• Title/Summary/Keyword: SEM-XRF 분석

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Applicability for Authenticity of Bronze Artefacts using Scientific Analyses (과학적 분석을 통한 전세품 청동기의 진위판별 적용 가능성 연구)

  • Do, Misol;Chung, Kwang Yong
    • Journal of Conservation Science
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    • v.29 no.4
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    • pp.355-366
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    • 2013
  • Diverse scientific analyses, including microstructure, ICP-AES, SEM-EDS, and P-XRF(Bench Top type and Gun type), were carried out on 6 bronze artefacts which handed from generation to generation. Also, we attempted to study applicability for authenticity of the bronze artefacts using scientific analyses based on the specific element. The results of ICP-AES analysis showed that the bronze were formed from an alloy of Cu, Sn, Pb with trace elements such as Ag, As, Co, Fe, but there were not Zn found. The result of P-XRF are 10~25% lower in Cu and 10~20% higher in Sn than that of ICP-AES. This is because of destannification that the compound of $SnO_2$ are present on the surface. The results of SEM-EDS represented that there is lead segregation. It was difficult to study applicability for authenticity of bronze artefact according to the microstructures and chemical components of the bronze artefacts. Therefore, as bronze artefacts have shown different corrosion materials depending on the buried environment and conserving environment, identifying the authenticity would be possible on the basis of the additional researches on the corrosion and comparative research of ancient art.

Study on the screening method for determination of heavy metals in cellular phone for the restrictions on the use of certain hazardous substances (RoHS) (유해물질 규제법(RoHS)에 따른 휴대폰 내의 중금속 함유량 측정을 위한 스크리닝법 연구)

  • Kim, Y.H.;Lee, J.S.;Lim, H.B.
    • Analytical Science and Technology
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    • v.23 no.1
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    • pp.1-14
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    • 2010
  • It is of importance that all countries in worldwide, including EU and China, have adopted the Restrictions on the use of certain Hazardous Substances (RoHS) for all electronics. IEC62321 document, which was published by the International Electronics Committee (IEC) can have conflicts with the standards in the market. On the contrary Publicly Accessible Specification (PAS) for sampling published by IEC TC111 can be adopted for complementary application. In this work, we tried to find a route to disassemble and disjoint cellular phone sample, based on PAS and compare the screening methods available in the market. For this work, the cellular phone produced in 2001, before the regulation was born, was chosen for better detection. Although X-ray Fluorescence (XRF) showed excellent performance for screening, fast and easy handling, it can give information on the surface, not the bulk, and have some limitations due to significant matrix interference and lack of variety of standards for quantification. It means that screening with XRF sometimes requires supplementary tool. There are several techniques available in the market of analytical instruments. Laser ablation (LA) ICP-MS, energy dispersive (ED) XRF and scanning electron microscope (SEM)-energy dispersive X-ray (EDX) were demonstrated for screening a cellular phone. For quantitative determination, graphite furnace atomic absorption spectrometry (GF-AAS) was employed. Experimental results for Pb in a battery showed large difference in analytical results in between XRF and GF-AAS, i.e., 0.92% and 5.67%, respectively. In addition, the standard deviation of XRF was extremely large in the range of 23-168%, compared with that in the range of 1.9-92.3% for LA-ICP-MS. In conclusion, GF-AAS was required for quantitative analysis although EDX was used for screening. In this work, it was proved that LA-ICP-MS can be used as a screening method for fast analysis to determine hazardous elements in electrical products.

