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Precipitation of calcium phosphates from electrolyte solutions

II. The formation and transformation of the precipitates

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Abstract

The kinetics of the formation and transformation of calcium phosphate precipitates obtained by mixing equal volumes of solutions, 6×10−3 M in total calcium and/or total phosphate was investigated at 25°. The phosphate solutions were preadjusted to pH 7.4. Changes of the pH and turbidity of the solutions were followed simultaneously as a function of time. Precipitates were isolated at various time intervals and characterized by different physicochemical methods. Initially a precipitate with a molar Ca/P ratio of 1.5, amorphous to X-ray and electron diffraction was formed. IR spectra indicated the presence of PO 3−4 and HPO 2−4 ions. After a period of metastability, precipitation of a crystalline material within or upon the amorphous matter occurred. Twenty four hours after sample preparation the precipitates showed mainly the characteristics of octacalcium phosphate.

Résumé

La cinétique de la formation et de la transformation des précipités de phosphate de calcium, obtenus en mélangeant de volumes égaux de solutions à 6×10−3 M de calcium total et/ou phosphate total est étudiée à 25°C. Les solutions de phosphate sont préajustées à un pH de 7.4. Les changements de pH et de turbidité des solutions sont suivis simultanément en fonction du temps. Les précipités sont isolés à des intervalles de temps variables et caractérisés par diverses méthodes physico-chimiques. Initialement un précipité avec un rapport molaire Ca/P de 1.5, amorphe aux rayons X et en diffraction électronique, est formé. Le spectre IR indique la présence de PO 3−4 et de HPO 2−4 . Après une période métastable, on observe la précipitation d'un matériel cristallin dans ou sur la phase amorphe. Vingt quatre heures après préparation de l'échantillon les précipités présentent surtout les caractères du phosphate octocalcique.

Zusammenfassung

Die Kinetik der Bildung und Transformation von Calciumphosphat-Niederschlägen wurde bei 25°C untersucht. Es wurden dazu gleiche Volumen von Lösungen gemischt, bei einer Konzentration von 6×10−3M totales Calcium und/oder totales Phosphat. Die Phosphatlösungen wurden zuerst auf pH 7,4 eingestellt. Veränderungen des pH und Trübung der Lösungen wurden gleichzeitig als eine Funktion der Zeit aufgezeichnet. Niederschläge wurden in verschiedenen Zeitintervallen isoliert und mit verschiedenen physiko-chemischen Methoden charakterisiert. Am Anfang wurde ein Niederschlag mit einem molaren Ca/P-Verhältnis von 1,5, im Röntgenbild und in der Elektronendiffraktion amorph, gebildet. Infrarotspektren deuteten die Anwesenheit von PO 3−4 - und HPO 2−4 -Ionen an. Nach einer metastabilen Periode erfolgte ein Niederschlag aus kristallinem Material innerhalb oder auf der amorphen Substanz. 24 Std nach der Herstellung der Proben zeigten die Niederschläge in der Hauptsache die Charakteristiken von Octocalciumphosphat.

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Authors and Affiliations

  1. Department of Physical Chemistry, “Rudjer Bošković” Institute, POB 1016, Zagreb, Croatia, Yugoslavia

    Lj. Brečević & H. Füredi-Milhofer

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  1. Lj. Brečević
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  2. H. Füredi-Milhofer
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Part of the M. Sc. thesis submitted to the Faculty of Science, University of Zagreb.

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Brečević, L., Füredi-Milhofer, H. Precipitation of calcium phosphates from electrolyte solutions. Calc. Tis Res. 10, 82–90 (1972). https://doi.org/10.1007/BF02012538

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  • DOI: https://doi.org/10.1007/BF02012538

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