• Title/Summary/Keyword: Structural Synthesis

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Enzymatic Synthesis of Flame Retardant Phenolic Polymers Catalyzed by Horseradish Peroxidase (Horseradish Peroxidase 효소촉매에 의한 난연성 페놀고분자의 합성)

  • Park, Han Sol;Park, Jung Hee;Lee, Hak Sung;Ryu, Keungarp
    • Korean Chemical Engineering Research
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    • v.51 no.1
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    • pp.111-115
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    • 2013
  • The optimum synthetic conditions of poly(p-phenylphenol) by horseradish peroxidase in dioxane:water (80:20 v/v) mixtures were studied. The stability against thermal degradation and structural properties of the synthesized phenolic resins were investigated by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC), respectively. The synthetic yield of poly(p-phenylphenol) increased upon the increase of the amount of enzyme up to 0.25 mg HRP/mL, then leveled off for further increase of the enzyme usage. When sodium acetate (100 mM, pH 4~6) and sodium phosphate (100 mM, pH 7~9) were used as the buffering salts for the aqueous component (20% v/v), the synthetic yield of the resin increased at higher pH of the aqueous buffer. But when the pHs of the aqueous buffer were 6 and 9, the synthetic yield strongly depended on the types of the buffering salts; if sodium phosphate was used instead of sodium acetate at pH 6, the yield decreased by about 15% and if sodium bicarbonate was used instead of sodium phosphate, the yield decreased by almost 20%. When the pH range of the aqueous buffer was from 4 to 7, the addition of a radical mediator, 2,2'-azinobis (3-ethylbenzothiazoline-6-sulfonate) (ABTS), up to 2 mM improved the synthetic yield of the resin by about 10%. TGA experiments revealed that the thermal stability of the resin synthesized in dioxane:water (100 mM sodium phosphate, pH 9) (80:20 v/v) was high having the char yield of 47% upon the heating at $800^{\circ}C$. DCS results showed that the structures of the polymers synthesized in acidic aqueous buffers were different from those of the polymers synthesized in the basic aqueous buffers. However, all the synthesized resins were found to have the property of the thermosetting resins.

Synthesis and Functional Properties of Plastein from the Enzymatic Hydrolysates of Filefish Protein 2. General Properties and IR Spectrum of Plasteins (말쥐치육 단백질의 효소적 가수분해물을 이용한 Plastein의 합성 및 그 물성 2. Plastein의 일반적 성상과 IR Spectrum)

  • KIM Se-Kwon;LEE Eung-Ho
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.20 no.5
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    • pp.431-440
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    • 1987
  • In order to develop a new type of food source for the effective utilization of fish protein, plastein reaction was applied to improve the functional properties of filefish protein. Plasteins were synthesized from a peptic filefish protein hydrolysate by papain, pepsin, $\alpha-chymotrypsin$ and protease(from Streptomyces griceus) under the optimum conditions of previous paper). Also, L-glutamic acid diethylester and L-leucine ethylester were incorporated into plastein during the plastein reaction by papain. And, General composition, yield, molecular weight, amino acid composition, color and IR spectrum of plasteins were measured. The protein, ash and lipid content of the plasteins were $72\~78\%,\;7.4\~11.8\%\;and\;0.3\~0.9\%$ respectively. The yield of plasteins were papain $55.0\%,\;pepsin\;47.6\%,\;\alpha-chymotrypsin\;38.3\%,\;protease\;23.6\%$, glutamic acid-incorporated plastein (Glu-Plastein) $35.0\%$, and leucine-incorporated plastein (Leu-plastein) $45.7\%$. The glutamic acid and leucine content in Glu-plastein and Leu-plastein were $38.7\%,\;41,7\%$, respectively, while the contents in the peptic filefish protein hydrolysate were $16.01\%\;and\;8.16\%$, respectively. The amino acid compositions were similar to that of the original filefish muscle protein. The major molecular weights of the peptic hydrolysate estimated by gel filteration were 2,000 and 310, and those of plasteihs were 21,000 and 4,900 for papain, 24,000 for pepsin, 18,500 for $\alpha-chymotrypsin$ 6,700 for protease, 24,000 for Glu-plastein and 17,000 for Leu-plastein. The structural changes in freeze-dried filefish meat, the FPC and hydrolysate were not observed on the IR spectrum. But plasteins showed amide I band in $1,600\~l,700cm^{-1}$ range and resulted in a strong band in $800\~850\;cm^{-1},\;700\~750\;cm^{-1}\;and\;650\~700\;cm^{-1}$. The amide I band of Glu-plastein was wider than those of other plasteins and had also a small band at $1,440\;cm^{-1}$.

