Phase Equilibrium in the CsCl + YbCl3 + HCl (∼11.3 %) + H2O

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Phase Equilibrium in the CsCl + YbCl3 + HCl (∼11.3 %) + H2O System at 298.2 K and Thermodynamic Properties of New Solid Phase Compounds Zhan-Ping Qiao,† Hai-quan Xie,† Xin Chen,† and Hui Wang*,‡ †

College of Chemistry and Pharmacy Engineering, Nanyang Normal University, Nanyang 473061, P. R. China Key Laboratory of Synthetic and Natural Functional Molecule Chemistry (Ministry of Education), College of Chemistry & Materials Science, Northwest University, Xi’an 710069, P. R. China

‡

ABSTRACT: Solubility was studied in the CsCl + YbCl3 + HCl + H2O quaternary system along the (∼11.3 %) HCl section at 298.2 K using the isothermal solubility method, and the corresponding phase diagram was plotted. The compositions of solid phases were determined by the Schreinemaker’s wet residues technique. The system was complicated with four equilibrium solid phases CsCl, Cs4YbCl7·4H2O, Cs2YbCl5· 5H2O, and YbCl3·6H2O. The compound Cs4YbCl7·4H2O was incongruently soluble, and the compound Cs2YbCl5·5H2O was congruently soluble in the system. The new solid phase compounds were characterized by chemical analysis, X-ray diffraction (XRD), and thermogravimetric/differential thermogravimetric (TG-DTG) techniques. The standard molar enthalpies of solution of Cs4YbCl7·4H2O and Cs2YbCl5·5H2O in water were measured to be (18.19 ± 0.47) and (13.22 ± 0.27) kJ·mol−1 by microcalorimetry under the condition of infinite dilution, and their standard molar enthalpies of formation were determined as being − (4039.2 ± 2.2) kJ·mol−1 and − (3469.2 ± 1.3) kJ·mol−1, respectively.

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INTRODUCTION As host lattices, the compounds which were made of RbX or CsX and REX3 (X = Cl, Br, I; RE = La, Ce, Pr, Nd, Sm−Lu) showed upconversion luminescence property. Some potential upconversion materials, such as Er3+-doped RbGd2C17 and RbGd2Br7,1 Cs3Yb2Cl9 and Cs3Yb2Br9,2 Cs3Y2Br9:10% Dy3+ and Cs3Dy2Br9,3 Cs3Er2X9 (X = Cl, Br, I),4 and Er3+ in Cs3Lu2Br95 have been continuously reported. The synthesis of these compounds was realized by means of the Bridgman technique. To investigate the formation of the compounds of the alkali metal halide/rare-earth metal trihalide in the equilibrium systems and provide the data of phase equilibrium for scientists and engineers, the phase equilibrium systems of CsCl + RECl3 + HCl (∼13 %) + H2O (RE = La, Ce, Pr, Nd, Sm, Eu, Gd, Tm, Tb, Y, Lu) at 298.15 K have been reported.6−16 Twenty-two new solid compounds were obtained, including Cs5RECl8· nH2O (RE = Eu, Tb, n = 14, 6) (5:1 type), Cs4RECl7·nH2O (RE = Gd, Lu, Y, n = 1, 5, 10) (4:1 type), Cs3RECl6·nH2O (RE = La, Ce, Pr, n = 3, 7) (3:1 type), Cs2RECl5·nH2O (RE = La, Nd, Sm, Eu, Gd, Tb, Lu, n = 2, 4, 6, 7, 9) (2:1 type), CsRECl4· nH2O (RE = La, Ce, Pr, Nd, n = 4, 6, 9) (1:1 type), Cs3RE2Cl9· 14H2O (RE = Tm, Y) (3:2 type), and Cs9Lu5Cl24·29H2O (9:5 type) (type means the molar ratio of CsCl to RECl3). In addition, the spectroscopy properties of the Cs3CeCl6·3H2O, CsCeCl 4 ·4H 2 O, Cs 5 EuCl 8 ·14H 2 O, and Cs 2 EuCl 5 ·4H 2 O showed that they all exhibited upconversion luminescence when being exited in the near-infrared or visible region. Relevant results of rare earth metal chlorides in aqueous systems have been evaluated importantly.17 © 2013 American Chemical Society

