• 제목/요약/키워드: elemental techniques

검색결과 118건 처리시간 0.023초

Template Synthesis and Characterization of Host (Nanocavity of Zeolite Y)-Guest ([Cu([18]aneN4S2)]2+, [Cu([20]aneN4S2)]2+, [Cu(Bzo2[18]aneN4S2)]2+, [Cu(Bzo2[20]aneN4S2)]2+) Nanocomposite Materials

  • Salavati-Niasari, Masoud;Mirsattari, Seyed Nezamodin;Saberyan, Kamal
    • Bulletin of the Korean Chemical Society
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    • 제30권2호
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    • pp.348-354
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    • 2009
  • Copper(II) complexes with tetraoxo dithia tetraaza macrocyclic ligands; [18]ane$N_4S_2$: 1,4,10,13-tetraaza-5,9,14,18-tetraoxo-7,16-dithia-cyclooctadecane, [20]ane$N_4S_2$: 1,5,11,15-tetraaza-6,10,16,20-tetraoxo-8,18-dithia-cyclocosane,Bzo2[18]ane$N_4S_2$: dibenzo-1,4,10,13-tetraaza-5,9,14,18-tetraoxo-7,16-dithia-cyclooctadecane, Bzo2[20]ane$N_4S_2$: dibenzo-1,5,11,15-tetraaza-6,10,16,20-tetraoxo-8,18-dithia-cyclocosane; were entrapped in the nanopores of zeolite-Y by a two-step process in the liquid phase: (i) adsorption of [bis(diamine)copper(II)] (diamine = 1,2-diaminoethane, 1,3-diaminopropane, 1,2-diaminobenzene, 1,3-diaminobenzene); $[Cu(N-N)_2]^{2+}$-NaY; in the nanopores of the zeolite, and (ii) in situ template condensation of the copper(II) precursor complex with thiodiglycolic acid. The obtained complexes and new host-guest nanocomposite materials; $[Cu([18]aneN_4S_2)]^{2+}-NaY,\;[Cu([20]aneN_4S_2)]^{2+}-NaY,\;[Cu(Bzo_2[18]aneN_4S_2)]^{2+}-NaY,\;[Cu(Bzo_2[20]aneN_4S_2)]^{2+}$-NaY; have been characterized by elemental analysis FT-IR, DRS and UV-Vis spectroscopic techniques, molar conductance and magnetic moment data, XRD and, as well as nitrogen adsorption. Analysis of data indicates all of the complexes have been encapsulated within nanopore of zeolite Y without affecting the zeolite framework structure.

Efficacy of various cleaning solutions on saliva-contaminated zirconia for improved resin bonding

  • Kim, Da-Hye;Son, Jun-Sik;Jeong, Seong-Hwa;Kim, Young-Kyung;Kim, Kyo-Han;Kwon, Tae-Yub
    • The Journal of Advanced Prosthodontics
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    • 제7권2호
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    • pp.85-92
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    • 2015
  • PURPOSE. This study aimed to investigate the efficacy of cleaning solutions on saliva-contaminated zirconia in comparison to air-abrasion in terms of resin bonding. MATERIALS AND METHODS. For saliva-contaminated air-abraded zirconia, seven cleaning methods)-no contamination (NC), water-spray rinsing (WS), additional air-abrasion (AA), and cleaning with four solutions (Ivoclean [IC]; 1.0 wt% sodium dodecyl sulfate [SDS], 1.0 wt% hydrogen peroxide [HP], and 1.0 wt% sodium hypochlorite [SHC])-were tested. The zirconia surfaces for each group were characterized using various analytical techniques. Three bonded resin (Panavia F 2.0) cylinders (bonding area: $4.5mm^2$) were made on one zirconia disk specimen using the Ultradent jig method [four disks (12 cylinders)/group; a total of 28 disks]. After 5,000 thermocycling, all specimens were subjected to a shear bond strength test with a crosshead speed of 1.0 mm/minute. The fractured surfaces were observed using an optical and scanning electron microscope (SEM). RESULTS. Contact angle measurements showed that groups NC, AA, IC, and SHC had hydrophilic surfaces. The X-ray photoelectron spectroscopy (XPS) analysis showed similar elemental distributions between group AA and groups IC and SHC. Groups IC and SHC showed statistically similar bond strengths to groups NC and AA (P>.05), but not groups SDS and HP (P<.05). For groups WS, SDS, and HP, blister-like bubble formations were observed on the surfaces under SEM. CONCLUSION. Within the limitations of this in vitro study, some of the cleaning solutions (IC or SHC) were effective in removing saliva contamination and enhancing the resin bond strength.

