Agric. Dcpt.
Issued October 30, 1909.
United States Department of Agriculture,
BUREAU OF CHEMISTRY— Circular No. 46. H. W. WILEY, Chief of Bureau.
THE OCCURRENCE OF PINENE IN LEMON OIL.
By E. M. CHACE, Chief, Food Technology Laboratory, Division of Foods.
INTRODUCTION.
In the winter and spring of 1907-8 extensive investigations were made by this Bureau in regard to the constituents of certain lemon oils imported into the United States from Sicily. The investigations made by the Bureau at that time led us to believe that the lemon oils referred to were not pure, but were adulterated either by the addition of turpentine or by some manipulation in the method of manufacture. At that time the importers made strong representations to the Bureau that the oils were absolutely genuine. They even went to the trouble and expense of sending a chemist from Messina, who made several visits to our laboratory and collaborated with our chemists and gave us the benefit of his skill. It was decided in order to settle the matter to send Mr. E. M. Chace to Sicily to investigate the method of handling the oil. Mr. Chace accordingly spent several months there making investigations and brought home samples which he could certify to be pure lemon oil. The results of his investigations fully sustain the original contentions of this Bureau.
I believe that the publication of the results of this investigation will be of great benefit not only to the people of the United States but to those of other countries importing or manufacturing lemon oil. I recommend that these results be published as Circular No. 46, Bureau of Chemistry.
Respectfullv,
H. W. WILEY,
Chief of I>ureav- Approved:
W. M. HAYS,
Acting Secretary of Agriculture.
WASHINGTON, D. C., September 15, 1909. 9965— Cir. 46—09 1
THE OCCURRENCE OF PINENE IN LEMON OIL.
In 1907, in the enforcement of the food and drugs act of June 30, 1906, this Bureau was making examinations of all consignments of lemon oil offered for importation at the custom-houses throughout the United States. Nothing unusual had been observed in these exam- inations until May of that year, when certain lots of oil were offered for entry at New York which contained substantial amounts of pinene and showed greatly abnormal physical constants. The Board of Food and Drug Inspection detained the shipments in question and requested the importers to show reason why they should not be reshipped on the ground of adulteration.
A preliminary hearing was held in New York in July and a further one requested by the importers before the Board of Food and Drug Inspection at Washington. At the latter the testimony of an Italian chemist was offered on their behalf, the question being mainly whether or not the quantity of pinene found in the oils under discussion could occur in normal oils. The expert from abroad testified that he was an inspector attached to the Chamber of Commerce at Messina, Italy, and that it was his duty, in a general wa}^, to inspect and supervise the manufacture of lemon oil; that he was thoroughly familiar with the situation with reference to the adulteration of oil and had made a study of the question of the presence of pinene in lemon oil for the past six or seven years. Pinene, according to his testimony, occurred in vary- ing quantities, sometimes not being detectable by ordinary methods, at other times being present to such an extent as to be readily detected. He had examined much of the oil at Messina that }Tear and had found pinene in almost all of it. He further stated that distilled oils entered into the final product exported from Messina to the extent of 3 or 4 per cent. It contained more pinene than hand- pressed oil, but would vary the total pinene content of the mixed oils but little. Other testimony by local chemists, and from literature, was offered to prove that pinene in considerable quantities was a normal constituent of lemon oil.
On behalf of this Bureau it was contended that while pinene was perhaps a normal constituent it did not occur in sufficient quantities to be detectable by methods using only ordinary means of distillation ; that wherever it had been reported it had been found only after
[Cir. 46] (3)
repeated distillation with special forms of apparatus, and that for some time there had been considerable discussion among experts as to whether or not it ever occurred; that besides the presence of pinene in these oils many of them were otherwise abnormal. These con- signments were confined to five importers; in fact, by far the larger part of them to one. The character of the oils had shown, during these months, a marked change; up to and including July 26 they had exhibited various other abnormalities aside from the presence of pinene. After that time, however, the physical constants became more or less normal and the amount of pinene found very much less, although con- siderable traces were always present.
