• 제목/요약/키워드: Sample preparation method

검색결과 461건 처리시간 0.029초

프탈로시아닌계 광전도성 유기박막의 제조에 관한 연구 (A study on the preparation of phthalocyanine optoelectric thin films)

  • 박구범;조기선;이덕출
    • E2M - 전기 전자와 첨단 소재
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    • 제7권5호
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    • pp.409-416
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    • 1994
  • A double layered photoreceptor using phthalocyanine dye was made by dip-coating method. The under cutting layer(UCL) was coated with A1$\_$2/O$\_$3/ or polyamide, and the charge generation layer(CGL) was formed by .tau.-type metal-free phthalocyanine. The oxadiazole was used as a charge transport layer(CTL) and polycarbonate and poly(vinyl butyral) was employed as a host polymer. The .tau.-H$\_$2/Pc had an absorption peak around 780nm, which coincided with the emitting wavelengths of GaAlAs diode lasers. Maximum charge acceptance of CTL that gives thickness of 12.mu.m was -900V by corona charge of -6.0kV. In photo-induced discharge measurements, residual potential was less than -20V and sufficient for ordinary use, and sample films using of poly(vinyl butyral) was showed good charge retention. In printing test, drum that was employed polycarbonate as a host polymer showed the good print quality.

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Purity assessment using quantitative NMR: establishment of SI traceability in organic analysis

  • Choi, Kihwan
    • 한국자기공명학회논문지
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    • 제24권1호
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    • pp.30-37
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    • 2020
  • Quantitative nuclear magnetic resonance (qNMR) has been gaining attention as a purity assessment method. In particular, qNMR is recognized as the primary method to realize the Internal System of Units (SI) in organic analysis. The capability of quantitative analysis is recognized as the beginning of NMR development. NMR signals are proportional to the number of nuclei and qNMR has been used in various fields, such as metabolomics and food and pharmaceutical analysis. However, careful sample preparation and thorough optimization of measurement parameters are required to obtain accurate and reliable results. In this review, quantitative methods used in qNMR are discussed, and the important factors to be considered also introduced. The recent development of qNMR techniques including combination with chromatography and, multidimensional NMR are also presented.

The comparison of relative reliability on biaxial and three point flexure strength methods of light curing composite resin

  • Seo, Deog-Gyu;Rho, Byoung-Duck
    • 대한치과보존학회:학술대회논문집
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    • 대한치과보존학회 2003년도 제120회 추계학술대회 제 5차 한ㆍ일 치과보존학회 공동학술대회
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    • pp.575-575
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    • 2003
  • The majority of studies comparing the mechanical properties of brittle dental restorative materials now include use of the Weibull Modulus (m). This modulus is determined from analysis of the statistical distribution of strength measurements, which can be determined using a variety of methods, including biaxial flexure, 3pt bend and 4pt bend. In comparing materials it is usually implicitly assumed that the modulus (m) is independent of test method although it is recognised to be highly dependent on flaw distributions. However, in some cases flaw distributions can be modified by sample preparation and test method may modify stressing patterns. This study investigated the pattern of strength and m in two light setting materials.

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Characterization of Spinel Lithium Manganite Prepared by Citrate Sol-Gel Method

  • 홍영식;박휴범;이지은;한치환;김시중
    • Bulletin of the Korean Chemical Society
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    • 제18권11호
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    • pp.1153-1158
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    • 1997
  • The powder characteristics of LiMn2O4 prepared by the citrate sol-gel method have been investigated. The optimum pH for the preparation of homogeneous citrate gel was calculated by the theoretical consideration of thermodynamic equilibrium constants for metal-citrate complexes and metal salts. The obtained citrate gel was prefired at 300 ℃ and calcined at 300-700 ℃ for 1 h. The obtained powders were characterized by TG/DSC, FT-IR spectrometer, X-ray diffractometer, SQUID magnetometer, SEM, and particle size analyzer. It was observed that the mixed phases of spinel LiMn2O4 and Mn3O4 were transformed into spinel LiMn2O4 phase and the vibrational bands due to the carbonate and nitrate were also disappeared over 400 ℃. At temperatures below 150 K, inverse molar susceptibilities of every sample began to show an antiferromagnetic ordering of Mn magnetic moments.

