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By Dr. J. K. GLADSTONE,Ph.D., F.R.S

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By Dr. J. K. GLADSTONE,Ph.D., F.R.S View Article Online / Journal Homepage / Table of Contents for this issue GLADSTONE ON PYROPHOSPHORIC ACID. 435 Published on 01 January 1867. Downloaded by University of Windsor 22/10/2014 03:36:55. XL.- On Pyropl~osphoricAcid. By Dr. J. K. GLADSTONE,Ph.D., F.R.S. IN the classic research of Graham, pyrophosphoric acid was viewed as a bibasic acid, having the conetitution 2H0.P05; but under the present view, that the atomic weight of oxygen is 16, we are compelled to recognize in it the exktence of two atoms of phosphorus, and to assign to it the formula 2H,O.P2O,, or’rather P,H,O,. This makes it a quadribasic acid, and that * Chem. SOC.Jour., six, 238. 2n2 View Article Online 436 GLADSTONE ON PYROPHOSPHORIO ACID. it actually is such, is indicated by its giving some double salts, in which the two metaJs exist in the proportion of 3 atoms of the one to 1 atom of the other. A still better proof of the above formula may be found in the fkt that amides of pyro- phosphoric acid exist., in which 1, 2, and 3 molecules of HO are replaced by NH,. It is my intention to treat in this paper of-1st. Some normal pyrophosphates ; 2ndly. An allotropic modification of these salts ; and, 3rdly, the formation of pyrophosphoric acid, and the theory of its constitution. Normal Salts. If solutions of a silver-salt and of pyrophosphate of eodium be mixed in any proportion, a permanent white precipitate is the result ; but if a solution of ferric chloride be added in small quantity to a solution of pyrophosphate of sodium, the white precipitate, produced at the moment of contact, dissolves in the excess of sodium-salt. If more ferric chloride be added, a per- manent, flocculent precipitate is obtained, If the addition be continued, the solid gyrophosphate is again dissolved, but now by the excess of ferric salt. On performing this experiment with solutions of known strength, it was found that the pyrophosphate of sodium con- tinued to dissolve the iron-salt, till the proportion of two atoms of ferric chloride, feC1," to one of pyrophosphate of' sodium, P2Na4O7,was arrived at ; then, the permanent precipitate in- Published on 01 January 1867. Downloaded by University of Windsor 22/10/2014 03:36:55. creased, with a milky appearance, until the proportion became four to one, at which time no more iron was found in solution, and the ferric salt' separated readily in flocculent masges. To dissolve this up again, many atoms of ferric chloride were found to be necessary. This suggests the existence of a soluble double salt, P2Na,fe20, ; and an insoluble normal pyrophosphate, P,fe,O,. Schwarzenbergt, long ago, gave the above, plus 3 atoms of water, as the composition of ferric pyrophosphate, and the following analysea confirm the conclusion :- I. 0.330 grrn., dried at loo* C., and heated to low redness, it To avoid great complexity of formulEe, I have adopted Williamson's fenicum with the atomic weight 18'66, and the symbol fe. t Ann. Ch. Pharm., lxv, 163. View Article Online GLADSTONE ON PYROPHOSPHORIC ACID. 437 gave off water, losing 0.058 grm. The residue boiled long with hydrochloric acid, and precipitated by magnesium-salt in the presence of citric acid, gave 0-234 grm. of pyrophosphate of magnesium. 11. 0.349 grm. gave 0.245 of pyrophosphate of magnesium. Calculated. Found. I. IT. 20.48 19.78 19.60 Phomhorus4 ........ Iron.. .............. 24.65 - - Oxygen ............ 37.03 - - Water ............. --17.84 17-57 100~00 The supposed double salt, P2Na,fe,07, being in solution, and &xed with chloride of aodium, a.nd, possibly, other combina- tions, could not be satisfactorily examined. An attempt wa8 made to separate it by dialysk. It was soon evident that the double salt remained in the dialyser, while the chloride of sodium passed through ; but when the chlorine had practically disap- peared, the salt partially gelatinized. The whole contents of the dialyser were, nevertheless, evaporated down, and the phos- phorus, iron, and water were estimated. There wa8 also a considerable amount of sodium, which could be determined by difference; but the numbers obtained did not agree well with the above formula. In the reaction8 described above, have spoken of ferric Published on 01 January 1867. Downloaded by University of Windsor 22/10/2014 03:36:55. I chloride and pyrophosphate of sodium, but the iron may be combined with other acids, or potassium may be substituted for the other alkali, without affecting the results. If a cupric salt be mixed with a soluble pyrophosphate, the precipitate first produced dissolves in excess of the phosphorus- compound, giving a deep-blue solution. On the further addi- tion of copper, a permanent green salt separates, which was found, on analysis, to be the normal pyrophosphate, P2Cu,07, combined with two atoms of water. I. 0.359 grm., dried at looo C., and heated to low redneas, gave off water, and lost 0.041 grm. The residue was boiled long with hydrochloric acid, and gave 0.238 pyrophosphate of magnesium. The copper had previously been separated by hydroaulphuric acid, and yielded 0.170 grm. of oxide, View Article Online 438 GLADSTONE ON PYROPHOSPHORIC ACID. 11. 