X 560 ■04l6 J U. S. DEPARTMENT OF AGRICULTURE. BUREAU OF CHEMISTRY -BULLETIN NO. 77 H. W. WILEY, CliicC of Bureau. OLIVE OIL AND ITS SUBSTITUTES. L. M. TOLMAN and L. S. MUNSON. Prepared under tlie direction of W. D. BIGELOW, Cliit'f of Food L'lhoriitorii. WASHINGTON: GOVERNMENT PRINTING OFFICl 1905. Monograph Class T X R (^ D Book^_Q^T6 1 i I /i.^ U. S. DEPARTMENT OF AGRICULTURE. BUREAU OF CHEMISTRY— BULLETIN NO. 77. II. W. WILEY, Chief of Bureau. OLIVE OIL AND ITS .SUBSTITUTES. L. M. TOLMAN and L S. MUNSON. Prepared under the direction of "W. D. BIGELOW, CliiiJ' (if Food L'lhoratorij. WASHINGTON: GOVERNMENT PRINTING OFFICE. 1905. "^ -1^ \ LETTER OF TRANSMITTAL U. S. Department of Agriculture, Bureau of Chemistry, WmJilngton, D. C, .My 3, 1903. Sir: I have the honor to tninsmit herewith for yoiir inspection and approval a manuscript relating to olive oils and their adulterations, and embodying the investigations made in this Bureau of American and imported pure olive oils and adulterations thereof. This work was done under the act of Congress authorizing the Secretary of Agri- culture "'to investigate the adulteration of foods, drugs, and liquors,'' and I recommend that the results as reported herein be published as Bulletin No. Y7 of the Bureau of Chemistry. Respectfullj% Hon. James Wilson, Secretary of Agriculture. H. W. Wiley, Chief of Bureau. SAN PI r- D. otD. INTRODUCTION. The work reported in this liulletin was begun on imported oils received throug-h the customs officers, with a vieM' to determinino- the nature of the products brought into the United States from abroad and sold as olive oil. It was then thought advisable to go into the open market and secure oils sold in retail stores under foreign labels in order to make a comparison of olive oil as it is received by the cus- toms officers and as it is sold to the consumer. Having thus collected considerable data on oils of otlier countries, it seemed expedient to make a study of American olive oils for the sake of comparison. Many samples were therefore purchased in the open market, and a number of representative manufacturers were requested to furnish samples of their product as it left the mill. These requests were quite generally complied with, and in each case the manufacturer sent with his sample an affidavit as to its purity. Employees of the Bureau visited New York, Philadelphia, Washington, Boston, New Haven, Rochester, Buffalo, Burlington, Vt., New Orleans, Chicago, St. Louis, and San Francisco, and purchased both American and foreign oils found in as man}' stores, selected at random, as it .seemed advisable to visit. The relatively low price at which imported oils are sold as compared with California oils may often be attributed to their inferior quality. In selecting material for the work reported in this bulletin no .sam- ples were taken which wei'e not sold as olive oil. Oils sold under other names, or simply as salad oil, were not included. It is a matter especially worthy of comment that the California oils bought in the open market were all of superior (luality, and that only two of the fifteen samples so obtained contained any oil other than olive oil. Of these two samples one was not labeled with the name of the manufac- turer, but instead l)ore the name of the dealer. Following the usual custom in such matters, all manufacturers resi- dent in the United States were notified of the results of the examina- tion previous to their publication, and no protests were received except those relating to the two oils mentioned. The dealer from whom one of these samples was obtained- replied that he supposed that he was handling a high-grade article, while the manufacturers of the other sample wrote us that they had ceased to make olive oil because, 4 INTRODUCTION. while