• Title/Summary/Keyword: 액상법

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Quantitative analysis of 3-MCPD in water using LC-MS (LC-MS를 이용한 수용액중의 3-MCPD 정량)

  • Park, Gyo-Beom;Kim, Yong-Hwa;Kim, Jin-Sung;Jeong, Ja-Young;Kim, Choong-Yong;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.198-203
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    • 2007
  • The analysis method of 3-Monochloropropane-1,2-diol (3-MCPD) compound in water was developed using liquid chromatography with mass spectrometric detection. Aqueous solution was controlled in strong basic condition with sodium hydroxide, and then $25{\mu}L$ of benzoyl chloride was added to the solution for the derivatization of 3-MCPD. The derivative was extracted using pentane and analyzed by the selected ion monitoring (SIM) method of LC-MS. The results of analyses showed that the calibration curves was in the range of 1.0 to $100{\mu}g/mL$ with a good linearity (correlation coefficient of $r^2=0.992$) and limit of detection was below $0.01{\mu}g/mL$. The recoveries of this analysis method by LC-MS were 92.3-98.0 %.

Separation of liquiritin, glycyrrhizic acid and glabridin from licorice by RP-HPLC (RP-HPLC를 이용한 감초에서 liquiritin, glycyrrhizic acid, glabridin의 분리)

  • Tian, Minglei;Yan, Hongyuan;Row, Kyung Ho
    • Analytical Science and Technology
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    • v.21 no.2
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    • pp.102-108
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    • 2008
  • Reversed-phase high performance liquid chromatography (RP-HPLC) was used for the simultaneous determination of liquiritin (LQ), glycyrrhizic acid (GA) and glabridin from licorice. An optimized run condition was selected with a binary gradient elution of methanol-water which ramped 35/65 to 80/20 (vol. %) in 0.0-8.0 min and a flow rate of 1.0 mL/min. A good linearity was obtained between 0.2 mg/mL and 1.0 mg/mL for LQ and GA, and 0.01 mg/mL-0.2 mg/mL for glabridin with the relative standard deviations less than 0.90% (n=5). The developed method was successfully applied to determination of the three components from licorice samples. The mean recoveries of three components are 80.79% for liquiritin, 89.71% for glycyrrhizic acid and 72.50% for glabridin.

A Study on Properties of SiC material Fabricated by Liquid Phase Sintering (액상소결법에 의해 제조된 탄화규소 재료의 특성에 대한 연구)

  • Sang-Pill Lee;Jae-Hwan Kwak;Jin-Kyung Lee
    • Journal of the Korean Society of Industry Convergence
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    • v.26 no.6_2
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    • pp.1019-1024
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    • 2023
  • Ceramic materials have excellent material properties such as stability at high temperatures, chemical stability, corrosion resistance, and wear resistance, so they are applicable even in extreme environments of high temperature and pressure. In particular, silicon carbide can be applied in the field of structural ceramics due to its characteristics of high strength, hardness, corrosion resistance, and heat resistance even at high temperatures. In this study, considering the application of silicon carbide materials to next-generation turbines, silicon carbide materials were manufactured using a liquid phase sintering method. When manufacturing liquid phase sintered silicon carbide, sintering additives were added to lower the sintering temperature and densify the material. In Al2O3-SiO2, it was confirmed that the secondary product of the sintering additive was observed as a slightly dark area and was evenly distributed overall, and the fracture surface of Al2O3-SiO2 was in the form of transgranular fracture in which cracks progressed along the crystal plane, and the flexural strength for Al2O3-SiO2 was about 445.6 MPa.