Application of Handheld Raman Spectroscopy for Pigment Identification of a Hanging Painting at Janggoksa Temple(Maitreya Buddha) (장곡사 미륵불 괘불탱의 채색 재료 분석을 위한 휴대용 라만 분광기의 적용성 연구)

  • LEE Na Ra;YOO Youngmi;KIM Sojin
    • Korean Journal of Heritage: History & Science
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    • v.56 no.4
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    • pp.216-228
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    • 2023
  • The purpose of this study is to apply the handheld Raman spectrometer to identify the coloring materials used in a large Buddhist painting (of Maitreya Buddha) at Janggoksa Temple through cross-validation with HH-XRF. An in situ investigation was performed together with use of a digital microscope and HH-XRF analysis to verify the properties of pigments used in the gwaebul ("large Buddhist painting") via a non-destructive method. However, the identification of coloring materials composed of light elements and mixed or overlaid pigments is difficult using only non-destructive analysis data. Unlike in situ investigation, laboratory analysis often required samples yet the sampling is restricted to a small quantity due to the cultural heritage characteristic. Thus, it is necessary to develop a non-destructive in situ method to supplement the HH-XRF data. The large Buddhist painting at Janggoksa Temple was painted mainly using white, red, yellow, green, and blue colors. The Raman spectroscopy provides molecular information, while XRF spectroscopy provides information about elemental composition of the pigments. Analysis results identified various coloring materials: inorganic pigment, such as lead white, minium, cinnabar, and orpiment, as well as organic pigment such as gamboge and indigo. Therefore, it is possible to obtain more information for the identification of pigments; organic pigment and mixed or overlaid pigments, while at the same time minimizing the collection sample and simplifying the analysis procedure compared to previously used methods. The results of this study will be used as basic data for the analysis of painting cultural heritage through a non-destructive in situ method in the future.

Color Enhancement of Freshwater Pearl by Heat Treatment (열처리에 의한 다양한 컬러 담수양식진주의 색 향상 연구)

  • Son, Soo-Jung;Seo, Jin-Gyo;Park, Jong-Wan
    • The Korean Journal of Malacology
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    • v.25 no.1
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    • pp.81-89
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    • 2009
  • In this study, we conducted heat-treatment on freshwater cultured pearls at various conditions in other to improve their color. Also, after heat treatment, we used the UV-Vis, ED-XRF and SEM to investigate changes freshwater cultured pearls' color, composition and internal structure. UV-Vis analysis showed the reflectivity of samples increased at most heat-treatment conditions although the reflectivity decreased at a certain temperature and duration. At $100^{\circ}c$/8 h, $120^{\circ}c$/6 h and $140^{\circ}c$/4 h, the reflectivity increased highest. In proportion to reflectivity increase, freshwater cultured pearls' color was improved. Ca, Mn, Sr and other micro elements were found from ED-XRF analysis. However, changes in composition of elements were not detected. It was found that the content of Mn in freshwater cultured pearl is higher than other micro elements. From SEM analysis, aragonite's shape was shown in narce and some of the narce were condensed after heat treatment.

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Characteristics of Asphalt Concrete using Waste Foundry Sand (주물고사 첨가 아스팔트 콘크리트의 특성에 관한 연구)

  • Kim, Kwang-Woo;Ko, Dong-Hyuk;Choi, Dong-Chon;Kim, Sung-Won;Kim, Joong-Yul
    • International Journal of Highway Engineering
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    • v.3 no.4 s.10
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    • pp.105-116
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    • 2001
  • This study was performed to evaluate the characteristics of waste foundry sand (WFS) and the asphalt mixture made of a foundry waste sand. To estimate the applicability of WFS, chemical and physical properties were measured by XRF(X-ray fluorescent), and SEM(Scanning electronic microfilm). To improve the stripping resistance of WFS asphalt mixture, anti-stripping agents (a hydrated lime and a liquid anti-stripping agent) were used. To improve tensile properties and durability of WFS asphalt concrete mixture, LDPE(low-density polyethylene) was used as an asphalt modifier Marshall mix design, indirect tensile strength, tensile strength ratio(TSR) after freezing and thawing, moisture susceptibility and wheel tracking tests were carried out to evaluate performance of WFS asphalt concrete. Comparing with conventional asphalt concrete, WFS asphalt concretes showed similar or the better qualify in mechanical properties, and satisfied all specification limits. Therefore, it Is concluded that waste foundry sand can be recycled as an asphalt pavement material.