making a high-grade article, they could not compete with infe- rior goods which were sold under the labels of iirst-class olive oil, and had decided to discontinue its manufacture. They sta,ted that they employed no cotton-seed oil or other substitute at any time. Dealers whose names appeared on the labels as importers or manufacturers' agents were also notified. For the lack of a better term, a number of salad oils are referred to in this bulletin as "olive oil substitutes." By this it is not intended to class them as inferior in any sense, or to disparage their legitimate use or their sale when labeled in such a way as to notify the purchaser of their nature. They are included in this bulletin, however, merely because, being cheaper oils, they are sometimes fraudulently substi- tuted for olive oil and sold either at a price above their relative value, or at a price whicii brings olive oil into unfair competition. Such practices are fraudulent, and it is highly important for those engaged in the manufacture of olive oil, which has become an important indus- trj- in California, that they be forbidden. Two Federal laws were passed by the last Congress which have a bearing on this subject. One of these (Public — No. 223) forbids the misbranding or false labeling of food products as to the place of their manufacture. The other (Public^7-No. 158) prohibits the importation into the United Stsites of foods which are "found to be dangerous to health, or which are forbidden to be sold or restricted in sale in coun- tries in which they are made or from which they are exported, or which shall be falsely labeled in any respect in regard to the place of manufacture or the contents of the package. "" With these laws on the statute books it becomes important that pur- chasers should carefully read the labels on their purchases and note that the name of the manufacturer and the place of manufacture are distinctly stated. It is altogether probable that in the future oils dis- tinctly labeled will l)e found to be as represented, as ordinaiily fraudu- lent manufacturers will attempt to evade the law by omitting the place cf manufacture rather than violate the law by making a false state- ment regarding it. As an illustration of this a label is reproduced (PI. 1, fig. 1) which was found on a bottle of maize oil puichased as olive oil. This label does not distinctly state that the t)ottlc contains olive oil, but it is worded in such a waj* that it is oidy upon close examination that the purchaser will note the fact that the oil is I'epre- sented not as '"supei'lor olive t)il," but as "superior to any olive (jil."' Among other instances of misbranded oil are a number which bear French or Italian laltels and contain cotton-seed oil. As illustrations of this two labels are reproduced (PI. J, fig. 2, and PI. II. fig. 2) which are believed to have originated in this country." The prevalence of the sale of cotton-seed oil under labels of this nature has led to frequent "See page 56." INTRODUCTION. rumors that the cotton-seed oil exported from the United States is largely used as an adulterant or substitute for olive oil, and is sentliack to us under another label and at greatly increased prices. It is difficult to understand how this idea could have gained credence. The ship- ment of the oil twice across the ocean would seem a needless expense. Oils of American origin are never subjected to a more rigid examina- tion tliun imi^orted oils. In view of these facts we would expect even foreign manufacturers to establish mixing and bottling establishments here, if they desire to handle American oil, and conline their impt)rtii- tion to the labels. In the following pages several instances of the presence of cheaper oils imported as olive oil are noted, but