Tripotassium Trimetaphosphimate

The x-ray powder diffraction patterns are available for comparison.5 For the trimer, absence of a line at d = 7.63 A. can be interpreted as absence of the tetramer for the tetramer, absence of a line at d = 5.66 A. shows absence of the trimer. 

Submitted by Morris L. Nielsen and T. J. Morrow Checked bt Oscar T. QuiMBYf 

In a 1-1. flask fitted with a stirrer is placed a solution of 60 g. of trimeric phosphonitrile chloride in 240 ml. of diox-ane and a solution of 300 g. of potassium acetate in 300 ml. of water. The temperature is held at 45 to 55°, cooling at first with a cold-water bath, later heating with a heating 

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To an ice-cold solution of 35.1 g. (0.1 mol) of tripotassium trimetaphosphimate in 95 ml. of water is added, slowly, 62 ml. of 72% perchloric acid so that the temperature does not exceed 25°. The potassium perchlorate is filtered off and washed with 15 ml. of 5% perchloric acid. The combined filtrates are transferred to a 200-ml. round-bottomed flask and evaporated at reduced pressure. A Dry Ice trap and potassium hydroxide pellets are used before the oil pump. The solution is stirred with a magnetic stirring bar and is heated in a water bath at not over 31°. When nearly but not quite dry, the solids are slurried in ethyl acetate-methanol (80/20 by volume) to remove any crystallized potassium perchlorate, transferred to a Buchner funnel and rinsed, using a total of 125 ml. of the above solvent, then... 

Ps06(NH)3K3 Tripotassium tri-metaphosphimate, 6 97 Pa06(NH)3Na8 Trisodium tri-metaphosphimate, 1-hydrate, 6 99 4-hydrate, 6 105 P,0 (NH)3Na,NaOH-7H20 Trisodium trimetaphosphimate, 6 80... 

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