A second hearing was later given by the Board of Food and Drug- Inspection, at which the Secretary of Agriculture was present, and the importers then requested that such of the importations as were held merely because they contained pinene should be released and that the whole question be investigated by the Department at the place of production. The Board finally decided to release those oils which were not greatly abnormal and to send a representative of the Depart- ment to Sicily to investigate the conditions there during the season of 1907-8. The writer went to the island of Sicily under instructions from the Chief of the Bureau of Chemistry for the purpose of making an investigation of the methods of production of essential oils and to collect authentic samples from the several districts from which data could be derived on which to base future conclusions.
THE LEMON-PRODUCING DISTRICTS.
The island of Sicily contains five, more or less, distinct lemon- producing districts, and there is also a small area on the adjacent mainland in Italy where they are grown. The lemon belt in Sicily lies along the northern and southern coast lines, never extending inland for any great distance. The most important section lies at the foothills of Mount Etna, extending from Catania on the south to Giardini on the north, and will be called the Etna district. The second district of importance is a continuation of the first, extending from Giardini on the south to Messina on the north, and is named from the latter city. Palermo, the largest city of Sicily, is the center of the third district and gives it its name. The region begins on the east at Ficarazzi and extends westward to Partinico, including the valley of the Conco D' Oro. The fourth, or Syracuse, district lies on the south side of the island, from Avola on the south to Augusta on the north. It extends farther inland than any^ of the others, is not so mountain- ous, and has more mild climatic conditions. The fifth district lies between Messina and Palermo, on the north coast. It consists of groups of orchards around individual center towns, the largest of
[Cir. 46]
5
which is Barcelona. The small mainland district of Calabria may be neglected for all practical purposes, as the output forms a very small
to
0
part of the total crop and is only interesting for the reason that the oil is made by machine instead of hand pressed.
tCir. 46]
COLLECTION OF SAMPLES.
The problem of collecting authentic samples in sufficient number to cover adequately not only the territory, but also the different periods of the season, was one of considerable difficulty. There seemed three possible ways to make satisfactory- collections: First, by purchasing the fruit and hiring workmen to produce the oil under such super- Vision as would preclude the possibility of anything but genuine samples; second, by arranging with the factories to produce, under closest personal supervision, samples of oil from the fruit which was on hand; third, by visiting the factories unannounced and requesting* samples at a stage in the manufacturing process where, beyond all reasonable doubt, no adulteration could have taken place.
It would seem, of course, that the first method was preferable to the others, but experience soon showed that it had many disadvan- tages. It was found practically impossible to hire workmen and space in which to manufacture the samples in other cities than Messina, except at excessive cost in both time and money. If either of the other methods would give the desired results they were much prefer- able on this account, and by using them it would be possible to collect two or more samples a day. If the first method were employed, the samples would average at most five or six a week, even if the oil were made at a central point. Moreover, the fruit is always somewhat damaged in shipping and very often delayed for some days, and thus abnormal oil might result. The second and third methods were open to the objection that no authentic information could be obtained rela- tive to the fruit used, although indications of abnormality might be revealed by the peel, which could always be examined. It was seldom possible, however, to have samples prepared in the factories. Owners did not care to change the routine of their work for such a purpose, and where such samples were obtained the fruit used was generally that prepared the day before. Fruit cut and worked up immediately yields a much smaller quantity of oil than that prepared in the ordi- nary way, and this fact makes the possibility of obtaining abnormal results greater. Furthermore, samples of oil taken during the pro- cess of manufacture would more nearly represent the average output of a district, as the fruit would be more thoroughly mixed, and sam- ples taken from several bowls in different parts of the pressing room would probably represent lemons from different lots purchased by the factory.