Simultaneous determination of 11-nor-Δ9-carboxy-tetrahydrocannabinol and 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide in urine samples by LC-MS/MS and its application to forensic science (LC-MS/MS를 이용한 소변 중 11-nor-Δ9-carboxy-tetrahydrocannabinol 및 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide의 동시 분석 및 법과학적 적용)

  • Park, Meejung;Kim, Sineun
    • Analytical Science and Technology
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    • v.34 no.6
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    • pp.259-266
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    • 2021
  • Cannabis (Marijuana) is one of the most widely used drugs in the world, and its distribution has been controlled in South Korea since 1976. Identification of 11-nor-Δ9-carboxy-tetrahydrocannabinol (THCCOOH) in urine can provide important proof of cannabis use, and it is considered scientific evidence in the forensic field. In this study, we describe a simultaneous quantitative method for identifying THCCOOH and THCCOOH-glucuronide in urine, using simple liquid-liquid extraction (LLE), and liquid chromatography-tandem mass spectrometry (LC-MS/MS). THCCOOH-D3 and THCCOOH-glucuronide-D3 were used as internal standards. Validation results of the matrix effect, as well as recovery, linearity, precision, accuracy, process efficiency, and stability were all satisfactory. No carryover, endogenous or exogenous interferences were observed. The limit of detection (LOD) of THCCOOH and THCCOOH-glucuronide were 0.3 and 0.2 ng/mL, respectively. The developed method was applied to 28 authentic human urine samples that tested positive in immunoassay screening and gas chromatography/mass spectrometry (GC/MS) tests. The ranges of concentrations of THCCOOH and THCCOOH-glucuronide in the samples were less than LOQ~266.90 ng/mL and 6.43~2133.03 ng/mL, respectively. The concentrations of THCCOOH-glucuronide were higher than those of THCCOOH in all samples. This method can be effectively and successfully applied for the confirmation of cannabinoid use in human urine samples in the forensic field.

Effects of chromium chloride addition on coloration and mechanical properties of 3Y-TZP (크롬염화물 첨가에 따른 지르코니아 색상 및 물리적 성질 변화에 관한 연구)

  • Oh, Gye-Jeong;Seo, Yoon-Jeong;Yun, Kwi-Dug;Lim, Hyun-Pil;Park, Sang-Won;Lee, Kyung-Ku;Lim, Tae-Kwan;Lee, Doh-Jae
    • The Journal of Korean Academy of Prosthodontics
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    • v.49 no.2
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    • pp.120-127
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    • 2011
  • Purpose: The purpose of this study was to examine the effects of chromium chloride addition on coloration, mechanical property and microstructure of 3Y-TZP. Materials and methods: Chromium chloride was weighed as 0.06, 0.12, and 0.25 wt% and each measured amount was dissolved in alcohol. $ZrO_2$ powder was mixed with each of the individual slurry to prepare chromium doped zirconia specimen. The color, physical properties and microstructure were observed after the zirconia specimen were sintered at $1450^{\circ}C$. In order to evaluate the color, spectrophotometer was used to analyze the value of $L^*$, $C^*$, $a^*$ and $b^*$, after placing the specimen on a white plate, and measured according to the International Commission on Illumination (CIE) standard, Illuminant D65 and SCE system. The density was measured in the Archimedes method, while microstructures were evaluated by using the scanning electron microscopy (SEM) and XRD. Fracture toughness was calculated Vickers indentation method and indentation size was measured by using the optical microscope. The data were analyzed with 1-way ANOVA test (${\alpha}$ = 0.05). The Tukey multiple comparison test was used for post hocanalysis. Results: 1. Chromium chloride rendered zirconia a brownish color. While chromium chloride content was increased, the color of zirconia was changed from brownish to brownish-red. 2. Chromium chloride content was increased; density of the specimen was decreased. 3. More chromium chloride in the ratio showed increase size of grains. 4. But the addition of chromium chloride did not affect the crystal phase of zirconia, and all specimens showed tetragonal phase. 5. The chromium chloride in zirconia did not showed statistically significant difference in fracture toughness, but addition of 0.25 wt% showed a statistically significant difference (P<.05). Conclusion: Based on the above results, this study suggests that chromium chlorides can make colored zirconia while adding in a liquid form. The new colored zirconia showed a slight difference in color to that of the natural tooth, nevertheless this material can be used as an all ceramic core material.

