• Title/Summary/Keyword: Volume of recovery water

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Separation of chlorine in a uranium compound by pyrohydrolysis and steam distillation, and its determination by ion chromatography (열가수분해 및 수증기증류에 의한 우라늄 화합물 중 염소 분리 및 이온크로마토그래피 정량)

  • Kim, Jung-Suk;Lee, Chang-Hun;Park, Soon-Dal;Han, Sun-Ho;Song, Kyu-Seok
    • Analytical Science and Technology
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    • v.23 no.1
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    • pp.45-53
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    • 2010
  • For the determination of chlorine in uranium compound, analytical methods by using a steam distillation and a pyrohydrolysis have been developed. The steam distillation apparatus was composed of steam generator, distilling flask and condenser etc. The samples were prepared with an aliquot of LiCl standard solution and a simulated spent nuclear fuel. A sample aliquot was mixed with a solution containing 0.2 M ferrous ammonium sulfate-0.5 M sulfamic acid 3 mL, phosphoric acid 6 mL and sulfuric acid 15 mL. The chloride was then distilled by steam at the temperature of $140^{\circ}C$ until a volume of $90{\pm}5\;mL$ is collected. The pyrohydrolysis equipment was composed of air introduction system, water supply, quartz reaction tube, combustion tube furnace, combustion boat and absorption vessel. The chloride was separated from powdered sample which is added with $U_3O_8$ accelerator, by pyrohydrolysis at the temperature of $950^{\circ}C$ for 1 hour in a quartz tube with a stream of air of 1 mL/min supplied from the water reservoir at $80^{\circ}C$. The chlorides collected in each absorption solution by two methods was diluted to 100 mL and measured with ion chromatography to determine the recovery yield. For the ion chromatographic determination of chlorine in molten salt retained in a metal ingot, the chlorine was separated by means of pyrohydrolysis after air and dry oxidation, and grinding for the sample.

Characteristics of Microwave-Assisted Extraction for Grape Seed Components with Different Solvents (추출용매에 따른 포도씨 성분의 마이크로웨이브 추출 특성)

  • Lee Eun-Jin;Kwon Joong-Ho
    • Food Science and Preservation
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    • v.13 no.2
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    • pp.216-222
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    • 2006
  • Microwave energy (2450 MHz) was applied to extract health-effective component (HEC) from grape seed. Three different solvents approved for grape seed extract such as water, ethanol and acetone, were confirmed in their microwave-heating properties and by which extraction efficiencies were determined. Microwave-assisted extraction (MAE) was performed under different parameters; microwave power : (0, 50, 100 and 150), time : (1, 3, 5, 7, and 9 min), the sample to solvent ratio : (1:20, 1:10, 1:5 and 1:2.5), and particle size(whole, 20, 40 and 60 mesh) and the subsequent extracts were used for determining their physicochemical properties, such as total yield : (TY), total phenolics : (TP), catechin content : (CC), electron donating ability : (EDA), and browning color. The heating properties of solvent demonstrated the optimal ranges of microwave and time as 100 W and 2 to 6 min. The TY and HFC content were higher with increasing powers in water and ethanol solvent, while HFC content were lower in acetone at over 100 W. The longer of extraction time up to 5 min, the higher extraction efficiency. Based upon the overall MAE efficiency and solvent recovery, it was found optimal to use 10 times volume of ethanol for 10 mesh of seed particle at 100 W.

Variation on Estimated Values of Radioactivity Concentration According to the Change of the Acquisition Time of SPECT/CT (SPECT/CT의 획득시간 증감에 따른 방사능농도 추정치의 변화)