not a single instance has been found of the use of cotton-seed oil as an adulterant or substitute for olive oil in goods known to be imported," although samples of imported olive oil were obtained from the customs officei-s of several of our leading ports, and everj^ effort was made to secure a fair representa- tion of the oils imported. We are therefore brought to the conclu- sion that cotton-seexl oil is not imported under olive oil labels, as is frequently stated. Since the completion of our work on this subject this idea has been confirmed by a report from Consul-General 11. P. Skinner, as a result of his inv^estigation of the manufacture of olive oil in France. Mr. Skinner calls attention to the fact that edible olive oil to the value of $1,200,000 is brought annually into the United States, and that Marseilles alone has sometimes imported $3,000,(100 worth of cotton oil in a single year. Mr. Skinner then says: "There- fore, if we also assume, a most improbable hypothesis, that these oils contain 25 per cent of cotton oil, we have accounted for cotton oil to the value of merely $300,000, a mere drop in the bucket as com- pared with the value of our cotton-oil exports." Another form of fraud is illustrated in Plate II, tig. 1, which is a reproduction of a label on a bottle received from the appraiser's stoi-es imported as olive oil, hut containing peanut oil. I take this opportunity to express our indebtedness to all the Ameri- can manufacturers who have cooperated in this work by furnishing the laboratory with samples of their oil, accompanied by affidavits as to their purity and descriptions of tlieir methods of manufacture; and also to V. Villavecchia, custom-house chemist, Rome; Giacomo Dellepiane fu Andrea, Genoa; G. E. Colby and W. C. Blasdale, of the University of California, Berkelej', Cal., who have supplied samples of olive oil of known purity from different regions, and the V. D. Anderson Com- pany, who prepared several samples of olive-oil substitutes for our laboratory. W. D. BiGELOW, Chief of J^ood Laboratory. o Nine samples out of 250 recently received from the custom-house have contained cotton-seed oil. CONTENTS. Page. Introduction 3 General discussion 9 Statistics of the olive oil trade 9 Manufacture of olive oil 11 Methods of analysis and interpretation of results 13 Specific gravity 13 Index of refraction 15 JIaumene number and specific temperature reaction 18 lodin absorption 20 Saponification or Koettstorfer number 25 Melting point of fatty acids 25 Solid fatty acirocess or processes. An exceedingly able English mechanic has tried two experiments with a new press this 12 OLIVE OIL AND ITS SUBSTITUTES. season here, and has since continued his experiments with oUves sent to San Fran- cisco, of which I have not as yet learned the result. I am eoniident that we shall before long have a machine which will avoid the costly process of partial evapora- tion and handle the olives as they come from the tree without sacks or the cider- press outfit, both of which mean much labor and expense. Yours, very truly, Edward E. Goodrich. Jamacha p. O., San Diego County, Cal., March 30, l'M2. Yours of March 22, asking for information in regard to olive oil, just received. I have no secret process. I inclose a printed description of my process, which very clearly shows our method. We use no heat at any stage of the process. This cold-water separator I consider a great improvement over the old way of storing in large settling vats and skimming iiff the oil as it rises. By this process the oil is separated from the lees as fast as pressed. E /ery morning the oil expressed the day before i.s taken from the separator and plt.ce :l in the racking tanks. I use only ripe olives and press them fresh from the tree. s. put up two