• Title/Summary/Keyword: elemental analysis

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Crystal Structure and Tautomerism Study of the Mono-protonated Metformin Salt

  • Wei, Xiaodan;Fan, Yuhua;Bi, Caifeng;Yan, Xingchen;Zhang, Xia;Li, Xin
    • Bulletin of the Korean Chemical Society
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    • v.35 no.12
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    • pp.3495-3501
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    • 2014
  • A novel crystal, the mono-protonated metformin acetate (1), was obtained and characterized by elemental analysis, IR spectroscopy and X-ray crystallography. It was found that one of the imino group in the metformin cation was protonated along with the proton transfer from the secondary amino group to the other imino group. Its crystal structure was then compared with the previously reported diprotonated metformin oxalate (2). The difference between them is that the mono-protonated metformin cations can be linked by hydrogen bonding to form dimers while the diprotonated metformin cations cannot. Both of them are stabilized by intermolecular hydrogen bonds to assemble a 3-D supermolecular structure. The four potential tautomer of the mono-protonated metformin cation (tautomers 1a, 1b, 1c and 1d) were optimized and their single point energies were calculated by Density Functional Theory (DFT) B3LYP method based on the Polarized Continuum Model (PCM) in water, which shows that the most likely existed tautomer in human cells is the same in the crystal structure. Based on the optimized structure, their Wiberg bond orders, Natural Population Analysis (NPA) atomic charges, molecular electrostatic potential (MEP) maps were calculated to analyze their electronic structures, which were then compared with the corresponding values of the diprotonated metformin cation (cation 2) and the neutral metformin (compound 3). Finally, the possible tautomeric mechanism of the mono-protonated metformin cation was discussed based on the observed phenomena.

Design of Oceanography Buoy - Part II: Mooring System (해양관측용 부이의 설계 건전성 평가 - Part II: 계류시스템 구조건전성 평가)

  • Keum, Dong-Min;Kim, Tae-Woo;Han, Dae-Suk;Lee, Won-Boo;Lee, Jae-Myung
    • Journal of Ocean Engineering and Technology
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    • v.23 no.1
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    • pp.89-95
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    • 2009
  • The purpose of the present study was to evaluate the safety under extreme environmental conditions and the dynamic safety under service environment conditions, of oceanographic buoy mooring systems consisting of a variety of materials, including chain, wire rope, nylon rope, and polypropylene rope. For the static safety assessment of a mooring system, after the calculation of external forces and the division of a mooring system into finite elements, the numerical integral was conducted to yield the elemental static tension until satisfying the geometrical convergence condition. To evaluate the dynamic safety, various processes were considered, including data collection about the anticipated areas for mooring, a determination of the parameters for the interpretation, the interpretation of the dynamic characteristics based on an analytic equation that takes into account the heave motion effect of a buoy hull and a mooring system, and a fatigue analysis of the linear cumulative damage. Based on the analysis results, a supplementary proposal for a wire rope that has a fracture in an actual mooring area was established.

Characterization of Large-sized Jar-coffins from Youngsan River by the Elemental Analysis (영산강유역 대형옹관의 태토 특성에 의한 분류)

  • Lee, Han-Hyoung;Hong, Jong-Ouk;Hwang, Jin-Ju;Park, Ji-Hee;Moon, Eun-Jung;Kim, Soo-Kyung;Chung, Yong-Sam;Moon, Jong-Hwa
    • 보존과학연구
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    • s.30
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    • pp.103-124
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    • 2009
  • Major and trace elements and cross section textures of the large-sized jar-coffins excavated in the Young San river area have been analyzed for categorization according to geochemical characteristics of the raw materials. As results, we have found out that the jar-coffins of the Oryang-dong and Ungok-dong have very similar characteristics, and those of Songwol-dong and Jangdeung show distinguishable characteristics from the others. In addition, similar characteristics have been detected in some U-shape jar-coffins from several sites such as Oryang-dong, Ungok-dong, Sinchon-ri, Mansu-ri and Yeon-ri posess on trace elements and cross section texture. These results indicate that there was active physical migration although the detail route of the physical migration is unclear at current stage.

