• Title/Summary/Keyword: X-Ray diffraction method

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Geochemical Characteristics of the Gyeongju LILW Repository II. Rock and Mineral (중.저준위 방사성폐기물 처분부지의 지구화학 특성 II. 암석 및 광물)

  • Kim, Geon-Young;Koh, Yong-Kwon;Choi, Byoung-Young;Shin, Seon-Ho;Kim, Doo-Haeng
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.6 no.4
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    • pp.307-327
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    • 2008
  • Geochemical study on the rocks and minerals of the Gyeongju low and intermediate level waste repository was carried out in order to provide geochemical data for the safety assessment and geochemical modeling. Polarized microscopy, X-ray diffraction method, chemical analysis for the major and trace elements, scanning electron microscopy(SEM), and stable isotope analysis were applied. Fracture zones are locally developed with various degrees of alteration in the study area. The study area is mainly composed of granodiorite and diorite and their relation is gradational in the field. However, they could be easily distinguished by their chemical property. The granodiorite showed higher $SiO_2$ content and lower MgO and $Fe_2O_3$ contents than the diorite. Variation trends of the major elements of the granodiorite and diorite were plotted on the same line according to the increase of $SiO_2$ content suggesting that they were differentiated from the same magma. Spatial distribution of the various elements showed that the diorite region had lower $SiO_2,\;Al_2O_3,\;Na_2O\;and\;K_2O$ contents, and higher CaO, $Fe_2O_3$ contents than the granodiorite region. Especially, because the differences in the CaO and $Na_2O$ distribution were most distinct and their trends were reciprocal, the chemical variation of the plagioclase of the granitic rocks was the main parameter of the chemical variation of the host rocks in the study area. Identified fracture-filling minerals from the drill core were montmorillonite, zeolite minerals, chlorite, illite, calcite and pyrite. Especially pyrite and laumontite, which are known as indicating minerals of hydrothermal alteration, were widely distributed in the study area indicating that the study area was affected by mineralization and/or hydrothermal alteration. Sulfur isotope analysis for the pyrite and oxygen-hydrogen stable isotope analysis for the clay minerals indicated that they were originated from the magma. Therefore, it is considered that the fracture-filling minerals from the study area were affected by the hydrothermal solution as well as the simply water-rock interaction.

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Alteration Zoning, Mineral Assemblage and Geochemistry of the Hydrothermal Clay Deposits Related to Cretaceous Felsic Magmatism in the Haenam Area, Southwest Korea (한국 서남부, 해남지역에서 백악기 산성마그마티즘에 관련된 열수점토광상의 누대분배, 광물조합의 지구화학적 연구)

  • Kim, In Joon
    • Economic and Environmental Geology
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    • v.25 no.4
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    • pp.397-416
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    • 1992
  • In the present study, three clay deposits, named the Seongsan, Ogmaesan and Haenam deposits, were investigated. The altered zones are recognized in the hydrothermally altered rocks of the clay deposits from the center of the alteration to the margin: Kaolin, Kaolin-Quartz, Quartz, Sericite and Chlorite zones in the Seongsan deposits; Quartz zone, Alunite zone, Kaolin zone, Sericite zone and Chlorite zone in the Ogmaesan deposits; Quartz zone, Pyrophyllite zone, Sericite zone and Chlorite zone in the Haenam deposits. These zones can be grouped into two types of alteration: Acidic alteration such as Pyrophyllite zone, Alunite zone, Quartz zone, Kaolin zone, Kaolin-Quartz zone and a part of Sericite zone; Propylitic alteration such as Chlorite zone and a part of Sericite zone. All clay deposits belong to high-sulfidation (acid-sulfate) system. The rocks of the acidic alterations are composed of pyrophyllite, alunite, kaolin minerals, sericite, quartz and pyrite. On the basis of bulk chemical compositions, it was found that some components such as $SiO_2$, $TiO_2$, $Fe_2O_3$, FeO, MgO, CaO, $K_2O$ and $Na_2O$ were mobilized considerably from the original rocks. The mobility of these major elements is related to, and controls, mineral assemblages in each altered zone. Polytypes of sericite are determined as $2M_1$ and 1M by X-ray diffraction method. The amount of $2M_1$ is nearly equal to that of 1M in the Seongsan deposits whereas $2M_1$ is less and higher than that of 1M in the Ogmaesan and the Haenam deposits. These facts indicate that formation temperature of sericite is relatively high in the Haenam deposits, moderate in the Seongsan deposits, and low in the Ogmaesan deposits. The ratios of Na/(K+Na) for alunite in the Ogmaesan deposits determined by electron microprobe analyzer (EPMA) are higher than those in the Seongsan deposits. Thus, the alunite of the Ogmaesan deposits must have been formed from the solutions with relatively high aqueous Na/(K+Na) ratios and low pH at a high temperature rather than that of the Seongsan deposits. From all data, it is clarified that alunite is hypogene in origin, and has been formed by oxidation of hydrogen sulfide in the steam-heated environment, and that alunite has been produced by the spectacular solfataric alteration observed at the surface of some present-day hydrothermal systems.