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Spectroscopic Studies on Crystallization of Na, TPA-ZSM-5 synthesized at Low Temperature and Atomospheric pressure (저온 상압에서 합성된 Na, TPA-ZSM-5의 결정화에 관한 분광학적 고찰)

  • Yun, Young Ja;Ha, Jae Mok
    • Analytical Science and Technology
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    • v.10 no.1
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    • pp.18-30
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    • 1997
  • Na, TPA-ZSM-5 with Si / Al mole ratio of about 130 was synthesized at low temperature and atmospheric pressure. These intermediate products were characterized by using XRD, XRF, FT-IR, NMR, and SEM. As a result, intermediate product were different from those that synthesized by autoclave method but spectroscopic characteristics of the final products showed to be in the typical ZSM-5 region. The defect sites were observed in the final product and removed by calcination at $540^{\circ}C$. Na, TPA-ZSM-5, aboveall, was synthesized at this condition within 48hr.

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Analysis of Ceramics Using Scanning Electron Microscopy (주사전자현미경을 활용한 세라믹의 분석)

  • Lee, Sujeong
    • Ceramist
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    • v.22 no.4
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    • pp.368-380
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    • 2019
  • A ceramic is used as a key material in various fields. Accordingly, the use of scanning electron microscopy is increased for the purpose of evaluating the reliability and defects of advanced ceramic materials. The scanning electron microscope is developed to overcome the limitations of optical microscopy and uses accelerated electrons for imaging. Various signals such as SE, BSE and characteristic X-rays provide useful information about the surface microstructure of specimens and, the content and distribution of chemical components. The development of electron guns, such as FEG, and the improved lens system combined with the advanced in-lens detectors and STEM-in-SEM system have expanded the applications of SEM. Automated SEM-EDS analysis also greatly increases the amount of data, enabling more statistically reliable results. In addition, X-ray CT, XRF, and WDS, which are installed in scanning electron microscope, have transformed SEM a more versatile analytical equipment. The performance and specifications of the scanning electron microscope to evaluate ceramics were reviewed and the selection criteria for SEM analysis were described.

Conservation Treatment and Study on Manufacturing Techniques of Jija Chongtong Gun in the Middle of Joseon Dynasty (조선 중기 제작된 지자총통의 보존처리와 제작기법 연구 -동아대학교 석당박물관 소장 보물 지자총통을 중심으로-)

  • Nam Dohyeon;Park Younghwan;Lee Jaesung
    • Conservation Science in Museum
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    • v.30
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    • pp.23-46
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    • 2023
  • The Jija Chongtong Gun, owned by Seokdang Museum of Dong-A University, is a tubedstyle heavy weapon of the battlefield in the mid-Joseon Dynasty and is the second largest firearm after Cheonja Chongtong. The original surface color of the Jija Chongtong Gun was obscured by foreign substances and therefore it was judged that its condition requires the conservation treatment. For stable conservation treatment, gamma ray and X-ray non-destructive transmission surveys was conducted to determine the internal structure and conservation condition. And the component analysis on the material components and surface contaminants of Jija Chongtong Gun was conducted by utilizing the p-XRF component analysis, SEM-EDS component analysis, and XRD analysis. As a result of the gamma-ray and X-ray non-destructive transmission investigation, a large amount of air bubbles was observed inside Jija Chongtong Gun, and the part that appeared to be a chaplet by visual observation was not identified. As a result of gamma-ray and p-XRF component analysis, it was confirmed that Jija Chongtong Gun was bronze made of copper (Cu), tin (Sn), and lead (Pb) alloy. As a result of surface analysis of foreign substances using SEM-EDS, it was confirmed that the main components of white foreign substances were calcium (Ca), sulfur (S), and titanium (Ti). Titanium was presumed to be titanium dioxide (TiO2), the main component of white correction fluid. The red foreign substance was confirmed to contain barium (Ba) as its main ingredient, and was presumed to be barium sulfate (BaSO4), an extender pigment in paint. White and red contaminants, mainly composed of titanium and barium, are presumed to have been deposited on the surface in recent years. The yellow foreign substances were confirmed to be aluminum (Al) and silicon (Si), and were presumed to have originated from soil components. As a result of SEM-EDS and XRD component analysis, the white foreign substance was confirmed to be gypsum (CaS). Based on the results of component analysis, surface impurities were removed, stabilization treatment, and strengthening treatment were performed. During the conservation process, unknown inscriptions Woo (右), Byeong (兵), Sang (上), and Yi (二) were discovered through a portable microscope and precise 3D scanning. In addition, the carving method, depth, and width of the inscription were measured. Woo Byeong Sang is located above Happo Fortress in Changwon, and Yi can be identified as the second hill.

