• 제목/요약/키워드: Sample preparation method

검색결과 461건 처리시간 0.03초

주사전자현미경상에서의 고분자 미세구조 관찰 (A New Sample Preparation Technique for SEM Observation of Polyolefin Microstructure)

  • 박제명
    • Applied Microscopy
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    • 제29권4호
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    • pp.405-415
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    • 1999
  • 일반적으로 고분자 미세구조 관찰은 microtomming, solution casting, carbon replica, staining법 등을 이용하여 시료를 전처리한 시료를 TEM을 이용하여 관찰한다. 이러한 시편 전처리 법은 높은 재연성 등으로 널리 이용되고 있으나 기기 의존적이거나 시편전처리 과정이 복잡한 단점이 있다. 본 연구는 주사전자현미경을 이용한 고분자미세구조 관찰 및 이를 위한 시편준비법에 관한 것이다. 이를 위하여 본 연구에서는 기존에 제한된 화학적에칭법을 개선하여 각종 polyolefin 종류 및 형상에 맞게 전처리하여 SEM을 이용한 고분자 미세구조 연구를 수행하였다. 본 연구를 통하여 과망간산 에칭방법이 주사전자현미경을 이용한 polyolefin 미세구조 관찰에 적합함을 알 수 있었으며, 에칭조건은 시료의 종류와 관찰대상에 맞게 과망간산/인산, 과망간산/인산/황산 등의 조성과 etchant 의 함량비, 에칭시간의 단순한 조절로 가능하다. 본 연구의 에칭법을 이용하여 관찰한 고분자의 미세구조는 iPP 구정의 characterization, 라멜라 특성연구, 고분자 blend 등 기존 연구의 관찰결과를 잘 재연하고 있어 고분자의 모폴로지 특성 뿐만 아니라 blend와 film등 상업적 제품 연구 및 개발에 유용한 방법임을 알 수 있었다.

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유자청을 첨가한 발아현미다식의 품질 특성 (Quality Characteristics of Sprouted Brown Rice Dasik with Yujacheong Added)

  • 이영숙;김애정;노정옥
    • 한국식품조리과학회지
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    • 제24권4호
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    • pp.494-500
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    • 2008
  • The principal objective of this study was to assess the quality characteristics of Sprouted Brown Rice Dasik(SBRD) manufactured with various addition levels of honey and Yujacheong(Yuja syrup and Yuja sarcocarp) in accordance with the traditional method for the preparation of Korean Dasik(a kind of cookie). The nutritional components, color value, physical tests, volatile compounds, and sensory evaluation of SBRD to which Yujacheong was added were conducted. The results were summarized as follows. In SBRD to which Yujacheong had been added, the moisture contents and crude fat content did not differ significantly among the sample groups, and the contents of crude protein and crude ash increased with increasing additions of Yuja syrup and Yuja sarcocarp. The pH(p<0.001) and sweetness(p<0.001) were significantly higher in sample D1 than in samples D2 and D4. The L color value was highest in D2, the a value was highest in D3, and the b value was highest in sample D2. The texture property analysis showed that the cohesiveness, springiness, gumminess, and chewiness of SBRD to which Yujacheong was added were all significantly higher compared to sample D1. According to the results of our volatile analysis, the D1 and other experimental groups evidenced different flavors and antibacterial compositions. According to the results of our sensory evaluation, the appearance of the D1 sample was superior to the other samples. However, flavor, taste, texture, and overall preference were higher in the samples to which Yuja syrup and Yuja sarcocarp were added. These results indicate that SBRD to which Yujacheong was added, and particularly those to which Yuja syrup was added, is superior to Dasik prepared with honey in terms of flavor and taste, and this method will improve the flavor and preparation time, due to its lower pH.

Effect of Preparation on Structure and Magnetic Properties of ZnFe2O4

  • Niyaifar, Mohammad
    • Journal of Magnetics
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    • 제19권2호
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    • pp.101-105
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    • 2014
  • In this work, Zinc ferrite nanoparticles have been prepared by various methods, conventional (ZC), mechanochemical processing (ZM) and Sol-Gel (ZS) method, to compare their structural and magnetic properties. The cation distribution obtained from XRD shows the degrees of inversions are 4%, 14.8%, and 16.4% from the normal $ZnFe_2O_4$ structure. Fourier transform infrared spectroscopy (FT-IR) confirms changes in cation distribution of $ZnFe_2O_4$ fabricated by sol-gel and mechanochemical processing. The $^{57}Fe$ M$\ddot{o}$ssbauer spectra of the samples were recorded at room temperature. The spectra exhibit a line broadening. The magnetic properties of the samples were studied by vibration sample magnetometer (VSM) at room temperature and the results show that the sample ZM has ferrimagnetic behaviour.