grades, only one of which we bottle. No. 2 is sold only in bulk to ou' local trade. The cost of production of course , but had 12.11 per cent of free acid, which explains the low gravity and excludes the oil from use for salad purposes. Eighteen samples of Italian oils gave a range of from 0.9155 to 0.9180. with an average of 0.9163. Blasdale' on 11 sam- ples of California oils found a variation of from 0.9161 to 0.9174. Milliau'' found on French oils a range of from 0.9169 to 0.9172, and for Tunis oils' a range of from 0.9170 to 0.9196, with an average on •19 samples of 0.9183. De Negri and Fabris-^ in a very exhaustive exam- ination of Italian oils found on 70 .samples a range of fi-oiii 0.9160 to 0.918(), and an average of 0.9166. These authoi's found one sample of oil made from I'otten olives which had a specific gravity- of 0:9145. This low figure was most likely due to the presence of free fatty acids, which were not determined, but which were probably present in suffi- cient amounts to materially iutlueiice this constant and to (exclude the product from edible oils. Colby" gives the range for California oils of 0.9140 to 0.9185, but in the absence of definite data regarding the amount of f r(>e acids present the lower limit can hardly be accepted for a normal oil. From tiie above figures it is apparent that there is but little variation in the specific gravity of edible oli\e oils from dif- ferent sources and from different varieties of olives. The specific gravity of California, French, and Italian olive oils varies from 0.9140 to 0.9185, while the oils from Algeria range as- "Allen, Com. Org. Anal., 3d ed., vol. 2, pt. 1, p. .3.3. Wintoii, Connecticut Agr. Expt. Sta. Kept., 1900, pt. 2, p. 149. ''U. S. Dept. Agr., Bureau of Chemistry Bui. 6.5, p. 21. '•.Tour. Amer. Chem. Soc, 189.5, 17: 935. ''Bui. du Ministere de 1' Agriculture, 1895, p. 139. ''Milliau, Bertainchand et Malet, Bui. de 1' Agriculture et Commerce de Tunia, " Rapport sur les huiles d'olive de Tunisie, 1900." ./"Annali del Lab. chim. centr. delle Gabelle, vol. 1, Gli Olii, jit. 1, p. 38. !/ California Agr. Expt. Sta. Kept., 1897-98, p. 169. METHODS OF ANALYSIS. 15 high as 0.rtl9fi. Zammit " called attention to the fact that the presence uf free acids in olive oils reduces the specitic gravity, and the following table taken from his results shows the effect of excessive amounts: Table III. — Effect of excessive amounts of free acids in olive oils on their specific gravity. Free acid as oleic. 12 per cent 13 per cent 14 per cent 15 per cent 20 per cent Specific gravity 15.5° C. 0. 9147 .9139 .9U3 .9144 . 9132 Free acid as oleic. 25 per cent 27 per cent 28 per cent 31 per cent Specific gravity 15.5° C. 0.9128 .9136 . 9124 . 9122 Table IV gives the range of specific gravity of all the oils considered in this bulletin. Oils having an excessive amount of free acids, and consequently abnormal specific gravity, have been excluded from the ranges given in the column of '•Results obtained in Bureau of Chem- i.stry." This explains in many cases the lack of agi"eement between the results from the two sources. An example of this is one sample of peanut oil having 13.51 per cent of free acids and a specific gi-avity of 0.9155. The other three samples of peanut oil have specific gravities of 0.9186 and above, which are considered about normal for this oil. Table IV. — Specific gravity of oils. Kind of oil. Results obtained in Bureau of Chemistry. Compiled results. 0.9162 to 0.9180 .9155 to .9180 0. 9140 to 0. 9185 .9158 10 .9180 . 9169 to . 9172 .9170 10 .9196 Lard . .914810 .9143 to .9147 to . 9186 to .9226 to .9233 to . 9201 to .9239 to .9175 .9163 .9193 .9186 .9188 .9236 .9218 .9256 .9205 .9244 .9150 to .9160 .9112 to .9184 . 9125 to . 9183 . 9151 to . 9200 .9110 to .9220 . 