After considering all sides of the question, it was decided to carry out the following plan: First, a large number of samples were col- lected from the bowls of the factory workmen while the factory was in operation. THis assured a sample taken at a stage of the process of manufacture where intelligent adulteration would be impossible, for only very skillful sophistication can be practiced successfully by the
[Cir. 46]
producer at this point, since all the oil must undergo examination by the chemist of the purchasing broker. As such sophistication could only take place after the oil had been separated and measured, it would seem that only genuine samples would be collected in this way, unless, of course, the factory operators had been warned of the inspection and bad deliberately adulterated the oil. Since, however, the prevailing opinion among the producers was that this investigation, if fairly con- ducted, would vindicate them, a great majority of manufacturers were anxious to see that samples obtained from their places were repre- sentative and genuine beyond all possible doubt. Many insisted on drawing a sample from their storage tank in addition to the one taken from the working room in order to show that the oils were in no way different.
The factories were visited immediately upon arriving at the town in which they were situated and samples collected as soon as possible, so that the news of what was being done would have little time to spread, Close watch was kept on every move of the factory operators after arrival, and where suspicions were aroused the circumstances were noted, and the sample classed as not authentic in considering the final results. The greater part of the samples were taken in this way, the analyses of 130 of them being included in the average of bowl and authentic samples given in Table XII.
In addition to these, a considerable number of samples were col- lected which were made in factories under close personal supervision from selected peel. This method was especially followed in the north coast and Palermo districts, owing to the peculiar methods of manufac- ture employed. Fifteen samples were taken in this way, the analyses being given in Table IV under the head of authentic samples made at factories. In addition to these, nine samples were made by hired work- men in a small laboratory established for the purpose at Messina. Fruit was shipped from the Syracuse, Etna, Messina, and north coast districts and worked up in a manner excluding to an unusual degree the possibilit}r of contamination This work was done late in Decem- ber and early in January and was not repeated later on account of the length of time required and the injury caused to the fruit by shipment in small parcels. The results of the analyses of these samples are not included in the averages for the reason that they can not be discussed as fully as desired, and the average result is affected by several abnor- mal oils. All were examined for pinene, however, and the absence of that body in detectable quantities proven in every case. Whenever samples could not be obtained under conditions which seemed to jus- tify their classification as authentic, they were purchased and classed as commercial. The 33 samples thus obtained are given in Table XL
The inspection work began early in December, and a complete cir- cuit of the district was made in that and the two following months.
[Cir. 46]
8
After the 15th of March the late Dr. A. S. Cheney, then consul at Messina, continued the collection of samples until the season closed, in May. Doctor Cheney had unusual qualifications for doing this work, being himself a trained chemist, and after a very successful collection had been made his samples were forwarded to Washington and are included with the others.
METHODS OF ANALYSIS.
The same methods of examination were used in the preliminary analysis of these samples as had been used on the oils under dispute,
PKJ. 2.— Photomicrographs of crystals from lemon oil ( x 100). a, 6, Limonene nitroso chlorid crystals from lemon oil; c, limoneneand pinene nitroso chlorid crystals from a lemon oil mixed with 5 per cent of turpentine; d, Pinene nitroso chlorid crystals from turpentine.
namely: (1) Specific gravity at 15.5° C., by means of a picnometer or Sprengel tube; (2) rotation at 20° C., on a Smith and Haensch instru- ment in a water-iacketed 50 mm tube and conversion of the readings to angular degrees; (3) refractive index on an Abbe refractometer at 20° C.
[Cir. 46]
9
A 50 cc portion of the oil was then distilled as described in Schimmel & Co.'s Reports for 1898, page 41. The rotation of this distillate was determined at 20° C., and it was then tested for pinene as follows:
The distillate was mixed with an equal volume of glacial acetic acid in a 2-ounce Erlenmeyer flask and immersed in a freezing mixture. Ten cubic centimeters of ethyl nitrite were next added and finally, slowly with constant stirring, 2 cc of a mixture of two parts of con- centrated hydrochloric acid and one part of water, all previously cooled. The whole was allowed to remain fifteen minutes in the freezing bath, then rapidly filtered on a Gooch crucible provided with a filter paper disk, using vacuum. The resulting crystals of nitroso chlorid of limonene were dissolved in the smallest possible amount of chloroform and reprecipitated with methyl alcohol. After filtering off these crystals they were mounted with olive oil and examined under the microscope, using a magnification of 100. (See fig. 2.) If present, pinene nitroso chlorid is easily detected by its compara- tively broad crystals having irregular pyramidal ends, limonene nitroso chlorid crystallizing in needle shapes or columns.
