• Title/Summary/Keyword: elemental analysis

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Synthesis and Characterization of Molybdeum Complexes with Schiff-Bases(II), Dioxobis(N-aryl-3-methoxysalicyaldiminato) Molybdenum(VI) Complexes (몰리브덴의 시프-염기착물의 합성과 그 성질 (제2보). 다이옥소비스(질소-아릴-3-메톡시살리실알디미나토)몰리브데늄(VI) 착물)

  • O, Sang O;Gu, Bon Gwon
    • Journal of the Korean Chemical Society
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    • v.29 no.3
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    • pp.257-264
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    • 1985
  • Dioxobis(3-methoxysalicyaldehydato)molybdeum(VI) complex has been synthesized by reactions of 3-methoxysalicylaldehyde and ammonium paramolybdate in methanol solution. With appropriate primary amine, the resulting complex gave schiff-base complexes, MoO$_2$(CH$_3$O-sal-N-R)$_2$ in which C=O oxide ligands had been replaced by nitrogen. The properties and possible molecular structure of these complexes were discussed by elemental analysis, spectroscopic studies and electric conductivities measurements. It was found that the Mo(VI) complexes contain a cis-MoO$_2$ group since their infrared spectra two Mo=O band at about 900cm$^{-1}$ and the combining ratios for MoO$_2$-ligand are 1 : 2. Also, electronic spectra of molybdenyl complexes assigned to ligand-to-metal charge transfer transition. All of these complexes are yellow or orange, depolar compound and slightly soluble in alcohol, dichloromethane, chloroform and N,N-dimethylformamide.

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Synthesis and Characterization of Molybdenum (V)-1, 6-Diaminohexane-N, N, N', N'-tetraacetic Acid Derivatives Complexes (몰리브덴 (V) 와 1, 6-Diaminohexane-N, N, N', N'-tetraacetic Acid 계 착물합성과 그 성질)

  • Sang Oh Oh;Sig Young Choi
    • Journal of the Korean Chemical Society
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    • v.33 no.1
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    • pp.90-96
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    • 1989
  • A new series of $dioxo-di-{\mu}-oxo-dimolybdate(V)(*image)$, has been prepared by the reaction of pyridinum oxoisothiocyanato-molybdate(V) with 1, 6-diaminohexane-N, N, N', N'-tetraacetic acid derivatives containing amine carboxyl groups. The properties and possible molecular structure of these complexes were discussed by elemental analysis, spectroscopic studies and magnetic susceptibility measurements. The infrared spectra of these complexes show two strong Mo=$O_t$ stretching modes in the $900-965cm^{-1}$, MoO$_2$Mo stretching bands at around 450∼500 and $740-765 cm^{-1}$ to symmetrical and asymmetrical O-bridge stretching, a coordinated $COO^-$ asymmetrical band in the $1600-1635 cm^{-1}$. The complexes synthesized were yellow or orange and diamagnetic.

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Synthesis and Characterization of Molybdenum(V)-Iminodiaceticacid Derivatives Complexes (몰리브덴(V)와 이미노디아세틱액시드계 착물 합성과 그 성질)

  • Sang-Oh Oh;Sik-Young Choi
    • Journal of the Korean Chemical Society
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    • v.31 no.6
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    • pp.520-526
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    • 1987
  • A new series of $dioxo-di-\mu-oxo-dimolybdate(V)$, has been prepared by reaction of pyridinum oxoisothiocyantomolybdate (V) with iminodiacetic acid derivatives containing amine carboxyl groups. The properties and possible molecular structure of these complexes were discussed by elemental analysis, spectroscopic studies and magnetic susceptibility measurements. The infrared spectra of these complexes all show two strong $Mo=O_t$ stretching bands in the 900∼$980cm^{-1}$, $MoO_2Mo$ very prominent strectching bands at around 410~425 and 735~$750cm^{-1}$ to symmetrical and asymmetrical O-bridge stretching, a coordinated $coo^-$ asymmetrical band in the 1585∼$1,640cm^{-1}$. Also, d-d transition of molybdenyl complexes corresponding to $^2B_2{\to}^2B_1$ occured in the 24,800~$28,000cm^{-1}$ region, charge transfer transition corresponding to ligand-to-molybdenum in the 32,500~33,800, 42,000~$47,500cm^{-1}$ region. The complexes synthesized were yellow or orange and diamagnetic.

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Study on the Corrosion Characteristics in the Slag Line of SEN Oxide Refractory (산화물계 SEN내화물의 슬래그 라인부 침식특성 연구)

