}m$. The size distribution of particles in the diatomite filtrate ranged from 1.26 to $101.1{\mu}m$ when pre-coated with diatomite filter-aid, at a content of $57.64g/m^2$. Diatomite filter aids, i.e., the particles that form the pre-coating layer, capture very fine particles as well as macromolecules, owing to their complex structure with numerous fine microscopic pores, and surface properties. The filtration process using diatomite and $Celpure^{(R)}100$ as filter aids, has been successfully applied, to recover water from sewage for reuse. The disadvantage of the process, is that the particle size of the filter-aid is spent, because of pressurization.

Comparative analysis of two methods of laser induced boron isotopes separation

  • K.A., Lyakhov;Lee, H.J.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.02a
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    • pp.407-408
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    • 2011
  • Natural boron consists of two stable isotopes 10B and 11B with natural abundance of 18.8 atom percent of 10B and 81.2 atom percent of 11B. The thermal neutron absorption cross-section for 10B and 11B are 3837 barn and 0.005 barn respectively. 10B enriched specific compounds are used for control rods and as a reactor coolant additives. In this work 2 methods for boron enrichment were analysed: 1) Gas irradiation in static conditions. Dissociation occurs due to multiphoton absorption by specific isotopes in appropriately tuned laser field. IR shifted laser pulses are usually used in combination with increasing the laser intensity also improves selectivity up to some degree. In order to prevent recombination of dissociated molecules BCl3 is mixed with H2S 2) SILARC method. Advantages of this method: a) Gas cooling is helpful to split and shrink boron isotopes absorption bands. In order to achieve better selectivity BCl3 gas has to be substantially rarefied (~0.01%-5%) in mixture with carrier gas. b) Laser intensity is lower than in the first method. Some preliminary calculations of dissociation and recombination with carrier gas molecules energetics for both methods will be demonstrated Boron separation in SILARC method can be represented as multistage process: 1) Mixture of BCl3 with carrier gas is putted in reservoir 2) Gas overcooling due to expansion through Laval nozzle 3) IR multiphoton absorption by gas irradiated by specifically tuned laser field with subsequent gradual gas condensation in outlet chamber It is planned to develop software which includes these stages. This software will rely on the following available software based on quantum molecular dynamics in external quantized field: 1) WavePacket: Each particle is treated semiclassicaly based on Wigner transform method 2) Turbomole: It is based on local density methods like density of functional methods (DFT) and its improvement- coupled clusters approach (CC) to take into account quantum correlation. These models will be used to extract information concerning kinetic coefficients, and their dependence on applied external field. Information on radiative corrections to equation of state induced by laser field which take into account possible phase transition (or crossover?) can be also revealed. This mixed phase equation of state with quantum corrections will be further used in hydrodynamical simulations. Moreover results of these hydrodynamical simulations can be compared with results of CFD calculations. The first reasonable question to ask before starting the CFD simulations is whether turbulent effects are significant or not, and how to model turbulence? The questions of laser beam parameters and outlet chamber geometry which are most optimal to make all gas volume irradiated is also discussed. Relationship between enrichment factor and stagnation pressure and temperature based on experimental data is also reported.

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Change of Calcium Carbonate Crystal Size at steady state in CMSMPR(Continuous Mixed Suspension Mixed Produce Removal) Crystallizer (연속식결정화기 정상상태에서 탄산칼슘 결정크기 변화)

  • Han, Hyun Kak
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.18 no.7
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    • pp.714-719
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    • 2017
  • The controlled synthesis of inorganic materials with a specific size and morphology is an important factor in the development of new materials in many fields, such as nanoparticles, medicine, electronics, semiconductors, pharmaceutical sand cosmetics. Solution crystallization is one of the most widely used separation processes in the chemical and pharmaceutical industries. Calcium carbonate has attracted a great deal of attention in industry because of its numerous applications. The mean crystal size, crystal size distribution and morphology are important factors in the continuous crystallization process. In this study, the continuous crystallization of calcium carbonate by the calcium chloride process was investigated. The mean crystal size and crystal size distribution data were obtained by a particle size analyzer. The morphological imaging of the crystalswasper formed by SEM. Under steady state operation, the mean crystal size change was small, but increasing the input concentration and mixing rate increased the crystal size. In this operation, some aragonite was found, but the main crystal phase was calcite.

Solution-Processed Inorganic Thin Film Transistors Fabricated from Butylamine-Capped Indium-Doped Zinc Oxide Nanocrystals

  • Pham, Hien Thu;Jeong, Hyun-Dam
    • Bulletin of the Korean Chemical Society
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    • v.35 no.2
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    • pp.494-500
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    • 2014
  • Indium-doped zinc oxide nanocrystals (IZO NCs), capped with stearic acid (SA) of different sizes, were synthesized using a hot injection method in a noncoordinating solvent 1-octadecene (ODE). The ligand exchange process was employed to modify the surface of IZO NCs by replacing the longer-chain ligand of stearic acid with the shorter-chain ligand of butylamine (BA). It should be noted that the ligand-exchange percentage was observed to be 75%. The change of particle size, morphology, and crystal structures were obtained using a field emission scanning electron microscope (FE-SEM) and X-ray diffraction pattern results. In our study, the 5 nm and 10 nm IZO NCs capped with stearic acid (SA-IZO) were ligand-exchanged with butylamine (BA), and were then spin-coated on a thermal oxide ($SiO_2$) gate insulator to fabricate a thin film transistor (TFT) device. The films were then annealed at various temperatures: $350^{\circ}C$, $400^{\circ}C$, $500^{\circ}C$, and $600^{\circ}C$. All samples showed semiconducting behavior and exhibited n-channel TFT. Curing temperature dependent on mobility was observed. Interestingly, mobility decreases with the increasing size of NCs from 5 to 10 nm. Miller-Abrahams hopping formalism was employed to explain the hopping mechanism insight our IZO NC films. By focusing on the effect of size, different curing temperatures, electron coupling, tunneling rate, and inter-NC separation, we found that the decrease in electron mobility for larger NCs was due to smaller electronic coupling.

