• Title/Summary/Keyword: purity analysis

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Mass Balance Method for Purity Assessment of Organic Reference Materials: for Thermolabile Materials with LC-UV Method

  • Lee, Joonhee;Kim, Byungjoo
    • Bulletin of the Korean Chemical Society
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    • v.35 no.11
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    • pp.3275-3279
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    • 2014
  • A mass balance method for purity assessment of thermolabile organic reference materials was established by combining several techniques, including liquid chromatography with UV/VIS detector (LC-UV), Karl-Fischer (K-F) Coulometry, and thermal gravimetric analysis (TGA). This method was applied to three fluoroquinolones like enrofloxacin, norfloxacin and ciprofloxacin. LC-UV was used to analyze structurally related organic impurities based on UV/VIS absorbance spectra obtained in combination with LC separation. For all three organic reference materials, the UV/VIS spectra of the separated impurities were similar to that of the major component of the corresponding materials. This indicates that the impurities are structurally related to the respective reference material sharing common chromophores. Impurities could be quantified by comparing their absorbances at the wavelength of maximum absorbance (${\lambda}_{max}$). The water contents of the reference materials were measured by K-F Coulometry by an oven-drying method. The total inorganic impurities contents were assayed from ash residues in TGA analysis with using air as a reagent gas. The final purities estimated from results of those analytical techniques were assigned as ($99.91{\pm}0.06$), ($97.09{\pm}0.17$) and ($91.85{\pm}0.17$)% (kg/kg) for enrofloxacin, norfloxacin and ciprofloxacin, respectively. The assigned final purities would be applied to the reference materials which will be used as calibrators for the certification of those compounds in matrix CRMs as starting points for the traceability of their certified values to SI units.

Automated radiochemical synthesis of [18F]FET on TRACERlab FX2N module and its quality control

  • Dong Hyun Kim;Eun-bi Shin;Iljung Lee;Heejung Kim;Kyo Chul Lee;Kyeong Min Kim;Joo Hyun Kang;Sang Moo Lim
    • Journal of Radiopharmaceuticals and Molecular Probes
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    • v.7 no.2
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    • pp.147-152
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    • 2021
  • C-11 Radiolabeled amino acid-based radiopharmaceuticals such as [11C]MET for brain tumor PET imaging have limitations due to their short half-life (20 min). F-18 radiolabeled amino acid derivatives have been developed to overcome for the short half-life, one of which is [18F]FET. Brain tumor imaging using [18F]FET showed high uptake in tumor region and no non-specific uptake in inflammatory tissue, which was useful in discriminating the difference between inflammation and tumor especially. In this study, [18F]FET was synthesized using an automatic synthesis module and quality tests were carried out including enantiomeric purity analysis with reference compounds. Radiochemical yield was 50.3 ± 4.9% (n=7, decay-corrected) with molar activity of 76 ± 17 GBq/mmol. The radiochemical purity of >99%. Enantiomeric purity of [18F]FET using chiral HPLC analysis showed >99%, which was confirmed by co-injection with the L-FET and D-FET authentic standards. [18F]FET was prepared with high radiochemical yield and molar activity including no racemate mixture.

Plasma Resistance and Etch Mechanism of High Purity SiC under Fluorocarbon Plasma

  • Jang, Mi-Ran;Paek, Yeong-Kyeun;Lee, Sung-Min
    • Journal of the Korean Ceramic Society
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    • v.49 no.4
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    • pp.328-332
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    • 2012
  • Etch rates of Si and high purity SiC have been compared for various fluorocarbon plasmas. The relative plasma resistance of SiC, which is defined as the etch rate ratio of Si to SiC, varied between 1.4 and 4.1, showing generally higher plasma resistance of SiC. High resolution X-ray photoelectron analysis revealed that etched SiC has a surface carbon content higher than that of etched Si, resulting in a thicker fluorocarbon polymer layer on the SiC surface. The plasma resistance of SiC was correlated with this thick fluorocarbon polymer layer, which reduced the reaction probability of fluorine-containing species in the plasma with silicon from the SiC substrate. The remnant carbon after the removal of Si as volatile etch products augments the surface carbon, and seems to be the origin of the higher plasma resistance of SiC.

