• Bulletin of the Korean Chemical Society
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• v.14 no.2
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• pp.258-262
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• 1993

Two single crystals of fully dehydrated $Rb^+$ -exchanged zeolite A have been prepared by the reduction of all $Ca^{2+}$ ions in dehydrated $Ca_6$-A by rubidium vapor. Their structures were determined by single crystal X-ray diffraction methods in the cubic space group Pm3m (a=12.160(2) $^{\AA}$ and 12.166(2) $^{\AA}$) at 22(1)$^{\circ}$C. In these structures, 12.4(2) to 13.3(2) Rb species are found per unit cell, more than 12 Rb$^+$ ions needed to balance the anionic charge of the zeolite framework, indicating that the sorption $Rb^0$ has occurred. In each structure, three $Rb^+$ ions per unit cell are located at the centers of the 8-rings. Six to eight $Rb^+$ ions are found opposite the 6-rings on threefold axes, and three $Rb^+$ ions are found in a sodalite unit. About 0.5 $Rb^+$ ion lies opposite a 4-ring. The structural analysis indicates the presence of a triangular rubidium cluster in the sodalite cavities. The triangular rubidium clusters may be stabilized by the coordination to two and/or three rubidium ions in the large cavity. Therefore, this cluster may be viewed as $(Rb_5)^{4+}$ and/or $(Rb_6)^{4+}$.

• Korean Journal of Materials Research
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• v.32 no.1
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• pp.36-43
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• 2022

Breakthrough analysis has widely been explored for the dynamic separation of gaseous mixtures in porous materials. In general, breakthrough experiments measure the components of a flowing gas when a gaseous mixture is injected into a column filled with an adsorbent material. In this paper, we report on the design and fabrication of a breakthrough curve measurement device to study the dynamic adsorptive separation of hydrogen isotopologues in porous materials. Using the designed system, an experiment was conducted involving a 1:1 mixture of hydrogen and deuterium passed through a column filled with zeolite 13X (1 g). At room temperature, both hydrogen and deuterium were adsorbed in negligible amounts; however, at a temperature of 77 K, deuterium was preferentially adsorbed over hydrogen. The selectivity was different from that in the existing literature due to the different sample shapes, measurement methods, and column structures, but was at a similar level to that of cryogenic distillation (1.5).

• Journal of the Mineralogical Society of Korea
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• v.4 no.2
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• pp.99-107
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• 1991

Three fully dehydrated fully Rb+-exchanged zeolite A single crystals have been prepared by the reduction of all Na+ ions in dehydrated Na12-A by rubidium vapor at various experimental conditions (220 $\leq$ T $\leq$ 33$0^{\circ}C$, 2 $\leq$ t $\leq$24 hours, and 0.1 $\leq$ PRb $\leq$ 1.1 Torr). Their structures were determined by single-crystal X-ray diffraction methods in the space group {{{{ RHO }}m3m (a=12.245(3) A) at 22(1)$^{\circ}C$. In these structures 12.6(2) to 13.5(2) Rb species are found per unit cell, more than the 12 Rb+ ions needed to balance the anionic charge of the zeolite framework, indication that the sorption of Rb0 has occurred. In each structure, three Rb+ ions per unit cell are located at the centers of 8-rings. Beyond that, the fractional occupancies observed are simply explained by two unit cell arrangments. In one, two Rb+ ions are in the sodalite unit near opposite 6-rings, six are in the large cavity near 6-ring, and one is in the large cavity near a 4-ring. In the other, three Rb species in the sodalite cavity (forming a triangle 3.7 A on an edge) each bond (3.4 A) through a 6-ring to an Rb species in the large cavity to give an (Rb6)4+ cluster of symmetry 3m (C3V). Five additional Rb+ ions fill the remaining large-cavity 6-ring sites.

• Bulletin of the Korean Chemical Society
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• v.30 no.8
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• pp.1703-1710
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• 2009