Characteristics of Sn-doped β-Ga2O3 single crystals grown by EFG method (EFG 법으로 성장한 β-Ga2O3 단결정의 Sn 도핑 특성 연구)

  • Tae-Wan Je;Su-Bin Park;Hui-Yeon Jang;Su-Min Choi;Mi-Seon Park;Yeon-Suk Jang;Won-Jae Lee;Yun-Gon Moon;Jin-Ki Kang;Yun-Ji Shin;Si-Yong Bae
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.33 no.2
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    • pp.83-90
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    • 2023
  • The β-Ga2O3 has the most thermodynamically stable phase, a wide band gap of 4.8~4.9 eV and a high dielectric breakdown voltage of 8MV/cm. Due to such excellent electrical characteristics, this material as a power device material has been attracted much attention. Furthermore, the β-Ga2O3 has easy liquid phase growth method unlike materials such as SiC and GaN. However, since the grown pure β-Ga2O3 single crystal requires the intentionally controlled doping due to a low conductivity to be applied to a power device, the research on doping in β-Ga2O3 single crystal is definitely important. In this study, various source powders of un-doped, Sn 0.05 mol%, Sn 0.1 mol%, Sn 1.5 mol%, Sn 2 mol%, Sn 3 mol%-doped Ga2O3 were prepared by adding different mole ratios of SnO2 powder to Ga2O3 powder, and β-Ga2O3 single crystals were grown by using an edge-defined Film-fed Growth (EFG) method. The crystal direction, crystal quality, optical, and electrical properties of the grown β-Ga2O3 single crystal were analyzed according to the Sn dopant content, and the property variation of β-Ga2O3 single crystal according to the Sn doping were extensively investigated.

Verification of Numerical Analysis Technique of Dynamic Response of Seabed Induced by the Interaction between Seabed and Wave (파랑-지반 상호작용에 의한 해저지반의 동적응답 수치해석법 검증)

  • Kang, Gi-Chun;Kim, Sung-Woung;Kim, Tae-Hyung;Kim, Do-Sam;Kim, Jae-Hong
    • Journal of the Korean Geotechnical Society
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    • v.31 no.1
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    • pp.5-14
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    • 2015
  • Seabed may undergo large excess pore water pressure in the case of long duration of high wave loading. This excess pore water pressure may reduce effective stress and, consequently, the seabed may liquefy. Thus, it is necessary to develop a numerical technique which can precisely evaluate the dynamic response of seabed due to wave action. In this study, a new numerical technique named mixed model (2D NIT & FLIP models) was proposed. The dynamic wave pressure and water flow velocity acting on the boundary between seabed and the wave field was estimated using 2D-NIT model. This result was used as input data in FLIP program for investigation of dynamic response of seabed. To secure the reliability of the mixed model, the numerical analysis results of the mixed model were compared with Yamamoto's solution and Chang's experiment results. The comparison results indicated that there were some differences between them, but the general trend of the effective stress increment and the excess pore water pressure along the depth of seabed was similar to each other. Thus, this study clearly supports the plausibility of the numerical analysis of the mixed model.

Thermal and Mechanical Evaluation of Environmental Barrier Coatings for SiCf-SiC Composites (SiCf-SiC 복합재료의 내환경 코팅 및 열, 기계적 내구성 평가)

