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Synthesis and X-ray diffraction study of calcium salts of some carboxylic acidsa)

Published online by Cambridge University Press:  05 March 2012

A. Valor ,
E. Reguera  and
F. Sa´nchez-Sinencio
A. Valor*
Affiliation:
Research Center of Applied Science and Advanced Technology (CICATA), Instituto Politecnico Nacional, Legaria 694, Colonia Irrigacio´n, México D.F. 11500, México and Faculty of Physics, University of Havana, Havana, Cuba
E. Reguera
Affiliation:
Research Center of Applied Science and Advanced Technology (CICATA), Instituto Politecnico Nacional, Legaria 694, Colonia Irrigacio´n, México D.F. 11500, México and Institute of Materials and Reagents, University of Havana, Havana, Cuba
F. Sa´nchez-Sinencio
Affiliation:
Research Center of Applied Science and Advanced Technology (CICATA), Instituto Politecnico Nacional, Legaria 694, Colonia Irrigacio´n, México D.F. 11500, México
*
b)Electronic mail: alma@esfm.ipn.mx
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Abstract

An experimental X-ray diffraction (XRD) study of calcium salts of four carboxylic acids is presented. Calcium salts of propionic, butyric, valeric, and caproic acids were synthesized mixing in a mortar Ca(OH)2 with the liquid acids. Measuring the thermogravimetric analysis curves it was determined that the salts were actually monohydrates. The densities of the synthesized samples were measured using a density gradient column. The measured values for the densities were as follows: Dm(propionate)=1.38 g/cm3, Dm(butyrate)=1.30 g/cm3, Dm(valerate)=1.26 g/cm3, Dm(caproate)=1.22 g/cm3. The XRD analysis revealed that these compounds have monoclinic cells with symmetry described by the P21/a space group. Calcium propionate hydrate has cell parameters: a=2.437 51(5) nm, b=0.681 24(1) nm, c=0.591 43(1) nm, β=95.320(2)°. For calcium butyrate hydrate the cell parameters are: a=2.966 84(8) nm, b=0.680 74(2) nm, c=0.589 29(2) nm, β=95.442(3)°. The cell parameters for calcium valerate hydrate are: a=3.566 36(4) nm, b=0.682 49(1) nm, c=0.592 77(1) nm, β=107.280(1)° and for calcium caproate hydrate a=4.180 30(5) nm, b=0.682 61(1) nm, c=0.592 13(1) nm, β=110.230(1)°. The calculated density values from the XRD results, taking into account that the number of chemical formulas in the unit cell equals four, agree very well with the measured ones. It was established that the unit cell parameter a grows with the increase of the number of carbon atoms in the aliphatic chain, while parameters b and c remain almost constant. This is an indication of the stacking layer character of the structure as has been suggested for calcium stearate monohydrate. This fact points to the possibility of the refinement of the crystalline structures taking as the starting point the reported structure for calcium stearate monohydrate.

Keywords

X-ray diffractioncarboxylic acidscalcium saltsTGA
Type
Technical Articles
Information
Powder Diffraction , Volume 17 , Issue 1 , March 2002 , pp. 13 - 18
Copyright
Copyright © Cambridge University Press 2002

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Footnotes

a)

Paper presented at SARX 2000, 19–24 November 2000, Sao Pedro-SP-Brazil.

References

Boultif, A., and Louër, D. (1991). “Indexing of powder diffraction patterns for low-symmetry lattices by the successive dichotomy method,” J. Appl. Crystallogr. JACGAR 24, 987–993. acr, JACGAR CrossRefGoogle Scholar
Charbonnier, F., Gobert-Ranchoux, R., and Faure, R. (1977). “Crystal data for two salts of propionic acid: Ca(C2H5CO2)2.H2O and Sr(C2H5CO2)2.H2OF,” J. Appl. Crystallogr. JACGAR 10, 357. acr, JACGAR Google Scholar
Kohlbeck, F., and Hörl, E. M. (1976). “Indexing program for powder patterns especially suitable for triclinic, monoclinic and orthorhombic lattices,” J. Appl. Crystallogr. JACGAR 9, 28–33. acr, JACGAR CrossRefGoogle Scholar
Laugier, J., and Bochu, B. (2000). “LMGP—Suite of programs for the interpretation of X-ray experiments.” Available at: http://www.inpg.fr/LMGP and http://www.ccp14.ac.uk/tutorial/lmgp/Google Scholar
Lelann, P., and Bérar, J.-F. (1993). “Synchrotron high resolution powder study of molecular packing in hydrate calcium stearate,” Mater. Res. Bull. MRBUAC 28, 329–336. mrb, MRBUAC CrossRefGoogle Scholar
Reguera, E., Yee-Madeira, H., Ferna´ndez-Bertra´n, J., and Sa´nchez-Sinencio, F. (2000). Topics in Contemporary Physics, edited by J. A. Heras and R. V. Jiménez (Editorial IPN, México. Printed by Monarch Litho Inc. USA), p. 222.Google Scholar
Shirley, R. (1999a). The CRYSFIRE System for Automatic Powder Indexing. User’s Manual (The Lattice Press, Guilford, Surrey GU2 5NL, England).Google Scholar
Shirley, R. (1999b). “A modified version of Visser’s ITO zone-indexing program, using Ishida & Watanabe PM criterion for zone evaluation” (unpublished).Google Scholar
Shirley, R., and Louër, D. (1978). “New powder indexing programs for any symmetry which combine grid-search with successive dichotomy,” Acta Crystallogr. Sect. A: Cryst. Phys., Difr., Theor. Gen. Crystgallogr. ACACBN A34, S382. aca, ACACBN Google Scholar
Smith, S., and Snyder, R. L. (1979). “FN: A criterion for rating powder diffraction patterns and evaluating the reliability of powder-pattern indexing,” J. Appl. Crystallogr. JACGAR 12, 60–65. acr, JACGAR CrossRefGoogle Scholar
Strewler, G. J., and Rosenblat, M. (1995). Endocrinology (McGraw–Hill, New York), p. 1407.Google Scholar
Taupin, D. (1973). “A powder-diagram automatic-indexing routine,” J. Appl. Crystallogr. JACGAR 6, 380–385. acr, JACGAR CrossRefGoogle Scholar
Visser, Jan (1969). “A fully automatic program for finding the unit cell from powder data,” J. Appl. Crystallogr. JACGAR 2, 89–95. acr, JACGAR Google Scholar
Werner, P.-E., Eriksson, L., and Westdahl, M. (1985). “TREOR, a semi-exhaustive trial-and-error powder indexing program for all symmetries,” J. Appl. Crystallogr. JACGAR 18, 367–370. acr, JACGAR CrossRefGoogle Scholar
de Wolf, P. M. (1968). “A simplified criterion for the reliability of a powder pattern indexing,” J. Appl. Crystallogr. JACGAR 1, 108–113. acr, JACGAR CrossRefGoogle Scholar