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Micromorphological and Mineral Characteristics of the Jang-won Series which have Fragipan in the soil Profile (경반층 토양인 장원통의 미세형태학적 및 광물학적 특성)

  • Moon, Yong-Hee;Zhang, Yong-Seon;Chun, Hyen-Chung;Sonn, Yeon-Kyu;Hyun, Byung-Keun;Park, Chan-Won;Song, Kwan-Cheol
    • Korean Journal of Soil Science and Fertilizer
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    • v.44 no.5
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    • pp.916-921
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    • 2011
  • This study was carry out on a Jang-Won series (fine loamy, mixed, mesic family of typic fragipan) that were established and classified as a fragipan soil in Korea. The morphological, physical, chemical and minerals characteristics of Jang-Won series were studied to determine the genesis of fragipan soils in natural environment. Each sample was analyzed for its physical, chemical and mineralogical characteristics. The particle size distribution of samples was measured using pipette method. Clay minerals were investigated on parallel-oriented specimens of the clay fraction ($<2{\mu}m$) from each horizon, separated by sieving and centrifugation, using X-ray diffraction (XRD) analysis. Micromorphological observations were made on thin sections prepared from soil blocks impregnated with Crystic Resin, cut and ground to less than $30{\mu}m$ in thickness, and finally polished with diamond paste. Most horizons have pH values in the range of fewer than 5.0 and have very low base-saturation values. Their textural classification ranges from silt loam to loam, the lower horizons being the finer. The clay fraction revealed the occurrence of illite, kaolinite, chlorite and vermiculite. The micro-morphological analysis carries out thin sections from each soil profile. The silt concentrations occur as extremely dense and homogenous bands or zones of silt-sized materials, brownish in colour in plane-polarized light and anisotropic in cross-polarized light, surrounding or adhering to skeleton grains. The genesis of fragipan in the Jangweon series assumed composition of clay fraction rather than silt concentration. Therefore, this results suggested an authentic interpretation which Jangweon series is classification as Typic Fragiochrepts.

Crystallographic Study on the Selectivity and Distribution of Sr2+ Ions Within Zeolite A In the Presence of Competing Na+ Ions in Aqueous Exchange Solution (Na+ 경쟁이온이 존재하는 수용액에서 Zeolite A 내 Sr2+ 이온의 선택성 및 분포에 관한 결정학적 연구)

  • kim, Hu Sik;Park, Jong Sam;Lim, Woo Taik
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.1
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    • pp.41-50
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    • 2022
  • To study the properties of Sr2+ exchange into zeolite A with increasing the molar concentration of Na+ in given exchange solution, four single crystals of fully dehydrated Sr2+- and Na+- exchanged zeolite A were prepared by the bath method using mixed ion-exchange solutions. The Sr(NO3)2:NaNO3 molar rations of the ion exchange solution were 1:1(crystal 1), 1:100(crystal 2), 1:250(crystal 3), and 1:500 (crystal 4), respectively, with a total concentration of 0.05 M. The single-crystals were then vacuum dehydration at 623 K and 1×10-4 Pa for 2 days. Their single-crystal structures were determined by single-crystal synchrotron X-ray diffraction techniques in the cubic space group Pm3-m, at 100(1) K, and were then refined to the final error indices of R1/wR2=0.047/0.146, 0.048/0.142, 0.036/0.128, and 0.040/0.156 for crystals 1, 2, 3, and 4, respectively. In crystals 1 and 2, the 6 Sr2+ ions are found at three different crystallographic sites. In crystal 3, 1 Sr2+ and 10 Na+ ions are found in large cavity and sodalite unit. In crystal 4, only 12 Na+ ions occupy three equipoints. The degree of Sr2+ ion-exchange decreased sharply from 100 to 16.7 to 0% as the initial Na+ concentration increase and the Sr2+ concentration decrease. In addition, the unit cell constant of the zeolite framework decreased with this lower level of Sr2+ exchange.