Multi-class Analysis of Exposure Chemicals in Deciduous Teeth by Liquid Chromatography-Mass Spectrometry: Preliminary Studies on Sample Preparation Methods

  • Lee, Yujin;Seo, Eunji;Park, Jun Young;Bae, Kwang-Hak;Lee, Jaeick;Cha, Sangwon
    • Mass Spectrometry Letters
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    • 제9권4호
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    • pp.110-114
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    • 2018
  • Since accumulation of chemicals in deciduous teeth can occur from the second trimester of fetal development to shedding, a deciduous tooth has been considered as an attractive biomatrix for estimating individual chemical exposures recently. Therefore, detection of organic chemicals from teeth has received an increasing attention in exposomics research. Most previous studies on organic chemical analysis of teeth not only focused on a few targeted chemicals but also ignored potential contaminants from an enamel surface or a dental pulp. Recently, our group started developing a multi-class organic analysis method for deciduous teeth and tried to find a proper incubation condition of tooth materials. Our results showed that incubation with methanolic HCl provided the best performance among tested.

Replacing critical point drying with a low-cost chemical drying provides comparable surface image quality of glandular trichomes from leaves of Millingtonia hortensis L. f. in scanning electron micrograph

  • Raktim Bhattacharya;Sulagna Saha;Olga Kostina;Lyudmila Muravnik;Adinpunya Mitra
    • Applied Microscopy
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    • 제50권
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    • pp.15.1-15.6
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    • 2020
  • Sample preparation including dehydration and drying of samples is the most intricate part of scanning electron microscopy. Most current sample preparation protocols use critical-point drying with liquid carbon dioxide. Very few studies have reported samples that were dried using chemical reagents. In this study, we used hexamethyldisilazane, a chemical drying reagent, to prepare plant samples. As glandular trichomes are among the most fragile and sensitive surface structures found on plants, we used Millingtonia hortensis leaf samples as our study materials because they contain abundant glandular trichomes. The results obtained using this new method are identical to those produced via critical-point drying.

시료 조건 및 측정방법에 따른 셀룰로오스의 결정화도 평가 (Determination of crystallinity index of cellulose depending on sample preparation and analysis instruments)

  • 안정언;윤혜정;정양진;김태영
    • 펄프종이기술
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    • 제44권4호
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    • pp.43-50
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    • 2012
  • The crystallinity index is an important characteristic of cellulose. The crystallinity value is different depending on the adopted instrument. In this study, we determined a crystallinity index of cotton and wood celluloses using wide-angle X-ray scattering (WAXS), powder X-ray diffractometer (PXRD), and cross polarization/magic angle spinning solid-state $^{13}C$ nuclear magnetic resonance spectroscopy (CP/MAS solid-state $^{13}C$ NMR). The specimen was prepared in forms of powder, sheet and pallet. With the comparison of the obtained crystallinity indices of the cellulose, the effects of the analysis instrument, the sample preparation and analysis method were investigated. Among three instruments, the crystallinity indices by PXRD and NMR had a good relationship and reproducibility, and WAXS gave the crystallinity index with poor reproducibility. In the case of analysis methods of crystallinity indices, the Segal method showed higher value than that of the Ruland-Vonk method. We expect that this study would be applicable to evaluate the crystallinity index of various cellulose materials with accuracy and reproducibility.

Effect of particle size and scanning cup type for near infrared reflection on the soil property measurement

  • Ryu, Kwan-Shig;Cho, Rae-Kwang;Park, Woo-Churl;Kim, Bok-Jin
    • Near Infrared Analysis
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    • 제1권2호
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    • pp.35-39
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    • 2000
  • The purpose of this research was to find out suitable soil sample preparation and sample holding tools for NIR reflection radiation for estimating soil components. NIR reflectance was scanned at 2nm intervals from 1,100 to 2,500nm with an InfraAlyzer 500(Bran+Luebbe Co.). Coarse(2.0mm) and fine(0.5mm) soil sample and various sample holding tools were used to obtain mean diffuse reflection of the soil for the calibration and validation of the calibration set in estimating moisture, organic matter and total nitrogen of the soils. Multiple linear regression was used to obtain the best correlation of NIR spectroscopy method. Correlation of NIR spectroscopy method. Correlation of NIR spectra for finely and coarsely sized soil did not show much difference. The standard errors of prediction(SE) using different types of sample holding tools for organic matter, total nitrogen and soil moisture were better than 0.765, 0.041 and 0.63% respectively. From the results it can be concluded that NIR spectroscopy with flow type cell could be used as a fast routine testing method in quantitative determination of organic matter, total nitrogen and soil moisture.