9160 to . 9362 . 9200 to . 92.50 Maize . . 9213 to . 9255 . 9240 to . 9262 . 9240 to . 9370 Index of Refraction. This determination was made with a Zei.ss butyro-ref ractometer, the readings being made as nearly at 15.5'-^ C. as possible. As it is not always convenient to make the readings at this temperature, the factor to be used for the correction for temperature was determined on oils likely to be used as substitutes for olive oil.* The buty ro-ref ractometer, on account of its ease of manipulation, is very widely used, but its empirical scale, with divisions of varying value in refractive indices, requires for an accurate correction for temperature that the scale read- ings be calculated to indices of refraction and the temperature correction applied thei'eto. The reason for this can be seen from Table V. «Rev. Int. Fals. Alim., 1899, 12: 84. ''Tolman and Munson, Jour. Amer. Chem. Soc, 1902, 24: 754. 16 OLIVE OIL AND ITS SUBSTITUTES. Table V. — Value of butyro-refractomeler degrees in refractive indices on different parts of the scale. Scale N,. division. 1.4220 10 1.4300 40 1.4.524 50 1.4593 90 1.4840 100 1.4896 Differ- ence. 0.0080 .0069 .0065 From thi.s it will be .seen that ten scale divisions from o to 10 on this instrument equal 0. 0080 in index of refraction, while from 90 to 100 they equal 0.0055. It is evident that if, as shown in Table VII, the change in the refractive index for 1° C. is practically a constant, then the change in the scale division of this instrument for 1° C. must be a vai'iable and will increase as the scale reading increases. This is shown in Table VI, which gives the readings on rape oil. The change for 1° C. decreases as the temperature rises. T.\BLE VI. — Variable temperature correction in butyro-refraclometer readings. Scale readings. Change for 1° C. Temperature. In scale reading. In re- fractive index. 2.3°C .... Degrees. 82.0 70.5 70.5 61.0 Degree. } 0.60 } .67 S1.8°C 0. 000360 21.8° C 38. 4° C , .000360 Table VII gives the determinations of the temperature corrections of vai'ious oils. Table VII. — Temperature corrections for various oils. Labo- ratory No. First reading. Second read- ing. Kind of oil. j Tem- pera- ture. Butyro- refrac- 1 Tem tometer pera read- ture. ing Butyro- refrac- tometer read ing. Third read- ing. Tem- pera- ture. Butyro- refrac- tometer read- ing, Increase for 1° C. Between first and second reading. Between second and third reading. In index of refrac- tion. 23605 506 23460 493 491 498 23624 496 490 486 495 487 22434 499 23656 492 489 436 Olive do do Poppy seed Maize Sunflower do Rape do Mustard Black mustard Lard do Peanut do Peanut and cotton seed Sesame Cotton seed Average . °C. 3.4 3.2 3.2 9.0 2.8 3.0 3.0 2.8 3.4 2.8 3.2 3.0 3.0 3.0 3.3 3.4 3.4 3.4 Degrees. 76.5 76.0 76.0 82.6 84. 5 81.0 81.2 82.0 82.2 84.6 84.5 74.5 75.2 78.5 76.0 82.0 81.2 81.5 °C: 22.0 22.2 22.2 19.9 21.8 21.8 22.0 21.8 22.0 22.0 22.0 22.0 22.0 22.0 22.0 22.0 22.0 22.2 Degrees. 65.6 64.8 66.0 7.5.6 73.0 69.5 70.0 70.5 71.0 72.6 73.0 63.4 64.0 67.2 64.5 70.6 70.0 70.0 37.8 36.8 43.3 41,0 39.6 39.0 39,0 38,4 38,8 38,0 39.4 37.6 39.2 37,2 44.2 42.5 38.2 37.6 Degrees. 56,5 56,5 53,0 63,2 62,5 69,5 60,0 61,0 61,4 63,2 63,0 64,6 54,0 68,5 52.3 88.8 60.5 61.2 Degree. 0.69 .69 .58 .63 .60 .61 .69 .60 .60 .62 .61 .68 .69 .69 .61 .61 .60 .61 0.67 .87 .66 .69 .59 ..58 .58 .,57 .67 .58 .57 .66 .67 .87 .56 .67 .58 .67 0. 000366 .000366 .000360 . 000369 .000366 ,000369 ,000364 .000363 .000364 ,000360 .000361 .000363 .000372 .000365 .000366 .000369 .000370 .000368 .000365 METHODS OF ANALYSIS. 