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Effect of Di(2-ethyl hexyl)phthalate(DEHP) on the Onset of Puberty in Female Rat (암컷 흰쥐의 사춘기 개시에 미치는 di(2-ethyl hexyl)phthalate(DEHP)의 효과)

  • Lee, Kyeung-Yeup;Lee, Sung-Ho
    • Development and Reproduction
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    • v.10 no.2
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    • pp.147-154
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    • 2006
  • Phthalates such as di(2-ethyl hexyl)phthalate(DEHP) are industrial chemicals with wide-ranging human exposures because of their use in plastics and other common consumer products. Consequently, their adverse effects as endocrine disruptor in the reproductive physiology of both laboratory rodents and human have been studied extensively. The present study was undertaken to examine whether prepubertal exposure to DEHP affects on the onset of puberty and the associated reproductive parameters such as hormone receptor expressions in female rats. DEHP(100mg/kg/day) was administered daily from postnatal day 25(PND 25) through the day when the first vaginal opening(VO) was observed, and the animals were sacrificed on the next day. Gross anatomy and weight of reproductive tissues were compared to test the DEHP's effects on the cell proliferation. Furthermore, histological studies were performed to assess the structural alterations in the tissues. Specific radioimmunoassay was carried out to measure serum LH levels. To determine the transcriptional changes in progesterone receptor(PR), total RNAs were extracted and applied to the semi-quantitative reverse transcription polymerase chain reaction(RT-PCR). As a result, delayed VO was shown in the DEHP group(PND $37.3{\pm}0.7$) compared to the control group(PND $35.3{\pm}0.7$; p<0.05). DEHP treatment significantly decreased the wet weight of ovaries and uteri compared to the control group(p<0.05). Interestingly, elevation of serum LH levels was shown in the DEHP group(p<0.05). Graafian follicles and corpora lutea were observed only in the ovaries from the control animals. Numerous primary, secondary follicles and small atretic follicles were observed in the ovaries from DEHP-treated animals. Similarly, hypotrophy of luminal and glandular uterine epithelium was found in the DEHP-treated group. These effects were probably due to the inhibitory effects of DEHP on the synthesis and secretion of estrogen from granulosa cells. In the semiquantitative RT-PCR studies, the transcriptional activities of PR in both ovary(p<0.05) and uterus(p<0.01) from DEHP-treated animals were significantly lower than those from the control animals. The present studies demonstrated that the acute exposure to DEHP during the critical period of prepubertal stage could inactivate the reproductive system resulting delayed puberty in female rats.

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Synthesis and Structural Characterization of Benzene-sorbed Cd2+-Y(FAU) Zeolite (벤젠이 흡착된 Cd2+-Y(FAU) 제올라이트의 합성 및 구조연구)