고속 액체 크로마토그라피에 의한 cis- 및 trans-Neopynamin과 Fenitrothion의 분리 정량에 관한 연구 (Studies on the Differential Determination of cis-, and trans-Neopynamin and Fenitrothion by High Pressure Liguid Chromatography)

  • 이왕규;정해수
    • 약학회지
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    • 제24권2호
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    • pp.117-122
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    • 1980
  • A new application of high pressure liquid chromatography for the determination of fenitrothion and cis- and trans-neopynamin in insecticidal preparations was investigated. Optimum conditions for a good separation and determination were determined; solvent system: dichloromethane + n-hexane = 17 + 83; Bow rate: 0.5ml/min; column: u-porasil ($4mm{\times}3Ocm$); absorbance wavelength: 254nm; 0.05 AUFS and sample size: 30 ul. Recovery of fenicrothion, cis- and trans-neopynamin from mixed artificial preparations was 99.6%, 99.7% and 99.8% respectively. Also reproducibility tests showed that the coefficient of variation was 0.89% for fenitrothion, 0.74% cis-neopynamin and 1.1% for trans-neopynamin. There was no interference with insecticidal preparation containing DDVP, allethrin, S-421 and kerosene. HPLC method was rapid, accurate and it gave better reproducibility and higher sensitivity than any other analytical method. It was considered that HPLC could be greatly applied to the analysis of fenitrothion and neopynamin in insecticidal preparations.

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Chiral Derivatization of Hydroxycarboxylic Acids Using 2,4,6-Trichlorobenzoyl Chloride as a Highly Efficient Regioselective Esterification Reagent for Gas Chromatography-Mass Spectrometry

  • Park, Jeong Hyeok;Han, Sang Yun
    • Mass Spectrometry Letters
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    • 제11권4호
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    • pp.103-107
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    • 2020
  • We report the application of 2,4,6-trichlorobenzoyl chloride (often referred to as Yamaguchi esterification reagent) for the selective derivatization of the carboxylic group for GC-MS with the sample preparation method optimized for GC-MS analysis. The reagent was shown to be capable of selectively turning the carboxylic group into a reaction center, i.e., anhydride, of which the further reaction was directed to a near complete formation of required esters by unique steric and electronic effects of the reagent. Using the developed method, the chiral separation of hydroxycarboxylic acids by GC-MS using non-chiral columns was successfully demonstrated.

High Pressure Freezing (HPF)을 이용한 조류 Ptilota filicina의 미세구조 관찰:HPF 고정법과 화학 고정법의 비교 (Ultrastructures of Ptilota filicina (Rhodophyta) by High Pressure Freezing(HPF): Comparison of HPF Fixation and Chemical Fixation)

  • 이상희;김윤중;정종만;김진규;김영민;권희석;문원진;이석훈
    • ALGAE
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    • 제21권4호
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    • pp.479-483
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    • 2006
  • In preparation of the biological samples for electron microscopy, the chemical fixation by glutaraldehyde, paraformaldehyde, and OsO4 has been generally used for a long time. However, the chemical fixation method has some problems: the infiltration time is a little bit long and the ultrastructure of cell or tissue transforms before complete fixation of sample. So, recently, cryo-fixation is considered more often in biomedical field. In this study, we compared High Pressure Freezing (HPF) method with chemical fixation method using a algal sample (Ptilota filicina J. Agardh), which was difficult to fix using chemical fixation method. In chloroplast, the ultrastructure of thylakoid lamella and phycobilisome can not show clearly by chemical fixation. In this study we could observe the ultrastructure of thylakoid lamella and phycobilisome of chloroplast very clearly using HPF fixation. An improved images of ultrastructures of nucleus, mitochondrion and floridean starch could obtain. These results suggest that HPF method is very useful method in algal specimen for electron microscopy.

Multi-class, Multi-residue Analysis of 59 Veterinary Drugs in Livestock Products for Screening and Quantification Using Liquid Chromatography-tandem Mass Spectrometry

  • Yu Ra Kim;Sun Young Park;Tae Ho Lee;Ji Young Kim;Jang-Duck Choi;Guiim Moon
    • 한국환경농학회지
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    • 제41권4호
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    • pp.288-309
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    • 2022
  • BACKGROUND: The objective of this study was to develop a comprehensive and simple method for the simultaneous determination of 59 veterinary drug residues in livestock products for safety management. METHODS AND RESULTS: For sample preparation, we used a modified liquid extraction method, according to which the sample was extracted with 80% acetonitrile followed by incubation at -20℃ for 30 min. After centrifugation, an aliquot of the extract was evaporated to dryness at 40℃ and analyzed using liquid chromatography combined with tandem mass spectrometry. The method was validated at three concentration levels for beef, pork, chicken, egg, and milk in accordance with the Codex Alimentarius Commission/Guidelines 71-2009. Quantitative analysis was performed using a matrix-matched calibration. As a results, at least 52 (77.6%) out of 66 compounds showed the proper method validation results in terms of both recovery of the target compound and coefficient of variation required by Codex guidelines in livestock products. The limit of quantitation of the method ranged from 0.2 to 1119.6 ng g-1 for all matrices. CONCLUSION(S): This method was accurate, effective, and comprehensive for 59 veterinary drugs determination in livestock products, and can be used to investigate veterinary drugs from different chemical families for safety management in livestock products.

