• 제목/요약/키워드: impurity analysis

검색결과 227건 처리시간 0.023초

A Comparison of Analytical Methods for the Content and Purity of Cefradine

  • Hyun, Myung-Ho;Jeong, Euh-Duck;Shin, Min-Seob;Jin, Jong-Sung
    • Bulletin of the Korean Chemical Society
    • /
    • 제29권6호
    • /
    • pp.1185-1189
    • /
    • 2008
  • Two HPLC methods such as cefadroxil and cefalexin methods were compared in their performance for the quantitative analysis of the content and purity of $\beta$ -lactamic antibiotic, cefradine, for six bulk drug samples. Between the two methods, the cefadroxil method prescribed by the European Pharmacopoeia (EP) for the determination of impurities in cefradoxil was superior to the cefalexin method prescribed by the EP and by the United States Pharmacopeia (USP) for the determination of cefalexin impurity in cefradine in terms of the greater stability of the chromatogram baselines and the higher precision, i.e., the lower % relative standard deviation (RSD). Based on the comparison of the two HPLC methods, the cefadroxil method was recommended to replace the TLC method, which has been prescribed by the EP as the official method for determination of extraneous impurities in cefradine.

열처리 분위기에 따른 $MgB_2$ 초전도의 특성 변화 ($MgB_2$ Superconducting Properties under Different Annealing Condition)

  • 정국채;김영국
    • 한국전기전자재료학회:학술대회논문집
    • /
    • 한국전기전자재료학회 2009년도 하계학술대회 논문집
    • /
    • pp.362-362
    • /
    • 2009
  • $MgB_2$ bulk samples were sintered at different ambient. In this work, high purity Ar gas was added with oxygen and hydrogen gas, which can be regarded as impurity in a sense, as a possible dopant in the $MgB_2$. It was found that oxygen in the sintering ambient leads to a decrease in the critical current density $J_c$ at self field and lower fields. However, we can obtained higher $J_c$ at higher fields. It was also noted that $MgB_2$ samples sintered with 5% hydrogen in Ar revealed the increased $J_c$ at all fields compared to those processed in pure Ar ambient. From the XRD and FESEM analysis, the impurity gas in Ar can refine the $MgB_2$ grain size and result in increased grain. boundary, which can act as a strong flux pinning sites in $MgB_2$ samples. Also discussed are the effects of sintering ambient on irreversibility field, $H_{irr}$ and the upper critical field, $H_{C2}$.

  • PDF

Preparation of Carbon Nanofibers by Catalytic CVD and Their Purification

  • Lim, Jae-Seok;Lee, Seong-Young;Park, Sei-Min;Kim, Myung-Soo
    • Carbon letters
    • /
    • 제6권1호
    • /
    • pp.31-40
    • /
    • 2005
  • The carbon nanofibers (CNFs) were synthesized through the catalytic decomposition of hydrocarbons in a quartz tube reactor. The CNFs prepared from $C_3H_8$ at $550^{\circ}C$ was selected as the purification sample due to the higher content of impurity than that prepared from other conditions. In this study, we carried out the purification of CNFs by oxidation in air or carbon dioxide after acid treatment, and investigated the influence of purification parameters such as kind of acid, concentration, oxidation time, and oxidation temperature on the structure of CNFs. The metal catalysts could be easily eliminated from the prepared CNFs by liquid phase purification with various acids and it was verified by ICP analysis, in which, for example, Ni content decreased from 2.51% to 0.18% with 8% nitric acid. However, the particulate carbon and heterogeneous fibers were not removed from the prepared CNFs by thermal oxidation in air and carbon dioxide. This result can be explained by that the direction of graphene sheet in CNFs is vertical to the fiber axis and the CNFs are oxidized at about the similar rate with the impurity carbon.