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Whether Pinhole Scan or Single Photon Emission Computed Tomography (SPECT) in the Diagnosis of Bone and Joint Diseases (골격계진단에 있어서 핀홀스캔의 우월성)

  • Bahk, Yong-Whee
    • The Korean Journal of Nuclear Medicine
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    • v.30 no.1
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    • pp.1-14
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    • 1996
  • Since the publication of the first bone scintiscans in 1962 three decades have elapsed. The bone scan has made great strides during this period, becoming one of the most commonly used nuclear imaging tests. In spite of the progress, however, the specificity of bone scan has remained relatively low. As the result it is a common practice to seek additional information from radiograph, CT scan and MR image, which is euphemistically termed as "image fusion or co-location." The basic reason is the inapplicability of the classical piecemeal analysis to interpreting planar and SPECT bone scans. Such analysis has its base on the observation of elemental features of morphology, which include the size, shape, contour, location, topography and internal architecture. The physiochemical profile may well also be included. Understandably, however, the miniatured images of the planar bone scan cannot provide these features in acceptable detail and the same holds true even with SPECT Images which are but sliced views of the reconstructed planar scans. Fortunately pinhole scanning has the capacity to portray both the morphological and chemical profiles of bone and joint diseases in greater detail through true magnification. The magnitude of pinhole scan resolution is practically comparable to that of radiography as far as gross anatomy is concerned. Thus, we feel strongly that pinhole scanning is a potential breakthrough of the long-lamented low specificity of bone scan. This presentation will discuss the fun-damentals, advantages and disadvantages and the most recent advances of pinhole scanning. It high-lights the actual clinical applications of pinhole scanning in relation to the diagnosis of infective and inflammatory diseases of bone and joint.

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Synthesis and Cure Behaviors of Diglycidylether of Bisphenol-S Epoxy Resins (Diglycidylether of Bisphenol-S 에폭시 수지의 합성 및 경화거동에 관한 연구)

  • 박수진;김범용;이재락;신재섭
    • Polymer(Korea)
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    • v.26 no.4
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    • pp.501-507
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    • 2002
  • In this work, diglycidylether of bisphenol-S (DGEBS) epoxy resin was prepared by alkaline condensation of bisphenol-S (BPS) with epichlorohydrin (ECH) in the presence of NaOH catalyst. The structure of the synthesized DGEBS epoxy resin was confirmed by IR, NMR spectra, and elemental analysis. The curing reaction and glass transition temperature ($T_g$) of DGEBS epoxy resin cured with phthalic anhydride (PA) and tetrahydrophthalic anhydride (THPA) at curing agents were studied by dynamic differential scanning calorimetry (DSC). The thermal stability of the cured specimen was investigated by thermogravimetric analysis (TGA). As a result, the activation energy ($E_a$) of DGEBS/PA system was higher than that of DGEBS/THPA system, whereas $T_g$, initial decomposed temperature (IDT), and decomposition activation energy ($E_t$) of DGEBS/PA were lower than those of DGEBS/THPA. This was probably due to the fact that the crosslinking density of DGEBS/THPA was increased by ring strain of curing agent.

Preparation and Properties of Modified Polyethylenes: 1. Preparation and Properties of Dispersions in Water (변성 폴리에틸렌의 제조 및 물성 : 1. 제조 및 수분산 특성)

