• Title/Summary/Keyword: elemental analysis

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Synthesis of Transition Metal Cu(II) Complexes and Their Electrochemical Properties (Cu(II) 전이금속 착물의 합성과 전기화학적 성질에 관한 연구)

  • Chae, Hee-nam;Choi, Yong-kook
    • Applied Chemistry for Engineering
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    • v.9 no.5
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    • pp.719-725
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    • 1998
  • Tridentate Schiff base ligands were prepared by the reactions of salicylaldehyde and 2-hydroxy-1-naphthaldehyde with 2-aminophenol and 2-amino-p-cresol. And then Cu(II) complexes of those ligands were synthesized. The structures and properties of ligands and their complexes were studied by elemental analysis, $^1H$-NMR, IR, UV-visible spectra, and thermogravimetric analysis. The mole ratio of Schiff base to the metal of complexes was found to be 1:1. Cu(II) complexes were contemplated to be four-coordinated square planar configuration containing one water molecule. The redox process of ligands and complexes in DMSO solution containing 0.1 M TBAP as a supporting electrolyte was investigated by cyclic voltammetry and differential pulse voltammetry with glassy carbon electrode. The redox process of the tridentate Schiff base ligands was totally irreversible. The redox process of Cu(II) complexes was quasi-reversible and diffusion-controlled as one electron by one step process Cu(II)/Cu(I). The reduction potentials of the Cu(II) complexes shifted in the positive direction in the order of [Cu(II)(HNIPC)($H_2O$)]>[Cu(II)(HNIP)($H_2O$)]>[Cu(II)(SIP)($H_2O$)]>[Cu(II)(SIPC)($H_2O$)].

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A Systematic Literature Review on the Domestic and Foreign Research Trends of Movable Modern and Contemporary Cultural Heritage Conservation (국내외 연구문헌 조사를 통한 근·현대 동산문화재 보존 연구 동향 분석)

  • Youm, Inkyung;Yu, Jaeeun;Lee, Hyeyoun
    • Korean Journal of Heritage: History & Science
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    • v.48 no.1
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    • pp.44-61
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    • 2015
  • The research on the conservation of the movable modern and contemporary cultural heritage have been actively performed internationally since late 20th century. In this study, the international research trends of movable modern and contemporary cultural heritage conservation in last decades were analyzed. Setting up the range of the period, research papers were collected through various databases based on the systematic literature review process. Samples of 45 domestic papers and 505 foreign papers were classified by materials as books and paper, metals, textiles and fibers, photographs and audio-visuals, woods, plastics and ceramics and glass. The types of treated artifacts, detailed materials of the treated artifacts, and the research subjects were investigated from each paper. The data were compiled statistically and analyzed. Number of papers are published domestically in the book and paper conservation and metals conservation fields, but there are needs for more diversified artifact types and extensive research subjects. The researches in foreign countries are active in conservation of organic materials such as paper, textile and photographs and deal with various research subjects on not only treatment techniques and elemental analysis but also preventive conservation and conservation ethics. It is expected that this study would contribute to the field as a preliminary data on the conservation of modern and contemporary cultural heritage.

Bronze Production Technology in the Early Iron Age: A comparative study of bronze artifacts recovered from the Hoam-dong site in Chungju and Chongsong-ri in Buyeo (초기철기시대 청동기의 제작기술 - 충주 호암동유적과 부여 청송리유적 출토 청동기의 비교 연구-)

  • Han, Woorim;Hwang, Jinju;Kim, Sojin
    • Korean Journal of Heritage: History & Science
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    • v.51 no.4
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    • pp.224-233
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    • 2018
  • Thirty-three Early Iron Age bronzes at the sites of Hoam-dong in Chungju and Cheongsong-ri in Buyeo were investigated in order to study the manufacturing technique and the provenance of lead. Chemical analysis using X-ray fluorescence showed that 33 bronzes consist of copper(Cu), tin(Sn) and lead(Pb) served as major elements. Major and minor elemental analyses by EPMA were performed on two mirrors and 2 weapons of the bronzes investigated. The results shows that bronze mirrors from Chungju and Buyeo were high-tin bronzes(> 30 wt%). And 20% of tin and 5% of lead were founded in bronze weapons. Iron, zinc, arsenic, silver, nickel, sulfur and cobalt detected in four bronzes as minor and trace elements. The four bronzes were alloyed considering their function and were not heat treated after casting due to their high tin content. Lead isotope analysis using TIMS indicates that thirty-three bronzes were distributed southern Korea peninsula except Zone 1. As a result, lead raw materials came from various regions in Korean Peninsula not from Gyeongsang-do regions. The manufacturing techniques of bronze ware generalized at this age, and bronze was produced in various sites using raw materials from various sources.