Hydrogneation and Electrochemical Characteristics of Gas-atomized Zr-based $AB_2$ Hydride for Ni-MH Secondary Battery (기체분무형 공정으로 제조된 Zr계 금속수소화물의 수소화반응 및 Ni-MH 2차전지 전극 특성에 관한 연구)

  • Kim, Jin-Ho;Hwang, Kwang-Taek;Kim, Byung-Kwan;Han, Jeong-Seb
    • Journal of Hydrogen and New Energy
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    • v.20 no.6
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    • pp.505-511
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    • 2009
  • The hydriding and electrochemical characteristics of Zr-based $AB_2$ alloy produced by gas atomization have been extensively examined. For the particle morphology of the as-cast and gas-atomized powders, it can be seen that the mechanically crushed powders are irregular, while the atomized powder particles are spherical. The increase of jet pressure of gas atomization process results in the decrease of hydrogen storage capacity and the slope of plateau pressure significantly increases. TEM and EDS studies showed the increase of jet pressure in the atomization process accelerated the phase separation within grain of the gas-atomized alloy, which brought about a poor hydrogenation property. However, the gas-atomized $AB_2$ alloy powders produced by jet pressure of 50 bar kept up the reversible $H_2$ storage capacity and discharge capacity similar to the mechanically crushed particles. In addition, the electrode of gas-atomized Zr-based $AB_2$ alloy of 50 bar showed improved cyclic stability over that of the cast and crushed particulate, which is attributed to the restriction of crack propagation by grain boundary and dislocation with ch/discharging cycling.

Process gas purification using cyclone recirculation and cooling process (싸이클론 재순환, 냉각공정을 이용한 공정가스 정제 연구)

  • Kim, Ju-Hoe;Jo, Woo-Jin;Choi, Young-Tae;Jo, Young-Min;Kim, Sang-Bum
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.19 no.1
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    • pp.25-33
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    • 2018
  • Renewable energy has been of interests in the area of modern alternative fuels. Biogas is produced in waste landfill sites through anaerobic digestion processes, including hydrolysis, acidogenesis, organic acid fermentation (acetogenesis), and methane fermentation (methanogenesis). High contents of fine dust and moisture limited its utilization for direct combustion, town gas and vehicle fuel. Thus, this study proposed a new design for a cooling device using a centrifugal cyclone for simultaneous removal of fine dust and moisture as a pretreatment in the purification processes. A heat exchanger and an ID fan, which are installed inside and outside of the cyclone, in order to cool the humid gas below the freezing point and form a foggy mist. Such an atmosphere enhanced to capture fine dust as recirculating the cold mist flow. The water removal rate was 80.8% at a relative humidity of 95%, and the particle removal efficiency was 98.3% for $2.5{\mu}m$. Simultaneous removal efficiency was 70.8% and 99.6% for particle and moisture respectively.

A Study on the Cobalt and Lithium Recovery from the Production Scraps of Lithium Secondary Battery by High Efficient and Eco-friendly Method (이차전지(二次電池) 제조공정(製造工程)스크랩으로부터 고효율(高效率) 親環境(친환경) 코발트(Co)와 리튬(Li)의 회수(回收)에 관(關)한 연구(硏究))

  • Lee, Jeong-Joo;Chung, Jin-Do
    • Resources Recycling
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    • v.19 no.6
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    • pp.51-60
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    • 2010
  • A study on the recovery of cobalt and lithium from Lithium Ion Battery(LIB) scraps has been carried out by a physical treatment - leaching - solvent extraction process. The cathode scraps of LIB in production were used as a material of this experiment. The best condition for recovering cobalt from the anode scraps was acquired in each process. The cathode scraps are dissolved in 2M sulfuric acid solution with hydrogen peroxide at $95^{\circ}C$, 700 rpm. The cobalt is concentrated from the leaching solution by means of a solvent extraction circuit with bis(2-ethylhexyl) phosphoric acid(D2EHPA) and PC88A in kerosene, and then cobalt and lithium are recovered as cobalt hydroxide and lithium carbonate by precipitation technology. The purity of cobalt oxide powder was over 99.98% and the average particle size after milling was about 10 lim. The over all recoveries are over 95% for cobalt and lithium. The pilot test of mechanical separation was carried out for the recovery of cobalt from the scraps. The $Co_3O_4$ powder was made by the heat treatment of $Co(OH)_2$ and the average particle size was about 10 ${\mu}m$ after grinding. The recovery was over 99% for cobalt and lithium each other and the purity of cobalt oxide was over 99.98%.