• Applied Microscopy
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• 제50권
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• pp.21.1-21.3
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• 2020

Sample preparation is significantly important to the high-resolution transmission electron microscopy (HRTEM) characterization of nanomaterials. However, many general organic solvents can dissolve the necessary organic polymer support layer in TEM grid, which causes it difficult to obtain high-quality samples of oil-soluble nanomaterials. In this study, a new sample preparation method for oil-soluble nanomaterials has been developed by using the sublimable material as a transition layer. Experiments also show that there is no damage to TEM grids and high-quality HRTEM images can be obtained via this method. This approach paves the way to applicable HRTEM sample preparation of oil-soluble nanomaterials.

• Applied Microscopy
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• 제46권2호
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• pp.110-115
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• 2016

Transmission electron microscopy (TEM) is a powerful tool for analyzing a broad range of materials and provides localized information about the microstructure. However, the analysis results are strongly influenced by the quality of the thin foil specimen. Sample preparation for TEM analysis requires considerable skill, especially when the area of interest is small or the material of interest is difficult to thin because of its high hardness and its mechanical instability when thinned. This article selectively reviews recent advances in TEM sample preparation techniques using a tripod polisher. In particular, it introduces two typical types (fl at type and wedge type) of TEM sample preparation and the benefits and drawbacks of each method; finally, a method of making better samples for TEM analysis is suggested.

• Applied Microscopy
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• 제42권1호
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• pp.49-52
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• 2012

For TEM study of biological samples or polymers that are contained in organic structure, it is often required that the sample is prepared by using ultramicrotome and stained with proper agents to increase the contrast of organic structure. In this study, we investigated an efficient TEM sample preparation method for ductile heterogeneity material by using ultramicrotomy. Cryo-ultramicrotomy is a suitable method that is capable of rendering sample hardness for various ductile materials. However, it has several factors to consider, such as experimental cost, working time and finding the optimal staining conditions. To satisfy these considerations, we prepared TEM sample by using ultramicrotome without cryofunction, and secured the sample hardness by applying the staining process prior to ultrathin sectioning. The cross-linked polyethylene structure in the sample was stained with the 2% $RuO_4$ solution in a sealed test tube for 24 hours at $4^{\circ}C$. After the sample staining, ultrathin sections of sample were prepared using ultramicrotome. As a result, it was revealed that the difficulties associated with staining of ultrathin sections prepared by low-temperature conditions were improved. In addition, appropriate staining depth of sample could be selected for sectioning process. The quality of TEM sample obtained by using this method was better than that of cryo-ultramicroscopy. Finally, it is expected that our method could be effectively applied in TEM sample preparation for a variety of nano-bio convergence materials.

• 한국어병학회지
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• 제34권2호
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• pp.261-269
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• 2021

This study presents the evaluation of sample extraction and purification procedure for the determination of residues of febantel and its metabolites, fenbendazole, oxfendazole and oxfendazole sulfone in rockfish (Sebastes schlegeli) muscle using liquid chromatography-tandem mass spectrometry. Residues of febantel and its metabolites in rockfish muscle were analyzed using each different sample preparation method from Korean Food Standards Codex (KFSC), Food Safety and Inspection Service (FSIS, USA), and the modified FSIS method using QuEChERS kit (FSIS-Q), respectively. Each method was compared for mean recoveries and repeatabilities. Since FSIS-Q showed higher repeatabilities (coefficient of variation, CV of 2.4%~10.9%) than those of FSIS method (CV of 4.6%~17.5%), recoveries from FSIS-Q were compared with those from KFSC method. FSIS-Q showed significantly higher recoveries of 83.1%~110.1% (P < 0.05) than those from KFSC method of 64.7%~107.4%. In addition, FSIS-Q showed a good linearity over the range of 2.5~200 ㎍/kg, and excellent sensitivities with limit of detection of 0.46~0.71 ㎍/kg and limit of quantification of 1.08~2.15 ㎍/kg. Although all the sample preparation methods turned out to be able to meet CODEX guideline for all the compounds, FSIS method and FSIS-Q validated in this study could be applied to screening and quantification for residues of febantel and its metabolites in rockfish muscle with efficient preparation procedures.

