• Title/Summary/Keyword: $^{27}Al$ NMR

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Synthesis of AlPO4-type Mesoporous Materials Using Alum Sludge (Alum 슬러지를 이용한 AlPO4-계 다공성 물질의 합성)

  • Kang, Kwang Cheol;Kim, Young Ho;Kim, Jin-man;Lee, Choul Ho;Rhee, Seog Woo
    • Applied Chemistry for Engineering
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    • v.22 no.2
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    • pp.173-177
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    • 2011
  • In this study, the formation of $AlPO_4$-type porous materials from alum sludge was investigated. The materials were synthesized by the reaction of aluminum hydroxide and phosphoric acid with an organic template. Cationic surfactant, natural humic acid, and amino acids were used for the organic template. The residual organic templates were removed by calcination at $600^{\circ}C$ in the air. Powder X-ray diffraction patterns showed the charicteristic patterns of the $AlPO_4$-type porous materials. The morphology of the material was examined using a scanning electron microscopy. The coordination environment of $Al^{3+}$ ion was investigated by $^{27}Al$ MAS NMR technique. Both tetrahedrally and octahedrally coordinated$Al^{3+}$ ions were found in the as-synthesized samples while all $Al^{3+}$ ions were tetrahedrally coordinated in the calcined products. The development of mesopore in the solid material was confirmed by the measurement of BET specific surface area. Finally, they were used for removal of toxic formaldehyde from the air and the formaldehyde molecules were adsorbed on the surface of pores. In conclusion, $AlPO_4$-type porous materials from alum sludge might be applicable in the removal of toxic volatile organic compounds from the air.

Pressure-load Calibration of Multi-anvil Press at Ambient Temperature through Structural Change in Cold Compressed Amorphous Pyrope (비정질 파이로프의 저온 압축에 따른 구조 변화를 이용한 멀티 앤빌 프레스의 상온 압력-부하 보정)

  • Lhee, Juho;Kim, Yong-Hyun;Lee, A Chim;Kim, Eun Jeong;Lee, Seoyoung;Lee, Sung Keun
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.1
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    • pp.65-73
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    • 2022
  • The proper estimation of physical and chemical properties of Earth materials and their structures at high pressure and high temperature conditions is key to the full understanding of diverse geological processes in Earth and planetary interiors. Multi-anvil press - high-pressure generating device - provides unique information of Earth materials under compression, mainly relevant to Earth's upper mantle. The quantitative estimation of the relationship between the oil load within press and the actual pressure conditions within the sample needs to be established to infer the planetary processes. Such pressure-load calibration has often been based on the phase transitions of crystalline earth materials with known pressure conditions; however, unlike at high temperature conditions, phase transitions at low (or room) temperatures can be sluggish, making the calibration at such conditions challenging. In this study, we explored the changes in Al coordination environments of permanently densified pyrope glasses upon the cold compression using the high-resolution 27Al MAS and 3QMAS NMR. The fractions of highly coordinated Al in the cold compressed pyrope glasses increase with increasing oil load and thus, the peak pressure condition. Based on known relationship between the peak pressure and the Al coordination environment in the compressed pyrope glasses at room temperature, we established a room temperature pressure-load calibration of the 14/8 HT assembly in 1,100-ton multi-anvil press. The current results highlight the first pressure-load calibration of any high pressure device using high-resolution NMR. Irreversible structural densification upon cold compression observed for the pyrope glasses provides insights into the deformation and densification mechanisms of amorphous earth materials at low temperature and high pressure conditions within the subducting slabs.

Synthesis and characterization of MCM-41 type aluminosilicates (MCM-41형태의 알루미노실리케이트의 합성특성)

  • Lee, Sung-Hee;Lee, Dong-Kyu;Park, Soo-Gil
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2003.07b
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    • pp.1231-1234
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    • 2003
  • A sample procedure has been described to room temperature synthesis, mesoporous aluminosilicate materials with strong surface acidity by using a cationic surfactnat cetyltrimethylammonium bromide(CTABr) as the template agent. All samples were charecterized by X-ray diffraction(XRD) and nitrogen adsorption. The crystallinity and surface area of MCM-41 type aluminosilicats decrease with decreasing of Si/Al ratio. The influence of the aluminum contents of MCM-41 on the coordination of Al and on the acidity is studied by $^{27}Al$ MAS NMR and temperature programmed desorption of ammonia(TPD). It was shown that the incorporation of Al atoms into the framework causes increasing of acid site surface. And then Al atoms in the framework were incorporated tetrahedrally in structure, which gave a rise to cationic sites in the framework.

