- 92 - | 



The complaints which have made themselves heard of late years with 

 regard to the deficient ester -content of petitgrain oil 1 ) appear to have 

 resulted in unscrupulous suppliers attempting to make good this deficiency 

 by the addition of terpinyl acetate, a practice which so far we had not 

 observed in the case of petitgrain oil. Lately two samples of oil thus 

 adulterated have been examined in our laboratory, and in the subjoined 

 table we quote these, together with two other oils which had also been 

 sophisticated, but in a different manner. 



Of the two samples which had been doctored with terpinyl acetate 

 (Nos. 1 and 2) the first shows a somewhat excessive specific gravity, but 

 for the rest it gives, as does No. 2, the analytical values of pure petit- 

 grain oils, and only fractional saponification made it possible to conclude 

 that it was adulterated. As the oils, when rectified with steam, showed 

 as great differences as did the original oils, the addition of the ester in 

 question was established. As determined by us from mixtures of known 

 composition (comp. Report October 1911, 116) this addition amounted to 

 from 9 to 12 p. c. An attempt to separate, by fractional distillation in 

 vacuo, the terpinyl acetate from 1 kilo of sample No. 2, in which the 

 addition was readily ascertainable from the odour, was unfortunately not 

 attended by the desired result, because at a pressure of 3 to 4 mm. the 

 boiling points of terpinyl acetate and of the esters which are naturally 

 present in petitgrain oil lie very closely together. Hence even repeated 

 fractionation was only able to establish the fact that the fractions in 

 question had been enriched with terpinyl acetate, although the addition 

 was considerable. 



The sample mentioned under No. 3 possessed normal constants, and 

 upon fractional saponification it showed a difference which was only 

 slightly greater than in normal oils, but on the other hand the difference 

 between acid v. II and the saponification value was 8,9, which indicated 

 adulteration with an ester of a sparingly-volatile acid. Further examination 

 established the fact that the oil contained several per cent, of a fatty oil, 

 for after distillation with steam the saponification value and the acid 

 value II agreed, from which it followed that the non-volatile acid must be 

 contained in the distillation-residue in the form of an ester. This residue 

 of 5,7 p. c. was liquid, insoluble in alcohol, and had sap. v. 172,2. 



Sample No. 4 was obviously also adulterated, inasmuch as its opt. rot. 

 ( — 12°) was altogether abnormal, its ester content was only 29,4 p. c. and 

 it was insoluble in alcohol of less than 90 p. c. But the quantity of oil 

 submitted to us was too small to permit of a more thorough investigation , 

 and it was therefore impossible to establish the cause of these abnormities. 



Pimento Oil has been maintained in price, for there have been but 

 few opportunities of securing cheap and suitable raw material. 



x ) Report October 1910, 106. 