Heat Shield Property of Nanostructural-regulated Fe2O3/TiO2 Composites Filled with Polyacrylate Paint (나노구조 변화에 의한 Fe2O3/TiO2 복합재료를 충전한 Poly Acrylate 도료의 열차단 특성)

  • Kim, Dae Won;Ma, Young Kil;Kim, Jong Seok
    • Applied Chemistry for Engineering
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    • v.31 no.1
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    • pp.43-48
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    • 2020
  • Fe2O3 nanoparticles with the mixed structure of cubic and nanorod were synthesized by precipitation, hydrothermal, sol-gel method, etching process and heat treatment. Fe2O3/TiO2 core-shell (CS) of type Fe2O3@TiO2 composite was fabricated on a 20 nm nanolayer of TiO2 coated on the surface of Fe2O3 nanoparticles. Fe2O3/TiO2 yolk-shell (YS) composite was prepared by chemical etching and heat treatment of Fe2O3/TiO2 CS nanoparticles. Physical properties of Fe2O3, Fe2O3@TiO2 CS and Fe2O3@TiO2 YS nanoparticles were characterized by FE-SEM, HR-TEM and X-ray diffraction. The solar reflectance, commission internationale de l'Elcairage (CIE) color coordinate and heat shield temperatures of Fe2O3, CS and YS type Fe2O3@TiO2 pigments filled with poly acrylate (PA) paints were investigated by UV-Vis-NIR spectrometer and homemade heat shield temperature measuring device. The Fe2O3@TiO2 YS red pigment filled PA composite exhibited excellent near infrared light reflecting performance and also reduced the heat shield temperature of 13 ℃ than that of Fe2O3 filled counterparts.

Luminescence properties of $(Y,\;Zn)_2O_3$:$Eu^{3+}$ red phosphor as the effect of Zn ion (Zn ion의 영향에 따른 $(Y,\;Zn)_2O_3$:$Eu^{3+}$ 적색 형광체의 발광특성)

  • Song, Y.H.;Moon, J.W.;Park, W.J.;Yoon, D.H.
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.18 no.6
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    • pp.253-257
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    • 2008
  • To enhance the luminescence properties, the red phosphor composed of $(Y,\;Zn)_2O_3$:$Eu^{3+}$ as doping concentration of Zn ion is synthesized at $1200^{\circ}C$ for 6 hrs in air atmosphere by conventional solid reaction method. As a result of the red phosphor $(Y,\;Zn)_2O_3$:$Eu^{3+}$ is measured X-ray diffraction (XRD), The main peak is nearly corresponded to the same as JCPDS card (No. 41-1105). When the doping concentration of Zn ion is more than 5 mol%, However, the ZnO peak is showed by XRD analysis. Therefore, when the doping concentration of Zn ion is less than 5 mol%, the Zn ion is well mixed in $Y_2O_3$ structure without the impurity phases. The photoluminescence (PL) properties is shown as this phosphor is excited in 254 nm region and the highest emission spectra of $(Y,\;Zn)_2O_3$:$Eu^{3+}$ has shown in 612 nm region because of a typical energy transition ($^5D_0{\rightarrow}^7F_2$) of $Eu^{3+}$ ion. As the doping concentration of Zn ion is more than 10 mol%, the emission peak is suddenly decreased. when the highest emission peak as doping concentration of Zn ion is shown, the composition of this phosphor is $(Y_{0.95},\;Zn_{0.05})_2O_3$:$Eu^{3+}_{0.075}$ and the particle size analyzed by FE-SEM is confirmed from 0.4 to $3{\mu}m$.

