• Title/Summary/Keyword: crystal form

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Effect of Salt on the Formation of $\alpha$-Calcium Sulfate Hemihydrate from by-Product Gypsum of Phosphoric Acid Process in Aqueous Salt Solution at Atmospheric Pressure (상압수용액중에서 인산석고로부터 $\alpha$형 반수석고의 생성에 미치는 염류의 영향)

  • 이구종;최상흘
    • Journal of the Korean Ceramic Society
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    • v.25 no.1
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    • pp.66-72
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    • 1988
  • The effect of salts on the formation of ${\alpha}$-hemihydrated gypsum at boiling temperature under atmospheric pressure was studied by the solubility measurement method, and the formation of ${\alpha}$-hemihydrated gypsum from by-product gypsum of phosphoric acid process in the salts solution were investigated. The order of catalytic effect of salt on the formation of ${\alpha}$-hemihydrated gypsum are as follows: NH4Cl>NaCl>NaNO3. In the salts solution of sodium nitrate, sodium chloride, and ammonium chloride, prismatic ${\alpha}$-hemihydrated gypsum was obtained and the crystal form was converted to needle form in complex solution with sulfuric acid. The P2O5 content in gypsum was largely decreased in this atmosphoric solution process.

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Synthesis and Crystal Structure of Lead Iodide in the Sodalite Cavities of Zeolite A (LTA)

  • Kim, Seok-Han;Lim, Woo-Taik;Kim, Ghyung-Hwa;Lee, Heung-Soo;Heo, Nam-Ho
    • Bulletin of the Korean Chemical Society
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    • v.27 no.5
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    • pp.679-686
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    • 2006
  • The positions of $PbI _2$ molecule synthesized into the molecular-dimensioned cavities of $\mid K_6 (Pb _4I_2)(PbI_2) _{0.67}-(H_2O)_2\mid [Si _{12}Al _{12}O _{48}]$-LTA have been determined. A single crystal of $\mid Pb _6\mid [Si _{12}Al _{12}O _{48}]$-LTA, prepared by the dynamic ion-exchange of $\mid Na _{12}\mid [Si _{12}Al _{12}O _{48}]$-LTA with aqueous 0.05 M $Pb _(NO _3)_2$ and washed with deionized water, was placed in a stream of flowing aqueous 0.05 M KI at 294 K for three days. The resulting crystal structure of the product $( \mid K_6 (Pb _4I_2)(PbI_2) _{0.67}(H_2O)_2\mid [Si _{12}Al _{12}O _{48}]$-LTA, a = 12.353(1) $\AA$) was determined at 294 K by single-crystal X-ray diffraction in the space group Pm3 m. It was refined with all measured reflections to the final error index $R_1$ = 0.062 for 623 reflections which $F_o$ > 4$\sigma$($F_o$). 4.67 $Pb ^{2+}$ and six $K^+$ ions per unit cell are found at three crystallographically distinct positions: 3.67 $Pb ^{2+}$ and three $K^+$ ions on the 3-fold axes opposite six-rings in the large cavity, three $K^+$ ions off the plane of the eight-rings, and the remaining one $Pb ^{2+}$ ion lies opposite four-ring in the large cavity. 0.67 $Pb ^{2+}$ ions and 1.34 $I^-$ ions per unit cell are found in the sodalite units, indicating the formation of a $PbI _2$ molecule in 67% of the sodalite units. Each $PbI _2$ (Pb-I = 3.392(7) $\AA$) is held in place by the coordination of its one $Pb ^{2+}$ ion to the zeolite framework (a $Pb ^{2+}$ cation is 0.74 $\AA$ from a six-ring oxygens) and by the coordination of its two $I^-$ ions to $K^+$ ions through six-rings (I-K = 3.63(4) $\AA$). Two additional $I^-$ ions per unit cell are found opposite a four-ring in the large cavity and form $Pb _2K_2I^{5+}$ and $Pb _2K_2I^{3+}$ moieties, respectively, and two water molecules per unit cell are also found on the 3-fold axes in the large cavity.

Drowning-out Crystallization of Calcium Lactate for Crystal Size Control (결정입자 제어를 위한 젖산칼슘 용석결정화 기술)

  • Kim, Jong-Min;Chang, Sang Mok;Kim, In-Ho;Koo, Yoon-Mo;Hong, Haehyun;Kim, Woo-Sik
    • Korean Chemical Engineering Research
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    • v.47 no.6
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    • pp.740-746
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    • 2009
  • In the present study, the drowning-out crystallization of L(+)-calcium lactate was investigated in order to develop the crystallization separation process. The crystallization of the calcium lactate was induced by injecting the alcoholic anti-solvent into the aqueous solution of calcium lactate and the control of the calcium lactate crystal size during the crystallization was primarily investigated under the consideration of the anti-solvent species, anti-solvent composition and agitation speed as the key operating factors. Alcohols of methanol, ethanol, n-propanol and i-propanol were used as the anti-solvent for the drowning-out crystallization. Prior to the crystallization experiment, the solubility of calcium lactate in the water-alcohol mixture was measured along with the variation of the alcohol species and composition, which was necessary to estimate the supersaturation level of the crystallization. By the drowning-out crystallization, the calcium lactate crystals of the fabric shape were obtained. Using the ethanol as the antisolvent, the fabric crystals close to the needle shape were produced. However, the hairy crystals were obtained by using the propanol as the anti-solvent. Due to such morphological features, the crystals was highly apt to form the aggregates. The aggregation of the crystals was intensified as increasing the alcohol fraction in the water-alcohol mixture. Meanwhile, the agitation caused the breakage of crystals, resulting in the decrease of the crystal size. Therefore, the crystal size in the crystallization was predominantly determined by the competition between the crystal aggregation and breakage.