The single-crystal structure of |$Ca_{35.5}$|[$Si_{121}Al_{71}O_{384}$]-FAU, $Ca_{35.5}Si_{121}Al_{71}O_{384}$ per unit cell, a = 24.9020(10) $\AA$, dehydrated at 673 K and 2 ${\times}\;10^{-6}$Torr, has been determined by single-crystal X-ray diffraction techniques in the cubic space group Fd$\overline{3}$m at 294 K. The large single crystals of zeolite Y (Si/Al = 1.70) were synthesized up to diameters of ${\mu}m\;and\;Ca^{2+}$-exchanged zeolite Y were prepared by ion exchange in a batch method of 0.05 M aqueous Ca($NO_3)_2$ for 4 hrs at 294 K. The structure was refined using all intensities to the final error indices (using only the 971 reflections for which $F_o\;>\;4{\sigma}(F_o))\;R_1$ = 0.038 (based on F) and $R_2$ = 0.172 (based on $F^2$). About 35.5 $Ca^{2+}$ ions per unit cell are found at an unusually large number of crystallographically distinct positions, four. Nearly filling site I (at the centers of the double 6-rings), 14.5 octahedrally coordinated $Ca^{2+}$ ions (Ca-O = 2.4194(24) $\AA$ and O-Ca-O = 87.00(8) and 93.00($8^o$) are found per unit cell. One $Ca^{2+}$ ion per unit cell is located at site II’ in the sodalite cavity and extends 0.50 $\AA$ into the sodalite cavity from its 3-oxygen plane (Ca-O = 2.324(13) $\AA$ and O-Ca-O = 115.5(10)o). The remaining twenty $Ca^{2+}$ ions are found at two nonequivalent sites II (in the supercages) with occupancies of 10 and 10 ions, respectively. Each of these $Ca^{2+}$ ions coordinates to three framework oxygens, either at 2.283(3) or 2.333(5) $\AA$, respectively, and extends either 0.24 or 0.54 $\AA$, respectively, into the supercage from the three oxygens to which it is bound. In this crystal, site I is the most populated; sites II’ and II are only sparsely occupied.$Ca^{2+}$+ appears to fit the octahedral site I best. No cations are found at sites III or III’, which are clearly less favorable for $Ca^{2+}$ ions in dehydrated zeolite Y.

• Journal of the Korean Chemical Society
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• v.13 no.1
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• pp.49-55
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• 1969

X-ray Fluorescence Spectrographic method has been applied for the rapid determination of main components, such as $SiO_2$, $Al_2O_3$, $Fe_2O_3$, CaO, MgO and $K_2O$ in Silicate Minerals. In this method, Boric Acid was used as a binder after fusion with Lithium Tetraborate in the briquet-making process. The Lithium Flubride, Ammonium di-Hydrogen Phosphate and Ethylene Diamine d-Tartrate crystals were used with Scintillation counter and Gas Flow counter as the detectors. Several influences on this method were discussed, including the particle size of samples and reducing of the matrix effects by dilution with Boric Acid and addition of Lanthanum Oxide with the diluent. In order to test the reproducibility of this method described above, the determination of the same kind of samples were carried out repeatedly, and the results obtained were presented in the table. Calibration curves for each element were presented, and the application of the method was tested with International Rock Standard T-Ⅰ. All the results obtained by X-Ray Fluorescence Spectrographic method were compared with the results by conventional chemical method.

• Bulletin of the Korean Chemical Society
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• v.13 no.1
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• pp.70-74
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• 1992

Two crystal structures of ethylene (a= 12.272(2) ${\AA}$) and acetylene (a = 12.245(2) ${\AA}$) sorption complexes of dehydrated fully $Ca^{2+}$-exchanged zeolite A have been determined by single crystal X-ray diffraction techniques in the cubic space group, Pm3m at $21(1)^{\circ}C$. Their complexes were prepared by dehydration at $360^{\circ}C$ and $2{\times}10^{-6}$ Torr for 2 days, followed by exposure to 200 Torr of ethylene gas and 120 Torr of acetylene gas both at $24^{\circ}C$, respectively. The structures were refined to final R (weighted) indices of 0.062 with 209 reflections and 0.098 with 171 reflections, respectively, for which I > 3${\sigma}$(I). The structures indicate that all six $Ca^{2+}$ ions in the unit cell are associated with 6-oxygen ring of the aluminosilicate framework. Four of these extend somewhat into the large cavity where each is coordinated to three framework oxide ions and an ethylene molecule and/or an acetylene molecule. The carbon to carbon distance in ethylene sorption structure is 1.48(7) ${\AA}$ and that in acetylene sorption structure 1.25(8) ${\AA}$. The distances between $Ca^{2+}$ ion and carbon atom are 2.87(5) ${\AA}$ in ethylene sorption structure and 2.95(7) ${\AA}$ in acetylene sorption structure. These bonds are relatively weak and probably formed by the electrostatic attractions between the bivalent $Ca^{2+}$ ions and the polarizable ${\pi}$-electron density of the ethylene and/or acetylene molecule.

• Proceedings of the Korean Nuclear Society Conference
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• 1996.05c
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• pp.409-414
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• 1996

Radionuclides such as Cs and Sr were removed from dilute aqueous solutions by means of inorganic adsorbents, 13X and chabazite. The physical adsorption obeyed the DA equation and non-equilibrium dynamic adsorption model, which describes surface diffusion mechanism with the DA equation, simulated the adsorption behavior of cesium and strontium on zeolite in fixed bed adsorbers. The dynamic model simulated the adsorption behavior of cesium and strontium.