  • Sung, Young Taek;Son, Jeong Hun;Lee, Sung Seok;Bae, Dong Sik
    • Korean Journal of Materials Research
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    • v.24 no.1
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    • pp.53-59
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    • 2014
  • The corrosion resistance of submerged entry nozzle (SEN) materials were investigated for high-class steel manufacturing. Composite samples were fabricated by mixing $ZrO_2$, $Al_2O_3$, MgO, mullite, spinel, and carbon. The raw materials were mixed with attrition milling, compacted in a uniaxial pressure of 200MPa and calcined at $1000^{\circ}C$ for 3 h in $N_2$ atmosphere. The bulk density and apparent porosity of the calcined samples were measured by the liquid displacement method in water using Archimedes's principle. The corrosion resistance of the samples were measured by cup test with mold powder at $1550^{\circ}C$ for 2 h. The microstructure and elemental analysis of samples were observed by scanning electron microscopy (SEM), energy dispersive spectrum (EDS), and X-ray diffraction pattern (XRD). The XRD result shows that the starting raw materials were crystalline phase. The microstructure of fabricated specimen was investigated before and after corrosion tests at $1000^{\circ}C$ and $1550^{\circ}C$ for 2h. $ZrO_2$-C composite showed good resistance in the slag corrosion test. Among the composite oxide materials, $ZrO_2-Al_2O_3$-C and $ZrO_2$-MgO-C showed better resistance than $ZrO_2$-C in the slag corrosion test. The diameter variation index of $ZrO_2$-C refractory was 16.1 at $1000^{\circ}C$ for 2 h. The diameter variation index of the $ZrO_2-Al_2O_3$-C refractory was larger than that of the $ZrO_2$-C refractory at $1550^{\circ}C$ for 2 h.

Performance of a Novel Sulfonate Flame Retardant Based on Adamantane for Polycarbonate (아드만탄 기반의 새로운 설포네이트 폴리카보네이트 난연제 성능 연구)

  • Guo, Jianwei;Wang, Yueqin;Feng, Lijuan;Zhong, Xing;Yang, Chufen;Liu, Sa;Cui, Yingde
    • Polymer(Korea)
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    • v.37 no.4
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    • pp.437-441
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    • 2013
  • A novel sulfonate flame retardant, 1,3,5,7-tetrakis(phenyl-4-sodium sulfonate)adamantane (FR-A), was successfully synthesized from 1-bromoadamantane in sequential four-step reactions involving Fiedel-Crafts phenylation, sulphonation, hydrolysis, and neutralization. The success of synthesis was confirmed by FTIR spectra, $^1H$ NMR spectra, elemental analyses and mass spectra. The effect of FR-A on the flame retardacy of polycarbonate (PC) has been studied. Limiting oxygen index (LOI) and thermogravimetric analysis (TGA) showed that this novel sulfonate flame retardant had effective flame retardancy on polycarbonate (PC). With a small amount (0.08 wt%) of FR-A, the flame retardancy of PC was improved obviously, which got to UL 94 V-0 rating. TGA and DTA curves demonstrated that the additive raised the degradation rate of PC by promoting the quick formation of an insulating carbon layer on the surface, and confirmed that the flame retardant mechanism of PC/FR-A system was similar to potassium diphenylsulfone sulfonate (KSS).

Synthesis and Microstructure of Fe-Base Superalloy Powders with Y-Oxide Dispersion by High Energy Ball Milling (고에너지 볼 밀링을 이용한 Y-산화물 분산 Fe-기초내열합금 분말의 합성 및 미세조직 특성)

  • Yim, Da-Mi;Park, Jong Kwan;Oh, Sung-Tag
    • Korean Journal of Materials Research
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    • v.25 no.8
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    • pp.386-390
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    • 2015
  • Fe-base superalloy powders with $Y_2O_3$ dispersion were prepared by high energy ball milling, followed by spark plasma sintering for consolidation. High-purity elemental powders with different Fe powder sizes of 24 and 50 mm were used for the preparation of $Fe-20Cr-4.5Al-0.5Ti-O.5Y_2O_3$ powder mixtures (wt%). The milling process of the powders was carried out in a horizontal rotary ball mill using a stainless steel vial and balls. The milling times of 1 to 5 h by constant operation (350 rpm, ball-to-powder ratio of 30:1 in weight) or cycle operation (1300 rpm for 4 min and 900 rpm for 1 min, 15:1) were applied. Microstructural observation revealed that the crystalline size of Fe decreased with an increase in milling time by cyclic operation and was about 15 nm after 3 h, forming a FeCr alloy phase. The cyclic operation had an advantage over constant milling in that a smaller-agglomerated structure was obtained. The milled powders were sintered at $1100^{\circ}C$ for 30 min in vacuum. With an increase in milling time, the sintered specimen showed a more homogeneous microstructure. In addition, a homogenous distribution of Y-compound particles in the grain boundary was confirmed by EDX analysis.

Characteristics of Thermophilic Bacteria and Secondary Materials Attached on the Pyrrhotite, Uljin (울진 자류철석 표면에 부착한 고온성박테리아와 2차 생성물의 특성)

  • Park, Cheon-Young;Kim, Bong-Ju
    • Journal of the Mineralogical Society of Korea
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    • v.23 no.4
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    • pp.315-329
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    • 2010
  • Characteristics of thermophilic bacteria and secondary materials on the pyrrhotite surface were investigated by using scanning electron microscopy (SEM). The thermophilic bacteria from an acid hot spring in Japan were incubated with pyrrhotite at $42^{\circ}C$, $52^{\circ}C$, and $62^{\circ}C$ respectively. SEM analysis of the reacted pyrrhotite showed that indigenous rod-shaped bacteria ranging from $0.4{\times}1.5{\mu}m$ to $0.3{\times}11.9{\mu}m$ in size were attached to the pyrrhotite surface at these temperatures with formation of secondary materials. Extracellular polymer substances were formed on the bacterial surface. We suggest that these polymers functioned as a capsule protecting bacteria from the extreme environment. Secondary materials such as elemental sulfur, Fe-hydroxide, S-Fe and O-P-Fe compounds were found on the pyrrhotite surface.