  • Chae, Yeon-Hwa;Moon, Heung Soo;Kim, Seyoung;Woo, Sang Kuk;Park, Ji-Yeon;Lee, Kee Sung
    • Composites Research
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    • v.30 no.2
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    • pp.84-93
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    • 2017
  • This study investigates thermal and mechanical characterization of environmental barrier coating on the $SiC_f-SiC$ composites. The spherical environmental barrier coating (EBC) powders are prepared using a spray drying process for flowing easily during coating process. The powders consisting of mullite and 12 wt% of Ytterbium silicate are air plasma sprayed on the Si bondcoat on the LSI SiC fiber reinforced SiC composite substrate for protecting the composites from oxidation and water vapor reaction. We vary the process parameter of spray distance during air plasma spray of powders, 100, 120 and 140 mm. After that, we performed the thermal durability tests by thermal annealing test at $1100^{\circ}C$ for 100hr and thermal shock test from $1200^{\circ}C$ for 3000 cycles. As a result, the interface delamination of EBC never occur during thermal durability tests while stable cracks are prominent on the coating layer. The crack density and crack length depend on the spray distance during coating. The post indentation test indicates thermal tests influence on the indentation load-displacement mechanical behavior.

Preparation of the TiO2 Coated Mica by Hydrolysis Method(I) (가수분해법에 의한 TiO2 피복 운모의 제조(I))

  • Park, Yoon-Chang;Kim, Hyo-Joong;Kwak, Chung-Heop;Suh, Tae-Soo
    • Applied Chemistry for Engineering
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    • v.8 no.5
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    • pp.709-714
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    • 1997
  • $TiO_2$ hydrate coating on mica in an aqueous solution of $TiOSO_4$ by the hydrolysis using ammonia water studied with emphasis on coating conditions for a uniform coating. For the uniform coating of $TiO_2$ film on mica surface, it was found that smaller mica particles were coated more uniformly compared to larger particles. It was necessary to suppress the rate of formation of hydrated $TiO_2$ particles in solution, which were deposited on mica and generate irregular coating. It was also necessary to control precipitation yield by varying the reaction temperature to obtain uniform coating. More uniform coating was obtained with higher precipitation yield. A uniform dense film was formed when mica particles of average size of $14.7{\mu}m$ is used for mica slurry solution, of which pH is 2.5, and the factor of acidity of $TiOSO_4$ solution is 291, and the solution was kept at $80^{\circ}C$ for 3 hours. The morphology of $TiO_2$ film formed on mica was little affected by firing at $900^{\circ}C$.

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Preparation of the Dexamethasone-incorporated Lipid Nanosphere: Characteristics of Lipid Nanosphere by Varying Species and Ratio of Lipid (덱사메타손이 봉입된 지질나노입자의 제조: 지질의 종류와 함량 변화에 따른 지질나노입자의 특성)

  • Jeong, Seok-Hyeon;Lee, Jeong-Eun;Seong, Ha-Su;Sin, Byeong-Cheol
    • Journal of the Korean Chemical Society
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    • v.50 no.6
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    • pp.464-470
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    • 2006
  • the coricosteroid drug dexamethasone is an efficacious antiinflammatory drug, it is difficult to formulate in an injectable formulation due to its poor aqueous solubility. A lipid-based nanosphere formulation containing dexamethasone was designed for solubilization of the drug in aqueous solution and sustained release of the drug from the nanosphere. The lipid nanospheres, composed of phospholipid, cholesterol and cationic lipid, were prepared by self emulsification-solvent diffusion method followed by diafiltration. Physicochemical characteristics such as mean particle diameter, zeta potential and drug loading efficiency of the lipid nanospheres were investigated according to the variation of either the kind of lipid or the lipid composition. The lipid nanospheres had a mean diameter 80-120 nm and dexamethasone loading efficiency of greater than 80%. The drug loading efficiency increased with the increase of the length of aliphatic chain attached to the phospholipid. However, the drug loading efficiency was inversely proportional to the increase of cholesterol content in the lipid composition. The lipid nanosphere could not be prepared without the use of cationic lipid and the drug loading efficiency was proportional to the increase of cationic lipid content. The lipid nanospheres containing dexamethasone are a promising novel drug carrier for an injectable formulation of the poorly water-soluble drugs.