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PDFOUTLINE SCHEME FOR THE ANALYSIS OF NITRO-EXPLOSIVES ____________________________________________________________
___________ | | | Exhaust dried substance with Anhydrous Ether in Soxhlet’s Fat | | Extraction Apparatus. | |___________________________________________________________
____________| | | | Solution--Divide into two parts A. and B. | |___________________________________________________________
____________| | | | A. | | | | Allow ether to evaporate spontaneously. Dry residue in vacuo over | | H_{2}SO_{4} and weigh. Equals nitro-glycerine, resin, camphor, and | | paraffin. | | | | The nitro-glycerine in this residue may be decomposed by heating | | with a solution of alcoholic potash. Water may then be added, and the | | alcohol evaporated off on the water bath. From this solution the | | resin may be precipitated by HCl, filtered off, dried, and weighed. | | Solution containing the paraffin is treated with AmS solution and | | heated. On cooling the paraffin separates, and may be separated. | | Residue may be shaken with CS_{2} to remove camphor. | |___________________________________________________________
____________| | | | B. | | | | Add phenol-phthalein and titrate with alcoholic potash, 1 c.c. normal | | KHO = .330 grm. resin, and add considerably more KHO. Evaporate, | | dissolve residue in water, shake with ether, and separate. | |___________________________________________________________
____________| | | | Ethereal Solution evaporated leaves paraffin. | |___________________________________________________________
____________| | | | Aqueous Solution-- | | Add bromide, acidify with HCl, separate any resin and precipitate, | | filtrate with BaCl_{2} BaSO_{4} x .1373 = Sulphur. | |___________________________________________________________
____________| | | | Residue-- |