The citral was determined by the fuchsin sulphite colorimetric method, which at the time of making the analyses was the most accu- rate method available. The method, in the hands of an expert manipulator, gives results within two-tenths of a per cent of the actual amount present, the error being uniformly positive.
EXPLANATION OF TABLES.
Table I contains the analyses of oils adjudged by the Bureau to be adulterated which were imported between May IT and July 26, 1907. Aside from the presence of considerable quantities of pinene, the oils are abnormal in other respects.
Table II contains the analyses of oils imported between July 30 and November IT, 1907. They were adjudged to be adulterated chiefly because of the presence of pinene, although, as is noted under 4 'Remarks" in this table, many of the oils are abnormal in other respects.
Table III contains analyses of oils imported between May 29 and October 11, 190T, which were adjudged to be unadulterated, and it was largely on these analyses that the judgment condemning the oils in Tables I and JI was based.
Table IV contains analyses of all of the authentic factory samples made as described on page T.
Table V contains analyses of the oils collected in the Syracuse dis- trict from the bowls of the workingmen, as described on page 6.
Table VI contains analyses of oils collected in the same manner in the Etna district, in which is situated the Mascali region. The oils
9965— Cir. 46—09 2
10
from this region were reported by the Italian expert as highly ab- normal.
Table VII contains analyses of oils collected in the same manner in the Messina district. The oils collected at Bauso on the north coast are included here, although their composition is more nearly like that of Barcelona and Patti oils.
Table VIII contains analyses of oils collected in the same manner in the Palermo district. Both distilled oil and oil from Bastardoni lemons are produced in this district. Presence of the latter may account for the abnormal physical constants observed in some of these samples.
Table IX contains the analyses of oils collected in the same manner in the Barcelona district. Oils from this district were also reported as abnormal and of high pinene content.
Table X contains analyses of oils collected in the same manner at Patti. The oils are similar to those of the Barcelona district.
Table XI contains samples of commercial oils collected throughout Sicily.
Table XII contains analyses of miscellaneous samples of oils which were collected on account of their general interest and the light which they throw on the question at issue.
The analytical work reported in these tables was done by Messrs. H. S. Bailey and C. O. Dodge, with the exception of the determina- tions given in Tables I, II, and III, which were made in the New York Food and Drug Inspection Laboratory by Messrs. A. F. Seeker and L. D. Havenhill.
[Cir. 46]
11
i
'c s
^
adulterated with turpentine ive index also below normal.
rac Do. Do. Do. Do. Do. Do. ssly rac Do. Do.
*
00 • &> O i-H -^ O 00 GO ••* Ol
01 cc w ci oi eo co T(! co CM
tCir. 46]
12
13
II
; : : ; :~oooooooooooooooooooooooo : : : : : gta -o -o-o-d-o-o -o-o -o-e-o-o -o-o-e-o-a •o-e-c-o-o -o _
I
a>
• o co 1-1 o CM •<»< • • 't^ • • '«o coicuni^ooo •* ^
tfiiJ^^o^otfJaJtdi-^tdottJ I - '-t^ '• '• '-X '• '• '• '• '• >^M«£W*lN «rf
e
.i^t^t^r^t^t^t^^i^FiFiFifi^-i^i-iS-iS.^.^^^^^^^^.^^^^^^ t<- _g
a
o
>COOi-l(NOSOi-l«DOOi-l
iioi>eoooi co
s
sG^C^O^CTiCiO '^ «OiCi<JiO3C^O*OT '
g"
[Cir. 46]
14
06 •
5 »o i d ui «o 10 i
o ^^
0 >> CD
re bo ^
, III
t^^ooooooooooooo
•g
.'O'O
HI4§
. . . . ..
nil!