A novel method for predicting the swelling potential of clay-bearing rocks

  • Moosavi, Mahdi;Ghadernejad, Saleh
    • Geomechanics and Engineering
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    • 제27권6호
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    • pp.615-626
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    • 2021
  • The main objective of this study is to present a fast and reliable approach to predict the swelling potential of clay-bearing rocks. Investigations showed that there is a good correlation between the swelling potential of a rock and its desire to absorb water due to its clay content which could be measured using the "Contact Angle" test as one of the most common ways to determine the wettability. In this test, the angle between a water drop and the flat rock surface on which it rests is measured. The present method is very fast and returns repeatable results and requires minimal sample preparation. Only having a saw-cut surface of a sample with any shape is all one needs to perform this test. The logic behind this approach is that the swelling potential of a rock is a function of its mineral content and molecular structure, which are not only distributed in the bulk of the sample but also reflected on its surface. Therefore, to evaluate swelling behavior, it is not necessary to wait for a sample to get wet all the way to its "internal structure" (which, due to the low permeability of clay-bearing rocks, is very slow and time-consuming). Instead, one can have a good sense of swelling potential by studying its surface. Parametric studies on the effect of moisture content, porosity, and surface roughness on the contact angle measurements showed that using a saw-cut oven-dried sample is a convenient way to evaluate the swelling potential by this method.

Alumina dummy 충전재를 이용한 GaN 기반 박막재료의 단면 TEM 시편준비 (Cross-sectional TEM Specimen Preparation of GaN-based Thinfilm Materials Using Alumina Dummy Filler)

  • 오상호;최주형;송경;정종만;김진규;유인근;유석재;김영민
    • Applied Microscopy
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    • 제39권3호
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    • pp.277-281
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    • 2009
  • Practical difficulties for preparing a good crosssectional specimen of GaN-based materials for transmission electron microscopy have arisen due to large difference of mechanical properties between hard ceramic substrate and soft GaN-layered materials. Uneven polishing, sudden cracking, delamination, and selective sputtering during the conventional wedge polishing technique are often encountered as experimental hindrances. The preparation technique based on Strecker's method can be applied to overcome these difficulties, which eventually leads to mechanically stable TEM samples independent of the mechanical properties of materials. The basic idea is to use hard ceramic dummy filler for embedding the sample of interest into the dummy frame. In this study, we applied this technique into preparing cross-sectional TEM specimen of the GaN-based materials with mechanical instability and demonstrated usefulness of this hard dummy filler method in which the possible modifications of the sample of interest during the preparation must be avoidable. In addition, practical precautions during the preparation were discussed.

버어리종 담배중 암모니아성 질소에 대한 불확도 측정 (Uncertainty Evaluation of Ammonia Determination in Burley Tobacco)

  • 이정민;이경구;한상빈
    • 한국연초학회지
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    • 제27권1호
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    • pp.107-114
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    • 2005
  • The uncertainty of measurement in quantitative analysis of ammonia by continuous-flow analysis method was evaluated following internationally accepted guidelines. The sources of uncertainty associated with the analysis of ammonia were the weighing of sample, the preparation of extracting solution, the addition of extracting solution into the sample, the reproducibility of analysis and the determination of water content in tobacco, etc. In calculating uncertainties, Type A of uncertainty was evaluated by the statistical analysis of a series of observation, and Type B by the information based on supplier's catalogue and/or certificated of calibration. It was shown that the main source of uncertainty was caused by the volume measurement of 1 mL and 2 mL, the purity of ammonia reference material in the preparation of standard solution, the reproducibility of analysis and the determination of water content of tobacco. The uncertainty in the addition of extraction solution, the sample weighing, the volume measurement of 50 mL and 100 mL, and the calibration curve of standard solution contributed relatively little to the overall uncertainty. The expanded uncertainty of ammonia determination in burley tobacco at $95\%$ level of confidence was $0.00997\%$.