  • Moon, Dae Jun;Suh, Jeong-Min;Park, Jong Sam;Choi, Sik Young;Lim, Woo Taik
    • Journal of the Mineralogical Society of Korea
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    • v.30 no.2
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    • pp.45-57
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    • 2017
  • Two single crystals of fully dehydrated $Cd^{2+}$-exchanged zeolites Y were prepared by the exchange of ${\mid}Na_{75}{\mid}[Si_{117}Al_{75}O_{384}]-FAU$ ($Na_{75}-Y$, Si/Al = 1.56) with aqueous $0.05M\;Cd(NO_3)_2$ (pH = 3.65) at 294 K, followed by vacuum dehydration at 723 K (crystal 1) and a second crystal, similarly prepared, was exposed to zeolitically dried benzene for 72 hours at 294 K and evacuated (crystal 2). Their structures were determined crystallographically using synchrotron X-rays and were refined to the final error indices using $F_o$>$4{\sigma}(F_o)$ of $R_1/wR_2=0.040/0.121$ and 0.052/0.168, respectively. In crystal $1({\mid}Cd_{36}H_3{\mid}[Si_{117}Al_{75}O_{384}]-FAU)$, $Cd^{2+}$ ions primarily occupy sites I and II, with additional $Cd^{2+}$ ions at sites I', II', and a second site II. In crystal $2({\mid}Cd_{35}(C_6H_6)_{24}H_5{\mid}[Si_{117}Al_{75}O_{384}]-FAU)$, $Cd^{2+}$ ions occupy five crystallographic sites. The 24 benzene molecules are found at two distinct positions within the supercages. The 17 benzene molecules are found on the 3-fold axes in the supercages where each interacts facially with one of site IIa $Cd^{2+}$ ions. The remaining 7 benzene molecules lie on the planes of the 12-rings where each is stabilized by multiple weak electrostatic and van der Waals interactions with framework oxygens.

Reduction of Mitochondrial Electron Transferase in Rat Bile duct Fibroblast by Clonorchis sinensis Infection (간흡충(Clonorchis sinensis)감염에 의한 흰쥐 담관 섬유모세포 미토콘드리아 전자전달효소의 감소)

  • Min, Byoung-Hoon;Hong, Soon-Hak;Lee, Haeng-Sook;Kim, Soo-Jin;Joo, Kyoung-Hwan
    • Applied Microscopy
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    • v.40 no.2
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    • pp.89-99
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    • 2010
  • Fibroblasts are the most common cells in connective tissue and are responsible for the synthesis of extracellular matrix components. The fibrosis associated with chronic inflammation and injury may contribute to cholangiocarcinoma pathogenesis, particularly through an increase in extracellular matrix components, which participate in the regulation of bile duct differentiation during development. Mitochondria produce ATP through oxidative metabolism to provide energy to the cell under physiological conditions. Also, mitochondrial dysfunction and oxidative stress have been implicated in cellular senescence and aging. Alternations in mitochondrial structure and function are early events of programmed cell death or apoptosis and mitochondria appear to be a central regulator of apoptosis in most somatic cell. Clonorchis sinensis, one of the most important parasite of the human bile duct in East Asia, arouses epithelial hyperplasia and ductal fibrosis. Isolated fibroblast from the bile ducts of rats infected by C. sinensis showed increase of cytoplasmic process. In addition, decrease of cellular proliferation was observed in fibroblasts which was isolated from normal rat bile duct and then cultured in media containing C. sinensis excretory-secretory product. However, the effects of C. sinensis infection on the mitochondrial enzyme distribution is not clearly reported yet. Therefore, we investigated the structural change of C. sinensis infected bile duct and mitochondrial enzyme distribution of the cultured fibroblast isolated from the C. sinensis infected rat bile duct. As a result, C. sinensis infected SD rat bile ducts showed the features of chronic clonorchiasis, such as ductal connective and epithelial tissue dilatation, or ductal fibrosis. In addition, fibroblast in ductal connective tissue was damaged by physical effect of fibrotic tissue and chemical stimulation. Immunohistochemically detected mitochondrial electron transferase (ATPase, COXII, Porin) was decreased in C. sinensis infected rat bile duct and cultured fibroblast from infected rat bile duct. It can be hypothesized that the reason why number of electron transferase decrease in fibroblast isolated from the rat bile duct infected with C. sinensis is because dysfunction of electron transport system is occurred mitochondrial dysfunction, increase of ROS (reactive oxygen species) and apoptosis after chemical damage on the cell caused by C. sinensis infection. Overall, C. sinensis infection induces fibrotic change of ductal connective tissue, mutation of cellular metabolism in fibroblast and mitochondrial dysfunction. Consequently, ductal fibrosis inhibits fibroblast proliferation and decreases mitochondrial electron transferase on fibroblast cytoplasm. It was assumed that the structure of bile duct could not normalized and ductal fibrosis was maintained for a long period of time according to fibroblast metamorphosis and death induced by mitochondrial dysfunction.

