1915] Charles J. Robinson and J. Howard Mueller 107 



out, washed with alcohol and ether, and dried. After securing 

 second and third crops of crystals, all were united and recrystallized 

 in the same way. After drying in a water-oven for some time at 

 100° C, the product, weighing about 7 gm., was a light, powdery 

 material. Part of this was dried at 105° C, in vacuum over phos- 

 phorus pentoxid, and analyzed. Analytic data : 



0.1400 gm. gave 0.0860 gm. MgaPsOi. 



0.1596 gm. gave o.iooi gm. BaSO«. 



0.2275 gm. gave 0.0575 gm. COo and 0.0399 gm. HjO. 

 Found: F, 17.12%; Ba, 37-77% ; C, 6.89% ; H, 1.96%. 



Calculated: for CeHisOiiPeBaj — 



P, 17-35% ; Ba, 38.43% ; C, 6.72% ; H, 1.69%. 



Preparation of the free acid from the crystallized material. The 

 entire amount of the crystalline material remaining, a little less 

 than 7 gm., was decomposed as follows. Somewhat more than the 

 calculated amount of normal sulfuric acid sol. was added to pre- 

 cipitate the barium and, af ter warming for some time, the liquid was 

 filtered. To this was added an excess of copper acetate sol, and 

 the precipitate filtered out and washed thoroughly with water. It 

 was finally suspended in water, and decomposed with hydrogen 

 Sulfid gas. After filtering from the copper sulfid, the liquid con- 

 taining phytic acid was concentrated to a small bulk by boiling in 

 vacuum, the temperature not rising above 65° C. The residue was 

 finally dried for ten days in vacuum over sulfuric acid at room 

 temperature. The residue, weighing about 3 gm., was a very thick, 

 amber colored syrup. For analysis a portion of it was dried at 

 105° C. in vacuum over phosphorus pentoxid. Analytic data: 



0.1208 gm. gave 0.1199 gm. MgjPoOr. 



0.2893 gm. gave 0.1156 gm. CO2 and 0.0917 gm. HjO. 

 Found: P, 27.67% ; Q 10.90% ; H, 3-54%. 



Calculated: for QH^^OsiP« — 



P, 27.92%; C, 10.81%; H, 3.63%. 



Calculated: for QHisOjiPs — 



P, 28.18% ; Q 10.90% ; H, 2.73%- 



Drying at 105° C. caused blackening, and, presumably, partial 

 decomposition of the material. Anderson^ ° shows, in the case of 

 10 Anderson : Jour. Biol. Chem., 1914, xvü, p. 171. 