Aminopropyl-Terminated Polydimethylsiloxane과 Trichlorogermyl 곁가지 그룹을 갖는 Polyamide 블록공중합체의 합성, 구조분석 및 열적거동 (Synthesis, Structural Characterization and Thermal Behaviour of Block Copolymers of Aminopropyl-Terminated Polydimethylsiloxane and Polyamide Having Trichlorogermyl Pendant Group)

  • Gill, Rohama;Mazhar, M.;Mahboob, Sumera;Siddiq, Muhammad
    • 폴리머
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    • 제32권3호
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    • pp.239-245
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    • 2008
  • Block copolymers of the general formula $[(-CO-R'-CO-HN-Ar-NH-CO-R'-CO)_xNH(CH_2)_3-(Me_2SiO)_y(CH_2)_3NH_2]_n$, [n=18.00 to 1175.0] where $R'=CH_2CH(CH_2GeCl_3)$;$CH_2CHGeCl_3CH_2$; and $Ar=-C_6H_4$;$-(o.CH_3C_6H_4)_2$;$-o.CH_3OC_6H_4)_2$;$-(o.CH_3C_6H_4)$ were prepared by a polycondensation reaction of polyamide containing a pendant trichlorogermyl group and terminal acid chloride $Cl(-CO-R'-CO-NH-Ar-NH-CO-R'-CO-)_xCl$ with aminopropyl-terminated polydimethylsiloxane $H_2N(CH_2)_3(Me_2SiO)_y-(CH_2)_3NH_2]$, (PDMS). These polymers were characterized by elemental analysis, $T_g$, FT-IR, $^1H$-NMR, solid state $^{13}C$-NMR, and molecular weight determination. The thermal stability of these copolymers was examined using thermal analysis techniques, such as TGA and DSC. Their molecular weights as determined by laser light scattering technique ranged $5.13{\times}10^5$ to $331{\times}10^5\;g/mol$. These polymers display their $T_g$ in the range of 337 to $393^{\circ}C$ with an average decomposition temperature at $582^{\circ}C$.

Chemical Doping of $TiO_2$ with Nitrogen and Fluorine and Its Support Effect on Catalytic Activity of CO Oxidation

  • Chakravarthy, G. Kalyan;Kim, Sunmi;Kim, Sang Hoon;Park, Jeong Young
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
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    • pp.142.2-142.2
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    • 2013
  • The effect of substrate on catalytic activity of CO oxidation with transition metal Platinum nanoparticles on doped and undoped TiO2 was investigated. Titanium dioxide was doped chemically with non-metal anions including nitrogen and fluorine. Undoped TiO2 was synthesized via simple conventional sol-gel route. Thin films of titania were developed by spin coating technique and the characterization techniques SEM, XRD, UV-Vis Absorption Spectroscopy and XPS were carried out to examine the morphology of films, crystal phase, crystallites, optical properties and elemental composition respectively. XPS analysis from doped TiO2 confirmed that the nitrogen site were interstitial whereas fluorine was doped into TiO2 lattice substitutionally. Catalytic activity systems of Pt/doped-TiO2 and Pt/undoped-TiO2 were fabricated to reveal the strong metal-support interaction effect during catalytic activity of CO oxidation reactions. By arc plasma deposition technique, platinum nanoparticles with mean size of 2.7 nm were deposited on the thin films of doped and undoped titanium dioxide. The CO oxidation was performed with 40 Torr CO and 100 Torr O2 with 620 Torr He carrier gas. Turn over frequency was observed two to three folds enhancement in case of Pt/doped TiO2 as compared to Pt/TiO2. The electronic excitation and the oxygen vacancies that were formed with the doping process were the plausible reasons for the enhancement of catalytic activity.