[Cir. 46]
15
^55
i
000000000000000000000^
2
f 10
0) K-<
i-l C<1 -* Tt< t^ T-H O O> IM O 00 iH t^ CO CO <M COrH t^ r-t OJ OO rH CO t- t--
O t>- O CC
OOCOGOOO
it? o
523,
gsa Sa
-
al
• •< •< • • i-- o • i— co
d 6 « d d
:^ :q : :
24£S§§£Jdl-li<S4.dl ^
l i
02 :<^ :^PH :•<•< :5<;S : : :<<OQ'-< : JCC'&H •«! j^c»'^ j<5 |<i
[Cir. 46]
16
OOOOOOO " O > O O O * bl O O
'
co" oo'co" -^ ie" • ,-T of in !5o~iC ioo • -ir
cq^lcslCNcl<N(Ncq'N<:vl 1"1
.»O . .'O .'O'O .'C'U'O'C'O .'C'O'O .'C'd .'O'O'C . .T3 .'O'O .
^•^••^••^.••J1^'0^'
03-3 :3 : :gs ; :.a :^ :«£ :*'3<s :
S^filS^-Sie-al
'l is isl ill ig Is 11131 ill i isle iss illll
ICir. 46]
17
9
v |
o
a
*
6
«T*«g(
__s
ll .. .
e a e
OTt<O'MCO(MtDOiO(Nt^Oa»t»(MOi'»<iOO5CO?OU7it^i-lt>TT<
»a^
J«M(N
* « i ^g8j8SS^S^§§iS§ii§§§ii§§SS§ii§i§i
Ife_d
c c S *§ o n'S o c' o o o o ^ o c o c o o o p o o :"^ p.ti'o o *i or
OOP XfO'££5rO'OrOfOrOl'C"c3
tio ojo£o jo o'ooo^oo'o'oo i -r^ : Jo o o o c o o
• : : • o
\
.ropd . .'6r3 .'S .'5'o _.|6'6'Or6 _.rp _.icio ,.'6'6 .. ,
|
§
c I
I
f|s8§«S ll ^«^!«ld^sJl|slj|l| "
[Cir. 46]
18
l
5*
rt 66666666C
eo ^ oo TJ< 10 ec co •* -<i< us -^
11
-2s o
IP
[Cir. 46]
oc oo oo t- oo r-
i-C if7 »O >C »O O »O
'o^oooooc
o'0 O "^ 'C -O 73 'C 13
' '
pjA^sj^jjt .b^S
|gg^ :33 :3a5
cj S S3 S S S'-S'0. PS ^ .
ilS :
SS!
;s^
ssg
o> >S"
9|
n^ O
co o >fi as •
liisi
o ' •
5 r- i^- 1^- -f r>- 1-1
3 lO iO >C iO lO I iO )00 COOO 00 3D OO
O O O O O
j" >oooooooo ''''''''
oooooooooo <^
19
[Cir. 46]
.g.H^C
M >'o'
5*
fid
III ip
'SS'S
Isa
.
<y C
eo^eo^eo-^^-TjiTji
•M" o 10 c4 o as 06 o
tOOtOOtOidiOO
o6x>Goaoccccoooo< d
; O O O '<& O O O 1 13 "0 »0 .5
' : : : es
ec" -l
oooooooo
20
3 1
o«s.»Ma
^a^alegl "iit.stf ^•3— a-a gfSo
^cl = S^^W
Jlfgs
'SZU
*Z3
CM o o
If
I" 1
T3 • • "O
2J JJS
o S o> S^"0. S'g'^ c
;SSS2 !g^ :s
p
• [Cir. 46]
21
I 1
1 a
M
o 2
5 £ g-
fl) -0} Ci)
•— S O r--4 Pi
CL, o C^ P
a a I
r-»
flg
all sgJ
CM CM
i>- r^
"g a o*
12 SJ
CO <O
H
lO CO Oi
i 11
0
S?5^t2
GO jo
iO II iC
QO I QO
iO O
CO 00
PH fcO
X O O 0-0 T3
O
£%
n oi
* s
|| "o*j m ® 3.«
[Cir. 46]
OtH
i-KO
22
DISCUSSION OF RESULTS.