0.344 grm. lost 0-038 grm. when hea€ed. 111. 0.378 gm. of a different preparation, lost 0941 p. when heated, and gave 0.230 grm. of pyrophosphate of mag- nesium, and 0.177 grm. of oxide of copper. These numbers indicate the composition P,Cu40,.2E,0. Calculated. Found, I. JI. 111. Phosphorus 18.43 18.51 7 18-47 Copper,. 37.57 37.78 - 37.36 Oxygen .. 33-29 - - -. Water . , . 10.71 11.42 11.04 lOd34 100.03 An attempt was made to isolate the doubIe pyrophosphate of copper and sodium by dialysis, but it Famed through the parch- ment paper about as readily as the sulphate of sodium did. Excess of pyrophosphate of sodium is also capable of dis- solving the precipitates produced by it with mercurous, ferrow, zinc, aluminium, and lead salt,s, but apparently not those with mercuric or chromic salts* These compounds are capable of being decomposed by free acids; 60 that, on the addition of a little sulphuric acid, for instance, to the sodio-ferric salt, the complete ferric pyrophosphate Reparates. Allotropic Xatts. Published on 01 January 1867. Downloaded by University of Windsor 22/10/2014 03:36:55. Many of these metallic pyrophoaphates are capable of existing in a different condition. Thus, the ferric salt already described is very soluble in acida. A few drops of sulphuric acid will dissolve a considerable quantity ; but if this solution be heated, it becomes turbid, and a white flocculent salt makelit its appearance, which is just like the original ferric compound, but no longer soluble either in pyrophosphate of sodium, ferric chloride, or dilute acids. Like the normal salt, however, it is easily dis- solved by ammonia. Analysis showed that this salt has the =me ultimate compo- sition as that from which it is prepared, namely, P2fe,0,.3H,0. I. 0.377 grm., dried at looo C., lost 0.065 grm. when strongly heated, and gave 0.277 grin. of pyrophosphate of magnesium. View Article Online GLADSTONE ON PYROPHOSPHORIC ACID. 439 11. 0.320 grm. gave 0.232 grm. of pyrophosphate of mag- nesium. 111. 0.255 grm. lost 0-044 grm. when strongly heated. IV. 0.200 grm. gave 0.071 grm. of ferric oxide. Calculated, Found. I. 11. 111. IV. PhorJpkrcrus 20.48 20.51 20.24 - - Iron .. .. 24.65 - - - 24.85 Oxygen.. 37-03 - - - - Water . 17-84 17.24 I 17.25 c -- 100~00 Other aci& may be used in the place of sulphuric acid to effect this change, but free acid is necessary. The normal salt may be boiled with water for a couple of hours without altera- tion, nor does the presence of neutral salts appear to have any effect. The temperature at which this allotropic salt forms depends upon the comparative amount of the different sub- stances present. If the acid and water be nearly saturated with the ferric compound, a temperature of 30" or 40" C. suf- fices. A means of testing for pyrophosphoric acid may be founded on this property. If the presence of that acid be suspected in a neutral solution, it is only necessary to add a drop or two of an iron-salt, sufficient sulphuric acid just to dissolve the pre- Published on 01 January 1867. Downloaded by University of Windsor 22/10/2014 03:36:55. cipitate, if any, and boil. The allotropic salt will reveal itself by a cloudiness appearing first in the warmer currents, and then extending itself a13 a gelatinous or flocculent white pre- cipitate throughout'the whole liquid. If it is necessary to employ acid in order to dissolve the substance to be tested, cold aulphuiic acid should be employed in as small a quantity as possible. An allotropic pyrophosphate of copper may be prepared in a way precisely analogous to that given above for the ferric salt. The following analyses confirm its formula as P,Cu,O,. 2H,O :- I. 0.407 grm., dried at 100°C., lost 0.044 grm. when strongly heated, and gave 0.193 of oxide of copper, and 0.269 of pyro- phosphate of magnesium. View Article Online 440 GLADSTONE ON PYROPHOSPHORIC ACID. Calculated. Found. Phosphorus ............ 18-43 18.45 Copper.. .............. 37-53 37-84 Oxygen .............. 33.29 - Water ................ 10.71 10.81 1oo*oo SimiIar precipitates are obtained when solutions of ferrous or zinc pyrophogphate in dilute sulphnric acid are heated, but the lead, chromium, and mercurous salts did not give precipitates under such circumstances.
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