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The orange solid  that  remained was  dissolved  in 50 ml of  water, concentrated to the first  appearance of  crystals  in a vacuum  desiccator over concentrated sulfuric acid, and then allowed to crystallize  further. The orange  crystals  that  formed  were  filtered, washed  with  water,  and  air  dried. The yield was 28 g. The crystalline acid effloresces slowly at room temperature; thus the amount of water of crystallization varied slightly from sample to sample.  Anal. Calcd for H4[PMo11VO40]32.5H20: P, 1.31; Mo,44.60; V, 2.15; H20,24.71.  Found:  P, 1.31; Mo, 44.54; V, 2.68; H2O (based on Mo), 24.86. The molar ratios are Mo to P, 10.97 to 1.00; and V to P, 1.24 to 1.00.  Similar analyses were All other reagents used were Baker Analyzed grade.
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