• Applied Microscopy
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• 제45권4호
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• pp.203-207
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• 2015

Sample preparation is very important for crystal structure analysis of novel nanostructured materials in electron microscopy. Generally, a grid dispersion method has been used as transmission electron microscope (TEM) sampling method of nano-powder samples. However, it is difficult to obtain the cross-sectional information for the tabular-structured materials. In order to solve this problem, we have attempted a new sample preparation method using focused ion beam. Base on this approach, it was possible to successfully obtain the electron diffraction patterns and high-resolution TEM images of the cross-section of tabular structure. Finally, we were able to obtain three-dimensional crystallographic information of novel zeolite nano-crystal of the tabular morphology by applying the new sample preparation technique.

• 자원환경지질
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• 제29권2호
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• pp.207-214
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• 1996

For many years oxygen and hydrogen isotope analysis have been used as one of the most valuable research tools to investigate many geological processes. There are many sample preparation techniques of oxygen and hydrogen isotope analysis for various geological samples. We introduce here several important sample preparation techniques for oxygen and hydrogen isotope analysis and discuss the problems of each method in detail.

• 한국세라믹학회지
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• 제55권4호
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• pp.376-380
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• 2018

Microstructural characterization of Ni-yttria-stabilized zirconia (YSZ) anodes using secondary electron images has been limited by a lack of contrast between Ni and YSZ phases. This paper reports a sample preparation method for obtaining secondary electron images that allow the detection of Ni, YSZ, and pore phases together. Ni-YSZ anode samples were obtained by reducing NiO-YSZ samples prepared by using the mixed oxide method. Colloidal silica polishing and electrolytic etching were performed on the Ni-YSZ samples. The morphological change of the sample surface after each polishing process is examined.

• Mass Spectrometry Letters
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• 제6권2호
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• pp.27-30
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• 2015

This article reviews the fundamentals of sample preparation used in matrix-assisted laser desorption/ionization-mass spectrometry (MALDI-MS). MALDI is a soft ionization method used to generate analyte ions in their intact forms, which are then detected in MS analysis. MALDI-MS boasts fast analysis times and easy-to-use operation. The disadvantages of MALDI-MS include the occurrence of matrix-associated peaks and inhomogeneous distribution of analyte within the matrix. To overcome the disadvantages of MALDI-MS, various efforts have been directed such as using different matrices, novel matrix systems, various additives, and different sample preparation methods. These various efforts will be discussed in detail. This article will benefit those who would like to obtain basic knowledge of MALDI sample preparation and those who would like to use MALDI-MS in their chemical analyses.

• Applied Microscopy
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• 제45권4호
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• pp.199-202
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• 2015

A simple and novel transmission electron microscopy (TEM) sample preparation method for phase change nanowire is investigated. A $Ge_2Sb_2Te_5$ (GST) nanowire TEM sample was meticulously prepared using nanomanipulator and gas injection system in a field emission scanning electron microscopy for efficient and accurate TEM analysis. The process can minimize the damage during the TEM sample preparation of the nanowires, thus enabling the crystallographic analysis of as-grown GST nanowires without unexpected phase transition caused by e-beam heating.

• 한국융합학회논문지
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• 제9권3호
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• pp.217-222
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• 2018

본 논문에서는 정확한 수의 희귀 세포 포집 및 이송을 위한 마이크로 폴리머 칩 플랫폼의 디자인과 제작, 그리고 프로토콜을 소개하고 있다. 본 플랫폼과 프로토콜은 기존의 통계학적인 샘플 준비 방법인 희석(Dilution)의 한계와 고가이며 형광염색이 요구되는 유세포분석기(Fluorescence activated cell sorter)의 단점을 극복하였다. 타켓 세포를 선택적으로 쉽고 간단하게 채집할 수 있으며 채집되는 세포의 수는 시각적으로 검증되므로 매우 정확한 방법이다. 또한, 채집된 세포들은 마이크로 챔버 등의 원하는 곳으로 세포의 손실 없이 이송 또는 주입 시킬 수 있다. 본 연구는 암진단 등을 목적으로 하는 칩 속의 실험실(Lab on a chip) 등에 필요한 희귀 세포 샘플 준비를 위해 활용 될 수 있을 뿐만 아니라 세포분석을 위한 싱글/더블/다수 세포 샘플의 준비에도 활용 가능하다. 본 논문에서 제시하는 세포 채집 플랫폼과 프로토콜을 검증하기 위해 5개의 인간 암세포(MCF-7)를 채집한 뒤 세포계수기(Hemocytometer) 안으로 주입시켜 세포의 수를 확인하였다.