  • Kim, Ji-Hyeon;Lee, Jooyoung;Son, Hyeon-Soo;Park, Hoon-Hee
    • The Korean Journal of Nuclear Medicine Technology
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    • v.25 no.2
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    • pp.15-24
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    • 2021
  • Purpose SPECT/CT was noted for its excellent correction method and qualitative functions based on fusion images in the early stages of dissemination, and interest in and utilization of quantitative functions has been increasing with the recent introduction of companion diagnostic therapy(Theranostics). Unlike PET/CT, various conditions like the type of collimator and detector rotation are a challenging factor for image acquisition and reconstruction methods at absolute quantification of SPECT/CT. Therefore, in this study, We want to find out the effect on the radioactivity concentration estimate by the increase or decrease of the total acquisition time according to the number of projections and the acquisition time per projection among SPECT/CT imaging conditions. Materials and Methods After filling the 9,293 ml cylindrical phantom with sterile water and diluting 99mTc 91.76 MBq, the standard image was taken with a total acquisition time of 600 sec (10 sec/frame × 120 frames, matrix size 128 × 128) and also volume sensitivity and the calibration factor was verified. Based on the standard image, the comparative images were obtained by increasing or decreasing the total acquisition time. namely 60 (-90%), 150 (-75%), 300 (-50%), 450 (-25%), 900 (+50%), and 1200 (+100%) sec. For each image detail, the acquisition time(sec/frame) per projection was set to 1.0, 2.5, 5.0, 7.5, 15.0 and 20.0 sec (fixed number of projections: 120 frame) and the number of projection images was set to 12, 30, 60, 90, 180 and 240 frames(fixed time per projection:10 sec). Based on the coefficients measured through the volume of interest in each acquired image, the percentage of variation about the contrast to noise ratio (CNR) was determined as a qualitative assessment, and the quantitative assessment was conducted through the percentage of variation of the radioactivity concentration estimate. At this time, the relationship between the radioactivity concentration estimate (cps/ml) and the actual radioactivity concentration (Bq/ml) was compared and analyzed using the recovery coefficient (RC_Recovery Coefficients) as an indicator. Results The results [CNR, radioactivity Concentration, RC] by the change in the number of projections for each increase or decrease rate (-90%, -75%, -50%, -25%, +50%, +100%) of total acquisition time are as follows. [-89.5%, +3.90%, 1.04] at -90%, [-77.9%, +2.71%, 1.03] at -75%, [-55.6%, +1.85%, 1.02] at -50%, [-33.6%, +1.37%, 1.01] at -25%, [-33.7%, +0.71%, 1.01] at +50%, [+93.2%, +0.32%, 1.00] at +100%. and also The results [CNR, radioactivity Concentration, RC] by the acquisition time change for each increase or decrease rate (-90%, -75%, -50%, -25%, +50%, +100%) of total acquisition time are as follows. [-89.3%, -3.55%, 0.96] at - 90%, [-73.4%, -0.17%, 1.00] at -75%, [-49.6%, -0.34%, 1.00] at -50%, [-24.9%, 0.03%, 1.00] at -25%, [+49.3%, -0.04%, 1.00] at +50%, [+99.0%, +0.11%, 1.00] at +100%. Conclusion In SPECT/CT, the total coefficient obtained according to the increase or decrease of the total acquisition time and the resulting image quality (CNR) showed a pattern that changed proportionally. On the other hand, quantitative evaluations through absolute quantification showed a change of less than 5% (-3.55 to +3.90%) under all experimental conditions, maintaining quantitative accuracy (RC 0.96 to 1.04). Considering the reduction of the total acquisition time rather than the increasing of the image acquiring time, The reduction in total acquisition time is applicable to quantitative analysis without significant loss and is judged to be clinically effective. This study shows that when increasing or decreasing of total acquisition time, changes in acquisition time per projection have fewer fluctuations that occur in qualitative and quantitative condition changes than the change in the number of projections under the same scanning time conditions.

New Analytical Method to Identify Chromium Species, Cr(III) and Cr(VI), and Characteristic Distribution of Chromium Species in the Han River (한강수계해서의 크롬(III,VI) 종(species) 분포 및 분석방법 정립)

  • Jeong, Gwan-Jo;Kim, Dok-Chan;Park, Hyeon
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.6
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    • pp.590-598
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    • 2005
  • An adequate method to identify chromium separation, Cr(III) and Cr(VI), in water samples were studied by using High Performance Liquid Chromatography(HPLC) coupled with Inductively Coupled Plasma Mass Spectometer(ICP-MS) equipped with Dynamic Reaction Cell(DRC). The characteristic distribution of Cr(III) and Cr(VI) in the raw water taken at the six water intake stations in Seoul, was analyzed by the method developed by the authors. The chromium species separated by HPLC was isocratically conducted by using tetrabutylammonium phosphate monobasic(1.0 mM TBAP), ethylenediaminetetraacetic acid(0.6 mM EDTA) and 2% v/v methanol as the mobile phase. 5% v/v methanol was used as flushing solvent. A reactive ammonia($NH_3$) gas was used to eliminate the potential interference of $ArC^+$. Several Parameters such as solvent ratio, pH, flow rate and sample injection volume were optimized for the successful separation and reproducibility. Although it has been reported thai the separation sensitivity of Cr(III) is superior to that of Cr(VI), the authors observed Cr(VI) was more sensitive than Cr(III) when ammonia($NH_3$) gas was used as the reaction gas. It took less than 3 minutes to analyze chromium species with this method and the estimated detection limits were $0.061\;{\mu}g/L$ for Cr(III) and $0.052\;{\mu}g/L$, for Cr(VI). According to the results from the analysis on chromium species in the raw water of the six intake stations, the concentrations of Cr(III) ranged from 0.048 to $0.064\;{\mu}g/L$(ave. $0.054\;{\mu}g/L$) while that of Cr(VI) ranged from 0.014 to $0.023\;{\mu}g/L$(ave. $0.019\;{\mu}g/L$). Recovery ratio was very high($90.1{\sim}94.1%$). There were two or three times more Cr(III) than Cr(VI) in the raw water.