As an extension of the work above, in this paper we reported the solubility of the system of CsCl + YbCl3 + HCl (∼11.3 %) + H2O at T = 298.2 K. The standard molar enthalpies of solution and standard molar enthalpies of formation of new solid phase compounds were obtained by microcalorimetry.

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EXPERIMENTAL SECTION Reagents. Cesium chloride (99.5+ mass % pure) purchased from Sinopharm Chemical Reagent Co., Ltd., Shanghai, China, was analytical reagent grade and without further purification. Ytterbium chloride (99.99 mass % pure) was extra pure grade, purchased from National Engineering Research Centre of Rare Earth Metallurgy and Function Materials, Baotou, China. Hydrochloric acid (guaranteed reagent) was purchased from Luoyang Haohua Chemical Reagent Company, Luoyang, China. Potassium chloride (99.99 mass % pure) was spectrum pure grade, purchased from Sinopharm Chemical Reagent Co., Ltd., Shanghai, China. Deionized water was used (resistivity = 5.7 MΩ·cm) in the present work. Investigations on the System at 298.2 K and Analysis Methods. The solubility of the system of CsCl + YbCl3 + HCl (∼11.3 %) + H2O system was investigated according to refs 15. All sealed samples were kept in a big water tank with an electrical stirrer at T = 298.2 K. The precision of the Received: June 20, 2013 Accepted: September 9, 2013 Published: September 26, 2013 3125

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Table 1. Solubility Data (in Mass Fraction) of the Saturated Solution of the Quaternary System CsCl−YbCl3−HCl(∼11 %)− H2O at (298.2 ± 0.1) K and Central Projection Data on the Trigonal Basal Face CsCl−YbCl3−H2Oa composition of solution/mass %

composition of residue/mass %

composition in the tetrahedral

composition in the trigonal basal faceb

no.

HCl

CsCl

YbCl3

CsCl

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 170 18 19

12.45 12.45 11.75 10.41 10.91 11.67 12.33 10.50 11.10 11.06 10.55 10.61 12.23 11.96 11.18 11.34 9.95 11.20 11.79

46.47 43.59 43.57 45.26 44.83 44.93 39.71 39.83 38.47 35.62 30.88 24.98 22.75 16.89 16.45 15.43 8.96 4.72 0.00

0.00 4.62 7.02 8.07 8.07 8.06 8.23 10.48 11.47 12.11 15.39 18.66 19.79 24.52 25.95 26.15 29.39 30.28 32.98

53.07 49.79 49.37 50.52 50.32 50.87 45.29 44.50 43.27 40.05 34.52 27.94 25.92 19.18 18.52 15.43 9.95 5.31 0.00

YbCl3

composition in the tetrahedral

composition in the trigonal basal face

HCl

YbCl3

CsCl

YbCl3

solid phasec

1.32 3.32 4.36 14.42 23.95 19.36 15.68 25.06 26.75 23.10 21.70 34.24 39.94 54.53 53.35 56.70 61.20

83.43 78.66 86.81 74.77 63.08 58.89 51.09 60.82 44.87 38.78 31.67 41.92 39.10 8.79 5.83 2.92 1.12

1.36 3.46 4.47 14.87 24.37 20.55 16.82 25.48 27.58 24.55 23.96 36.00 41.58 56.04 55.34 58.82 63.02

