 y i | 
amy 
60" 7 REPORT OF SCHIMMEL & Co. OCTOBER 1915. 
ought to be thoroughly shaken, filled up to the mark, filtered immediately, and the 
excess of silver determined as the German Pharmacopoeia, 4‘ edition, indicates. 
According to this method, Wegener found only 82.73, 85.62 and 84.37 p.c. of the 
mustard oil used. 
Pénau') recommended to determine the excess of silver by weight as sive 
chloride, not titrimetrically by sulphocyanide solution. Wegener thus obtained 98.95 
to 100.03 p.c. in four tests. , | 
Following the indications of the Swedish Pharmacopoeia, 9t" edition”), Wegener 
found in three cases 99.54 to 100 p.c. of the mustard oil used, whereas according to 
the prescriptions of the pharmacopoeias of the United States, 8th edition, Belgium 
and Russia, 6th edition far too low values were found. 
As the result of his investigations regarding the question: In which way can the 
greatest yield of mustard oil be obtained from mustard seed and mustard seed pre- 
parations? Wehrmann states that the best yield is arrived at, and the investigation 
carried out most quickly and reliably, as follows: 5 g. of mustard powder are mixed with 
100 g. of water and left standing for 2 hours, when 20 cc. of alcohol are added and, if 
necessary, 2 cc. of olive oil. The mixture is then distilled on a water-bath, preferably 
on a glycerin-bath of 120°, a Liebig condenser being used, until 50 cc. have passed 
over into the receiver filled with 10 cc. of ammonia solution. This almost corresponds 
to what the German Pharmacopoeia recommends. 
It becomes clear from the investigations of Wehrmann and Wegener that the 
method of the 5th edition of the German Pharmacopoeia for estimating mustard oil in 
mustard powder, mustard oil, spirit of mustard and mustard paper affords very good 
results and is easily carried out. Meyer likewise thinks this method to be the best 
and the most reliable. 4 
. 
; 
a 
; 
Some years ago we studied the influence of the rate of saponification on the 
estimation of the ester value in linalyl and terpinyl acetates, as well as on bergamot 
oils to which terpinyl acetate had been added, working out a method for proving the 
presence of terpinyl acetate which is now in general use’). While investigating the 
speed of saponification of linalyl, terpiny! and geranyl acetates, C. L. Barrillet and 
R. Berthelé*) arrived at the same result as we. They saponified the esters, which had 
previously been purified by fractionation, at the temperature of the water-bath as well 
as at 15 and 0°. On boiling, the linalyl acetate was completely saponified after — 
10 minutes, terpinyl acetate only after 1 hour. It further resulted that at 15° 16.9 p.c. 
of the linalyl acetate, 1.9 p.c. of the terpinyl acetate and 71.2 p.c. of the geranyl acetate 
had been saponified. The numbers were after 4 hours: 43.1, 8.4 and 86.8; after 15 hours: 
74.4, 24.1 and 88.2, and after 48 hours: 84.2, 49.6 and 88.2 p.c., whereas after 3 hours’ 
boiling the percentages established were: 85.5, 92.1 and 88.2. Consequently, geranyl : 
acetate is the most easily saponifiable. Of terpinyl acetate, 53.5 p.c. after 3 days, 
62.7 p.c. after 4 days, 71.2 p.c. after 5 days, 77 p.c. after 6 days and 83.6 p.c. after | 
7 days were found to have been reacted upon (temperature 13 to 14°). q 
Further, mixtures of linalyl and terpinyl acetates as well as of bergamot oil with : 
terpinyl and linalyl acetates were saponified for 3 hours in the heat, and for 24 hours 
at room temperature (15 to 16°). The difference between the figures thus obtained 
corresponds to the quantities of terpinyl acetate contained in the mixtures. For pure , 
1) Journ. de Pharm. et Chim. VII. 6 (1912), 160. — 2%) Comp. Report April 1909, 102. — 3%) Reports. 
October 1910, 60; October 1911, 116. — 4) Bull. Soc. chim. IV. 17 (1915), 20. 