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반응성 밀링에 의해 제조된 Cr2O3 분산강화형 Cu 합금의 미세조직과 입자조대화 (The Microstructure and Coarsening Behavior of Cr2O3 Dispersoid in ODS Cu Produced by Reactive Milling)

  • 박은범;황승준
    • 열처리공학회지
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    • 제31권4호
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    • pp.171-179
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    • 2018
  • Copper powder dispersed with 4 vol.% of $Cr_2O_3$ was successfully produced by a simple milling at 210 K with a mixture of $Cu_2O$, Cu and Cr elemental powders, followed by Hot Pressing (HP) at 1123 K and 50 MPa for 2h to consolidate the milled powder. The microstructure of the HPed material was characterized by standard metallographic techniques such as XRD (X-ray Diffraction), TEM and STEM-EDS. The results of STEMEDS analysis showed that the HPed materials comprised a mixture of nanocrystalline Cu matrix and $Cr_2O_3$ dispersoid with a homogeneous bimodal size distribution. The mechanical properties of the HPed materials were characterized by micro Vickers hardness test at room temperature. The thermodynamic considerations on the heat of formation, the incubation time to ignite MSR (Mechanically induced Self-sustaining Reaction), and the adiabatic temperature for the heat of displacement reaction between the oxide-metal are made for the delayed formation of $Cr_2O_3$ dispersoid in terms of MSR suppression. The results of TEM observation and hardness test indicated that the relatively large dispersoids in the HPed materials are attributed to the significant coarsening for the high temperature consolidation; this leads to the low Vickers hardness value. Based on the thermodynamic calculation for the operating processes with a limited number of parameters, the formation kinetics and coarsening of the $Cr_2O_3$ dispersoid are discussed.

New Cryptand Complexes of Lanthanides(Ⅲ) and Dioxouranium(Ⅵ) Nitrates

  • Oh-Jin Jung;Chil-Nam Choi;Hak-Jin Jung
    • Bulletin of the Korean Chemical Society
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    • 제12권2호
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    • pp.130-137
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    • 1991
  • The following new cryptand 221 complexes of lanthanides(Ⅲ) and dioxouranium(Ⅵ) nitrate have been synthesized: $(Ln(C_{16}H_{32}N_2O_5)(H_2O)_2(NO_3)_3\ and \((UO_2)_2(C_{16}H_{32}N_2O_5)(H_2O)_4(NO_3)_4$. These complexes have been identified by elemental analysis, moisture titration, conductivity measurements and various spectroscopic techniques. The proton and carbon-13 NMR as well as calorimetric measurements were used to study the interaction of cryptand 221 with La(Ⅲ), Pr(Ⅲ ), Ho(Ⅲ) and $UO_2(Ⅱ)$ ions in nonaqueous solvents. The bands of metal-oxygen atoms, metal-nitrogen atoms and O-U-O in the IR spectra shift upon complexation to lower frequencies, and the vibrational spectra ({\delta}NMN$) of metal-amide complexes in the crystalline state exhibit lattice vibrations below 300 $cm^{-1}$. The NMR spectra of the lanthanides(Ⅲ) and dioxouranium(Ⅵ) nitrate complexes in nonaqueous solvents are quite different, indicating that the ligand exists in different conformation, and also the $^1H$ and $^{13}C-NMR$ studies indicated that the nitrogen atom of the ring has greater affinity to metal ions than does the oxygen atom, and the planalities of the ring are lost by complexation with metal ions. Calorimetric measurements show that cryptand 221 forms more stable complexes with $La^{3+}$ and $Pr^{3+}$ ions than with $UO^{22+}$ ion, and $La^{3+}/Pr^{3+}$ and $UO^{22+}/Pr^{3+}$ selectivity depends on the solvents. These changes on the stabilities are dependent on the basicity of the ligand and the size of the metal ions. The absorption band (230-260 nm) of the complex which arises from the direct interaction of macrocyclic donor atoms with the metal ion is due to n-{\delta}*$ transition and also that (640-675 nm) of $UO^{22+}$-cryptand 221 complex, which arises from interaction between two-dioxouranium(Ⅵ) ions in being out of cavity of the ligand ring is due to d-d* transition.