A A A A+B A+B B B B B+C C C C C C+D C+D D D D D

CsCl

w(HCl) = ∼11.34 mass % 0.00 5.28 3.21 80.76 7.96 4.07 75.46 9.01 2.54 84.60 9.06 3.04 72.50 9.12 1.74 61.98 9.38 5.80 55.48 11.71 6.80 47.62 12.90 1.63 59.83 13.62 3.03 43.51 17.20 5.91 36.49 20.87 9.44 28.68 22.55 4.90 39.87 27.85 3.95 37.56 29.21 2.69 8.56 29.50 3.60 5.62 32.64 3.60 2.82 34.01 2.89 1.09 37.38

a The estimated accuracy (in the mass fraction) for HCl, CsCl, and YbCl3 is ± 0.25 %, ± 0.35 %, and ± 0.15 %, respectively. bDouble saturation point (average): E1: CsCl 50.42 %, YbCl3 9.03 %; E2: CsCl 43.27 %, YbCl3 12.90 %; E3: CsCl 18.85 %, YbCl3 28.53 %. cCompounds: A: CsCl; B: Cs4YbCl7·4H2O; C: Cs2YbCl5·5H2O; D: YbCl3·6H2O.

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RESULTS AND DISCUSSION Quaternary System of CsCl + YbCl3 + HCl (∼11.3 %) + H2O at 298.2 K and Characterization of New Solid Phase Compounds. Table 1 shows the solubility data of the quaternary system of CsCl + YbCl3 + HCl (∼11.3 %) + H2O and the central projection data on the trigonal basal face of the CsCl + YbCl3 + H2O at 298.2 K. The ion concentration values in the saturated solution and the corresponding wet residue were expressed as mass fraction. Figure 1 displays the corresponding phase diagram. The phase diagram of the quaternary system of CsCl + YbCl3 + HCl (∼11.3%) + H2O presented three invariant points (E1, E2, E3) and four saturated liquid curves corresponding to the four equilibrium solid phases CsCl, Cs4YbCl7·4H2O, Cs2YbCl5· 5H2O, and YbCl3·6H2O, respectively. Besides the initial components CsCl and YbCl3·6H2O, two new solid phase compounds Cs4YbCl7·4H2O (4:1 type) and Cs2YbCl5·5H2O (2:1 type) crystallized from the saturated solutions. Cs4YbCl7· 4H2O was incongruently soluble, and Cs2YbCl5·5H2O was congruently soluble in ∼11.3 % HCl. The two new compounds were synthesized, and the compositions were determined by chemical analysis. Their compositions were 51.62 % Cs, 16.98 % Yb, and 24.42 % Cl for Cs4YbCl7·4H2O (theoretical, 51.87 % Cs, 16.88 % Yb, and 24.21 % Cl), 37.51 % Cs, 24.62 % Yb, and 25.29 % Cl for Cs2YbCl5·5H2O (theoretical, 37.64 % Cs, 24.50 % Yb, and 25.10 % Cl). The reaction of CsCl with YbCl3·6H2O led to Cs4YbCl7· 4H2O and Cs2YbCl5·5H2O, respectively. Figures 2 and 3 show XRD diffraction patterns for Cs4YbCl7·4H2O and Cs2YbCl5· 5H2O. The XRD diffraction patterns for Cs4YbCl7·4H2O and Cs2YbCl5·5H2O differed from those of CsCl and YbCl3·6H2O.