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Dissolution Mechanism of Abandoned Metal Ores and Formation of Ochreous Precipitates, Dalseong Mine (달성광산의 폐금속 광석의 용해메커니즘과 하상 침전물의 형성특징)

  • Choo, Chang-Oh;Lee, Jin-Kook;Jeong, Gyo-Cheol
    • The Journal of Engineering Geology
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    • v.18 no.4
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    • pp.577-586
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    • 2008
  • The formation of acid mine drainage is closely related to water chemistry and ochreous sprecipitates formed at the bottom of creeks because it is initially derived from the possible water-rock interaction in abandoned waste metals at the mine. According to analyses on water, precipitates, and alteration characters of ore metals in Dalseone mine, whitish precipitates formed at pHs above 5 while schwertmannite formed at pH $3{\sim}4$. Water chemistry vary with seasons. The water chemistry of the treatment site measured ir Octoter 2002 is characterized by lower pH, and higher Al, Zn, Cu contents relative to those in March, 2003. In the latter case, As and Cl contents are very high. $^{27}Al$ MAS NMR data show the presence of predominant octahedral Al in whitish precipitates. Metal ore minerals dissolve at margins, cleavage, or comer of crystals where reactive sites are potential. Pyrite dissolves, forming etch pits or smooth faces on the edge.

Development of Fly Ash/slag Cement Using Alkali-activated Reaction(2) - Reaction products and microstructure - (알칼리 활성반응을 이용한 플라이 애쉬/슬래그 시멘트 개발(2) - 반응생성물과 미세구조 -)

  • Park, Sang-Sook;Kang, Hwa-Young;Han, Kwan-Su
    • Journal of Korean Society of Environmental Engineers
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    • v.29 no.7
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    • pp.810-819
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    • 2007
  • Investigation of alkali activation of fly ash and blast furnace slag was carried out using waterglass and sodium hydroxide. XRD, FTIR, $^{29}Si$ and $^{27}Al$ NMR, TGA and SEM were used to observed the reaction products and microstructure of the fly ash/slag cement (FSC) pastes. The reaction products were amorphous or low-ordered calcium silicate hydrate and aluminosilicate gel produced from alkali activation of blast furnace slag and fly ash, respectively. On the basis of this investigation, waterglass solution with a modulus(Ms) of 1.0 and 1.2 is recommended for alkali activation of fly ash and blast furnace slag. Morphology of FSC pastes alkali-activated with Ms of 1.0 and 1.2 shows a more solid and continuous matrix due to restructuring of gel-like reaction products from alkali-activated fly ash and blast furnace slag together with another hydrolysis product(i.e., silica gel) from water glass.

Catalytic Cracking of n-Octane over H-ZSM-5 Catalysts: Effect of Calcination and Steam Treatment (H-ZSM-5 촉매에서 n-옥탄의 촉매분해반응: 소성 및 스팀 처리 효과)

  • Lee, Hyun-Ju;Shin, Chae-Ho;Choi, Won Choon;Lee, Chul Wee;Park, Yong Ki
    • Korean Chemical Engineering Research
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    • v.46 no.2
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    • pp.291-300
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    • 2008
  • Catalytic cracking of n-octane was carried out over H-ZSM-5 zeolite catalysts after calcination with air and steaming with 100% steam in the temperature range of $550-750^{\circ}C$ for 24 h and compared with the results of thermal cracking. The increase of calcination and steaming temperature resulted in the decrease of surface area, pore volume, and strong acid sites, which was mainly caused by the dealumination of H-ZSM-5 framework. It was found by $^{27}Al$ and $^{29}Si$ MAS NMR that the dealumination was proceeded through the transformation process of tetrahedral framework Al${\rightarrow}$penta-cordinated Al ${\rightarrow}$ octahedral framework Al and the phenomena was much more severe in steaming conditions than that of calcination. In the catalytic cracking of n-octane, as the temperatures of calcination and steaming were increased, the conversion of n-octane, the selectivity of light olefins and ethylene to propylene ratio were decreased due to the dealumination of framework aluminum resulting the loss of acidic strengths. The conversion, selectivity of light olefins and ethylene to propylene ratio reached almost to the level of thermal cracking after steaming at $750^{\circ}C$ for 24 h.

Structural and Chemical Characterization of Aquatic Humic Substances in Conventional Water Treatment Processes (재래식 정수처리 공정에서 수질계 휴믹물질의 구조 및 화학적 특성분석)

  • Kim, Hyun-Chul;Yu, Myong-Jin
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.1
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    • pp.11-16
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    • 2005
  • Humic substances(HS) from raw and process waters at a conventional water treatment plant were isolated and extracted by physicochemical fractionation methods to investigate their characteristics. They are characterized for their functionality, chemical composition, and spectroscopic characteristics using FT-IR(Fourier transform infrared) and $^1H-NMR$(proton nuclear magnetic resonance) spectroscopy. Humic fraction gradually decreased from 47.2% to 26.4%(from 0.97 to 0.54 mgC/L) through conventional water treatment processes. Concentration of phenolic groups in the HS fraction gradually decreased from 60.5% to 21.8%(from 12.2 to $6.0\;{\mu}M/L$ as phenolic-OH) through water treatment. In the case of carboxylic groups, the concentration increased from 39.5% to 46.9%(from 7.9 to $10.6\;{\mu}M/L$ as COOH) by pre-chlorination, but gradually decreased to 34.2%($9.4\;{\mu}M/L$ as COOH) through sedimentation and sand filtration. From the results of the FT-IR and $^1H-NMR$ spectra of HS, the content of carboxylic groups increased and ratio of aliphatic protons to aromatic protons($P_{Al}/P_{Ar}$) also increased through water treatment, which indicated the increase of aliphatic compounds.