Methacrylamidohistidine in Affinity Ligands for Immobilized Metal-ion Affinity Chromatography of Human Serum Albumin

  • Odaba, Mehmet;Garipacan, Bora;Dede, Semir;Denizli, Adil
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.6 no.6
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    • pp.402-409
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    • 2001
  • Different bioligands carrying synthetic adsorbents have been reported in the literature for protein separation, We have developed a novel and new approach to obtain high protein ad-sorption capacity utilizing 2-methacrylamidohistidine(MAH) as a bioligand. MAH was synthe-sized by reacting methacrylocholride and histidine, Spherical beads with an average size of 150-200㎛ were obtained by the radical suspension polymerization of MAH and 2-hydrosyethyl-methacrylate(HEMA) conducted in an aqueous dispersion medium. p(HEMA-co-MAH) beads had a specific surface area of 17.6㎡/g . Synthesized MAH monomer was characterized by NMR. p(HEMA-co-MAH) beads were characterized by swelling test, FTIR and elemental analysis. Then Cu(II) ions were incorporated onto the beads and Cu(II) loading was found to be 0.96 mmol/g.These affinity beads with a swelling ration of 65% and containing, 1.6 mmol MAH/g were used in the adsorption/desorption of human serum albumin(HSA) from both aqueous solutions and hu-man serum. The adsorption of HSA onto p(HEM-co-MAH) was low(8.8 mg/g). Cu(II) chelation onto the beads significantly increased the HSA adsorption (56.3 mg/g). The maximum HSA ad-sorption ws observed at pH 8.0 Higher HSA adsorption was observed from human plasma(94.6 mgHSA/g) Adsorption of other serum proteins were obtained as 3.7 mg/g for fibrinogen and 8.5mg/g for γ-globulin. The total protein adsorption was determined as 107.1mg/g. Desorption of HSA was obtained using 0.1 M Tris/HCl buffer containing 0.5 M NaSCN, High desorption rations(up to 98% of the adsorbed HSA) were observed. It was possible to reuse Cu(II) chelated-p(HEMA-co-MAH) beads without significant decreases in the adsorption capacities.

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Detailed Abundance Analysis for Plant Host Stars

  • Kang, Won-Seok;Lee, Sang-Gak;Kim, Kang-Min
    • The Bulletin of The Korean Astronomical Society
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    • v.36 no.1
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    • pp.27.1-27.1
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    • 2011
  • We obtained the spectra of 93 Planet host stars and 73 normal field stars in F, G, K type using BOES at BOAO. We measured the equivalent width of Fe and 25 elements lines using the automatic EW measurement program, TAME(Tools for Automatic Measurement of Equivalent-widths) and estimated the elemental abundances by synth and abfind driver of MOOG code. Since the absence of planets in the normal field stars cannot be "completely" proved, this work focused on the chemical abundances and planet properties of planet host stars, which have the massive planets close to the parent star relatively. We carried out an investigation for the difference of abundances between stars with "Hot Jupiter" and normal field stars with no known planets. We examined the chemical composition of 25 elements, such as C, N, O, S, Na, Mg, Al, Si, K, Ca, Sc, Ti, V, Cr, Mn, Co, Ni, Cu, Zn, Sr, Y, Zr, Ba, Ce, Nd, and Eu by EW measurements, and the S abundances were estimated using synthetic spectrum. We have found that [Mg/Fe] and [Al/Fe] for planet host stars have lower limit comparing with those of comparison stars, and [Ca/Fe] of host star with Neptunian planets is relatively lower than the other host stars with massive planets. We have performed the Kolmogorov-Smirnov test, and examined the ratio of planet host stars to all stars for each bin of [X/H]. As a result, we noted that the O, Si, and Ca abfor undances are strongly related with the presence of planets.

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A Study on the Application of Cost Risk Exposure methods by the Probabilistic Evaluation on the Construction Projects (확률적 평가에 의한 건설공사 비용 위험도 측정의 적용성에 관한 연구)

  • Cho Jea-Ho;Chun Jae-Youl
    • Korean Journal of Construction Engineering and Management
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    • v.1 no.1 s.1
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    • pp.63-71
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    • 2000
  • The paper considers two non-deterministic methods of analysing the risk exposure in a cost estimate The fist method(referred to as the 'conventional statistical' method) analyses cost data directly, to describe a probability distribution for total cost. The second method(referred to as the 'Monte Carlo simulation' method) interprets cost data directly, to generate a probability distribution for total costs from the descriptions of elemental cost distribution. The common practice of allowing for risk through an all-embracing contingency sum or percentage addition is challenged. Rather than excluding conventional, non-deterministic methods, they are here presented as possibly the only of effective foundation on which to risk management in cost estimating.

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