• Bulletin of the Korean Chemical Society
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• v.28 no.2
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• pp.251-256
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• 2007

The crystal structure of fully dehydrated partially Cs+-exchanged zeolite X, [Cs52Na40Si100Al92O384], a = 24.9765(10) A, has been determined by single-crystal X-ray diffraction techniques in the cubic space group Fd3 at 21 °C. The crystal was prepared by flow method for 5 days using exchange solution in which mole ratio of CsOH and CsNO3 was 1 : 1 with total concentration of 0.05 M. The crystal was then dehydrated at 400 °C and 2 × 10-6 Torr for 2 days. The structure was refined to the final error indices, R1 = 0.051 and wR2 (based on F2) = 0.094 with 247 reflections for which Fo > 4σ (Fo). In this structure, about fifty-two Cs+ ions per unit cell are located at six different crystallographic sites with special selectivity; about one Cs+ ion is located at site I, at the centers of double oxygen-rings (D6Rs), two Cs+ ions are located at site I', and six Cs+ ions are found at site II'. This is contrary to common view that Cs+ ions cannot pass sodalite cavities nor D6Rs because six-ring entrances are too small. Ring-opening by the formation of ?OH groups and ring-flexing make Cs+ ions at sites I, I', and II' enter six-oxygen rings. The defects of zeolite frameworks also give enough mobility to Cs+ ions to enter sodalite cavities and D6Rs. Another six Cs+ ions are found at site II, thirty-six are located at site III, and one is located at site III' in the supercage, respectively. Forty Na+ ions per unit cell are located at two different crystallographic sites; about fourteen are located at site I, the centers of D6Rs and twenty-six are also located at site II in the supercage. Cs+ ions and Na+ ions at site II are recessed ca. 0.34(1) A and 1.91(1) A into the supercage, respectively. In this work, the highest exchange level of Cs+ ions per unit cell was achieved in zeolite X by conventional aqueous solution methods and it was also shown that Cs+ ion could pass through the sixoxygen rings.

• Applied Chemistry for Engineering
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• v.20 no.1
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• pp.80-86
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• 2009

In this study, binderless zeolite BaX granule, an effective adsorbent for the separation of p-xylene was made. This adsorbent which has a sufficient strength, high specific surface area and selectivity to p-xylene was prepared by various steps, such as granulation process, calcination, binderless treatment, ion-exchange, and activation. In the granulation, the concentration of colloidal silica solution was controlled in order to confirm the effect of $SiO_2$ contents after binderless treatment. As a result, we confirmed that the compressive strength of granule after binderless treatment was increasing with increasing proportion of $SiO_2$ in the granule. And then Na-ion in granule was exchanged with Ba-ion by successive batch ion-exchange process. And then prepared adsorbents were tested for p-xylene separation by batch adsorption at $90^{\circ}C$. As a results of batch adsortion test, we confirmed that prepared adsorbents have a high selectivity to p-xylene. Also, it could be conformed that the prepared binderless zeolite BaX has a sufficient compressive strength (0.450 kgf), high specific surface area $(647.57m^2/g)$, high crystallinity (98.5% compared with zeolite NaX powder), and selectivity to p-xylene.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.11 no.1
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• pp.14-19
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• 2001

The crystal size was determined as a function of reaction temperature, during the crystallization process of NaX zeolite. The measured rate constants for linear growth were as 0.0441$\mu\textrm{m}$/h at $80^{\circ}C$, 0.0595$\mu\textrm{m}$/h at $90^{\circ}C$ and 0.0972$\mu\textrm{m}$/h at $100^{\circ}C$, respectively. The activation energy calculated from the relation between the linear growth rate an the reaction temperature was 43.243kJ/mol. The reaction of crystal growth were revealed as 20 days at $80^{\circ}C$, 16 days at $90^{\circ}C$ and 9 days at $100^{\circ}C$, respectively. Both the final product crystal size an the crystallization time were decreased with increasing reaction temperature.