Formation of Cadmium(II) Nitrate Complexes with Macrocycles

  • Ho-Doo Kim;Hak-Jin Jung;Oh-Jin Jung
    • Bulletin of the Korean Chemical Society
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    • 제14권5호
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    • pp.561-567
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    • 1993
  • The twelve macrocycle (L) complexes of cadmium(II) nitrate have been synthesized: $CdL(NO_3)_2$. All the complexes have been indentified by elemental analysis, electric conductivity measurements, IR and NMR spectroscopic techniques. The molar electric conductivities of the complexes in water and acetonitrile solvent were in the range of 236.8-296.1 $cm^2{\cdot}mol^{-1}{\cdot}ohm^{-1}$ at 25$^{\circ}$C. The characteristic peaks of macrocycles affected from Cd(II) were shifted to lower frequencies as compared with uncomplexed macrocycles. A complex with 1,4,8,11-tetrakis(methylacetato)-1,4,8,11-tetraaza cyclodecane (L4) exhibited two characteristic bands such as strong stretching (1646 $cm^{-1})$, and weaker symmetric stretching band (1384 $cm^{-1})$. NMR studies indicated that all nitrogen donor atoms of macrocycles have greater affinity to cadmium(II) metal ion than do the oxygen atoms. The $^{13}$C-resonance lines of methylene groups neighboring the donor atom such as N and S were shifted to a direction of high magnetic field and the order of chemical shifts were $L_1 < L_2 < L_3 < L_6 < L_4$. Also the chemical shifts values were larger than those of methylene groups bridgeheaded in side-armed groups. This result seems due to not only the strong interaction of Cd(Ⅱ) with nitrogen donors according to the HSAB theory, but weak interaction of Cd(Ⅱ) and COO- ions or sulfur which is enhanced by the flexible methylene spacing group in side-armed groups. Thus, each additional gem-methyl pairs of L_3, L_4\;and\; L_6$ macrocycles relative to $L_1, L_2,\;and\;L_5$ leads to an large enhancement in Cd(II) affinity. ^{13}C$-NMR spectrum of the complex with $L_{12}$ (1,5,9,13-tetracyclothiacyclohexadecane-3,11-diol) reveals the presence of two sets of three resonance lines, and intensities of the each resonance line have the ratio of 1 : 2 : 2. This molecular conformation is predicted as structure of tetragonal complex to be formed by coordinating two sulfur atoms and the other two sulfur atoms which is affected by OH-groups.

거푸집 종류에 따른 콘크리트 표면 특성 (Surface Characteristics of Concrete According to Types of Formworks)

  • 박세언;최정일;이봉기;이방연
    • 한국건설순환자원학회논문집
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    • 제9권4호
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    • pp.499-505
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    • 2021
  • 이 연구의 목적은 거푸집 종류별로 콘크리트 표면의 물리/화학적 특성을 실험적으로 조사하는 것이다. 이를 위하여 건설공사에 일반적으로 사용되는 합판 거푸집과 코팅된 합판 거푸집을 준비하였고, 추가로 콘크리트 표면 열화나 거친 표면을 모사하기 위해 사포를 부착한 합판 거푸집을 준비하였다. 콘크리트는 일반 콘크리트를 사용하였다. 콘크리트 표면 특성은 육안관찰, 주사전자현미경 관찰, 성분 이미지 맵핑, 화학성분 분석, 2차원과 3차원 표면 형상 분석, 그리고 제타 전위 측정을 통해 조사하였다. 실험결과 코팅된 거푸집과 접한 콘크리트 표면이 가장 매끄럽고, 사포를 부착한 거푸집과 접한 콘크리트 표면이 가장 거친 것으로 나타났다. 이외에도 거푸집 종류별로 표면 특성에 뚜렷한 차이가 나타났다. 다만 표면 거칠기가 화학 성분이나 제타 전위에 비하여 차이가 크게 나타났다.

