Phase Formation in the Systems A(+)–Y(3+)–WO_4(2–) –H(+)–H_2O (A(+) = NH_4(+), K(+) and M(2+)–Y(3+)–WO_4(2–) –H(+)–H_2O (M(2+) = Mg(2+), Zn(2+)). Synthesis, FT-IR Spectroscopy, and Crystal Structure Determination of Salts with Paratungstate B Anion, Na2(NH4)8[W12O40(OH)2]∙12H2O and K10[W_12O_40(OH)_2]∙13H_2O
DOI:
https://doi.org/10.15330/pcss.26.2.285-295Keywords:
polyoxometalates, heteropoly tungstate, yttrium, Peacock–Weakley type of structure, paratungstate B anion, scanning electron microscopy, single-crystal X-ray diffraction, synthesisAbstract
A new procedure for the synthesis of sodium heteropoly decatungstoyttriate(III) Na9[Y(W5O18)2]·35H2O (I) from an aqueous solution of sodium tungstate, acidified to Z = ν(H+)/ν(WO42–) = 0.80 with ratio of ν(Y):ν(W) = 1:10 and with 2-propanone adding, has been developed. The presence of the Peacock–Weakley type anion in the obtained salt has been confirmed by FTIR spectroscopy. The micromorphology of the surface was studied using scanning electron microscopy (SEM); it was found that the grain size of (I) is in the range of 200–450 nm. The single-phase nature of the synthesized salt was confirmed by the uniform contrast of the surface in the backscattered electron mode.
The conditions for the synthesis of salts with the paratungstate B anion Na2(NH4)8[W12O40(OH)2]∙12H2O (II), K10[W12O40(OH)2]∙13H2O (III), and M5[W12O40(OH)2]∙nH2O (M2+ = Mg2+ (IV), and Zn2+ (V)) from acidified with Z = 0.80 aqueous solutions of the systems A+–Y3+–WO42––H+–H2O (A = NH4+, K+) and M2+–Y3+–WO42––H+–H2O (M2+ = Mg2+, Zn2+) have been established. Elemental analysis, SEM, and FTIR spectroscopy characterized the obtained salts.
The crystal structure of Na2(NH4)8[W12O40(OH)2]∙12H2O (II) (Mr = 3286.72, orthorhombic, Pbca, a = 14.0631(6) Å, b = 15.6713(5) Å, c = 22.9147(16) Å, V = 5050.1(4) Å3 at T = 200(2) K, Z = 4, dcalcd = 4.323 g/cm3) and К10[W12O40(OH)2]∙13H2O (III) (Mr = 3489.42, monoclinic, P21/c, a = 11.5049(6) Å, b = 14.3008(7) Å, c = 15.4567(10) Å, β = 105.889(7)°, V = 2445.9(2) Å3 at T = 293(2) K, Z = 2, dcalcd = 4.738 g/сm3) was determined by single crystal X-ray analysis.
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