Kinetic Study of Proton Exchange between Al($H_2O$)$_6^{3+}$ Ion and Bulk Water Molecules (Ⅰ) (Al($H_2O$)$_6^{3+}$ 이온과 물 용매 분자 사이에서의 수소 이온 교환의 반응속도론적 연구 (Ⅰ))

  • Moon-Hwan Cho;Jin-Ho Kim;Chang-Ju Yoon
    • Journal of the Korean Chemical Society
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    • v.32 no.5
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    • pp.436-442
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    • 1988
  • The $^1H-nmr$ lineshapes of $H_2O$ in the solution containing $Al^{3+}$ ion have been measured as a function of temperature and $H^+$-ion concentration. Above [$H^+$] = 0.06, the lineshape were analyzed by the uncoupled two-site exchange model. From the proton exchange rate between hexaaquaaluminium ion and bulk water as a function of H-ion concentration. These kinetic data could be fitted to a following linear rate law; that is; 1/${\tau}$ = k$_1$/12 + $k_2$[$H^+$]/6. The following proton exchange parameters were obtained; $k_1^{298}$ = 38.5s$^{-1}$ ${\{Delta}H_1^{\neq}$ = $42.9kJ mole^{-1}$ ${\{Delta}S_1^{\neq}$ = -48.6J $mole^{-1}K^{-1}$ $k_2^{298}$ = $172s^{-1}mole^{-1}$ ${\{Delta}H_2^{\neq}$ = 27.8kJ $mole^{-1}$ ${\{Delta}S_2^{\neq}$ = -90.3J $mole^{-1}K^{-1}$ These activation parameters are indicating an associative interchange, Ia, mechanism for the acid-hydrolysis of hexaaquaaluminium ion and the proton exchange between the hydration spheres of $Al^{3+}$ and $H^+$.

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Comparison of Organic Carbon Composition in Profile by Using Solid 13C CPNMR Spectroscopy in Volcanic Ash Soil

  • Sonn, Yeon Kyu;Kang, Seong Soo;Ha, Sang Keun;Kim, Yoo Hak;Lee, Chang Hoon
    • Korean Journal of Soil Science and Fertilizer
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    • v.46 no.5
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    • pp.391-398
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    • 2013
  • Soil organic carbon (SOC) has the potential to promote the soil quality for sustainability and mitigation of global warming. There is little information on organic carbon composition despite of having resistance of carbon degradation in soil. In this study, to understand the effect of volcanic ash on organic carbon composition and quantity in soil, we investigated characteristics of volcanic soil and compared organic carbon composition of soil and humic extract by using $^{13}C$-CPMAS-NMR spectra under soil profiles of Namweon series in Jeju. SOC contents of inner soil profiles were 134.8, 101.3, and 27.4 g C $kg^{-1}$ at the layer of depth 10-20, 70-80 and 90-100 cm, respectively. These layers were significantly different to soil pH, oxalate Al contents, and soil moisture contents. Alkyl C/O-alkyl C ratio in soil was higher than that of humic extracts, which was decreased below soil depth. Aromaticity of soil and humic extract was ranged from 29-38 and 24-32%, which was highest at the humic extract of 70-80 cm in soil depth. These results indicate that the changes of SOC in volcanic ash soil resulted from alteration of organic composition by pyrolysis and stability of organic carbon by allophane in volcanic ash soil.

Synthesis, Characterization and Biological Studies of New Mn(II), Ni(II), Co(II), Cu(II) and Zn(II) of 2-(benzothiazol-2-yl)-N'-(2,5-dihydroxybenzylidene)acetohydrazide (2-(Benzothiazol-2-yl)-N'-(2,5-dihydroxybenzylidene)acetohydrazide의 Mn(II), Ni(II), Co(II), Cu(II) 및 Zn(II) 착물의 합성, 특성 및 생물학적 연구)

  • El-Tabl, Abdou S.;Shakdofa, Mohamad M.E.;El-Seidy, Ahmed M.A.;Al-Hakimi, Ahmed N.
    • Journal of the Korean Chemical Society
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    • v.55 no.1
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    • pp.19-27
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    • 2011
  • New series of Mn(II), Ni(II), Co(II), Cu(II) and Zn(II) of the 2-(benzothiazol-2-yl)-N'-(2,5-dihydroxybenzylidene) acetohydrazide have been synthesized and characterized by elemental analysis, IR, UV-vis, $^1H$-NMR, mass and ESR spectra, magnetic susceptibility and molar conductivity measurements. The spectral data and magnetic measurements of the complexes indicate that, the geometries are either square planar or octahedral. The biological activity of the ligand and its complexes against fungi (Aspergillus nigar and Fusarium oxysporium) were investigated. The metal complexes exhibited higher activity than both the parent ligand and the corresponding metal ion.