temperature was 0.1 K. The phase equilibrium of the system of CsCl + YbCl3 + HCl (∼11.3 %) + H2O can be reached in about 5 days. For the analysis methods of saturated solutions and the corresponding solid phases of the samples, see refs 15 and 18. The concentration of Yb3+ was determined by complexometry titration with ethylenediaminetetraacetic acid (EDTA); the concentration of Cs+ was determined by gravimetry with the precipitation of CsB(C6H5)4, and the concentration of Cl− by titration with a standard solution of silver nitrate. The solidphase compositions in the system were determined by Shreinemaker’s graphical method.19 Equipment and Conditions. Thermogravimetric/differential thermogravimetric (TG-DTG) analysis was undertaken with a NETZSCH STA449C thermal analysis apparatus with a heating rate of 10 K·min−1 under a N2 atmosphere with a flow rate of 100 cm3·min−1. X-ray diffraction (XRD) measurements were performed by a D/Max-3C diffractometer using Cu Kα radiation at room temperature. Calorimetric Technique. An RD496-2000 heat conduction microcalorimeter (Mianyang CP Thermal Analysis Instrument Co., Ltd., China) was employed to measure the enthalpies of solution of Cs4YbCl7·4H2O and Cs2YbCl5·5H2O, which has been described in detail previously.20 To check the performance of the calorimeter, the enthalpy of solution of KCl (mass fraction ⩾ 0.9999) in distilled water was measured to be (17.41 ± 0.10) kJ·mol−1, which was in excellent agreement with that of 17.234 kJ·mol−1 reported in the lierature.21 This indicated that the calorimeter used for measuring the enthalpy of solution in this work was reliable. 3126

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Figure 4. Thermogravimetry and differential thermogravimetry (TG, DTG) curves of Cs4YbCl7·4H2O. Figure 1. Solubility diagram of the quaternary system CsCl−YbCl3− HCl(∼11.3 mass %)−H2O projected on CsCl−YbCl3−H2O at (298.2 ± 0.1) K. The E1, E2, and E3 stand for double saturation points. The B, C, and D stand for the compounds Cs4YbCl7·4H2O, Cs2YbCl5·5H2O, and YbCl3·6H2O, respectively.

Cs2YbCl5·5H2O (Figure 5), at the temperature range from 312 K to 511 K, Cs2YbCl5·5H2O showed two obvious

Figure 5. Thermogravimetry and differential thermogravimetry (TG, DTG) curves of Cs2YbCl5·5H2O. Figure 2. XRD spectrum of Cs4YbCl7·4H2O.

dehydration steps. The experimental mass-loss value (13.17 %) was in good agreement with calculation data (12.76 %). Calorimetry. The molar enthalpies of solution of Cs4YbCl7· 4H2O (s) and Cs2YbCl5·5H2O (s) in 5.00 cm3 of water at 298.15 K are listed in Table 2, respectively. In Table 2, m is the mass of the sample, and ΔsolHΘm is the molar enthalpy of solution of the sample. Standard Molar Enthalpies of Formation of Cs4YbCl7· 4H2O and Cs2YbCl5·5H2O. The molar enthalpies of formation of Cs4YbCl7·4H2O and Cs2YbCl5·5H2O can be calculated according to the following equations: Δf Hm Θ(Cs4YbCl 7 · 4H 2O)(s) = 4Δf Hm Θ(Cs+)(aq) + Δf Hm Θ(Yb3 +)(aq) + 7Δf Hm Θ(Cl−)(aq) Figure 3. XRD spectrum of Cs2YbCl5·5H2O.

+ 4Δf Hm Θ(H 2O)(l) − Δsol Hm Θ(Cs4YbCl 7 ·4H 2O)(s) Δf Hm Θ(Cs2YbCl5· 5H 2O)(s) = 2Δf Hm Θ(Cs+)(aq)

TG-DTG curves of Cs4YbCl7·4H2O (Figure 4) indicated that the mass loss was 7.41 % (theoretical 7.03 %) from T = 308 K to 433 K, which corresponded to the continuous loss of the crystallization water molecules. For TG−DTG graphs of

+ Δf Hm Θ(Yb3 +)(aq) + 5Δf Hm Θ(Cl−)(aq) + 5Δf Hm Θ(H 2O)(l) − Δsol Hm Θ(Cs 2YbCl5·5H 2O)(s) 3127

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Table 2. Molar Enthalpies of Solution of ΔsolHΘm (Cs4YbCl7·4H2O) and ΔsolHΘm (Cs2YbCl5·5H2O) in Deionized Water at (298.15 ± 0.01) Ka

a

no.