  • Lee, Jae Heung;Lee, Sang-Hun
    • Journal of Adhesion and Interface
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    • v.3 no.3
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    • pp.7-14
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    • 2002
  • Modified polyethylenes with polar side groups of -COOK, $-CONH_2$, and -COOH were prepared at a dispersion state in water by reacting poly(ethylene-co-methylacrylate) (PEMA) with aqueous solution of KOH and ammonia. Types and their contents of side groups were investigated by infrared spectroscopy, elemental analysis and atomic absorption analysis. Solution viscosity and surface tension were also measured as a function of solid contents. Stability and transparency of the dispersions were greatly affected by the content of COOK in the side groups. The stable dispersion could be prepared at a composition of COOK of 20 mole% at least. The transparency was increased with increasing the COOK contents, but decreased with increasing the amide content at a constant composition of COOK. Solution viscosities increased abruptly at a lower solid content when the COOK contents were increased, implying higher entanglement between the chains in dispersions with higher content of hydrophilic COOK group. The dispersions of higher COOK content revealed lower surface tension values.

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Synthesis of Tridentate Schiff base Molybdenum(Ⅴ) Complexes and Their Electrochemical Properties in Aprotic Solvents (세자리 Schiff base 몰리브데늄(Ⅴ) 착물들의 합성과 비수용매에서의 전기화학적 성질)

  • Choi, Young-Kook;Song, Mi-Sook;Rim, Chae-Pyeong;Chjo, Ki-Hyung
    • Journal of the Korean Chemical Society
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    • v.39 no.1
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    • pp.47-56
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    • 1995
  • Tridentate Schiff base molybdenum(V) complexes such as [Mo(Ⅴ)2O(SOHB)4], [Mo(Ⅴ)2O3(SOIP)2(NCS)2] and [Mo(Ⅴ)2O3(SOTB)2(H20)2](SOHB: Salicylidene-o-imino hydroxybenzene, SOIP; Salicylidene-o-imino pyridine, SOTB; Salicylidene-o-imino thiolbenzene) were synthesized and identified by elemental analysis, spectroscopy, and thermogravimetric analysis (TGA). It was found that the mole ratio of Schiff base ligand to the metal in these complexes is 1 : 1 or 1 : 2. The redox processes of the complexes were investigated by cyclic voltammetric and differential pulse polarographic techniques in nonaquous solvent containing 0.1 M tetraethylammonium perchlorate (TEAP) as supporting electrolyte at glassy carbon electrode. It was found that diffusion controlled reduction processes with one electron were Mo(Ⅴ)Mo(Ⅴ)e-→ Mo(Ⅴ)Mo(Ⅳ)e-→Mo(Ⅳ)Mo(Ⅳ)e-→Mo(Ⅳ)Mo(Ⅲ).

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Characteristics of Bio-oil by Pyrolysis with Pig Feces (돈분을 이용한 열분해공정 바이오오일의 특성)

  • Kun, Zhu;Choi, Hong L.
    • Journal of the Korea Organic Resources Recycling Association
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    • v.16 no.4
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    • pp.57-63
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    • 2008
  • The characteristics of the bio-oil produced by the pyrolysis process with pig feces was investigated in this paper. The continuous auger-type reactor produced bio-oil was maintained at the temperature range of 400 to $600^{\circ}C$, which was higher than a typical that in a conventional pyrolysis system. The pig feces was used as the feedstock. The bio-oil and its compositions were characterized by water analysis, heating values, elemental analysis, bio-oil compounds, by Gas Chromatography/Mass Spectrometry (GC/MS), and functional group by $^1H$ NMR spectroscopy. It was found that the maximum bio-oil yields of 21% w.t. was achieved at $550^{\circ}C$. This result suggested that this auger reactor might be a potential technology for livestock waste treatment to produce bio-oil because it is able to be improved to reach higher efficiency of bio-oil production in further study. The pyrolysis system reported herein had low heat transfer into the feedstock in the auger reactor so that it needs improve the heat conduction rate of the system in further study.