Synthesis and Structural Characterization of Optically Active Bis(L-Prolinato)(2,2'-bipyridine)Co(Ⅲ) and Bis(L-Prolinato)(1,10-phenanthroline)Co(Ⅲ) (광학활성 비스(L-Prolinato)(2,2'-bipyridine)코발트(Ⅲ)와 비스(L-Prolinato)(1,10-phenanthroline)코발트(Ⅲ)의 합성과 구조적인 특성)

  • Oh, Chang Eon;Kim, Bok Jo;Yoon, Doo Cheon;Doh, Myung Ki;Heo, Nam Ho
    • Journal of the Korean Chemical Society
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    • v.39 no.9
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    • pp.715-721
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    • 1995
  • Reaction between trans-$[Co(py)_4/Ci_2]^+(py=pyridine)$ and L-proline and diimine (=2,2'-bipyridine, 1,10-phenanthroline) gives two products, $[Co(L-pro)_2/(bipy)]^+$ and $[Co(L-pro)_2(phen)]^+$ complexes, respectively. On column chromatography, $[Co(L-pro)_2(bipy)]^+$ was obtained only as $Lambda$-trans(N) and $[Co(L-pro)_2(phen)]^+$ was obtained both as ${\Delta}$-trans(N) and $Lambda$-cis(O)cis(N) due to the stereoselectivity of L-prolinato which was stereospecific. Crystal data are as follows: $Lambda$-trans(N)-$[Co(L-pro)_2(bipy)]CIO_4{\cdot}2H_2O$ (1): monoclinic, space group $P2_1(#4)$, a=9.807(3), b=10.421(1), c=12.778(2) ${\AA}$, ${\beta}=109.90(2)^{\circ}$, V=1227.8(5) ${\AA}^3$, Z=2; 1571 data with I > 3.0${\sigma}$(I) were refined to R=0.060, $R_W = 0.067$; ${\Delta}$-trans(N)-$[Co(L-pro)_2(phen)]Cl{\cdot}_3H_2O$(2): monoclinic, space group $P2_1(#4)$, a=9.838(2), b=12.892(2), c=10.747(2)${\AA}$, ${\beta}=113.79(2)^{\circ}$, V=1247.2(4) ${\AA}^3$, Z=2; 2433 data with I > 3.0${\sigma}$(I) were refined to R=0.043, $R_W = 0.050$.

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PREPARATION OF AMORPHOUS CARBON NITRIDE FILMS AND DLC FILMS BY SHIELDED ARC ION PLATING AND THEIR TRIBOLOGICAL PROPERTIES