• The Journal of Natural Sciences
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• v.8 no.2
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• pp.119-127
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• 1996

The effect of sodium hydroxide treatment on some physicochemical properties of zeolite mordenite mineral was studied with chemical analyses, powder X-ray diffraction, thermal analyses, infrared analysis, measurement of carbon dioxide adsorption and gas chromatography. Mordenite mineral from tuffaceous rocks in Yeongil and Wolsung area was used as a starting material and treated with 0.1-5N NaOH aqueous solution at about $95^{\circ}C$ in the water bath for three hours.At the concentration of sodium hydroxide below 0.5N, all chemical compositions in the tuff were virtually insoluble and the mordenite structure did not change. At the concentration above 1N, the chemical compositions such as silica, alumina, etc., were dissolved. The dissolution ratio of silica was lager than that of alumina, and the ratio of silica to alumina in the tuff decreased sharply in the concentration range of 2 to 3N. Intensity of X-ray diffraction peak of mordenite (202) plane and the adsorbed amount of carbon dioxide also decreased with the increasing concentration of sodium hydroxide above 1N. These decreases corresponded to the degree of mordenite structure collapsed.The separation of gas chromatography of nitrogen, oxygen and carbon monoxide was not affected by the sodium hydroxide treatment, but elution peaks of methane and krypton tended to be broadened and their retention time was shortened. The elution peaks of both methane and krypton tended to be overlapped with those of nitrogen and oxygen.

• Journal of Environmental Science International
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• v.29 no.12
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• pp.1261-1274
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• 2020

The characteristics of ammonia-nitrogen (NH4+-N) adsorption by a zeolitic material synthesized from Jeju scoria using the fusion and hydrothermal method was studied. The synthetic zeolitic material (Z-SA) was identified as a Na-A zeolite by X-ray diffraction, X-ray fluorescence analysis and scanning electron microscopy images. The adsorption of NH4+-N using Jeju scoria and different types of zeolite such as the Z-SA, natural zeolite, and commercial pure zeolite (Na-A zeolite, Z-CS) was compared. The equilibrium of NH4+-N adsorption was reached within 30 min for Z-SA and Z-CS, and after 60 min for Jeju scoria and natural zeolite. The adsorption capacity of NH4+-N increased with approaching to neutral when pH was in the range of 3-7, but decreased above 7. The removal efficiency of NH4+-N increased with increasing Z-SA dosage, however, its adsorption capacity decreased. For initial NH4+-N concentrations of 10-200 mg/L at pH 7, the adsorption rate of NH4+-N was well described by the pseudo second-order kinetic model than the pseudo first-order kinetic model. The adsorption isotherm was well fitted by the Langmuir model. The maximum uptake of NH4+-N obtained from the Langmuir model decreased in the order of Z-CS (46.8 mg/g) > Z-SA (31.3 mg/g) > natural zeolite (5.6 mg/g) > Jeju scoria (0.2 mg/g).

• Journal of Korean Society of Environmental Engineers
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• v.39 no.2
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• pp.66-73
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• 2017

This study was to evaluate the influential parameters such as intial Cs concentration, reaction temperature, contact time and pH variation of solution on Cs adsorption. Using the experimental data, adsorption kinetics, isotherms and thermodynamic properties were analyzed. The Cs ion adsorption of the zeolite X was effective in the range from pH 5 to 10 and reached equilibrium after 60 minutes. The adsorption kinetics and isotherms of Cs ion with the zeolite X was described well by the pseudo-second-order kinetic and Langmuir isotherm model. The maximum adsorption capacities of Cs ion calculated from Langmuir isotherm model at 293~333 K were from 303.03 mg/g to 333.33 mg/g. It was found that thermodynamic property of Cs ion absorption on the zeolite X was spontaneous and endothermic reaction. The experimental data were fitted a second-order polynomial equation by the multiple regression analysis. The values of the dependent variable calculated by this best fitted model equation were in very good agreement with the experimentally obtained values.

• The Journal of Engineering Research
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• v.5 no.1
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• pp.57-62
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• 2004

Korean natural zeolite with feldspar and illite as impurities was purified by an air classification method. X-ray powder diffraction analyses showed that the air classification effectively separated zeolite and impurities, and reduce the amount of impurity of the natural zeolite. The zeolite with air classification was treated with 1N NaOH solutions at temperatures at 100, 150, $200^{\circ}C$ for 17hours. The obtained hydrothermal treatment of phase change to phillilsite and analcime from mordenite and clinoptilolite.

• Journal of Environmental Health Sciences
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• v.33 no.4
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• pp.317-324
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• 2007

The sewage treatment sludge disposal has become a serious environmental problem because of restricted direct land-filling and oceandumping in spite of their large amounts discharged. So the recycling of sewage treatment sludge is very useful alternative for waste management. Here, we studied the feasibility of zeolite synthesis in open system from the sewage treatment sludge incinerator fly ash by means of hydrothermal synthesis. We considered the concentration of NaOH, reaction time, reaction temperature and reaction step as synthesis variables. The phase of zeolite products was identified by X-ray diffractometer(XRD) and ammonium ion exchange test was performed for the raw fly ash and two zeolite products(Z-3 and Z-5). In leaching test of the raw fly ash, hazard metal is detected very low level compared with regulatory leaching test standard. But in total recoverable test, the total contents of the fly ash were very high in terms of the standard for waste-derived fertilizer. Through hydrothermal reaction, small amount of zeolite P was synthesied in 1 N of NaOH solution and relatively large amount of hydroxysodalite was synthesied in 3 N and 5 N of NaOH solution with similar peak intensity. Addition of an aging step in the synthesis didn't increase the amount of zeolite phase. Maximum $NE_4^+-N$ exchange capacity is 1.49 mg $NH_4^+-N/g$ in Z-3 and 1.38 mg $NH_4^+-N/g$ in Z-5. Most of the ammonium ion is exchanged in 30 minutes and disorption did not occur until 5 hours.