17 From these results it i.s seen that the correction of the index of refraction for 1 - C. is practically a constant for all of the oils examined, while the correction in scale divisions varies from 0.55 to 0.63 for 1° C. For great changes of temperature it is not accurate to use the scale division factor, but the results must be reduced to indices of refraction and the correction applied to them. The following formula may be used to correct for a range of 10 degrees: R =R' + X (T'-T). K = reading corrected to T. R' = reading at T'. T = desired temperature. T' = temperature at which readings are made. X = change in scale division caused by a change of temperature of 1° 0. (X = 0.55 for butters; 0.58 for oils that read from 60° to 70° on the scale; and 0.62 for oils that read from 70° to 80°. ) The determination of the index of refraction has much the .same value in the detection of tidulteration as the determination of specific gravity. The forty-two samples of California oils examined had a range of from 1.4703 to 1.1:718, with an average of 1.4711. These limits exclude one sample having -11 per cent of free acid and an index of 1.-1672, as free acid reduces the index of refraction of an oil. Blasdale" on eleven samples of California oils obtained a range of 1.4710 to 1.4716. Colby* gives a range for California oils of from 1.4689 to 1.4717, but this is probably too wide for oils which can be classed as salad oils. On eighteen samples of pure Italian oils reported in this bulletin there was found a range of from 1.4703 to 1.4713. There is therefore a total variation in the determinations made in this laboratory of from 1.4703 to 1.4713, with no difference between the California and Italian oils. Table VIII gives the index of refrac- tion obtained on various oils. Table VIII. — Bulyro-refntctometer readings and refractive indices of oils. Kiurt of nil. Number of samples. Butyro-refrac- tometer readings at 15.6° C. Index of refrac- tion at 15.5° C. California olive 42 IS 4 1 3 5 4 1 1 4 4 1 Degrees. 66.9 to 69. 2 67. 3 to 68. 5 68. 8 to 69. 5 70.9 70. to 71. 3 74. 5 to 76. 5 74. 1 to 74. 8 73.3 72.7 75.6 to 77.5 72.3 to 75. 6 77.8 1 4703 to 1 4718 Lnnl 1 4702 to 1 4720 .^.Imond 1 472S Mustard 1 4750 to 1 47IV2 Rape 1 4748 to 1 4752 Sunflower 1 4739 Cotton-seed . . 1 4737 to 1 4757 Poppy. 1 4770 «Jour. Amer. Chem. Soc, 1895, 17: 935. 6 California Agri. Expt. Sta. Rept., 1897-98, p. 169. I' One sample of peanut oil containing 13.51 per cent of free acids had an index of refraction of 1.4707. 20128— No. 77—05 3 18 olive oil asd its substitutes. Maumexk Number" and Specific Temperature Reaction.* The method used in making this determination was that described in the Provisional Methods for the Analysis of Foods/ The specific temperature number was calculated by the following formula: ^. 100 A ^ = T— S = Specific temperature number. A = i\Iaumenc number. B = The rise of temperature obtained with jiure water under tlie same conditions as those used in the Maumeno test. This simple test if carried out properly is a most valuable and rapid means of judging the puritj' of olive oil. Lard oil is practically the only oil which would be used as a substitute that lias as low a figure. Different analysts have obtained wideh' varying figures for this test, but it is easily shown that these are due to the use of acids of varying .strength. Colby.'' in preparing standards for the Association of Official Agricultural Chemists, gives from published results a range for this test of 32 to i7; but such figures as these have no value as thcv represent results obtained by different methods and different strengths of acid. BlasdalC found on a numl)er of California oils a range of 4.5 to -±7. With the ■±2 .samples of California oils of known purity examined in this laboratory a range of -i'S.o to 52.1 was found, with an average of Itj.S. In contrast to these results, Milliau,'' in his report on the oils of Tunis, gives a range of 30 to 36. These figures represent the