  • Takai, Osamu
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2000.11a
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    • pp.3-4
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    • 2000
  • Many researchers are interested in the synthesis and characterization of carbon nitride and diamond-like carbon (DLq because they show excellent mechanical properties such as low friction and high wear resistance and excellent electrical properties such as controllable electical resistivity and good field electron emission. We have deposited amorphous carbon nitride (a-C:N) thin films and DLC thin films by shielded arc ion plating (SAIP) and evaluated the structural and tribological properties. The application of appropriate negative bias on substrates is effective to increase the film hardness and wear resistance. This paper reports on the deposition and tribological OLC films in relation to the substrate bias voltage (Vs). films are compared with those of the OLC films. A high purity sintered graphite target was mounted on a cathode as a carbon source. Nitrogen or argon was introduced into a deposition chamber through each mass flow controller. After the initiation of an arc plasma at 60 A and 1 Pa, the target surface was heated and evaporated by the plasma. Carbon atoms and clusters evaporated from the target were ionized partially and reacted with activated nitrogen species, and a carbon nitride film was deposited onto a Si (100) substrate when we used nitrogen as a reactant gas. The surface of the growing film also reacted with activated nitrogen species. Carbon macropartic1es (0.1 -100 maicro-m) evaporated from the target at the same time were not ionized and did not react fully with nitrogen species. These macroparticles interfered with the formation of the carbon nitride film. Therefore we set a shielding plate made of stainless steel between the target and the substrate to trap the macropartic1es. This shielding method is very effective to prepare smooth a-CN films. We, therefore, call this method "shielded arc ion plating (SAIP)". For the deposition of DLC films we used argon instead of nitrogen. Films of about 150 nm in thickness were deposited onto Si substrates. Their structures, chemical compositions and chemical bonding states were analyzed by using X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy and infrared spectroscopy. Hardness of the films was measured with a nanointender interfaced with an atomic force microscope (AFM). A Berkovich-type diamond tip whose radius was less than 100 nm was used for the measurement. A force-displacement curve of each film was measured at a peak load force of 250 maicro-N. Load, hold and unload times for each indentation were 2.5, 0 and 2.5 s, respectively. Hardness of each film was determined from five force-displacement curves. Wear resistance of the films was analyzed as follows. First, each film surface was scanned with the diamond tip at a constant load force of 20 maicro-N. The tip scanning was repeated 30 times in a 1 urn-square region with 512 lines at a scanning rate of 2 um/ s. After this tip-scanning, the film surface was observed in the AFM mode at a constant force of 5 maicro-N with the same Berkovich-type tip. The hardness of a-CN films was less dependent on Vs. The hardness of the film deposited at Vs=O V in a nitrogen plasma was about 10 GPa and almost similar to that of Si. It slightly increased to 12 - 15 GPa when a bias voltage of -100 - -500 V was applied to the substrate with showing its maximum at Vs=-300 V. The film deposited at Vs=O V was least wear resistant which was consistent with its lowest hardness. The biased films became more wear resistant. Particularly the film deposited at Vs=-300 V showed remarkable wear resistance. Its wear depth was too shallow to be measured with AFM. On the other hand, the DLC film, deposited at Vs=-l00 V in an argon plasma, whose hardness was 35 GPa was obviously worn under the same wear test conditions. The a-C:N films show higher wear resistance than DLC films and are useful for wear resistant coatings on various mechanical and electronic parts.nic parts.

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Study on Synthesis and Characterization of Magnetic ZnFe2O4@SnO2@TiO2 Core-shell Nanoparticles (자성을 가진 ZnFe2O4@SnO2@TiO2 Core-Shell Nanoparticles의 합성과 특성에 관한 연구)

  • Yoo, Jeong-yeol;Park, Seon-A;Jung, Woon-Ho;Park, Seong-Min;Tae, Gun-Sik;Kim, Jong-Gyu
    • Applied Chemistry for Engineering
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    • v.29 no.6
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    • pp.710-715
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    • 2018
  • In this study, $ZnFe_2O_4@SnO_2@TiO_2$ core-shell nanoparticles (NPs), a photocatalytic material with magnetic properties, were synthesized through a three-step process. Structural properties were investigated using X-ray diffraction (XRD) analysis. It was confirmed that $ZnFe_2O_4$ of the spinel, $SnO_2$ of the tetragonal and $TiO_2$ of the anatase structure were synthesized. The magnetic properties of synthesized materials were studied by a vibrating sample magnetometer (VSM). The saturation magnetization value of $ZnFe_2O_4$, a core material, was confirmed at 33.084 emu/g. As a result of the formation of $SnO_2$ and $TiO_2$ layers, the magnetism due to the increase in thickness was reduced by 33% and 40%, respectively, but sufficient magnetic properties were reserved. The photocatalytic efficiency of synthesized materials was measured using methylene blue (MB). The efficiency of the core material was about 4.2%, and as a result of the formation of $SnO_2$ and $TiO_2$ shell, it increased to 73% and 96%, respectively while maintaining a high photocatalytic efficiency. In addition, the antibacterial activity was validated via the inhibition zone by using E. Coli and S. Aureus. The formation of shells resulted in a wider inhibition zone, which is in good agreement with photocatalytic efficiency measurements.

