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Download Article (PDF) An X-Ray Diffraction Study on the Structure of Concentrated Aqueous Caesium Iodide and Lithium Iodide Solutions Yusuke Tamura, Toshio Yamaguchi *, Isao Okada. and Hitoshi Ohtaki Department of Electronic Chemistry, Tokyo Institute of Technology, Nagatsuta, Midori-ku, Yokohama 227, Japan Z. Naturforsch. 42 a, 367-376 (1987); received December 8, 1986 X-Ray scattering measurements of 2.78 and 5.56 molal aqueous solutions of caesium iodide and 2.78 and 6.05 molal lithium iodide were carried out at 293 and 343 K Differences in the radial distribution functions (DRDFs) have been obtained between the caesium iodide and lithium iodide solutions of similar composition, the latter being taken as a reference for the data analysis of the former. The DRDFs show a peak arising from Cs-I contact-ion-pairs at 390 pm for all the caesium iodide solutions. The hydration structure of the caesium and iodide ions has been revealed. Effects of the concentration and temperature on the formation of ion-pairs and on the hydration structure of the ions are discussed. 1. Introduction cept Li+ increases. However, the above studies have given only indirect information with respect to The structure of electrolyte solutions, in partic- structural properties of hydrated ions. Recently, ular alkali halide solutions, has widely been in- Heinzinger et al. have obtained direct structural vestigated by means of X-ray and neutron diffrac- information on the effect of temperature and pres- tion [1] and Monte Carlo and molecular dynamics sure on the hydration shells of Li+ and I- and on the simulations [2], from which the structure and prop- bulk water by means of molecular dynamics (MD) erties of hydrated ions have been revealed. How- simulations of a 0.55 molal Lil solution at 308 and ever, almost all of these studies are limited to the 508 K [11]. systems at room temperature. Ionic association is another essential factor in The temperature dependence of the structure of understanding the physico-chemical properties of hydrated ions in aqueous solution has extensively concentrated alkali halide solutions. The formation been investigated by NMR [3, 4], conductivity [5], of ion-pairs in aqueous alkali halide solutions has thermochemical measurements [6,7], neutron been predicted on the basis of thermodynamic data scattering [8], and density measurements [9]. From [12, 13]. The first direct evidence of contact-ion-pairs these it has been concluded that ions which display has been obtained by Lawrence and Krüh [14] from negative hydration at room temperature change to their X-ray diffraction studies of concentrated alkali positive hydration with increasing temperature at solutions. Among the solutions of LiCl, LiBr, Lil, a so-called cross-over temperature. Buslaeva and Nal, CsCl, CsBr and Csl they found contact-ion- Samoilov [10] examined the temperature depen- pairs only in the caesium salts solutions. In X-ray dence of the hydration number of alkali metal and measuremets of concentrated aqueous KI solutions, halide ions in dilute solutions by a thermochemical Fishkis and Soboleva [15] reported the formation of + method, the results showing that with an increase in K -I" ion-pairs. Szäsz and Heinzinger [16] dis- + temperature the hydration number of these ions ex- cussed the formation of short lived Cs -F~ ion- pairs formed in a 2.2 molal aqueous CsF solution from an MD simulation. Neutron diffraction studies on concentrated aqueous LiCl solutions have revealed Reprint requests to Prof. H. Ohtaki, Department of Elec- + tronic Chemistry, Tokyo Institute of Technology, Naga- that Li — Cl~ contact-ion-pairs are formed [17, 18]. tsuta, Midori-ku, Yokohama 227, Japan. A recent MD simulation has also shown the forma- * Present address: Department of Chemistry, Faculty of tion of Li+-Cl" pairs in an aqueous LiCl solution Science, Fukuoka University, Nanakuma, Jonan-ku, having the [H 0]/[LiCl] molar ratio of four [19]. In Fukuoka 814-01, Japan. 2 0340-4811 / 87 / 0400-381 $ 01.30/0. - Please order a reprint rather than making your own copy. 368 Y. Tamura et al. • Structure of Aqueous Csl and Lil Solutions an aqueous solution with the [H20]/[LiCl] molar corrected scattering intensities to the electron units ratio of 3 (18.5 molal), more extensive ion-pair were carried out in the same way as previously formation between Li+ and Cl~ ions has been described [22, 23], revealed by both X-ray diffraction experiment and The structure function i(s) is obtained by sub- MD simulations [20,21], To our knowledge, no tracting the independent scatterings from all atoms investigation on ion-pair formation has yet been in the sample solutions from the scaled intensities carried out in aqueous alkali halide solutions at 7(5): elevated