variation found in 50 samples of oilsfroui varied sources and processes of manufacture. Milliau,'' in an earlier report on the olive oils of Europe, gives a range for the Maumene figure of 30 to 35. This wide difference in results is due entirely to the strength of the acid used in making the test. The actual limits where the same method and the same strength of acid are used are quite narrow. In prepar- ing acid for this test Milliau'' diluted 9.5 parts by volume of pure 66° Baume acid with 5 parts of distilled water. The acid prepared in this way gives a rise of temperature with water of about 38^ C, and com- pares satisfactorily when calculated to the specific temperature number with results obtained by the use of .strong acid giving a ri.se of tem- perature with water of 45 to l-B"^ C. In this laboratory an acid with a specific gravity of 1.8M was used, which gave a rise of temperature "Comp. Rend., 1852, 35: 572. ''Thomson and Ballantyne, Jour. Soc. Clieni. Ind. 1S91, 10: 233. <^U. S. Dept. Agr., Bureau of Chemistry Bui. 65, p. 31. rf California Expt. Sta. Kept., 1897-98, p. 169. fJour. Amer. Chem. Soc, 1895, 17: 935. / Milliau, Bertainchand and Malet, Rapport sur les liuiles d'olive de Tunisie, 1900. ?Bul. du Ministere de 1' Agriculture, 1895, p. 139. '' Buletinul camerei de comerciu si Industrie din Bucuresci, 1900. METHODS OF ANALYSIS. 19 with water of 45° C. Thus it can be seen that the Maumene numbers alone have no comparative value. Either the exact strength of the acid must be given, or, perhaps better, the rise of temperatui-e with water under .standard conditions. Thomson and Ballantyne," in order to give these results a compara- tive value, proposed to report them as specific temperature numbers. They showed that with acid varying from 95.4 to 99 per cent there was only a very .slight difference in results when calculated to specific temperature numbers, the stronger acid giving slightly higher results. Sherman, Danziger, and Kohnstamm'' showed that if there was a much greater variation in the strength of acid used there was also a wider variation in the specific temperature numbers. With acid vai'ying in strength from 89 to 95 per cent thej' found an average of from 90 to 103 in specific temperature numbers on the same olive oil. The Maumene numbers oljtained by the writers on 32 samples of olive oil of known puritj' using different strengths of acid are given in Table IX. T.\BLB IX. — Maumene and specific temperature numbers of olive, oilx. Rise of , tempera- Serial I til re number. | given JnSer. 962. 960. 934. 836. 931. 932. 933. 935. 9.55. 961. 936. with pure| water. Specific tempera- ture nuifiber. 33.3 33.3 33.3 34.0 34.0 34.0 34.4 34.4 34.4 34.4 34.4 31.4 29.8 29.6 30,0 29.8 30.6 27.4 27.1 I 27.5 . 28.7 I 28.6 ! 94.3 89.4 88.9 88.2 87.6 90.0 79.6 78.8 79.9 83.4 83.1 959 953 954. 956 957 952 958. ... 835 838 837 840 839 834 833 832. 831 796 797 ...1 798 1 Maximum Minimum Difference 34.4 31.4 94.3 33.3 27.1 78.8 1.1 4.3 15.5 Rise of tempera- ture given with pure water. °C. Man- menu number. Specific tempera- ture number. 36.6 1 33.2 I 33.4 88.0 88.6 35. 35. 35. 35. 35. 36. 35. 37.' 37.- 37.' 37.' 37. ■ 38. i 28.8 31.6 31.3 31.5 29.0 28.0 29.4 35.9 37.7 35. 4 37.5 38.9 36.1 36.8 37.1 36.0 37.7 39.1 38.4 39.1 80.9 88.8 88.0 88.5 81.4 78.6 82.6 95.2 100.0 93.9 99.5 103.1 93.8 96.5 96.4 93.5 97.8 tOl.5 99.7 101.5 Rise of ''"re'"" ^^''"- given I ="«?« wlfh pSre' "'^■"ber. water. 1 °C. 43.9 43.9 43.9 45.6 45.6 4S.6 45.6 45.6 I 45.6 : 45.6 1 45.6 47.5 47.5 I 47.5 1 47.5 ; 47.5 47.5 ' 47.5 ! 15.0 ; 45.5 I 45.5 45.5 45.5 47.5 47.5 47.5 47.5 47.5 47.5 47.5 47.5 38.5 35.6 2.9 39.1 28.0 11.1 103.1 78.6 M.6 47.6 43.9 S.6 43.5 +4.7 42.5 48.2 44.4 44.4 43.5 44.2 44.2 43.5 44.8 46.2 47.0 48.3 49.1 45.0 45.0 48.0 44.8 19. 