In questioning the purity of the samples reported in Tables 1 and II it would seem that the first point to be considered is the presence of pinene. It will be noted from perusal of the remainder of the tables that the other sample-s of oil imported during this period gave negative results when tested for pinene. . Absolutely no traces of it were found in the 15 authentic samples manufactured under personal supervision at the factories in Sicily, nor was it detected in the 130 samples, designated as bowl samples, from the six districts of Sicily. Moreover, of the 33 commercial samples, it was found in but one, No. 89, pur- chased at Bauso. The dealer claimed that this sample had been pro- duced the same day and had been taken from the factory to the store- room situated in another part of the town, but had not been mixed with oil held in stock. This is the only instance in which pinene was detected in the samples collected, and it would seem that the only conclusion possible to draw is that the oil had been adulterated by the dealer. This had been very skillfully done, as the sample is normal in every respect except the considerable quantities of pinene, which class it as on a par with the oils of Table I.
Of the miscellaneous samples, none was found to contain pinene. Nevertheless, four of these were distilled oils, which, according to the testimony of the Italian expert who appeared on behalf of the importers at the hearings above referred to, should be found to con- tain considerably larger quantities of pinene than the hand-pressed samples. This fact is not borne out by the analyses; for while the oils are highly abnormal in other respects, no traces of pinene were found in any of them.
Aside from the strongly positive tests for pinene, the next most striking feature of the oils of Table I are their abnormally low refract- ive indices. It will be seen from the entire average of all the sam- ples examined (Table XII) that the average for this determination is 1.4748, the minimum 1.4743, and the maximum 1.4758. For all of the oils in Table I, the refractive index is below the minimum figure in Table XII. None of them is over 1.4740, and the average is 1.4734, or 0.0009 below the lower limit for the genuine oils. The next abnormal point in the oils in Table I is the uniformly low per- centage of citral present. But two of the eleven oils have a good content of citral, and to one of these that substance was undoubtedly added, as the other data conclusivel}7 show that the sample had been grossly adulterated with turpentine, to such an extent that it could not contain 6 per cent of natural citral. It will be seen from the tables that the average percentage of citral in all of the samples exam- ined was 5.33 per cent, with a maximum of 7.03 per cent and a mini- mum of 4.07 per cent. The amount of this constituent seems to vary somewhat with the district and the season of the year in which the oil
[Cir. 46]
23
is produced. In the Messina and Syracuse districts the average citral content is slightly over 5.5 per cent, while in the Etna and Palermo districts it is but little over 5 per cent. The samples from Barcelona and Patti contain less than 5 per cent of citral, the percentage in the latter case being but slightly over 4.5.
In considering the citral content of the oils in question it should be remembered that it is not usual to export from Sicily a consignment of oil produced in one district solely, such consignments, in a great majority of cases, being made up of mixtures of oil from several districts. Three of the oils in Table I contain less than 4 per cent of citral and could have been rejected solely on this ground. A fourth oil containing 4. 1 per cent should also be classed with them. Three of the oils contained 4.7 per cent and one other 4.5 percent, which is an unu- sually low figure except for oils of the Barcelona and Patti districts.
The specific gravity of the oils, while in every case within the figures usually given for genuine oils, is uniformly high, the average of the 11 being 0.8602, compared with the entire average of 0.8577 and a maximum of 0.8606 and minimum of 0.8557, this figure being unusually uniform on the authentic samples, as the district averages show.
Considering the rotation of the oils, it will be seen that four of them would fall below 58° if determined at 20° C.° This figure does not, however, seem to be unusual in the case of oils from the Messina and Palermo districts. The entire average rotation is above 60°, while the lowest district average, that of Palermo, is 58.4°. Individual samples often show lower rotations, although in many instances explanation of their abnormal character is not wanting, as in the case of Palermo oils, where the oil from Bastardoni lemons is largely responsible for low rotations; oils produced late in the season are also often abnormal in this respect.