  • PDF

금속간화합물 Ti-51at%Al 분말 내의 불순물 분석 (Impurity Analysis of Intermetallic Ti-51at% Al Powders Produced by Plasma Rotating Electrode Process)

  • 최국선;이동희
    • 한국재료학회지
    • /
    • 제2권2호
    • /
    • pp.157-160
    • /
    • 1992
  • 플라즈마 회전전극법으로 제조된 Ti-51at%Al 금속간화합물 분말에 함유된 불순물의 함량변화를 분석하였다. 산소와 탄소의 함량은 각각 600 및 200ppm 정도로 분말입도에 따라 변하였으며, 이는 주로 원재료에 포함된 불순물의 영향이었다. AES 분석에 의하면 분말표면 산화물은 주로 Ti 및 Al과 산소 및 탄소의 복합화합물로 구성되었으며, 그 두께는 약 100 및 $200{\mu}m$ 크기의 분말에 대하여 각각 7 및 3.4nm 정도로 측정되었다. 분말의 제조로 산소와 탄소의 함량이 오히려 감소되는것의 구체적인 기구는 아직 확인되지 않았으나 플라즈마 고열에 의한 정련현상에 기인하는 것으로 생각된다.

  • PDF

A Technique to Minimize Impurity Signal from Blank Rhenium Filaments for Highly Accurate TIMS Measurements of Uranium in Ultra-Trace Levels

  • Park, Jong-Ho;Choi, In-Hee;Song, Kyu-Seok
    • Mass Spectrometry Letters
    • /
    • 제1권1호
    • /
    • pp.17-20
    • /
    • 2010
  • As background significantly affects measurement accuracy and a detection limit in determination of the trace amounts of uranium, it is necessary to minimize the impurities in the filaments used for thermal ionization mass spectrometry (TIMS). We have varied the degassing condition such as the heating currents and duration times to reduce the backgrounds from the filaments prepared with zone-refined rhenium tape. The most efficient degassing condition of the heating current and the duration time was determined as 3.5 A and 60 min, respectively. The TIMS measurement combined with the isotope dilution mass spectrometry (IDMS) technique showed that the uranium backgrounds were determined to be in a few fg level from blank rhenium filaments. The background minimized filaments were utilized to measure the uranium isotope ratios of a U030 (NIST) standard sample. The excellent agreement of the measurement with the certified isotope ratios showed that the degassing procedure optimized in this study efficiently reduced the impurity signals of uranium from blank rhenium filaments to a negligible level.

A Study on Reusable Metal Component as Burnable Absorber Through Monte Carlo Depletion Analysis

  • Muth, Boravy;Alrawash, Saed;Park, Chang Je;Kim, Jong Sung
    • 방사성폐기물학회지
    • /
    • 제18권4호
    • /
    • pp.481-496
    • /
    • 2020
  • After nuclear power plants are permanently shut down and decommissioned, the remaining irradiated metal components such as stainless steel, carbon steel, and Inconel can be used as neutron absorber. This study investigates the possibility of reusing these metal components as neutron absorber materials, that is burnable poison. The absorption cross section of the irradiated metals did not lose their chemical properties and performance even if they were irradiated over 40-50 years in the NPPs. To examine the absorption capability of the waste metals, the lattice calculations of WH 17×17 fuel assembly were analyzed. From the results, Inconel-718 significantly hold-down fuel assembly excess reactivity compared to stainless steel 304 and carbon steel because Inconel-718 contains a small amount of boron nuclide. From the results, a 20wt% impurity of boron in irradiated Inconel-718 enhances the excess reactivity suppression. The application of irradiated Inconel-718 as a burnable absorber for SMR core was investigated. The irradiated Inconel-718 impurity with 20wt% of boron content can maintain and suppress the whole core reactivity. We emphasize that the irradiated metal components can be used as burnable absorber materials to control the reactivity of commercial reactor power and small modular reactors.

SIMS와 GDMS를 이용한 구리와 탄탈 박막내의 주요불순물 분석 (Analysis of dominant impurities in Cu and Ta films using SIMS and GDMS)

  • 임재원
    • 한국진공학회지
    • /
    • 제13권2호
    • /
    • pp.79-85
    • /
    • 2004
  • 본 논문은 구리와 탄탈 박막내에 불순물로써 함유되기 쉬운 수소와 탄소, 그리고 산소 원소에 대해 이차이온 질량분석기(secondary ion mass spectrometry)와 글로우방전 질량분석기(glow discharge mass spectrometry)를 이용하여 분석하였고, 이들의 분석결과에 대해서 고찰하였다. 구리와 탄탈 박막은 실리콘 기판 위에 비질량 분리형 이온빔 증착장비를 이용하여 기판 바이어스를 걸지 않은 경우와 -50 V(구리 박막) 또는 -125 V(탄탈 박막)의 기판바이어스를 걸은 상태에서 증착하였다. 세슘 이온빔을 이용하여 분석한 SIMS 결과에서, 기판 바이어스를 걸지 않은 경우, 상당히 많은 피크들이 강하게 관찰되었는데 이는 위의 주요불순물들의 결합에 의한 상태로 검출된 것으로 이들 주요불순물들의 조합에 의해 가능한 질량번호를 산출하여 SIMS 결과의 모든 피크들을 해석할 수 있었다. 또한, 박막 내의 주요불순물들의 정량적인 GDMS 분석에 의해 SIMS 결과와의 일치성을 확인할 수 있었다.

