THE PHYSICAL PKOPEPTIES OF METHYL-ALCOHOL. 511 



to lose time by a systematic elaboration of the process, we at once carried it 



out with quantities of 3-4 litres of crude spirit, and in each case adjusted the 



proportion of caustic soda according to our judgment. A so-called Papin 



digestor, as sold for the boiling of meat under pressure, served as a retort, and 



worked well. The best results, on the whole, we obtained in an operation in 



which 3 - 5 litres of crude spirit were worked up with 1400 grammes of 



powdered caustic soda. The crude product, when distilled out of a boiling 



water-bath, yielded 15 litres of a highly acetonic distillate, which was put 



aside. The residue, when distilled with 175 litres of water over a naked 



flame, yielded 19 litres of a strong methyl-alcohol, free from acetone and free 



of unpleasant odour. From their specific gravity, and assuming them to be 



aqueous methyl-alcohol, the 1*9 litres of distillate contained 1396 grammes of 



real CH 4 as against the 2354 of CH 4 which the 3*5 litres of spirit contained 



according to the iodide test. In other cases the yield was considerably less, 



no doubt through partial oxidation of the methyl-alcohol into formate or 



oxalate, 



CH 4 + NaOH = CHNa0 2 + 2H 2 

 and 



2CHNa0 2 = C 2 Na 2 4 + H 2 . 



We, of course, do not recommend the process for manufacturing purposes ; 

 but it did good service to us by placing us in possession of some 6 litres of 

 very strong and almost acetone-free methyl-alcohol. From it we prepared 

 crystallised oxalate of methyl (or rather a mixture of this ester and methyl- 

 oxalic acid) by a method which Mr Alexander Watt many years ago worked 

 out in Dr Crum Brown's laboratory, and which we will describe shortly 

 because we believe it is little known to chemists generally. 



Purified alcohol, 400 c.c. 



Oil of vitriol, 200 c.c. 



Oxalic acid crystals, 500 grammes. 



The oxalic acid is mixed with the vitriol, the spirit is then added, and the 

 whole cautiously heated over a water-bath until the oxalic acid is dissolved. 

 The liquid, on cooling and standing over night, deposits an abundant crop of 

 methylic crystals, which are collected and squeezed out in a powerful press. 



For the regeneration of the alcohol the crystals were heated with water in a 

 flask connected more directly with an inverted condenser, kept at 70° C. ; what 

 remains uncondensed there passes down a condenser, and is collected in a 

 receiver. The resulting distillate is sufficiently strong to be fit for immediate 

 treatment with carbonate of potash, which latter was applied repeatedly as long 

 as it acted visibly. 



The resulting product was dehydrated further, first by distillation over 

 quicklime, and then by distillation over baryta-lime, a quasi apology for baryta, 