Understanding the Mechanism of Indomethacin-Saccharin Co-crystal Formation Using In-line Monitoring System based on PVM and FBRM (PVM 및 FBRM 기반 인라인 모니터링을 통한 indomethacin-saccharin 공결정의 생성 메커니즘이해)

  • Kim, Paul;Cho, Min-Yong;Choi, Guang J.
    • Korean Chemical Engineering Research
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    • v.55 no.2
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    • pp.180-189
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    • 2017
  • Pharmaceutical co-crystals primarily to improve the solubility as well as stability of insoluble drug are to be investigated more intensively for IMDs as US FDA has reclassified co-crystal as a special case of solvates in August this year. In this study, we proposed a mechanism of indomethacin-saccharin co-crystal formation and the creation of transient indomethacin meta-stable form using in-line monitoring tools with the addition rate of anti-solvent as a critical process parameter. Among various instruments, we combined PVM (particle vision measurement) and FBRM (focused beam reflectance measurement) for the in-line monitoring of anti-solvent co-crystallization process. The off-line characterization of resulting powders was carried out employing the PXRD (powder x-ray diffraction) and DSC (differential scanning calorimeter). It was observed that the pathway to the final IMC-SAC co-crystal was significantly dependent upon the anti-solvent addition rate. The process conditions to obtain high quality co-crystal powder effectively were established. Consequently, we concluded that in-line monitoring combing the PVM and FBRM should be useful for the in-line monitoring of pharmaceutical co-crystallization processes.

Structure Development and Dynamic Properties in High-speed Spinning of High Molecular Weight PEN/PET Copolyester Fibers

  • Im, Seung-Soon;Kim, Sung-Joong
    • Fibers and Polymers
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    • v.3 no.1
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    • pp.18-23
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    • 2002
  • The structure development and dynamic properties of fibers produced by high-speed spinning of P(EN-ET) random copolymers were investigated. The as-spun fibers were found to remain amorphous up to the spinning speed of 1500 m/min, and subsequent increases in speed resulted in the crystalline domains containing primarily $\alpha$ crystalline modification of PEN. The f modification was not found up to spinning speeds of 4500 m/min. On the other hand, annealing of constrained fibers spun at the 2100 m/min at 180,200, and 240^{\circ}C$ exhibited $\beta$-form crystalline structure, while the annealed fibers spun in 600-1500 m/min range exhibited dominantly $\alpha$-form. However $\beta$-form crystals disappeared above the spinning speed of 3000 m/min. With increasing spinning speeds from 600 to 4500 m/min, the storage modulus of as-spun fibers increased continuously and reached a value of about 10.4 spa at room temperature. The tan $\delta$curves showed the $\alpha$-relaxation peak at about 155-165^{\circ}C$, which is considered to correspond to the glass transition. The $\alpha$-relaxation peaks became smaller and broader, and shift to higher temperatures as the spinning speed increases, meaning that molecular mobility in the amorphous region is restricted by increased crystalline domain.

Crystal Structure of DsbA from Corynebacterium diphtheriae and Its Functional Implications for CueP in Gram-Positive Bacteria

  • Um, Si-Hyeon;Kim, Jin-Sik;Song, Saemee;Kim, Nam Ah;Jeong, Seong Hoon;Ha, Nam-Chul
    • Molecules and Cells
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    • v.38 no.8
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    • pp.715-722
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    • 2015
  • In Gram-negative bacteria in the periplasmic space, the dimeric thioredoxin-fold protein DsbC isomerizes and reduces incorrect disulfide bonds of unfolded proteins, while the monomeric thioredoxin-fold protein DsbA introduces disulfide bonds in folding proteins. In the Gram-negative bacteria Salmonella enterica serovar Typhimurium, the reduced form of CueP scavenges the production of hydroxyl radicals in the copper-mediated Fenton reaction, and DsbC is responsible for keeping CueP in the reduced, active form. Some DsbA proteins fulfill the functions of DsbCs, which are not present in Gram-positive bacteria. In this study, we identified a DsbA homologous protein (CdDsbA) in the Corynebacterium diphtheriae genome and determined its crystal structure in the reduced condition at $1.5{\AA}$ resolution. CdDsbA consists of a monomeric thioredoxin-like fold with an inserted helical domain and unique N-terminal extended region. We confirmed that CdDsbA has disulfide bond somerase/reductase activity, and we present evidence that the N-terminal extended region is not required for this activity and folding of the core DsbA-like domain. Furthermore, we found that CdDsbA could reduce CueP from C. diphtheriae.