The Heterogeneity of Flow Distribution and Partition Coefficient in [15O-H2O] Myocardium Positron Emission Tomography ([15O-H2O] 심근 양전자 단층 촬영에서 혈류 분포의 비균일성과 분배계수)

  • Ahn, Ji Young;Lee, Dong Soo;Kim, Kyung Min;Jeong, Jae Min;Chung, June-Key;Shin, Seung-Ae;Lee, Myung Chul;Koh, Chang-Soon
    • The Korean Journal of Nuclear Medicine
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    • v.32 no.1
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    • pp.32-49
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    • 1998
  • For estimation of regional myocardial blood flow with O-15 water PET, a few modifications considering partial volume effect based on single compartment model have been proposed. In this study, we attempted to quantify the degree of heterogeneity and to show the effect of tissue flow heterogeneity on partition coefficient(${\lambda}$) and to find the relation between perfusable tissue index(PTI) and ${\lambda}$ by computer simulation using two modified models. We simulated tissue curves for the regions with homogeneous and heterogeneous blood flow over a various flow range(0.2-4.0ml/g/min). Simulated heterogeneous tissue composed of 4 subregions of the same or different size of block which have different homogeneous flow and different degree of slope of distribution of blood flow. We measured the index representing heterogeneity of distribution of blood flow for each heterogeneous tissue by the constitution heterogeneity(CH). For model I, we assumed that tissue recovery coefficient ($F_{MME}$) was the product of partial volume effect($F_{MMF}$) and PTI. Using model I, PTI, flow, and $F_{MM}$ were estimated. For model II, we assumed that partition coefficient was another variable which could represent tissue characteristics of heterogeneity of flow distribution. Using model II, PTI, flow and ${\lambda}$ were estimated. For the simulated tissue with homogeneous flow, both models gave exactly the same estimates, of three parameters. For the simulated tissue with heterogeneous flow distribution, in model I, flow and $F_{MM}$ were correctly estimated as CH was increased moderately. In model II, flow and ${\lambda}$ were decreased curvi-linearly as CH was increased. The degree of underestimation of ${\lambda}$ obtained using model II, was correlated with CH. The degree of underestimation of flow was dependent on the degree of underestimation of ${\lambda}$. PTI was somewhat overestimated and did not change according to CH. We conclude that estimated ${\lambda}$ reflect the degree of tissue heterogeneity of flow distribution. We could use the degree of underestimation of ${\lambda}$ to find the characteristic heterogeneity of tissue flow and use ${\lambda}$ to recover the underestimated flow.

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Removal of residual VOCs in a collection chamber using decompression for analysis of large volatile sample