Visual Signal Luminance Analysis and Light Source Color Application Study for Escape Guidance in Underground Common Duct (지하공동구 내 탈출 유도를 위한 비주얼 시그널 휘도 분석 및 광색 적용 연구)

  • Jongmin Lim;Hyojoo Kong;Jinsoo Shin;Sangwuk Shin;Seongsik Yoo
    • Journal of the Society of Disaster Information
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    • v.18 no.4
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    • pp.806-816
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    • 2022
  • Purpose: In this study, the luminance measurement analysis results of the smoke generation state are considered for visual signal display light color for real-time escape guidance in the underground common area. Method: We will analyze the scattering characteristics of light in the atmosphere and optical technology based on the visibility theory, and try to classify the elemental technology as a guidance function through a prototype of a visual signal display device for evacuation guidance. Result: In the experiment conducted under the smoke-generating condition, the results were derived with low luminance ratio and good visibility in the order of red, green, and yellow. However, this result is different from general lighting in which color rendering is considered, and is limited to signals for signals and detection. Conclusion: A conclusions were drawn by reflecting both the luminance measurement results in the smoke generation situation and the preference survey results conducted in previous studies for the light color of the visual signal for signal and detection. When events such as smoke occur, it is better to use the escape guidance visual signal in red or green.

Layered structure of sialoliths compared with tonsilloliths and antroliths

  • Buyanbileg Sodnom-Ish;Mi Young Eo;Yun Ju Cho;Mi Hyun Seo;Hyeong-Cheol Yang;Min-Keun Kim;Hoon Myoung;Soung Min Kim
    • Journal of the Korean Association of Oral and Maxillofacial Surgeons
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    • v.50 no.1
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    • pp.13-26
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    • 2024
  • Objectives: The aim of this study was to perform a comparative analysis of the ultrastructural and chemical composition of sialoliths, tonsilloliths, and antroliths and to describe their growth pattern. Materials and Methods: We obtained 19 specimens from 18 patients and classified the specimens into three groups: sialolith (A), tonsillolith (B), and antrolith (C). The peripheral, middle, and core regions of the specimens were examined in detail by histology, micro-computed tomography (micro-CT), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy, and transmission electron microscopy (TEM). Results: In the micro-CT, group A showed alternating radiodense and radiolucent layers, while group B had a homogeneous structure. Group C specimens revealed a compact homogeneous structure. Histopathologically, group A showed a laminated, teardrop-shaped, globular structure. Group B demonstrated degrees of immature calcification of organic and inorganic materials. In group C, the lesion was not encapsulated and showed a homogeneous lamellar bone structure. SEM revealed that group A showed distinct three layers: a peripheral multilayer zone, intermediate compact zone, and the central nidus area; groups B and C did not show these layers. The main elemental components of sialoliths were O, C, Ca, N, Cu, P, Zn, Si, Zr, F, Na, and Mg. In group B, a small amount of Fe was found in the peripheral region. Group C had a shorter component list: Ca, C, O, P, F, N, Si, Na, and Mg. TEM analysis of group A showed globular structures undergoing intra-vesicular calcification. In group B, bacteria were present in the middle layer. In the outer layer of the group C antrolith, an osteoblastic rimming was observed. Conclusion: Sialoliths had distinct three layers: a peripheral multilayer zone, an intermediate compact zone and the central nidus area, while the tonsillolith and antrolith specimens lacked distinct layers and a core.

Quantitative Elemental Analysis in Soils by using Laser Induced Breakdown Spectroscopy(LIBS) (레이저유도붕괴분광법을 활용한 토양의 정량분석)