Turning to Table II, the chief cause of complaint against the oils is the presence of pinene. Of the 26 oils, all but 4 contain pinene in what was considered by the analyst as more than traces. With one excep- tion the refractive indices of these oils are normal and the average is approximately that of the entire average for authentic samples. The citral content is again unusual and uniformly low; three of the sam- ples having below 4 per cent could have been rejected on this abnor- mality alone. The average of the 18 samples upon which citral was determined is but 4.3 per cent. The specific gravity is again uni- formly high, the minimum figure, 0.8579, being slightly above the average of the authentic samples. Some of the samples are unusually low in rotation; in comparing these figures with those on the authentic samples, however, it is to be noted that the rotation of imported sam- ples was determined at 25° C., while that on the authentic samples was determined at 20° C., so that a correction of —1.1° should be made.
« Apply correction of —1.1° C, as determinations were made at 25° C. [Cir. 46]
24
Comparing- the oils of Tables I and II with those of Table III, which are the importations of other firms offered for entry during the same period of time, it will be seen that but two of the latter samples are abnormally low in refraction. One of these oils had not been tested for pinene, and it is possible, of course, that had this test been made it would have been included in the other tables. The second sample is but 1 point in the fourth decimal place below the mini- mum obtained on the authentic samples. The citral is uniformly much higher, but one sample falling- below 4.5 per cent, while the average is approximately that obtained on the authentic samples. The specific gravity is not uniformly so high, the average being but 5 points in the fourth decimal place above that obtained on the authentic samples.
It is not the purpose in this circular to discuss the data on the genuine samples given herewith except as it bears on the question under dis- cussion, and, indeed, it would seem that the case presented is sufficiently strong to need very little discussion. The matter will therefore be closed with a summary of the evidence submitted.
In all, there were 37 lots of oil detained at the port of New York pending the settlement of this controversy. Eleven of these oils, offered for entry between May 17 and June 26, gave very strong posi- tive tests for pinene and were otherwise abnormal. The remaining 26 lots offered for entry between July 30 and November 17, contained considerable pinene, except in four cases, where the analysts reported traces only and were otherwise abnormal.
During this same period of time 35 samples of lemon oil were offered for entry by other importers at New York, 25 of which contained no pinene, the remainder not having been tested for that substance. In practically every case these oils presented normal physical and chem- ical constants. Fifteen samples of oil manufactured under the per- sonal supervision of the writer in several districts throughout Sicily not only gave no test for pinene, but showed none of the abnormal physical constants which the oils in question gave. Analyses of 130 bowl samples are given, all of which gave negative results in the tests for pinene, and while in some cases certain of the physical constants are abnormal, the great majority of them are closely uniform and in no way present the abnormal figures obtained on the other oils under discussion. Wherever the miscellaneous samples bear on the ques- tion at issue, their testimony undoubtedly goes to prove that the oils were adulterated.
The only reasonable conclusion would seem to be that where pinene is found in lemon oil, using only ordinary means of distillation, it is prima facie proof of adulteration, whether or not the physical con- stants of the oil are abnormal.
[Cir. 46]
o
14 DAY USE
RETURN TO DESK FROM WHICH BORROWED
LOAN DEPT.
This book is due on the last date stamped below, or
on the date to which renewed. Renewed books are subject to immediate recall.
|
!OSep'63tf |
RECEIVtD |
NOV 0 2 1995
RECTD rn-RCULATI°N
-DOE
SEP 7 Q W
FEB - 8
SEP18'64-5P
JUN 13 1976
K&CW. Mr 17 7|
SUBJECT TO RECALL IMMEDIATELY
JULI0 19
FEB 01 1996
LD 21A-50m-ll,'62 (D3279slO)476B
General Library
University of California
Berkeley
1931
6*5407
U. C. BERKELEY LIBRARIES