Hydrothermal synthesis and structural characterization of framework microporous mixed tin-zirconium silicates with the structure of umbite

Inorganic Chemistry Communications

Volumn 5, Issue 10, 2002, Pages 824-828

  Pertierra, Pilar ^a   Salvadó, Miguel A ^a   García Granda, Santiago ^a   Bortun, Anatoly I ^b   Khainakov, Sergei A ^a   García, José R ^a  

^a UNIVERSITY OF OVIEDO   (Spain)

^b Magnesium Elektron Ltd   (United States)

Author keywords

Crystal structure; Hydrothermal synthesis; Microporous materials; Silicates

Indexed keywords

MINERAL; POTASSIUM ION; SILICON DERIVATIVE; SODIUM ION; TIN DERIVATIVE; UMBITE; UNCLASSIFIED DRUG; ZIRCONIUM DERIVATIVE;

ARTICLE; CHEMICAL ANALYSIS; CRYSTAL STRUCTURE; POROSITY; STRUCTURE ANALYSIS; SYNTHESIS;

EID: 0036826466     PISSN: 13877003     EISSN: None     Source Type: Journal    
DOI: 10.1016/S1387-7003(02)00574-9     Document Type: Article

References (16)

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13. -1, flow of nitrogen) shows a total weight loss up to 800 °C of 4.4% (calcd. 4.26%).
14. 2O with a 2 M NaCl solution (V:m = 200 ml:1 g, contact time 2 h) under static condition and ambient temperature. Ion exchange was controlled by periodic elemental analysis of the solid. Addition of flesh portions of NaCl solution was discontinued when >96% substitution was achieved. The solid obtained was filtered off, washed with an excess of distilled water and dried in air at 70-80 °C. Elemental analysis (wt%): Na 11.4, Sn 7.7, Zr 17.5, Si 21.3 (calcd. Na 11.78, Sn 7.60, Zr 17.53, Si 21.59). Weight loss up to 800 °C of 4.9% (calcd. 4.61%).
15. 2O [9] with Zr/Sn occupancies fixed from analytical values. Refinement was carried out with the FULLPROF program [see J. RodríguezCarvajal, In Collected Abstracts of Powder Diffraction Meetings, Toulouse, France, 1990, p. 127]. The quality of the refinements was somewhat limited by the presence of severe peak broadening. A Thompson-Cox-Hastings function was used to describe the peak shape, including isotropic size/strain and anisotropic size broadening effects. Soft constraints were applied for the bond distances M-O 2.06(2) Å (M = 75% Zr, 25% Sn) and Si-O 1.61(1) Å, calculated from the Shannon ionic radii [16]. For 1, all the atoms were refined with an isotropic overall temperature factor, B = 0.42(8). For 2, the temperature factor of each discrete atom type was refined. In the latter stages of refinement, Zr/Sn occupancies were allowed to refine, but these do not vary significantly from the departure values. Fig. 2 shows the powder X-ray diffraction patterns and the difference between the calculated patterns, including the interpolated backgrounds, and the observed patterns. Crystallographic parameters are presented in Table 1. Final atomic coordinates, isotropic displacement parameters, bond distances and angles are reported in Tables 2-5. A projection of the structure along the c-axis is shown in Fig. 3.
16. R.D. Shannon, Acta Crystallogr. A 32 (1976) 751.