Nitro-Explosives: A Practical Treatise eBook

This eBook from the Gutenberg Project consists of approximately 310 pages of information about Nitro-Explosives.

Nitro-Explosives: A Practical Treatise eBook

This eBook from the Gutenberg Project consists of approximately 310 pages of information about Nitro-Explosives.

[Footnote A:  Organic matter up to .6 per cent. is not always prejudicial to the nitrating quantities of a glycerine.]

Silver Test. A portion of the sample of glycerine to be tested should be put in a small weighing bottle, and a quarter of its bulk of N/10 silver nitrate solution added to it, then shake it, and place in a dark cupboard for fifteen minutes.  It must be pronounced bad if it becomes black or dark brown within that time (acrolein, formic, and butyric acids).

The German official test for glycerine for pharmaceutical purposes is much more stringent, 1 c.c. of glycerine heated to boiling with 1 c.c. of ammonia solution and three drops of silver nitrate solution must give neither colour or precipitate within five minutes.

Nitration. Fifty grms. of the glycerine are poured from a beaker into a mixture of concentrated nitric acid (specific gravity 1.53) and sulphuric acid (1.84), mixed in the proportions of 3 HNO_{3} to 5 H_{2}SO_{4} (about 400 c.c. of mixed acids).  The mixed acids should be put into a rather large beaker, and held in the right hand in a basin of water, and the glycerine slowly poured into them from a smaller one held in the left.  A constant rotatory motion should be given to the beaker in which the nitration is performed.  When all the glycerine has been added, and the mixture has been shaken for a few minutes longer, it is poured into a separator, and allowed to stand for some time.  It should, if the glycerine is a good one, have separated from the mixed acids in ten minutes, and the line of demarcation between the nitro-glycerine and the acid should be clear and sharp, neither should there be any white flocculent matter suspended in the liquid.  The excess of acids is now drawn off, and the nitro-glycerine shaken once or twice with a warm solution of carbonate of soda, and afterwards with water alone.  The nitro-glycerine is then drawn off into a weighed beaker, the surface dried with a piece of filter paper, and weighed; 100 parts of a good glycerine should yield about 230 of nitro-glycerine.  A quicker method is to take only 10 c.c. of the glycerine, of which the specific gravity is already known, nitrate as before, and pour into a burette, read off the volume of nitro-glycerine in c.c. and multiply them by 1.6 (the specific gravity of nitro-glycerine), thus:  10 grms. gave 14.5 c.c. nitro-glycerine, and 14.5 x 1.6 = 23.2 grms., therefore 100 would give 232 grms. nitro-glycerine.  The points to be noted in the nitration of a sample of glycerine are:  the separation should be sharp, and within half an hour or less, and there should be no white flocculent matter formed, especially when the carbonate of soda solution is added.

Total Acid Equivalent. Mr G.E.  Barton (Jour.  Amer.  Chem.  Soc., 1895) proposes to determine thus:  100 c.c. of glycerine are diluted to 300 c.c. in a beaker, a few drops of a 1 per cent. solution of phenolphthalein and 10 c.c. of normal caustic soda solution are added; after boiling, the liquid is titrated with normal hydrochloric acid (fatty acids are thus indicated and roughly determined).

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