  • Zhang, Yong-Seon;Lee, Gye-Jun;Lee, Jeong-Tae;Hwang, Seon-Woong;Jin, Yong-Ik;Park, Chan-Won;Moon, Yong-Hee
    • Korean Journal of Soil Science and Fertilizer
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    • v.42 no.5
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    • pp.399-407
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    • 2009
  • Laser induced breakdown spectroscopy(LIBS) is an simple analysis method for directly quantifying many kinds of soil micro-elements on site using a small size of laser without pre-treatment at any property of materials(solid, liquid and gas). The purpose of this study were to find an optimum condition of the LIBS measurement including wavelengths for quantifying soil elements, to relate spectral properties to the concentration of soil elements using LIBS as a simultaneous un-breakdown quantitative analysis technology, which can be applied for the safety assessment of agricultural products and precision agriculture, and to compare the results with a standardized chemical analysis method. Soil samples classified as fine-silty, mixed, thermic Typic Hapludalf(Memphis series) from grassland and uplands in Tennessee, USA were collected, crushed, and prepared for further analysis or LIBS measurement. The samples were measured using LIBS ranged from 200 to 600 nm(0.03 nm interval) with a Nd:YAG laser at 532 nm, with a beam energy of 25 mJ per pulse, a pulse width of 5 ns, and a repetition rate of 10 Hz. The optimum wavelength(${\lambda}nm$) of LIBS for estimating soil and plant elements were 308.2 nm for Al, 428.3 nm for Ca, 247.8 nm for T-C, 438.3 nm for Fe, 766.5 nm for K, 85.2 nm for Mg, 330.2 nm for Na, 213.6 nm for P, 180.7 nm for S, 288.2 nm for Si, and 351.9 nm for Ti, respectively. Coefficients of determination($r^2$) of calibration curve using standard reference soil samples for each element from LIBS measurement were ranged from 0.863 to 0.977. In comparison with ICP-AES(Inductively coupled plasma atomic emission spectroscopy) measurement, measurement error in terms of relative standard error were calculated. Silicon dioxide(SiO2) concentration estimated from two methods showed good agreement with -3.5% of relative standard error. The relative standard errors for the other elements were high. It implies that the prediction accuracy is low which might be caused by matrix effect such as particle size and constituent of soils. It is necessary to enhance the measurement and prediction accuracy of LIBS by improving pretreatment process, standard reference soil samples, and measurement method for a reliable quantification method.

Element Dispersion and Wallrock Alteration Analysis Using Portable XRF and SWIR in the Samgwang Au Deposit (휴대용 XRF와 단파장적외선 분광분석을 이용한 삼광 금광상의 원소분산 및 모암변질 분석)

  • Kim, Junkyum;Shin, Dongbok;Yoo, Bongchul;Im, Heonkyung;Kim, Ilkyu
    • Economic and Environmental Geology
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    • v.52 no.4
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    • pp.259-274
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    • 2019
  • Using portable XRF and SWIR analyzer, the characteristics of element dispersion and wallrock alterations induced by interaction between hydrothermal fluids and host rocks were investigated and ore exploration factors were estimated for the orogenic-type Samgwang Au deposits. On this purpose, in-situ measurements were conducted for 804 spots at regular intervals with a total of 4,824 times for host rocks, consisting of schist and gneiss, and altered wallrocks contacted with quartz veins in the Bonhang adit of the deposit, and the results were compared with quantitative data obtained by XRF and ICP analysis. The regression coefficients are 0.88 for major elements and 0.56 for trace elements, excluding V. For polished rock slabs, better results came out for major elements, 0.97 and for trace elements, 0.65. In altered wallrocks contacted with quartz veins, elements such as Fe, Zn, and Rb exhibit positive correlations with As in concentrations, while V forms a negative trend. Contour maps demonstrate that As, Zn, Rb, Fe, Ti, Cr, and Ni are enriched together near quartz veins, showing similar elemental behaviors. In-situ analysis using portable SWIR analyzer represents that schist and gneiss contain mica, illite, chlorite, sericite, amphibole, and epidote, while illite, sericite, gypsum, and mica are present in the altered rocks contacted with quartz veins. In contour maps, chlorite occurs mostly in host rocks, while sericite is concentrated near quartz veins. These results are similar to those of previous studies for element dispersion and hydrothermal alteration, and support the possibility for application of in-situ analysis on the exploration of orogenic gold deposit.

Semi-quantitative Analysis of Manganese Oxide Mineral in Manganese Nodule From the East Siberian Sea (동시베리아해 망가니즈단괴의 산화망가니즈광물 반정량 분석)