  • Lee, In-Ho;Byun, Chang Kyu;Eum, Chul Hun;Kim, Taewook;Lee, Sam-Keun
    • Analytical Science and Technology
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    • v.34 no.1
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    • pp.23-35
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    • 2021
  • In order to measure the volatile organic compounds (VOCs) of a sample which is too large to use commercially available chamber, a stainless steel vacuum chamber (VC) (with an internal diameter of 205 mm and a height of 50 mm) was manufactured and the temperature of the chamber was controlled using an oven. After concentrating the volatiles of the sample in the chamber by helium gas, it was made possible to remove residual volatile substances present in the chamber under reduced pressure ((2 ± 1) × 10-2 mmHg). The chamber was connected to a purge & trap (P&T) using a 6 port valve to concentrate the VOCs, which were analyzed by gas chromatography-mass spectrometry (GC-MS) after thermal desorption (VC-P&T-GC-MS). Using toluene, the toluene recovery rate of this device was 85 ± 2 %, reproducibility was 5 ± 2 %, and the detection limit was 0.01 ng L-1. The method of removing VOCs remaining in the chamber with helium and the method of removing those with reduced pressure was compared using Korean drinking water regulation (KDWR) VOC Mix A (5 μL of 100 ㎍ mL-1) and butylated hydroxytoluene (BHT, 2 μL of 500 ㎍ mL-1). In case of using helium, which requires a large amount of gas and time, reduced pressure ((2 ± 1) × 10-2 mmHg) only during the GC-MS running time, could remove VOCs and BHT to less than 0.1 % of the original injection concentration. As a result of analyzing volatile substances using VC-P&T-GC-MS of six types of cell phone case, BHT was detected in four types and quantitatively analyzed. Maintaining the chamber at reduced pressure during the GC-MS analysis time eliminated memory effect and did not affect the next sample analysis. The volatile substances in a cell phone case were also analyzed by dynamic headspace (HT3) and GC-MS, and the results of the analysis were compared with those of VC-P&T-GC-MS. Considering the chamber volume and sample weight, the VC-P&T configuration was able to collect volatile substances more efficiently than the HT3. The VC-P&T-GC-MS system is believed to be useful for VOCs measurement of inhomogeneous large sample or devices used inside clean rooms.

Simultaneous Analysis of Cold Medicine Component by High-Performance Liquid Chromatography(HPLC) (고성능 액체크로마토그래피(HPLC)를 이용한 Cold Medicine 성분의 동시 분석)

  • Wonju Lee;Seung-Tae Choi;Keun-Sik Shin;Jin-Young Park;Jae-Ho Sim
    • The Journal of the Convergence on Culture Technology
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    • v.9 no.6
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    • pp.867-873
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    • 2023
  • In this study, for the purpose of standardized quality control of a cold medicine, we simultaneous analyzed four main chemical components of a cold medicine: acetaminophen, caffeine, methyl paraben, and propyl paraben. The sample was subjected to quantitative analysis using high performance liquid chromatography (HPLC), after pretreatment of four components. The experiment was carried out by using Isocratic elution at wavelength of 270nm. Acetonitrile and water (H2O) were used as a mobile phase at a flow rate of 1.0mL/min in a commercial C18 reversed-phase column. A volume of 10uL cold medicine were injected into the column with column oven temperature at 35℃. As a result of the experiment, the values of Resolution were 4.983, 1.596, 5.519, and 1.678 respectively-well over Rs >1.5, which indicates that the separation of four components were efficient. In addition, value of symmetry factor of the components was 1.056, 1.069, 1.032, and 1.133 respectively, to show its symmetrical stability. The calibration curve of all four components exhibits good linearity with R2 >0.9995 to 0.9999. Furthermore, the limit of detection(LOD) were between 0.0118 to 1.5973 mg/mL, while the limit of quantification (LOQ) were between 0.0353 to 4.7919 ㎍/mL with the recovery rate of 79.6% ~ 120.5%. The results of this study showed an efficient quality evaluation of a simultaneous analysis method for cold medicine components.

Simultaneous determination of baicalin and glycyrrhizin in Sosiho-tang by HPLC and anti-inflammatory activity (소시호탕에서 baicalin과 glycyrrhizin 동시 분석 및 항염 활성)

  • Kim, Jung-Hoon;Ha, Hye-Kyung;Seo, Chang-Seob;Lee, Jin-Ah;Shin, Hyeun-Kyoo
    • The Korea Journal of Herbology
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    • v.26 no.1
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    • pp.41-46
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    • 2011
  • Objectives : To quantitate the main compounds and investigate the biological activity of Sosiho-tang (Xiao-Chai-Hu-Tang, SST), simultaneous determination of baicalin and glycyrrhizin, and anti-inflammatory activity were estimated. Methods : A quantitative analysis was performed using a high performance liquid chromatography (HPLC). Reference compounds were separated on a reversed-phase column using gradient elution with water and acetonitrile each containing acetic acid at a flow rate of 1 mL/min. And the productions of nitric oxide (NO) and prostaglandin $(PE)E_2$ were examined by lipopolysaccharide (LPS)-treated RAW 264.7 cells in the presence of the SST. The anti-inflammatory activity of SST was investigated by carrageenin-induced paw edema in rats. The paw volume was measured at 2 and 4 hr following carrageenin-induced paw edema in rats. Results : The correlation coefficients of the compounds showed good linearity ($r^2$ > 0.9992) over the linear range. The precisions of intra- and inter-day were less than 7.0% of relative standard deviation (RSD) values for baicalin and less than 3.5% of RDS valuse for glycyrrhizin. Recovery rates were within the range of 95.41-101.5%. The contents of baicalin and glycyrrhizin in SST were average 70.52, 6.18 mg/g, respectively. And SST exhibited inhibitory effect on NO production in LPS-treated RAW 264.7 cells but not on $PGE_2$ production. Oral administration of SST (1 g/kg) showed a reduction in carrageenin-induced paw edema on rats. Conclusions : The analytical method was applied successfully to measure the contents of baicalin and glycyrrhizin in SST which exhibited anti-inflammatory activities.

