Proceedings of the Korean Society of Toxicology Conference
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2006.11a
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pp.65-74
/
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.
An apparatus was made for the electrodeposition of alpha emitting actinide nuclides, $^{207}Bi$ and $^{210}Po$. The electrodeposition was made on a polished stainless steel plate cathode. The anode was made of platinum wire and to stir the solution. With the ammonium chloride as electrolyte initial pH = 4, chloride concentration = 0.6M and solution volume = 15ml, a current of 1.5 ampere(current density = 0.59A/$cm^2$) was flowed for 100 minutes for the quantitative recovery of electrodeposition and on average recovery of 98.3% was obtained within ${\pm}$0.7% uncertainty. Alpha spectrometry of the electrodeposited sample showed alpha peaks from $^{210}Po, ^{234}U$ and $^{239}Pu$ having energy resolution (FWHM) of 18.3, 21.8 and 36.0 keV respectively. The electrodeposition and alpha spectrometry for a natural uranium sample of domestic origin gave $^{238}U : ^{234}U = 1 : 6.1{\times}10^{-5}$ and for a neutron-irradiated uranium sample did $^{238}U : ^{239}Pu : ^{241}Am = 100 : 0.0263 : 5.20{times}10^{-5}$. The result of $^{238}U$ determination in the irradiated sample by electrodeposition-alpha spectrometry was in accord within ${\pm}1.6%$ of relative error with the results of solid fluorimetry and mass spectrometry. For $^{239}Pu$ the result of electrodeposition-alpha spectrometry was in accord within ${\pm}$4.0% of relative error with the results of anion exchange separation and the thenoyltrifluoroacetone(TTA) extraction both followed by alpha spectrometries.
The deterioration and structural damage such as exfoliation, cracks, and separation of painted layer on the wall paintings of Maitreya Hall in Geumsan-sa temple have been accelerated since it was re-positioned to the original place after the dismantling from the building in 1993. The examination of which result and analysis described in this study, is a preliminary survey for establishing conservation plan of the wall paintings. It aimed at the understanding of the physical and chemical characteristics of the materials applied in the 1993 conservation. The research focused on the south walls which displayed the worst condition compared to other walls. Samples for the examination for the understanding of micro-structure, chemical composition, cristalisation, and particle distribution, were collected for finishing, middle, and consolidated layers of the walls between pillars and the ones between brackets. Those samples were collected from separated fragments of the walls. The sample analysis displayed that: 1. the 1993 conservation used the similar type of weathered soil as the original for the finishing layer, and such soil and sand for the middle layer; 2. those walls are composed of a group of mineral particles which are relatively equal in size and shape and in their distribution; 3. the mineral particles were cohered forming solid aggregate due to the application of acrylic resin for the reinforcement on the wall. The main composition of crystalisation on the first and the second reinforcement layers of the back walls were lime plaster ($CaSO_4{\cdot}2H_2O$). The overall examination confirmed that the priority of the future conservation treatment should be given to the removal of the first and the second layers of reinforcement and the treatment on the back walls which were partially consolidated.
Purple sweet potato pigment extract was concentrated using both membrane separation method and vacuum concentration method. The pigment extract (anthocyanin content 1.6 g/L) was concentrated $({\times}25)$ after 5 hr of continuous operation of a nanofiltration to get anthocyanin content of 10.6 g/L. Total solid content also increased continuously while the flux decreased continuously during the concentration process. Degradation index (DI) changes of concentrated pigment solution were insignificant during the whole concentration process which is indicating that the nanofiltration method does not affect color degradation of anthocyanin pigment. For the comparison test, the same pigment extract was concentrated using a rotary vacuum evaporator at temperatures of 40 and $60^{\circ}C$. At both temperatures, pigment content increased in a similar manner during concentration $({\times}5)$. However, DI value at $60^{\circ}C$ increased while that at $40^{\circ}C$ did not change appreciably. Total color difference value changed only slightly by nanofiltration and $40^{\circ}C$ while changed significantly by $60^{\circ}C$. These indicate that a membrane filtration method is more effective in concentrating purple sweet potato pigment extract than a vacuum concentration method by high temperature.
This study was carried out to estimate the performance of modified sequencing batch reactor (SBR) process by the application of SBR process for small advanced wastewater treatment plant. Organic, nitrogen and phosphorus were able to remove in the unit reactor by SBR process and it would be able to select the suitable operation method. The plant was operated to achieve high performance with influent control, optimum anoxic/oxic condition using intermediate aeration method, and solid (sludge) /liquid (effluent) separation by modified decanter. The optimum operating mode was 3Cycles a day and intermediate input and aeration. Under these conditions, the treatment efficiencies were good with 60% of designed flow rate and low influent quality. When the influent concentrations of BOD and CODMn were 120.4 mg/L and 95.7 mg/L, respectively. The effluent concentrations of BOD and CODMn were 6.8 mg/L and 11.0 mg/L, respectively. The average removal efficiencies of BOD and CODMn were 94.4% and 88.5%, respectively. The removal efficiencies of T-N and T-P were 69.6% and 73.6%, respectively when the average T-N and T-P concentrations were 32.2mg/L and 4.65mg/L, respectively. The T-N and T-P removal efficiencies were slightly decreased to 58.8% and 68.5%, respectively in the winter season but its were also stable efficiencies. BOD, T-N and T-P were removed by 90%. 67% and 46% respectively in the first anoxic/oxic condition, in addition to T-P was removed by 70% in the second anoxic/oxic condition. From the results, modified sequencing batch reactor (SBR) process is suitable for small advanced wastewater treatment.