m/mg

Qs/mJ

ΔsolHΘm (Cs4YbCl7·4H2O)/kJ·mol−1

m/mg

Qs/mJ

ΔsolHΘm (Cs2YbCl5·5H2O)/kJ·mol−1

1 2 3 4 5 6 meanb

43.72 43.32 43.57 43.83 44.08 43.42

804.1 761.9 781.2 752.8 753.0 796.2

18.85 18.02 18.37 17.60 17.51 18.79 18.19 ± 0.47

29.26 29.95 30.02 31.22 29.45 29.42

538.6 568.4 560.8 606.1 554.4 530.8

13.00 13.40 13.19 13.71 13.29 12.74 13.22 ± 0.27

In each experiment, 5.0 cm3 of water was used. bThe uncertainty is twice the standard deviation of the mean.

The standard molar enthalpies of formation of Cs+, Yb3+, and Cl− were taken from NBS tables,22 namely, −(258.28 ± 0.50) kJ·mol−1, −(674.5 ± 0.5) kJ·mol−1, and −(167.159 ± 0.10) kJ· mol−1, respectively. That of H2O was −(285.83 ± 0.042) kJ· mol−1 taken from the CODATA Key Values.23 Using these schemes above, the standard molar enthalpies of formation of Cs4YbCl7·4H2O and Cs2YbCl5·5H2O were calculated to be −(4039.2 ± 2.2) kJ·mol−1 and −(3469.2 ± 1.3) kJ·mol−1, respectively.

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CONCLUSION

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AUTHOR INFORMATION

(3) Aebersold, M. A.; Güdel, H. U.; Furrer, A.; Blank, H. Inelastic Neutron Scattering and Optical Spectroscopy of Dy3+ Single Ions and Dimers in Cs3Y2Br9:10% Dy3+ and Cs3Dy2Br9. Inorg. Chem. 1994, 33, 1133−1138. (4) Hehlem, M. P.; Krämer, K.; Güdel, H. U. Upconversion in Er3+Dimer Systems: Trends with the Series Cs3Er2X9 (X = Cl, Br, I). Phys. Rev. B: Condens. Matter 1994, 49, 12475−12483. (5) Hehlen, M. P.; Güdel, H. U.; Quagliano, J. R. Electronic Energy Level Structure and Correlation Crystal Field Effects of Er3+ in Cs3Lu2Br9. J. Chem. Phys. 1994, 101, 10303−10312. (6) Li, Y. H.; Ran, X. Q.; Chen, P. H. Studies on Solvent System of Cesium Chloride and Lanthanum Chloride and Synthesization of Four Types of New Compounds. J. Rare Earths 1997, 15 (2), 113−116. (7) Wang, H.; Duan, J. X.; Ran, X. Q.; Gao, S. Y. Study on the Phase Diagram of CsCl−CeCl3−HCl(11%)−H2O System at 298.15 K and the Fluorescence Properties of its Compounds. Chin. J. Chem. 2002, 20 (9), 904−908. (8) Li, Y. H.; Ran, X. Q.; Chen, P. H. Studies on Quaternary Systems CsCl−PrCl3−13% HCl−H2O (298 K) and CsCl−PrCl3−42% HAc− H2O (303 K). Chem. J. Chin. Univ. 1997, 18 (3), 353−356 (in Chinese). (9) Jiao, H.; Wang, H.; Ran, X. Q.; Chen, P. H. Study on the quaternary system of CsCl−NdCl3−13%HCl−(42%HOAc) −H2O. Acta Chim. Sin. 1998, 56, 854−858 (in Chinese). (10) Li, Y. H.; Ran, X. Q.; Chen, P. H. Phase Behavior of Hydrochloric Aqueous Solution Containing Cesium and Samarium Chloride and Two Sub-Group Effect of The Light Rare Earth Element. Zh. Neorg. Khim. 1999, 44, 1207−1209. (11) Wang, H.; Duan, J. X.; Ran, X. Q. Study on Phase Diagram of Cesium Chloride + Europium Trichloride + Hydrogen Chloride + Water Quaternary System at T = 298.15 K and the Fluorescence Spectra of its Compounds. J. Chem. Thermodyn. 2002, 34, 1495−1506. (12) Wang, H.; Ran, X. Q.; Chen, P. H. A Study on Quaternary Systems MCl−GdCl3−HCl−H2O (M = K, Rb, Cs) (20 °C). Acta Chim. Sin. 1994, 52, 789−796 (in Chinese). (13) Qiao, Z. P.; Zhuo, L. H.; Zhang, S. S.; Wang, H. CsCl−TmCl3− HCl−H2O at 25 °C: Phase Equilibrium and New Solid Phase Compound. Chin. Inorg. Chem. 2006, 22, 1545−1549 (in Chinese). (14) Wang, H.; Yang, Q. C.; Li, L. Phase Equilibrium System of CsCl−TbCl3−HCl(∼7.6 mass %)−H2O at 298.2 ± 0.1 K and Fluorescent and Thermal Properties of Its Solid-Phase Compounds in the System. J. Chem. Eng. Data 2013, 58, 1034−1038. (15) Qiao, Z. P.; Xie, H. Q.; Zhuo, L. H.; Xin, C. Study on Phase Equilibrium in the Quaternary System CsCl−LuCl3−HCl (10.06%)− H2O at 298.15 ± 0.1 K and New Solid-Phase Compounds. J. Chem. Eng. Data 2007, 52, 1681−1685. (16) Wang, H.; Duan, J. X.; Ran, X. Q.; Gao, S. Y. Phase Equilibrium System of CsCl−YCl3−(9.5%) HCl−H2O at T = 298.15 K and Its Compounds. Chin. J. Chem. 2004, 22, 1129−1132. (17) Mioduski, T.; Gumiński, C.; Zeng, D. W. IUPAC-NIST Solubility Data Series. 87. Rare Earth Metal Chlorides in Water and Aqueous Systems. J. Phys. Chem. Ref. Data 2008, 37, 1765−1853; 2009, 38, 441−562; 2009, 38, 925−1011.