Strength Development Characteristics of Clay Stabilized with Electric Furnace Steel Slag (전기로 제강슬래그로 안정화된 연약점토의 강도 발현 특성)

  • Hyeongjoo Kim;Taegew Ham;Taewoong Park;Taeeon Kim
    • Journal of the Korean GEO-environmental Society
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    • v.25 no.5
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    • pp.29-37
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    • 2024
  • This study aimed to investigate the changes in chemical components that occur when weak clay is mixed with steel slag modified with calcium oxide, and to understand the expression characteristics of compressive strength according to hydrophilicity and curing time. XRF testing, SEM imaging, vane shear strength and uniaxial compressive strength testing were conducted. Calcium (Ca) released from the steel slag increases the Ca content in clay by increasing the number of crystal particles and forming a coating layer known as calcium silicate hydrate (CaO-SiO2-H2O) through chemical reactions with SiO2 and Al2O3 components. The weak clay stabilized with steel slag is classified into an initial inactive zone where strength relatively does not increase and an activation zone where strength increases over curing time. The vane shear strength of the initial inactive area was found to be 4.4 to 18.4 kN/m2 in the state of the weight mixing ratio Rss 30% (steel slag 30% + clay 70%). In the case of the active area, the maximum uniaxial compressive strength increased to 431.8 kN/m2 after 480 hours of curing time, which increased due to the apparent adhesion strength of clay through pozzolanic reaction. Therefore, considering the strength expression characteristics of stabilized mixed clay based on the mixing ratio (Rss) during the recycling of steel slag can enhance its practicality in civil engineering sites.

Production Techniques for Goryeo Wooden Lacquerware (고려시대 목심칠기 木芯漆器의 제작기법 연구)

  • Yi, Yonghee;Park, Suzin;Yun, Eunyoung;Jung, Hyejin
    • Conservation Science in Museum
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    • v.15
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    • pp.78-95
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    • 2014
  • To examine the materials, production techniques, and key features of Goryeo wooden lacquerwares, scientific analysis was conducted on six relevant lacquerware items. All of the items, except for a lacquered bowl duksu 4123, were found to have been made by first covering the surface of the wood with cloth and then varnishing with lacquer. The wooden frames of flower-shaped lacquered case and pine leaves shape lacquered case were made by wrapping thin wood around either the lid or bottom panel. In most cases, microscopic analysis revealed a lower layer of lacquer mixed with bone ash and bone dust, followed by an upper varnish layer of lacquer. SEM-EDS analysis and μ-XRF Micro-X-ray Fluorescence analysis showed that vermilion lacquer mixed with cinnabar was used on the surface. A lid decorated with a dot pattern was made by first varnishing the surface with yellow lacquer mixed with orpiment, and then irregular dot pattern with a mixture of black lacquer and soot. The vermilion lacquer used to varnish the side of the lacquered bowls was composed of lacquer mixed with cinnabar and minium Red Lead.