Establishing and validating an HPLC protocol for pralsetinib impurities analysis, coupled with HPLC-MS/MS identification of stress degradation products

  • Rajesh Varma Bhupatiraju;Pavani Peddi;Venkata Swamy Tangeti;Battula Sreenivasa Rao
    • 분석과학
    • /
    • 제37권5호
    • /
    • pp.280-294
    • /
    • 2024
  • This study introduces a novel analytical method for the assessment of pralsetinib impurities and degradation products (DPs), addressing critical gaps in existing methodologies. This research aims to develop a robust HPLC method for impurity analysis, characterize degradation products using LC-MS, and evaluate the environmental impact of the method. The study began by optimizing HPLC conditions with various columns and buffers, ultimately achieving successful separation using an XBridge® RP-C18 column with ethanol as solvent A and 50 mM formic acid at pH 2.9. This setup provided excellent peak resolution and symmetry, essential for reliable stability studies. The developed HPLC method was then adapted for HPLC-MS/MS, enhancing sensitivity and detection efficiency of DPs. Stress degradation studies of pralsetinib under different conditions (acidic, basic, oxidative, thermal, and photolytic) revealed significant degradation under acidic (29.3 %) and basic (21.5 %) conditions, with several DPs identified. Oxidative stress resulted in 19.8 % degradation, while thermal and photolytic conditions caused minimal degradation. HPLC-MS/MS analysis identified structures of five degradation products, providing detailed insights into pralsetinib's stability and degradation pathways. Method validation followed ICH guidelines Q2(R1), confirming method's specificity, selectivity, sensitivity, linearity, accuracy, precision, and robustness. The method exhibited strong linearity with a coefficient of determination (r2) greater than 0.999 for pralsetinib and its impurities. This method advances impurity detection and DPs characterization, ensuring the quality and safety of pralsetinib. Additionally, method's environmental impact was assessed, aligning with sustainable analytical practices. These findings provide essential data on pralsetinib's stability, guiding storage conditions and ensuring its efficacy and safety in pharmaceutical applications.

[Li]/[Nb]조성비 변화에 따른 iron-doped $LiNbO_3$ 결정의 특성분석

  • 한지웅;원종원;오근호
    • 한국결정성장학회:학술대회논문집
    • /
    • 한국결정성장학회 1997년도 Proceedings of the 13th KACG Technical Meeting `97 Industrial Crystallization Symposium(ICS)-Doosan Resort, Chunchon, October 30-31, 1997
    • /
    • pp.111-115
    • /
    • 1997
  • Iron-doped LiNbO$_3$ crystals were grown by floating zone(FZ) method with different [Li]/[Nb] ratio in order to investigate doping effects of transition metal impurity in LiNbO$_3$ crystal. The grown crystals were analyized edge in UV/VIS/IR spectrometry and EPMA(electron probe micro-analysis). The absorption edge in UV-VIS region and OH-absorption peak in IR region were investigated. The change of Fe concentration along the solidification direction was also investigated

  • PDF

홍천산(洪川産) Silica의 특성연구(特性硏究) (Characterization of Silica in Hongcheon)

  • 신건철
    • 산업기술연구
    • /
    • 제4권
    • /
    • pp.55-60
    • /
    • 1984
  • Silicastone of Hongcheon in Kangweon province was characterized by means of chemical analysis, scanning electron microscope, polarization microscope and x-ray diffractometer. The results showed that the purity of $SiO_2$ is over 97.64 in Wt-%. It also contains 0.046-0.417 Wt-% $Fe_2O_3$ and some others as impurity. The impuity exist as a isolated mineral type of hematite, sericite, apatite etc.

  • PDF