Improved Electrochemical Performance and Minimized Residual Li on LiNi0.6Co0.2Mn0.2O2 Active Material Using KCl (KCl을 사용한 LiNi0.6Co0.2Mn0.2O2계 양극활물질의 잔류리튬 저감 및 전기화학특성 개선)

  • Yoo, Gi-Won;Shin, Mi-Ra;Shin, Tae-Myung;Hong, Tae-Whan;Kim, Hong-kyeong
    • Journal of the Korean Electrochemical Society
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    • v.20 no.1
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    • pp.7-12
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    • 2017
  • Using a precursor of $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ as a starting material, a surface-modified cathode material was obtained by coating with KCl, where the added KCl reduces residual Li compounds such as $Li_2CO_3$ and LiOH, on the surface. The resulting electrochemical properties were investigated. The amounts of $Li_2CO_3$ and LiOH decreased from 8,464 ppm to 1,639 ppm and from 8,088 ppm to 6,287 ppm, respectively, with 1 wt% KCl added $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ that had been calcined at $800^{\circ}C$. X-ray diffraction results revealed that 1 wt% of KCl added $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ did not affect the parent structure but enhanced the development of hexagonal crystallites. Additionally, the charge transfer resistance ($R_{ct}$) decreased dramatically from $225{\Omega}$ to $99{\Omega}$, and the discharge capacity increased to 182.73mAh/g. Using atomic force microscopy, we observed that the surface area decreased by half because of the exothermic heat released by the Li residues. The reduced surface area protects the cathode material from reacting with the electrolyte and hinders the development of a solid electrolyte interphase (SEI) film on the surface of the oxide particles. Finally, we found that the introduction of KCl into $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ is a very effective method of enhancing the electrochemical properties of this active material by reducing the residual Li. To the best of our knowledge, this report is the first to demonstrate this phenomenon.

Phase Transitions of $LiMn_2O_4$ on $CO_2$ Decomposition (($CO_2$ 분해시 $LiMn_2O_4$의 상변화)

  • Kwoen, Tae-Hwan;Yang, Chun-Mo;Park, Young-Goo;Cho, Young-Koo;Rim, Byung-O
    • Journal of the Korean Applied Science and Technology
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    • v.20 no.1
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    • pp.33-43
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    • 2003
  • $LiMn_2O_4$ catalyst for $CO_2$ decomposition was synthesized by oxidation method for 30 min at 600$^{\circ}C$ in an electric furnace under air condition using manganese(II) nitrate $(Mn(NO_3)_2{\cdot}6H_2O)$, Lithium nitrate ($LiNO_3$) and Urea $(CO(NH_2)_2)$. The synthesized catalyst was reduced by $H_2$ at various temperatures for 3 hr. The reduction degree of the reduced catalysts were measured using the TGA. And then $CO_2$ decomposition rate was measured using the reduced catalysts. Phase-transitions of the catalysts were observed after $CO_2$ decomposition reaction at an optimal decomposition temperature. As the result of X-ray powder diffraction analysis, the synthesized catalyst was confirmed that the catalyst has the spinel structure, and also confirmed that when it was reduced by $H_2$, the phase of $LiMn_2O_4$ catalyst was transformed into $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase. After $CO_2$ decomposition reaction, it was confirmed that the peak of $LiMn_2O_4$ of spinel phase. The optimal reduction temperature of the catalyst with $H_2$ was confirmed to be 450$^{\circ}C$(maximum weight-increasing ratio 9.47%) in the case of $LiMn_2O_4$ through the TGA analysis. Decomposition rate(%) using the $LiMn_2O_4$ catalyst showed the 67%. The crystal structure of the synthesized $LiMn_2O_4$ observed with a scanning electron microscope(SEM) shows cubic form. After reduction, $LiMn_2O_4$ catalyst became condensed each other to form interface. It was confirmed that after $CO_2$ decomposition, crystal structure of $LiMn_2O_4$ catalyst showed that its particle grew up more than that of reduction. Phase-transition by reduction and $CO_2$ decomposition ; $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase at the first time of $CO_2$ decomposition appear like the same as the above contents. Phase-transition at $2{\sim}5$ time ; $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase by reduction and $LiMn_2O_4$ of spinel phase after $CO_2$ decomposition appear like the same as the first time case. The result of the TGA analysis by catalyst reduction ; The first time, weight of reduced catalyst increased by 9.47%, for 2${\sim}$5 times, weight of reduced catalyst increased by average 2.3% But, in any time, there is little difference in the decomposition ratio of $CO_2$. That is to say, at the first time, it showed 67% in $CO_2$ decomposition rate and after 5 times reaction of $CO_2$ decomposition, it showed 67% nearly the same as the first time.