Fabrication and Characterization of High Purity Al2O3 by Decomposition of Selicite (세리사이드 분해에 의한 고순도 Al2O3의 제조 및 특성에 관한 연구)

  • 이경희;박한수;송명신
    • Journal of the Korean Ceramic Society
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    • v.24 no.5
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    • pp.431-436
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    • 1987
  • High purity Al2O3 has been extracted from serlcite of clayminerals, selicite was treated by H2SO4(2N∼18N) solution, NH4OH treatment(PH8.5∼10.0) and metallic impurities such as Fe were removed by NaOH treatment. The tendency of extraction yield of ${\alpha}$-Al2O3 have been investigated by relating reaction time, acid concentration. Reaction products were analyzed by DT-TGA, chemical analysis and X-ray diffractometer. Prepared ${\alpha}$-Al2O3 power is fired in air at 1400$^{\circ}C$, 1600$^{\circ}C$ 2hr. The results are as follows; 1. The most suitable extracting conditions of ${\alpha}$-Al2O3 from Selicite were N-H2SO4, 120 min acidtreating time. 2. The optimum pH condition was 9.0. 3. Physical properties of sintered Al2O3 bodies were as follows. Relative density is 99%. Water absorption is 0.26%. Rock well hardness is 89.

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Fabrication of fine BSCCO-2223 precursor powder by spray pyrolysis process (분무 열분해방법에 의한 미세 BSCCO-2223 전구분말의 제조)

  • 김성환;유재무;고재웅;김영국;박기호
    • Progress in Superconductivity
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    • v.5 no.1
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    • pp.65-69
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    • 2003
  • Many researches on fabrication process for BSCCO precursor powders have been developed for high J$_{c}$ BSCCO-2223 tape. Spray pyrolysis method for fabrication of precursor powder has many advantages, such as high purity, fine particle size and low carbon content of BSCCO precursor powder. Fine, spherical powders were prepared by ultrasonic spray pyrolysis from the aqueous solution of metal nitrates. BSCCO precursor powders were synthesized with various solutes concentration and heat treatment conditions. Average particle size for spray pyrolysis powders was $1.5∼3\mu\textrm{m}$. Bi-2223/Ag tape was prepared by PIT method and followed by various sintering conditions. BSCCO precursor powders were characterized by XRD, SEM, EDS, Carbon content and particle size analysis.s.

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Consolidation and casting technology of fine poly-Si powders for economical production of Si ingot (경제적인 Si 잉곳 생산을 위한 poly-Si 미세분말의 성형과 용해주조기술)

  • Moon, Byung-Moon;Kim, Bong-Hwan;Shin, Je-Sik;Lee, Sang-Mok;Park, Gi-Seong;Kim, Dae-Suk;Kim, Ki-Young
    • 한국신재생에너지학회:학술대회논문집
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    • 2007.06a
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    • pp.261-264
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    • 2007
  • In this study, the consolidation and casting processes of fine Si powders, by-products of making high purity Poly-Si rods in the current method, were systematically investigated for use as economical solar-grade feedstock. Morphology, size, and contamination type of the poly-Si fine powders were inspected by combined analysis of SEM, particle size analyzer, and FT-IR. Poly-Si powder compacts were tried to fabricate by a consolidation process without a binding agent and then their density ratio and strength were evaluated. Finally, the electrical resistivity of the specimens prepared by an electromagnetic casting method was examined for purity assessment.