temperatures. i(s) = I(s)-Y,x f (s)2, (1) In the present paper, we report the results of i i X-ray diffraction studies on aqueous 2.78 and where Xj is the number of the /'-th atom in the 6.05 molal Lil solutions and 2.78 and 5.56 molal Csl stoichiometric volume V containing one iodine solutions at different temperatures. The ions Li+ atom and ft(s) is the coherent scattering factor cor- + and Cs were chosen in order to see the difference rected for the real and imaginary parts of the of ionic size. anomalous dispersion. The coherent and incoherent scattering factors of neutral atoms were taken from the International Tables [24], The structure func- 2. Experimental tions multiplied by the scattering vector 5 of the sample solutions are shown in Figs. 1 a and 2 a for Commercially available caesium iodide (min. the Lil and Csl solutions, respectively. 99.5%) was recrystallized once from water, and The radial distribution function (RDF) is calcu- reagent grade lithium iodide was used without lated by the Fourier transform of the structure further purification. The concentrations of the function: solutes were determined by gravimetry of iodide 2 y ^max 2 ions using an AgN03 solution. The densities of the D(r) = 4nr Q0 + J si(s) M(s) sin(sr) ds , (2) solutions were measured at 293 and 343 K by the n o pycnometric and Archimedes methods, respectively. where is the average electron density in the Data of the sample solutions are given in Table 1. stoichiometric volume V containing one iodine Solutions E and G are almost saturated at 293 and atom, and 5max is the maximum s-value attained in 343 K, respectively. the measurements. A modification function, M(s), A 6-6 diffractometer was used with MoA^ a with regard to one iodine atom, of the form radiation (/. = 71.07 pm) for the X-ray diffraction [./i (0)2//i(^)2] exp(- 100 52) was applied to all of measurements. The measured range of the scatter- the structure functions in common. ing angle (16) was 2— 140°, corresponding to an The synthetic structure function based on a model 1 5-range of 0.003-0.16 pm" (s = An sin 0//.). At is obtained by angles 6 below 1 ° the measured intensities were linearly extrapolated to zero at 6 = 0°. 80 000 counts v sin (sru) , i COsyn =LL xinijfifj exp (~ b^S1) at each data point were accumulated in the whole S I j j scan range. The diffractometer and details of data collection have been described in [22], Corrections _ y y 4 7^ sin (sR;) - s Rj cos (sRj) for absorption, polarization, double scattering and L XiXjJiJi V (sRj)3 incoherent scattering, and subsequent scaling of the •exp (-Bjs2). (3) 3 Table 1. Concentrations (mol/kg H20), water/salt molar ratios, densities (g/cm ), and temperatures (K) of the sample solutions. Solution Lil [H20]/[LiI] d T Solution Csl [H:0]/[CsI] d T A 2.78 20.0 1.25 293 E 2.78 20 1.47 293 B 2.78 20.0 1.22 343 F 2.78 20 1.44 343 C 6.05 9.19 1.49 293 G 5.56 10 1.79 343 D 6.05 9.19 1.45 343 369 Y. Tamura et al. • Structure of Aqueous Csl and Lil Solutions 4 6 8 10 12 14 16 s / 10-2prrH 4 6 8 10 12 14 16 s / 10-2pm-1 A Xv / \ / . \ / VY W. \ B ./ V A/V . 01 23456789 10 r / 102 pm \ c Fig. 2. a) Structure functions of the aqueous Csl solutions: experimental (dots) and calculated (solid lines), b) Radial 2 distribution functions in the form of D(r) - 4nr g0 of the aqueous Csl solutions: experimental (solid lines) and calculated (dashed lines). A D Fig. 1. a) Structure functions of the aqueous Lil solutions: experimental (dots) and calculated (solid lines), b) Radial 2 distribution functions in the form of D(r) — 4 nr g0 of the 01 23456789 10 aqueous Lil solutions: experimental (solid lines) and cal- r / 102pm culated (dashed lines). 370 Y. Tamura et al. • Structure of Aqueous Csl and Lil Solutions Table 2. Parameter values used for the model calculations on the Lil solutions of Fig. 1: the interatomic distance r (pm), the temperature factor 106 (pm2), the number of interactions n, and the parameters of the continuum electron distribution R (pm) and 10B (pm2). The values in parentheses are their standard deviations estimated from the least-squares fits. The parameter values without parentheses were fixed during the calculations. A B C D 2.78 molal 2.78 molal 6.05 molal 6.05 molal 293 K 343 K 293 K 343 K Li-0 r 220(8) — 228(3) — 10 b 10 — 10 — n 4 - 4 - 1-0 r 357.7(5) 358.2(2) 355.0(2) 359.1(2) 10 b 46(2) 33.8(5) 18.5(4) 16.4(3) n 8.3(1) 7.73(4) 5.58(5) 4.72(3) 0-0 r 279.9(4) 286.9(3) 283.2(4) 280(1) 10 b 8.3(7) 7.0(4) 5.8(5) 21(2) n * 3.39(4) 2.27(2) 2.34(3) 1.63(4) Li R 450(30) 330(20) 330(10) 290(30) 10 B 10 10 10 10 1 R 394(2) 385(1) 380(1) 363(1) 10 B 21(7) 29(4) 34(2) 84(5) H R 297(4) 242(3) 288(3) 234(4) 10 B 30(20) 80(20) 40(20) 10(20) O R 316(1) 301(1) 311(1) 286(1) 10 B 46(4) 87(3) 100(4) 92(5) * Per H20 molecule.
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