Glycerol Steam Reforming for Hydrogen Production on Metal-ceramic Core-shell CoAl2O4@Al Composite Structures (금속-세라믹 Core-Shell CoAl2O4@Al 구조체를 적용한 불균일계 촉매의 글리세롤 수소전환 반응특성)

  • Kim, Jieun;Lee, Doohwan
    • Clean Technology
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    • v.21 no.1
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    • pp.68-75
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    • 2015
  • In this study, we investigated the structure and properties of a highly heat conductive metal-ceramic core-shell CoAl2O4@Al micro-composite for heterogeneous catalysts support. The CoAl2O4@Al was prepared by hydrothermal surface oxidation of Al metal powder, which resulted in the structure with a high heat conductive Al metal core encapsulated by a high surface area CoAl2O4 shell. For comparison, CoAl2O4 was also prepared by co-precipitation method and also utilized for a catalyst support. Rh catalysts supported on CoAl2O4@Al and CoAl2O4 were prepared by incipient wetness impregnation and characterized by N2 adsorption, X-ray diffraction (XRD), scanning electron microscopy (SEM), CO chemisorption, and temperature-programmed reduction (TPR). The properties of catalysts were investigated for glycerol steam reforming reaction for hydrogen production at 550 ℃. Rh/CoAl2O4@Al exhibited about 2.8 times higher glycerol conversion turnover frequency (TOF) than Rh/CoAl2O4 due to facilitated heat transport through the core-shell structure. The CoAl2O4@Al and CoAl2O4 also showed some catalytic activities due to a partial reduction of Co on the support, and a higher catalytic activity was also found on the CoAl2O4@Al core-shell than CoAl2O4. These catalysts, however, displayed deactivation on the reaction stream due to carbon deposition on the catalysts surface.

Site Competition of Ca2+ and Cs+ Ions in the Framework of Zeolite Y (Si/Al = 1.56) and Their Crystallographic Studies (제올라이트 Y (Si/Al = 1.56) 골격 내의 Ca2+과 Cs+ 이온의 자리 경쟁 및 그들의 결정학적 연구)

  • Kim, Hu Sik;Park, Jong Sam;Lim, Woo Taik
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.4
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    • pp.235-248
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    • 2018
  • The present work was performed in order to study the effect of competing cation of $Ca^{2+}$ ion on ion exchange of $Cs^+$ on zeolite Y (Si/Al = 1.56). Three single-crystals of fully dehydrated and partially $Cs^+$-exchanged zeolites Y (Si/Al = 1.56) were prepared by the flow method using mixed ion-exchange solutions. The $CsNO_3:Ca(NO_3)_2$ molar ratios of the ion exchange solution were 1 : 1 (crystal 1), 1 : 100 (crystal 2), and 1 : 250 (crystal 3) with a total concentration of 0.05 M. The single-crystals were then vacuum dehydrated at 723 K and $1{\times}10^{-4}Pa$ for 2 days. The structures of the crystals were determined by single-crystal synchrotron X-ray diffraction technique in the cubic space group $Fd{\bar{3}}m$, at 100(1) K. The unit-cell formulas of crystals 1, 2, and 3 were ${\mid}Cs_{21}Ca_{27}{\mid}[Si_{117}Al_{75}O_{384}]-FAU$, ${\mid}Cs_2Ca_{36.5}{\mid}[Si_{117}Al_{75}O_{384}]-FAU$, and ${\mid}Cs_1Ca_{37}{\mid}[Si_{117}Al_{75}O_{384}]-FAU$, respectively. In all three crystals, the $Ca^{2+}$ ions preferred to occupy site I in the D6Rs, with the remainder occupying sites I', II', and II. On the other hand, the significant differences in the fractional distribution of $Cs^+$ ions are observed depending on the intial $Cs^+$ concentrations in given ion exchange solution. In Crystal 1, $Cs^+$ ion are located at sites II', II, III, and III', and in crystal 2, at sites II, IIIa, and IIIb. In crystal 3, $Cs^+$ ions are only located at sites IIIa and IIIb. The degree of $Cs^+$ ion exchange decreased sharply from 28.0 to 2.7 to 1.3 % as the initial $Ca^{2+}$ concentration increases and the $Cs^+$ content decreases.