일반소비자들의 고기 요리에 대한 기호도 및 소비행태 (Preferences and Consumption Patterns of General Consumers of Meat Dishes)

  • 김은미;서상희;이민아;권기현;전기홍
    • 한국식생활문화학회지
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    • 제25권3호
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    • pp.251-261
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    • 2010
  • This paper examines the dining tendencies of Koreans toward meat dishes and their related factors, with 301 people residing in Korea as subjects. We questioned this population on their restaurant choices, eating habits, preferences and a dislike with respect to method of cooking. All age groups, with the exception of 50~60 year-olds, were found to consume meat dishes in specialized restaurants. The selection factor for restaurants varied, depending on the age group: affordable cost was the most important factor for whom under 20 year-old. Whereas 20-40 year-old people considered taste and ambience the most for choosing restaurant. The 50-60 year-old people found to seek for convenient restaurant. In terms of the most preferred parts of beef, 20-30 year-old people preferred tenderloin (42.3%) while 40-60 year-old people preferred sirloin (45.6% and 41.2% each). All the other age groups preferred ribs the most (It was also found that) men preferred the rib parts and women preferred tenderloin. With respect to pork, all age groups preferred pork belly, with the highest response rate in the under 20 age group. When consuming meat dishes, 91.0% of respondents pointed to roasting as the most frequent preparation method, the reason being good taste was deemed the highest number of responses. In a survey on preference for stewed meats, 74.8% of the sample pool was found to prefer stew dishes but 24.9% of respondents provided negative answers, the reason for dislike was found to be poor taste for women, and both a long preparation time and poor taste for men. In fact, regardless of marital status, a high number of responses were given for poor taste as the reason for disliking stew dishes. Based on the examined factors for inconveniences in preparing meat dishes, the most common inconvenience factor was the odor of meat left on clothes after the dining experience, followed by the smoke generated in roasting meat, and the safety risk involved with changing the grill. In terms of stir fry preparation, the negative thoughts were due to the splashing of food and spices while cooking, followed by the meat odor left on clothes after dining experience, and the sanitation level of the cooking containers. For deep frying the sanitation level of cooking containers was the biggest reason for dislike, followed by splashing of food when preparing. Lastly, it was indicated that the problem of steaming method was a difficulty of judging the portion, on the top of this, people found that the sanitation level of cooking container and a long preparation time were also the problem of this cooking method.

원소별 함량결정을 위한 PIXE 스펙트럼 분석에 관한 연구 (A Study on PIXE Spectrum Analysis for the Determination of Elemental Contents)

  • ;배영덕
    • Nuclear Engineering and Technology
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    • 제22권2호
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    • pp.101-107
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    • 1990
  • PIXE(Proton Induced X-ray Emission)법을 수도물, 적포도주, 소변 및 흑분시료의 미량원소분석에 적용하여 보았다. SNU 1.5-MV 탄뎀 반데 그라프 가속기에서 얻은 1.202 MeV 양성자빔을 시료에 조사시켰으며 X-선 스펙트럼은 Si(Li) 스펙트로미터로 측정하였다. 분석의 감도를 높이기 위해 수도물은 증발법을 사용하여 농축하였다. 표준시료로서 흑분에는 Ni가루를 섞었고 다추 시료에는 yttrium용액을 첨가하였다. PIXE 스펙트럼은 AXIL(Analytical X-ray Analysis by Iterative Least-squares) 컴퓨터 프로그램을 사용하여 분석하였는데, 최소자승법은 Marquardt 알고리즘에 기초하고 있다. 수도물에서는 Mg, Al, Si, Ti, Fe, Zn등과 같은 원소들이 ppm이하의 함량으로 분석되었다 농축을 하지 않은 적포도주 시료에서는 Ti 원소가 3 ppm의 함량으로 검출되었다. 결론적으로 표준시료를 쓴 상대측정법에 의한 수용액시료분석에 PIXE법이 적합함을 입증할 수 있었으며, 정확한 X-선 발생단면적을 사용하고 시료준비기술을 개발하면 이 분석법을 향상시킬 수 있으리라 기대한다.

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