The average specific cake resistance, the most important indicator for cake filtration and solid-liquid separation, is measured by filtration experiment. But the exact value is difficult to measure because of the other influences such as sedimentation during filtration. This study, a little more stable method named filtration-permeation is proposed for measuring average specific cake resistance. The filtration-permeation is composed of permeation of particle eliminated water through pre-formed cake by filtration. Using 1 wt% calcium carbonate suspension, the filtration-permeation experiments were performed for 8 kinds of filter media at the conditions of 0.5 atm and 0.2 atm, 1 and 3 sheets of filter media. At each specific condition, three to five times filtration-permeation were accomplished. As a result, stable permeation speed is measured. According to this experimental result, the characteristics of permeation and the effect of sedimentation are analyzed with Ruth's equation. The one way analysis of variance (one way ANOVA) is applied to the average specific cake resistances of filtration and permeation obtained with the selected three kinds of filter media. The average specific cake resistances between 0.5 atm and 0.2 atm by filtration do not distinguished, but those by permeation is perfectly distinguished. The experimental results during permeation have a very narrow distribution than that measured during filtration. The analysis of filtration experiments, it was verified that the resistance of filter medium by traditional method is of no significance. Finally, the migration of small particles through the medium composed of fiber glass at low pressure was studied.
Son, Minah;Kim, Gookhee;Han, Kunwoo;Lee, Min Woo;Lim, Jun Taek
Korean Chemical Engineering Research
/
v.55
no.2
/
pp.141-155
/
2017
In the present paper, we investigated the development status of precipitated calcium carbonate (PCC) production using steel slag, which is one of mineral carbonation (MC) technologies, from the standpoint of $CO_2$ utilization. Principle, feature, and global and domestic development status of the mineral carbonation technology were discussed together with the overview of the production method and market of PCC. Mineral carbonation is known as stable and environmentally-friendly technology enabling economical treatment of industrials wastes. Typically, PCC is produced by the reaction of $CO_2$ with supernatant solution after Ca extraction from steel slag followed by the separation of solid and liquid. The development status of MC using steel slag is at the pilot stage (Slag2PCC at Aalto University), and there remains the process economics improvement for commercialization. Key technologies for the further development are efficient extraction of Ca ions from steel slag including impurities removal, valorization of PCC via shape and size control, usage development and value-addition of residual slag, and optimization of reaction conditions for continuous process setup, etc.
Park, Se Hyung;Sonn, Jong Suk;Lee, Hong Joo;Park, Jung Hoon
Korean Chemical Engineering Research
/
v.53
no.4
/
pp.407-411
/
2015
Dense ceramic membranes have been prepared using the commercial perovsikite $Ba_{0.5}Sr_{0.5}Co_{0.8}Fe_{0.2}O_{3-{\delta}}$, powders synthesized by the solid state reaction method. The as-synthesized powders were compressed into disks with 1.0 mm of thickness and the disk was sintered at $1,100^{\circ}C$ for 2 hr. The oxygen permeation flux of $Ba_{0.5}Sr_{0.5}Co_{0.8}Fe_{0.2}O_{3-{\delta}}$ membrane increased with the increasing temperature and oxygen partial pressure. The activation energy for oxygen permeation was increased with the increasing oxygen partial pressure. Oxygen permeation flux at $950^{\circ}C$ were measured at various flow rates of feed and sweep gas. It has been demonstrated that oxygen permeability increased at elevated flow rates of both gases, but the sweep gas is more influential.
Kim, Jong-Pyo;Son, Sou-Hwan;Park, Jung-Hoon;Lee, Yong-Taek
Membrane Journal
/
v.21
no.1
/
pp.55-61
/
2011
$BaCo_{0.7}Fe_{0.22}Nb_{0.08}O_{3-{\delta}}$ oxide was synthesized by solid state reaction method. Dense ceramic membrane was prepared using as-prepared powder by pressing and sintering at $1,200^{\circ}C$. XRD result of membrane showed single perovskite structure. Leakage and oxygen permeation test were conducted on the membrane sealed by glass ring as a sealing material. The oxygen permeation flux increased with increasing temperature and pressure difference and maximum oxygen permeation flux was $2.3mL/min{\cdot}cm^2$ at $950^{\circ}C$ with $Po_2$ = 0.63 atm of oxygen partial pressure. The oxygen permeation in the condition of air with $CO_2$ (300 ppm) as feed stream decreased as much as only maximum 2.9% in comparison with air feed stream. It indicated $BaCo_{0.7}Fe_{0.22}Nb_{0.08}O_{3-{\delta}}$ membrane is more stable than another membrane for carbon dioxide.
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.
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