Liquid-Phase Sintered SiC Ceramics with Oxynitride Additives

  • Rixecker, G.;Biswas, K.;Wiedmann, I.;Sldinger, F.
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 2000.06a
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    • pp.1-33
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    • 2000
  • Silicon carbide ceramics with sintering additives from the system AlN-Y$_2$O$_3$ can be gas-pressure sintered to theoretical density. While commonly a combination of sesquioxides is used such as Al$_2$O$_3$-Y$_2$O$_3$, the oxynitrid additives offer the advantage that only a nitrogen atmosphere is require instead of a powder. By starting form a mixture of ${\beta}$-SiC and ${\alpha}$-SiC, and by performing dedicated heat treatments after densification, anisotropic grain growth is obtained which leads to a platelet microstructure showing enhance fracture toughness. In the present work, recent improvement of the mechanical behaviour of these materials at ambient and high temperatures is reported. By means of a surface oxidation treatment in air it is possible to obtain four-point bending strengths in excess of 1 GPa, and the strength retention at high temperatures is significantly improved.

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Structural Diversity of Five New Lanthanide Coordination Polymers Tuned by Different Salt Anions

  • Tao, Yinhua;Lou, Yongbing;Li, Yang;Chen, Jinxi
    • Bulletin of the Korean Chemical Society
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    • v.35 no.5
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    • pp.1417-1421
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    • 2014
  • Five new lanthanide coordination polymers, $[Ln_2(1,4-NDC)_2(1,4-HNDC)_2(phen)_2]_n$ (Ln = Er (1), Yb (2)), and $[Ln_2(1,4-NDC)_3(phen)_2(H_2O)_2]_n$ (Ln = Nd (3), Gd (4), Er (5)) ($1,4-H_2NDC$ = 1,4-naphthalenedicarboxylic acid, phen = 1,10-phenanthroline), have been successfully prepared via the reaction of corresponding trivalent lanthanide salt, $1,4-H_2NDC$ and phen in the presence of NaOH and pyridine under hydrothermal condition. Pyridine plays a key role in the synthesis of these lanthanide coordination polymers. Single-crystal X-ray diffraction analyses indicate that compounds 1-5 all form a 2-D network while different salt anions result in the diversity of crystal structures. These lanthanide coordination polymers showed a considerable thermal stability in TGA analyses.

Regulation Mechanism of Redox Reaction in Rubredoxin

  • Tongpil Min;Marly K. Eidsness;Toshiko Ichiye;Kang, Chul-Hee
    • Journal of Microbiology
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    • v.39 no.3
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    • pp.149-153
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    • 2001
  • The electron transfer reaction is one of the most essential processes of life. Not only does it provide the means of transforming solar and chemical energy into a utilizable form for all living organisms, it also extends into a range of metabolic processes that support the life of a cell. Thus, it is of great interest to understand the physical basis of the rates and reduction potentials of these reactions. To identify the major determinants of reduction potentials in redox proteins, we have chosen the simplest electron transfer protein, rubredoxin, a small (52-54 residue) iron-sulfur protein family, widely distributed in bacteria and archaea. Rubredoxins can be grouped into two classes based on the correlation of their reduction potentials with the identity of residue 44; those with Ala44 (ex: Pyrococcus furiosus) have reduction potentials that are ∼50 mV higher than those with Va144 (ex: Clostridium pasteurianum). Based on the crystal structures of rubredoxins from C. pasteurianum and P. furiosus, we propose the identity of residue 44 alone determines the reduction potential by the orientation of the electric dipole moment of the peptide bond between 43 and 44. Based on 1.5 $\AA$ resolution crystal structures and molecular dynamics simulations of oxidized and reduced rubredoxins from C. pasteurianum, the structural rearrangements upon reduction suggest specific mechanisms by which electron transfer reactions of rubredoxin should be facilitated.

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New Mechanism of Thin Film Growth by Charged Clusters

  • Hwang, Nong-Moon;Kim, Doh-Yeon
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1999.06a
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    • pp.115-127
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    • 1999
  • The charged clusters or particles, which contain hundreds to thousands of atoms or even more, are suggested to form in the gas phase in the thin film processes such as CVD, thermal evaporation, laser ablation, and flame deposition. All of these processes are also used in the gas phase synthesis of the nanoparticles. Ion-induced or photo-induced nucleation is the main mechanism for the formation of these nanoclusters or nanoparticles inthe gas phase. Charged clusters can make a dense film because of its self-organizing characteristics while neutral ones make a porous skeletal structure because of its Brownian coagulation. The charged cluster model can successfully explain the unusual phenomenon of simultaneous deposition and etching taking place in diamond and silicon CVD processes. It also provides a new interpretation on the selective deposition on a conducting material in the CVDd process. The epitaxial sticking of the charged clusters on the growing surface is gettign difficult as the cluster size increases, resulting in the nanostructure such as cauliflowr or granular structures.

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