Methanol Extraction of Nitrogen Heterocyclic Compound Contained in Model Coal Tar Fraction of Nine Components System (9성분계 모델 콜타르 흡수유 중에 함유된 질소고리화합물의 메탄올 추출)

  • Kim, Su Jin;Kang, Ho Cheol
    • Applied Chemistry for Engineering
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    • v.25 no.2
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    • pp.142-146
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    • 2014
  • The separation of nitrogen heterocyclic compound (NHC) contained in a model coal tar fraction of nine components system was investigated by distribution equilibrium. The model coal tar fraction comprising NHC group (NHCs; indole (In), quinoline (Q), iso-quinoline (iQ), quinaldine(Qu)), bicyclic aromatic compound group (BACs; 1-methylnaphthalene (1MN), 2-methylnaphthalene (2MN), dimethylnaphthalene (DMN)), biphenyl (Bp) and phenyl ether (Pe) and the aqueous methanol were used as the raw materials and the solvent of this work, respectively. A batch-stirred tank was used as the liquid-liquid contact unit of this work. The distribution coefficient of NHCs increased by increasing the equilibrium operation temperature, whereas the selectivity of NHCs with respect to BACs decreased. Decreasing the initial volume ratio of water to the solvent resulted in deteriorating the selectivity of NHCs in reference to BACs, but improving the distribution coefficients of NHCs. At a fixed experimental condition, the sequence of the distribution coefficient and the selectivity with reference to BACs for each groups was increased in order of NHCs > Bp > BACs > Pe and NHCs > Bp> Pe, respectively. Also, the sequence of the distribution coefficient for entire compounds was in order of In > iQ = Q > Qu > Bp > 1MN = 2MN > Pe > DMN. The maximum yield of NHCs and the selectivity of NHCs based on BACs obtained by methanol extraction were 94 and 23%, respectively. Furthermore, the recovery process for NHCs from coal tar was studied by using the experimental results from this work.

Preconcentration and Extraction of Copper on Activated Carbon Using 4-Amino-2, 3-dimethyl-1-phenyl-3-pyrazoline or 4-(4-methoxybenzylidenimin) thiophenole (4-Amino-2,3-dimethyl-1-phenyl-3-pyrazoline 또는 4-(4-Methoxybenzylidenimin)thiophenole을 이용한 활성탄에서의 구리의 예비 농축 및 추출)

  • Ghaedi, Mehrorang;Ahmadi, Farshid;Karimi, Hajir;Gharaghani, Shiva
    • Journal of the Korean Chemical Society
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    • v.50 no.1
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    • pp.23-31
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    • 2006
  • carbon modified methods were used for the preconcentration and determination of copper in some real samples using the flame atomic absorption spectrometry. The copper ions was adsorbed quantitatively on the activated carbon due to their complexation with 4- amino-2, 3-dimethyl-1-phenyl-3-pyrazoline (ADMPP) or 4-(4- methoxybenzylidenimin) thiophenole (MBITP). The adsorbed copper on solid phase was eluted quantitatively using small amount of nitric acid. The influence of important parameters including pH, amount of carrier, flow rate, amount of activated carbon and type and concentration of eluting agent for obtaining maximum recovery were investigated. The methods based on ADMPP and MBITP at optimum conditions is linear over concentration range of 0.05-1.5 g mL-1 and 0.05-1.2 g mL-1 of copper with correlation coefficient of 0.9997 and 0.9994 and both detection limit of 1.4 ng mL-1, respectively. The preconcentration leads to enrichment factor of 310 and break through volume of 1550 mL for both ligands. The method has a good tolerance limit of interfering ion and a selectivity that has been successfully applied for the determination of copper content in real sample such as tap, spring, river and waste water.