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Extraction Chromatograph Separation Spark Source Mass Spectrometric Analysis of 14 Rare Earth Impurities in High Purity Rare Earth Oxide

  • Sui, Xiyun;Wang, Zishu;Shao, Baohai
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.553-559
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    • 1995
  • An extraction chromatographic method of separating rare earth impurities from high purity $Nd_2O_3$, $Sm_2O_3$, $Gd_2O_3$, $Er_2O_3$, $Dy_2O_3$ and $Yb_2O_3$ was studied by using $HCl-NH_4Cl$ as moving phase and P507 as stationary phase. After the impurities were enriched from the eluate by chelant-activated carbon, the active carbon was ashed and the ignited residue was used to prepare the sample electrode for spark source mass spectrometric determination. The impurities in 99.9999% rare earth oxide can be determined by the proposed method with recovery over 80%.

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Luminescent characteristics with coupling structure of Eu for ZnO:Eu Phosphor (Zno:Eu 형광체의 Eu 결합 구조에 따른 발광 특성)

  • 박용규;한정인;조황신;주성후
    • Electrical & Electronic Materials
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    • v.10 no.8
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    • pp.763-769
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    • 1997
  • In this study we have synthesized Zno:Eu phosphors under various sintering atmospheres and temperatures. The analysis of X-ray diffractometer measurement indicates that for Zno:EuCl$_3$ phosphors sintered in air and vacuum 뗘 exists in the host lattice as Eu$_2$O$_3$and EuOCl respectively. From the photoluminescence for the phosphors sintered in vacuum Eu removes the broad-band emission of the ZnO host consequently isolating the red emission due to Eu$^{3+}$ ion and improves the color purity of red emission. The photoluminescence excitation and time resolving spectrum measurements suggest that energy-transfer process occurres from the self-activated defect center in ZnO host the Eu$^{3+}$ ion which exist in the host lattice in the form of EuOCl.

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Synthesis, Characterization and Antimicrobial Activity of Novel Pharmacophores Incorporating Imidazoline-Oxazoline Scaffold

  • Barakat, Assem;Al-Majid, Abdullah Mohammed;Al-Qahatany, Faisal M.;Islam, Mohammad Shahidul;Al-Agamy, Mohamed H.M.
    • Bulletin of the Korean Chemical Society
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    • v.35 no.2
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    • pp.562-568
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    • 2014
  • In this work, synthesis, characterization and antimicrobial activity of series of imidazolines-oxazolines scaffolds 5a-f and 10a-d have been investigated. All the imidazolines-oxazolines derivatives were prepared from acid derivatives 1 and 6a-c, and enantiomerically pure (S)-2-amino-3-methyl-1-butanol in four steps with excellent optical purity. The structures of all newly synthesized compounds have been elucidated by $^1H$, $^{13}C$ NMR, GCMS, and IR spectrometry. Their purity was confirmed using elemental analysis. Some newly synthesized compounds were examined to in-vitro antimicrobial activity. Among the prepared products 10d was found to exhibits the most active against all tested bacteria and fungi with minimal inhibitory concentration (MIC) ranged between 21.9 and $42.6{\mu}g/mL$.

A Study on the Symbolism Shown by the Costumes in the Portraits of Elizabeth I (엘리자베스 1세의 초상화에 내재된 복식요소의 상징성 연구)

  • 배수정
    • Korean Journal of Human Ecology
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    • v.3 no.1
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    • pp.73-87
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    • 2000
  • The purpose of this thesis is to make clear the symbolism expressed by the gorgeous costume elements in the portraits of Elizabeth 1. After English paintings in 16th century and the Portraits of Elizabeth I being investigated in view of its characteristics, the symbolism in the costume of the portraits was studied in analysis. The flowers, the pearls and the sieve denoting a pure virgin predominantly appeared, snake for discretion and wisdom, phoenix for eternal youth and renewal, pelican for motherhood, and eyes and ears for almightiness and sound judgement as an utmost power was found. The color was mainly of black or white and sometimes of these two mixtures. The white means a purity and black, eternity and the mixture of them signifies a virtue of purity. This thesis may help people understand the gorgeous costume of Elizabeth 1. not as an external extravagance, but as an internal emblem or signs delivering its specific significance.

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