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USGS · 70010604

Crystal chemistry and structure refinement of five hydrated calcium borates

J. R. Clark·D.E. Appleman·C. L. Christ
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Abstract

The crystal structures of the five known members of the series Ca 2 B 6 O 11 ·xH 2 O (x = 1, 5, 5, 7, 9, and 13) have been refined by full-matrix least-squares techniques, yielding bond distances and angles with standard errors of less than 0·01 Å and 0·5°, respectively. The results illustrate the crystal chemical principles that govern the structures of hydrated borate compounds. The importance of hydrogen bonding in the ferroelectric transition of colemanite is confirmed by more accurate proton assignments.

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J. R. Clark, D.E. Appleman, C. L. Christ. 1964. Crystal chemistry and structure refinement of five hydrated calcium borates. https://doi.org/10.1016/0022-1902(64)80234-7

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USGS1967

The ternary system K2SO4 MgSO4 CaSO4

Melting and subsolidus relations in the system K 2 SO 4 MgSO 4 CaSO 4 were studied using heating-cooling curves, differential thermal analysis, optics, X-ray diffraction at room and high temperatures and by quenching techniques. Previous investigators were unable to study the binary MgSO 4 CaSO 4 system and the adjacent area in the ternary system because of the decomposition of MgSO 4 and CaSO 4 at high temperatures. This problem was partly overcome by a novel sealed-tube quenching method, by hydrothermal synthesis, and by long-time heating in the solidus. As a result of this study, we found: (1) a new compound, CaSO 4 ·3MgSO 4 (m.p. 1201°C) with a field extending into the ternary system; (2) a high temperature form of MgSO 4 with a sluggishly reversible inversion. An X-ray diffraction pattern for this polymorphic form is given; (3) the inversion of β-CaSO 4 (anhydrite) to α-CaSO 4 at 1195°C, in agreement with grahmann ; (1) (4) the melting point of MgSO 4 is 1136°C and that of CaSO 4 is 1462°C (using sealed tube methods to prevent decomposition of the sulphates); (5) calcium langbeinite (K 2 SO 4 ·2CaSO 4 ) is the only compound in the K 2 SO 4 CaSO 4 binary system. This resolved discrepancies in the results of previous investigators; (6) a continuous solid solution series between congruently melting K 2 SOP 4 ·2MgSO 4 (langbeinite) and incongruently melting K 2 SO 4 ·2CaSO 4 (calcium langbeinite); (7) the liquidus in the ternary system consists of primary phase fields of K 2 SO 4 , MgSO 4 , CaSO 4 , langbeinite-calcium langbeinite solid solution, and CaSO 4 ·3MgSO 4 . The CaSO 4 field extends over a large portion of the system. Previously reported fields for the compounds (K 2 SO 4 ·MgSO 4 ·nCaSO 4 ), K 2 SO 4 ·3CaSO 4 and K 2 SO 4 ·CaSO 4 were not found; (8) a minimum in the ternary system at: 740°C, 25% MgSO 4 , 6% CaSO 4 , 69% K 2 SO 4 ; and ternary eutectics at 882°C, 49% MgSO 4 , 19% CaSO 4 , 32% K 2 SO 4 ; and 880°, 67·5% MgSO 4 , 5% CaSO 4 , 27·5% K 2 SO 4 .

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