• Proceedings of the KAIS Fall Conference
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• 2012.05a
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• pp.33-35
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• 2012

본 연구에서는 전이금속 Cu, Mn이 함침된 제올라이트를 사용하여 일산화탄소의 흡착능을 연구하였다. 금속 복합 산화물촉매 제조는 Cu, Mn을 서로 다른 비율로 물리 혼합하여 지지체에 담지하였다. 제올라이트 분자체는 상용 13X를 사용하였다. 함침방법은 과잉용액 함침법을 사용하였고, 건조 후 소성 하여 산화물 형태로 담지하였다. 합성된 개질 흡착제의 표면특성 분석은 $N_2$흡착 및 탈착곡선을 통한 질소흡착 특성 분석으로 기공크기, 기공분포, 비표면적을 구하였으며, FT-IR, X-선 회절분석, 전자주사현미경, $NH_3$-TPD/TPR 으로 특성을 분석하였다. 흡착 실험은 고정층 반응기에서 수행하였으며, 내경 4 mm 석영관에 흡착제를 충진하고 흡착파과곡선을 Gas Chromatograph로 측정하여 Cu-Mn 제올라이트 촉매의 일산화탄소 흡착 성능을 연구하였다. Cu-Mn 함량 비율과 흡착조업조건에 따른 흡착능을 측정하여 최적 흡착조건을 구하였다.

• Journal of the Korean Chemical Society
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• v.39 no.1
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• pp.7-13
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• 1995

The crystal sructures of $X(Ca_{46}Al_{92}Si_{100}O_{384})$ and $Ca_{32}K_{28}-X(Ca_{32}K_{28}Al_{92}Si_{100}O_{384})$ dehydrated at $360^{\circ}C$ and $2{\times}10^{-6}$ Torr have been determined by single-crystal X-ray diffraction techniques in the cubic space group Fd3 at $21(1)^{\circ}C.$ Their structures were refined to the final error indices, R_1=0.096,\;and\;R_2=0.068$ with 166 reflections, and R_1=0.078\;and\;R_2=0.056$ with 130 reflections, respectively, for which I > $3\sigma(I).$ In dehydrated $Ca_{48}-X,\;Ca^{2+}$ ions are located at two different sites opf high occupancies. Sixteen $Ca^{2+}$ ions are located at site I, the centers of the double six rings $(Ca(1)-O(3)=2.51(2)\AA$ and thirty $Ca^{2+}$ ions are located at site II, the six-membered ring faces of sodalite units in the supercage. Latter $Ca^{2+}$ ions are recessed $0.44\AA$ into the supercage from the three O(2) oxygen plane (Ca(2)-O(2)= $2.24(2)\AA$ and $O(2)-Ca(2)-O(2)=119(l)^{\circ}).$ In the structure of $Ca_{32}K_{28}-X$, all $Ca^{2+}$ ions and $K^+$ ions are located at the four different crystallographic sites: 16 $Ca^{2+}$ ions are located in the centers of the double six rings, another sixteen $Ca^{2+}$ ions and sixteen $K^+$ ions are located at the site II in the supercage. These $Ca^{2+}$ ions adn $K^+$ ions are recessed $0.56\AA$ and $1.54\AA$, respectively, into the supercage from their three O(2) oxygen planes $(Ca(2)-O(2)=2.29(2)\AA$, $O(2)-Ca(2)-O(2)=119(1)^{\circ}$, $K(1)-O(2)=2.59(2)\AA$, and $O(2)-K(1)-O(2)=99.2(8)^{\circ}).$ Twelve $K^+$ ions lie at the site III, twofold axis of edge of the four-membered ring ladders inside the supercage $(K(2)-O(4)=3.11(6)\AA$ and $O(1)-K(2)-O(1)=128(2)^{\circ}).$

• Membrane Journal
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• v.23 no.6
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• pp.409-417
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• 2013

Adsorptive permeation hollow fiber membrane (APM) has been developed for effectively separating $CO_2$ from gas mixture. Inside the APM, zeolite 13X particles were uniformly dispersed without covering their surfaces by a symmetric porous structure of polypropylene lattice. In this study, $CO_2/N_2$ mixture was used as a simulated gas mixture. Separation was achieved by adsorbing $CO_2$ on the zeolite particles in the APM and then permeating $N_2$ into permeate side in passing all the feed gas through the APM. Adsorptive permeation tests were carried out with a set of APM modules, and the adsorptive permeation performances of the modules were analyzed from the test results. After saturation of the adsorbent with $CO_2$, the APM was regenerated by desorption of $CO_2$ from it through vacuuming both inside of outside of the APM hollow fiber, and the regeneration process of the APM by vacuuming was discussed in terms of regeneration efficiency and energy consumption.