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Study on quantitative & trace element analysis of metal objects (고대 청동기의 성분조성 및 산지추정 연구)

  • Chung, Kwang-Yong;Kang, Hyung-tae;Chong, Dong-Chan;Yun, Yong-hyun;Lee, Hoon
    • 한국문화재보존과학회:학술대회논문집
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    • 2004.10a
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    • pp.137-153
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    • 2004
  • We have analyzed the ingredients of 17 pieces of Bronze Age bronze ware, and an additional 22 pieces of Koryo and Chosun dynasty bronze ware. We have also conducted analysis of the extraction sites where these bronze ware items were found. For analyzing the main ingredient the bronze ware items have been divided into 3 groups - Cu-Sn(70?75:20), Cu-Pb-Sn(70:10:10), Cu-Pb-Sn(60:10:20) type respectively. In tile cases of the Cu-Pb-Sn groups the division comes down to differences in the Cu content as the main component, and elements such as Ni, Fe, Co contribute as a micro ingredient. The geographical and periodic characteristics of ancient bronze ware items show that theircompositional element changes from Cu:Sn to Cu:Pb:Sn and the Cu content decreases with the period,while the Pb content increases with the period. Bronze ware items from Suchon Ri, Gongju (that were used in 3 B.C.) form very different categories from 3rd ${\~}$ 2nd B.C.. They additionally formed very different categories from those bronze ware items analyzed in this research. These bronze ware itemsare shown to be geographically close and periodically overlapped, but made of a new elemental composition. This shows an inflow of a production technical culture present in the new bronze wares. The main component content of Cu is lower, and the Co and Fe contents (as microelements) are much higher than that of other bronze ware items. Such facts showthat those bronze ware items used completely different materials from bronze ware items in other cultural areas, or that there were differences in smelting techniques In the places where ancient bronze ware items have been extracted, it is presumed that the materials originated from the southern parts of Korea andnorthern parts and southern parts of China. .As more bronze ware scientific research is compiled one can conclude that that there will be enough scientific evidence to study the Bronze Age culture of Koreasystematically.

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Cr(III)-Tetraaza Macrocyclic Complexes Containing Auxiliary Ligands (Part III); Synthesis and Characterization of Cr(III)-Isothiocyanato, -Azido and -Chloroacetato Macrocyclic Complexes

  • Byun, Jong-Chul;Han, Chung-Hun;Park, Yu-Chul
    • Bulletin of the Korean Chemical Society
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    • v.26 no.7
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    • pp.1044-1050
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    • 2005
  • The reaction of cis-[Cr([14]-decane)($OH_2)_2]^+$ ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) with auxiliary ligands {$L_a$ = isothiocyanate ($NCS^-$), azide ($N3^-$) or chloroacetate(caa)} leads to a new cis-[Cr([14]-decane)($NCS)_2]ClO_4{\cdot}H_2O$ (1), cis-[Cr([14]-decane)($N_3)_2]ClO_4$ (2) or cis-[Cr([14]-decane)($caa)_2]ClO_4$ (3). These complexes have been characterized by a combination of elemental analysis, conductivity, IR and Vis spectroscopy, mass spectrometry, and X-ray crystallography. Analysis of the crystal structure of cis-[Cr([14]-decane)($NCS)_2]ClO_4{\cdot}H_2O$ reveals that central chromium(III) has a distorted octahedral coordination environment and two $NCS^-$anions are bonded to the chromium(III) ion via the Ndonor atom in the cis positions. The angle $N_{axial}-Cr-N_{axial}$ deviates by 13$^{\circ}$ from the ideal value of 180$^{\circ}$ for a perfect octahedron. The bond angle N-Cr-N between the Cr(III) ion and the two nitrogen atoms of the isothiocyanate ligands is close to 90$^{\circ}$. The bond lengths of Cr-N between the chromium and $NCS^-$groups are 1.964(5) and 2.000(5) $\AA$. They are shorter than those between chromium and nitrogen atoms of the macrocycle. The IR spectra of 1, 2 and 3 display bands at 2073, 1344 and 1684 $cm^{-1}$ attributed to the $NCS^-$, ${N_3}^-$ and caa groups stretching vibrations, respectively.