Characterization of Synthesized Carbonate and Sulfate Green Rusts: Formation Mechanisms and Physicochemical Properties (합성된 탄산염 및 황산염 그린 러스트의 형성 메커니즘과 이화학적 특성 규명)

  • Lee, Seon Yong;Choi, Su-Yeon;Chang, Bongsu;Lee, Young Jae
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.2
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    • pp.111-123
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    • 2022
  • Carbonate green rust (CGR) and sulfate green rust (SGR) commonly occur in nature. In this study, CGR and SGR were synthesized through co-precipitation, and their formation mechanisms and physicochemical properties were investigated. X-ray diffraction (XRD) and Rietveld refinement showed both CGR and SGR with layered double hydroxide structure were successfully synthesized without any secondary phases under each synthetic condition. Refined structural parameters (unit cell) for two green rusts were a (=b) = 3.17 Å and c = 22.52 Å for CGR and a (=b) = 5.50 Å and c = 10.97 Å for SGR with the crystallite size 57.8 nm in diameter from (003) reflection and 40.1 nm from (001) reflections, respectively. Scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) results showed that both CGR and SGR had typical hexagonal plate-like crystal morphologies but their chemical composition is different in the content of C and S. In addition, Fourier transform infrared (FT-IR) spectroscopy analysis revealed that carbonate (CO32-) and sulfate (SO42-) molecules were occupied as interlayer anions of CGR and SGR, respectively. These SEM/EDS and FT-IR results were in good agreement with XRD results. Changes in the solution chemistry (i.e., pH, Eh and residual iron concentrations (Fe(II):Fe(III)) of the mixed solution) were observed as a function of the injection time of hydroxyl ion (OH-) into the iron solution. Three different stages were observed in the formation of both CGR and SGR; precursor, intermediator, and green rust in the formation of both CGR and SGR. This study provides co-precipitation methods for CGR and SGR in a way of the stable synthesis. In addition, our findings for the formation mechanisms of the two green rusts and their physicochemical properties will provide crucial information with researches and industrials in utilizing green rust.

Synthesis and Structural Study of Extraframework ZrI6Tl119+ Cationic Cluster in Zeolite A (제올라이트 A 동공 내 비골격 ZrI6Tl119+ 양이온 클러스터의 합성과 구조 연구)

  • Hyeon Seung, Lim;Jong Sam, Park;Cheol Woong, Kim;Woo Taik, Lim
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.4
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    • pp.447-455
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    • 2022
  • Fully dehydrated Tl12-LTA (|Tl12|[Si12Al12O48]-LTA,Tl12-A) was treated with 6.0×103 Pa of ZrI4 (g) at 623 K for 72 hr under anhydrous conditions. The crystal structure of product, |Zr0.25I1.5Tl12|[Si12Al12O48]-LTA, was determined by single-crystal crystallography using synchrotron X-radiation in the cubic space group Pm3m (a = 12.337(2) Å). It was refined using all data to the final error index (for the 712 unique reflections for which Fo> 4σ(Fo) R1/wR2= 0.055/0.189. In this structure, octahedral ZrI62- ions center about 25% of the large cavities (Zr-I = 2.91(4) Å). Each coordinates to eight Tl+ ions and they are further bridged by Tl+ ions in the planes of 8-rings to form a cubic three-dimensional ZrI6Tl119+ cationic cluster. About 1.5 Tl+ ions per unit cell moved to deeper side of sodalite cavity after reaction with ZrI4(g). The remaining Tl+ ions occupy well-established cation positions near 6- and 8-rings.