Expression and Purification of Transmembrane Protein MerE from Mercury-Resistant Bacillus cereus

  • Amin, Aatif;Sarwar, Arslan;Saleem, Mushtaq A.;Latif, Zakia;Opella, Stanley J.
    • Journal of Microbiology and Biotechnology
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    • 제29권2호
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    • pp.274-282
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    • 2019
  • Mercury-resistant ($Hg^R$) bacteria were isolated from heavy metal polluted wastewater and soil collected near to tanneries of district Kasur, Pakistan. Bacterial isolates AZ-1, AZ-2 and AZ-3 showed resistance up to $40{\mu}g/ml$ against mercuric chloride ($HgCl_2$). 16S rDNA ribotyping and phylogenetic analysis were performed for the characterization of selected isolates as Bacillus sp. AZ-1 (KT270477), Bacillus cereus AZ-2 (KT270478) and Bacillus cereus AZ-3 (KT270479). Phylogenetic relationship on the basis of merA nucleotide sequence confirmed 51-100% homology with the corresponding region of the merA gene of already reported mercury-resistant Gram-positive bacteria. The merE gene involved in the transportation of elemental mercury ($Hg^0$) via cell membrane was cloned for the first time into pHLV vector and transformed in overexpressed C43(DE3) E. coli cells. The recombinant plasmid (pHLMerE) was expressed and the native MerE protein was obtained after thrombin cleavage by size exclusion chromatography (SEC). The purification of fusion/recombinant and native protein MerE by Ni-NTA column, dialysis and fast protein liquid chromatography (FPLC/SEC) involved unfolding/refolding techniques. A small-scale reservoir of wastewater containing $30{\mu}g/ml$ of $HgCl_2$ was designed to check the detoxification ability of selected strains. It resulted in 83% detoxification of mercury by B. cereus AZ-2 and B. cereus AZ-3, and 76% detoxification by Bacillus sp. AZ-1 respectively (p < 0.05).

시맨틱 네트워크 분석을 이용한 국내외 언플러그드 활동 관련 연구 비교 (Comparison of Unplugged Activities at Home and Abroad using Semantic Network Analysis)

  • 강두봉
    • 컴퓨터교육학회논문지
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    • 제22권4호
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    • pp.21-34
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    • 2019
  • 최근 2015개정 교육과정의 적용으로 소프트웨어 교육이 학교 현장에서 이루어지고 있다. 소프트웨어 교육의 목적은 컴퓨팅 사고력 신장에 있으며, 이를 위해 언플러그드 활동, 교육용 프로그래밍언어, 피지컬 컴퓨팅 등의 방법을 활용하고 있다. 이 중 언플러그드 활동과 관련된 국내 73편, 해외 85편의 연구물들을 시맨틱 네트워크 분석 기법을 활용하여 비교 분석하였다. 주제어 분석 결과 해외에서는 1998년부터, 국내에서는 2006년부터 연구가 시작되었으나, 4차 산업 혁명의 이슈와 맞물려 전 세계적으로 컴퓨팅 사고력이 미래 사회를 위한 핵심역량으로 인식되면서 국내외 모두 2016년 이후 연구가 급증하고 있음을 알 수 있었다. 국내 연구에서 소프트웨어 교육에서 활용되는 '언플러그드 활동', '로봇 활용', '교육용 프로그래밍 언어' 등의 수단적 요소에 관한 주제어가 많이 나타난 것으로 분석되었다. 언플러그드 활동이 컴퓨팅 사고력을 함양시키기 위한 방법으로 활용되어야할 것이며 이를 위해 컴퓨터 과학의 목적인 '컴퓨팅 사고력' 에 대한 고찰을 바탕으로 연구가 진행될 필요가 있다.