• Journal of Environmental Science International
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• v.28 no.6
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• pp.561-570
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• 2019

A zeolitic material (Z-Y2) was synthesized from Coal Fly Ash (CFA) using a fusion/hydrothermal method under low-alkali condition (NaOH/CFA = 0.6). The adsorption performance of the prepared zeolite was evaluated by monitoring its removal efficiencies for Sr and Cs ions, which are well-known as significant radionuclides in liquid radioactive waste. The XRD (X-ray diffraction) patterns of the synthesized Z-Y2 indicated that a Na-A type zeolite was formed from raw coal fly ash. The SEM (scanning electron microscope) images also showed that a cubic crystal structure of size $1{\sim}3{\mu}m$ was formed on its surface. In the adsorption kinetic analysis, the adsorption of Sr and Cs ions on Z-Y2 fitted the pseudo-second-order kinetic model well, instead of the pseudo-first-order kinetic model. The second-order kinetic rate constant ($k_2$) was determined to be $0.0614g/mmol{\cdot}min$ for Sr and $1.8172g/mmol{\cdot}min$ for Cs. The adsorption equilibria of Sr and Cs ions on Z-Y2 were fitted successfully by Langmuir model. The maximum adsorption capacity ($q_m$) of Sr and Cs was calculated as 1.6846 mmol/g and 1.2055 mmol/g, respectively. The maximum desorption capacity ($q_{dm}$) of the Na ions estimated via the Langmuir desorption model was 2.4196 mmol/g for Sr and 2.1870 mmol/g for Cs. The molar ratio of the desorption/adsorption capacity ($q_{dm}/q_m$) was determined to be 1.44 for Na/Sr and 1.81 for Na/Cs, indicating that the amounts of desorbed Na ions and adsorbed Sr and Cs ions did not yield an equimolar ratio when using Z-Y2.

• Bulletin of the Korean Chemical Society
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• v.19 no.1
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• pp.98-103
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• 1998

The crystal structure of dehydrated $Rb^+$-exchanged zeolite X, stoichiometry $Rb_{71}Na_{21}-X\; (Rb_{71}Na_{21}Si_{100}Al_{92}O_{384})$ per unit cell, has been determined from single-crystal X-ray diffraction date gathered by counter methods. The structure was solved and refined in the cubic space group Fd3, a=25.007(3) Å at 21(1) ℃. The crystal was prepared by ion exchange in a flowing stream using a 0.05 M aqueous RbOH solution (pH=12.7). The crystal was then dehydrated at 360 ℃ and $2{\times}10^{-6}$ torr for two days. The structure was refined to the final error indices, $R_1=0.047$ and $R_2=0.040$ with 239 reflections for which I> 3σ(I). In this structure, 71 $Rb^+$ ions per unit cell are found at six different crystallographic sites and 21 $Na^+$ ions per unit cell are found at two different crystallographic sites. Four and a half $Rb^+$ ions are located at site Ⅰ, the center of the hexagonal prism. Nine $Rb^+$ ions are found at site Ⅰ' in the sodalite cavity (Rb-O=2.910(15) Å and O-Rb-O=78.1(4)°). Eighteen $Rb^+$ ions are found at site Ⅱ in the supercage (Rb-O=2.789(9) Å and O-Rb-O=92.1(4)°). Two and a half $Rb^+$ ions, which lie at site Ⅱ', are recessed ca. 2.07 Å into the sodalite cavity from their three O(2) oxygen planes (Rb-O=3.105(37) Å and O-Rb-O=80.6(5)°). Thirty-two $Rb^+$ ions are found at site Ⅲ deep in the supercage (Rb-O=2.918(12) Å and O-Rb-O=71.9(4)°), and five $Rb^+$ ions are found at site Ⅲ'. Seven $Na^+$ ions also lie at site Ⅰ. Fourteen $Na^+$ ions are found at site Ⅱ in the supercage (Na-O=2.350(19) Å and O-Na-O=117.5(6)°).