  • Yu, Hye Jin;Shin, Eun Ju;Koo, Hyo Jin;Cho, Hyen Goo
    • Korean Journal of Mineralogy and Petrology
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    • v.33 no.4
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    • pp.427-437
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    • 2020
  • Manganese nodules, which are evaluated as potential metal resources, have been found in the Arctic Ocean as well as in the abyssal plains of the Pacific and Indian Oceans. Manganese nodules exhibit strong variations in the morphology, internal texture, chemical composition and mineralogy as they grow. The relationship between the texture and chemical elemental composition during the growth process is well documented, but the mineral composition variation during the growth process is not. Because the manganese oxide minerals in nodules are fine-grained and poorly crystalline, quantitative analysis for the mineral composition is challenging for the bulk nodule sample. This study investigated the internal texture and Mn-oxide mineral composition of manganese nodules obtained from the East Siberian Sea. Semi-quantitative analysis was attempted for three main Mn-oxide minerals constituting the manganese nodules (i.e., todorokite, buserite and birnessite) using the peak area ratio of X-ray diffraction analysis graphs. In the East Siberian Sea manganese nodules, birnessite is more abundant than buserite or todorokite, and no correlation is found between the mineral composition and the internal texture. Instead a correlation is found between the relative content of todorokite and the lamellae depth. The todorokite content tends to increase from the surface to the core of the nodules, which can be attributed to a recrystallization process or difference in the growth rate within the nodule. This study shows that semi-quantitative analysis of manganese oxide minerals using the peak area ratio is useful in the mineralogical study of manganese nodules.

Preparation and Characterization of Dimeric Molybdenum(Ⅴ) Complexes with Bis(hydroxyethyl)dithiocarbamate (Bis(Hydroxyethyl)dithiocarbamate 의 이핵 몰리브덴 (Ⅴ) 착물 합성과 그 성질)

  • Yeh Gyung-Hak;Koo Bon-Kweon
    • Journal of the Korean Chemical Society
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    • v.34 no.5
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    • pp.452-459
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    • 1990
  • A series of oxo-and sulfido-bridged molybdenum (V) complexes, Mo$_2$O$_4$L$_2$, Mo$_2$O$_3$L$_4$, Mo$_2$O$_2$S$_2$L$_2$, and Mo$_2$OS$_3$L$_2$ [L = bis(hydroxyethyl)dithiocarbamate] have been prepared. The complexes with bridging and terminal oxo groups have been synthesized by the reactions of (PyH)$_2$MoOCl$_5$ or MoCl$_5$ and ligand in water. One of the rest two complexes, in which bridging and terminal oxo groups have been replaced by sulfido in Mo$_2$O$_4^{2+}$ core, Mo$_2$O$_2$S$_2$L$_2$ have been prepared by addition of triphenylphosphine to a chloroform solution of Mo$_2$OS$_3$L$_2$. While, Mo$_2$OS$_3$L$_2$ is obtained from aqueous solution of (NH$_4$)$_2$MoS$_4$ and ligand in the presence of sodium dithionite. The complexes are identified by elemental analysis, and spectral data of IR, UV-vis, nmr, and mass. Also, the electrochemical behaviour for the complexes in dimethylsulfoxide has been investigated by the cyclic voltammograms.

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Synthesis and Characterization of Tetranuclear Molybdenum(Ⅵ) Complexes with Butylamidoxime Derivatives (부틸아미드옥심 유도체의 몰리브덴(Ⅵ) 사핵 착물의 합성과 성질)

  • Roh, Soo-Gyun;Oh, Sang Oh
    • Journal of the Korean Chemical Society
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    • v.39 no.7
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    • pp.552-558
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    • 1995
  • The tetranuclear complexes, $X_2[M_{O4}O_12{R'C(NH_2)NO}_2](X= n-Bu_4N^+$, $R'=(CH_3)_2CH$, $CH_3CH_2CH_2$, $CH_3SCH_2$; $X=(CH_3)_2CHC(=NH_2)NH_2^+$, $R'=(CH_3)_2CH$; $X = CH_3CH_2CH_2C(=NH_2)NH_2^+$, $R'=CH_3_CH_2CH_2$; $X=CH_3SCH_2C(=NH_2)NH_2^+$, $R'=CH_3SCH_2)$ have been synthesized by the reactions of monomeric and polynuclear complexes with isobutyl-, butyl- and thiomethylacetamidoxime. The prepared complexes were identified by elemental analysis, infrared, $^1H$ NMR and $^{13}C$ NMR spectroscopy. The structure of complex ${(CH_3)_2CHC(NH_2)_2}_2[M_{O4}O_{12}{(CH_3)_2CHC(NH_2)NO}_2]$ was determined by X-ray single crystal diffraction. Crystal data are follows: Monoclinic, $P2_{1/c}$, $a=10.168(3){\AA}$, $b=11.768(1){\AA}$, $c=13.557(1){\AA}$, ${\beta}=102.08(1)^{\circ}$, $V=1586.2(5){\AA}^3$, Z=2, final R=0.026 for 2951($F_0>3s(F_0)$). This complex is composed of a planar cyclic $[Mo_4({\mu}-O)_4]$ and two ${\mu}_4$-amidoximate.

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