The quaternary system of CsCl + YbCl3 + HCl (∼11.3 %) + H2O was investigated, and the corresponding phase diagram was constructed. In the quaternary system, Cs4YbCl7·4H2O and Cs2YbCl5·5H2O were found. Cs4YbCl7·4H2O was incongruently soluble, and Cs2YbCl5·5H2O was congruently soluble in an average medium of ∼11.3 mass % HCl. The phase diagram of the quaternary system could provide the fundamental basis and serve as a guide for the preparation of Cs4YbCl7·4H2O and Cs2YbCl5·5H2O. The standard molar enthalpies of solution for the two compounds of Cs4YbCl7· 4H2O and Cs2YbCl5·5H2O were measured, and their standard molar enthalpies of formation were calculated. Among the systems CsCl + RECl3 + HCl (∼13 %) + H2O (RE = La, Ce, Pr, Nd, Sm, Eu, Gd, Tm, Tb, Yb, Y, Lu) reported by us, it was found that the compounds of RECl3 (before Gd element) and CsCl formed in the systems were mainly 1:1 type (CsRECl4·nH2O, RE = La, Ce, Pr, Nd), 2:1 type (Cs2RECl5· nH2O, RE = La, Nd, Sm, Eu, Gd), and 3:1 type (Cs3RECl6· nH2O, RE = La, Ce, Pr), while those compounds (after Gd) were mainly 3:2 type (Cs3RE2Cl9·14H2O, RE = Tm, Y) and 4:1 type (Cs4RECl7·nH2O, RE = Gd, Lu, Yb, Y). The results showed “the effect of two groups” before and after Gd in which lanthanide rare earth elements were bordered by the Gd element in aqueous phase equilibrium.

Corresponding Author

*E-mail: [email protected]. Notes

The authors declare no competing financial interest.

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