45.0 48.2 48.4 46.2 48.0 47.0 46.0 50.0 .52.1 .50.2 51.0 Specific tempera- ture number. .52.1 42.5 9.6 99.1 101.8 96.8 105, 7 97.4 97.4 95.4 97.0 97.0 95.4 98.2 97.2 99.0 101.7 103.4 94.7 94.7 101.0 98.5 108.8 98.9 105.9 106.4 97.2 101.0 100.1 98.1 105.2 109.7 105. 6 107.3 109.7 94.7 15.0 The results given in this table show that when there is a wide dif- ference in the strength of acids used the specific temperature numbers «Jour. Soc. Chem. Ind., 1891, 10: 2.3S. SJour. Amer. Chem. Soc, 1902, 24: 266. 20 OLIVE OIL AND ITS SUBSTITUTES. are not of much value for comparative purposes, but if there is onlj- a slight difference in strength they give very satisfactory results. The variation is least when a strong acid is used, giving a rise of tempera- ture with water of 43.9^ C. to 47. 5"^ C, showing that the Maumcni' number obtained on olive oils with strong acid is more uniform than with the wealter acid. However, the strong acid is not satisfactor}- for use on seed oils, as the reaction becomes too violent and the oil is broken up. With seed oils a weaker acid was used, as suggested by Sherman, Danziger, and Kohnstamm." The following tal)lc gives the results obtained in this laboratory on various oils. The strongest acid was used on the olive and lard oils, and a weaker acid on the seed oils. Table X. — Maumeni' and specific temperature numbers of rarious oils. Kind of oil. Maumpnii ' Specific tem- Kind of oil. Maumcni number. Specific tem- perature num- ber.o California olive 42. 6 to 52.0 94. 7 to 109. 7 42. .5 to 49. 1 , 95.6 to IW. 7 46. 5 to 47. 8 103. 3 to 106. 2 61.0 to 63. 2 135.5 to 140. 2 61.0 to 79. 4 1 130.9 to 190. 3 54.610 67.8 1 135.0 to 152. 5 Almond 46.3 61.3 60.0 75. 2 to 89. 2 66. 2 to 73. 4 75. 8 to 85. 5 117.6 170. 3 Lard Sunflower Maize . 166.7 190. 2 to 212 5 Mustard Cotton seed Poppy 172.4 to 191.1 Kape . .. 213. to 237. a Acids of quite widely differing strengths were used in these determinations. loDiN Absorption. The method used for this determination was the modified Hiibl method, as adopted by the Association of Official Agricultural Chem- ists,* in which the iodin solution is allowed to stand in contact with the oil for three hours. The iodin number was found to be exceedingly variable. On 42 samples of California oil examined the range was 78.-5 to 89.8, with an average of 85.1. IJiasdale'' found a range of from 80 to 86.5, with an average of 84. Colby '' gives a range of 77.7 to 93.5 for California oils of known purity. On 17 .samples of Italian oils the variation was from 79.2 to 86.1, with an average of 81.5. De Negri and Fabris' found on 88 samples of pure Italian oils a range of from 79.1 to 89.8, with an average of 83.7. Milliau'" found for French oils a range of from 84 to 85, and for the oils of southern Europe and Tunis a range of from 81.4 to 85.2. Later'' he found on Tunis oils a range of 79.3 to 89.5, with an average of 85, figures which are very similar to the oJonr.Amer. Cheiii.Soc.,1902, 24: 266. t>V. S. Dept. Agr., Division of Chemistry Bui. 46, p. 50; Bui. 65, p. 24. fjour. Amer. Chem. Soc, 1895, 17: 9.35. <* California Agr. Expt. Sta. Rept., 1897-98, p. 168. « Annali del Labor, chira. centr. delle Gabelle, vol. 1, Gli Olii, pt. 1, p. 38. f Bu\. du Ministere de r Agriculture, 189.5, p. l:-i9. ?Milliau, Bertainchand, and Malet, Rapport sur les huiles d'olive de Tunisie, 1900. METHODS OF ANALYSIS. 21 results obtained on California oils. From these results it would seem that the range of iodin numbers on California oils is from 78 to 90, a little wider than that found on French oils, but about the same as on Italian and Algerian oils. Table XI gives the range of iodin values found in this laboratory and by other analysts on various oils of known purity. With all these oils this range is extremely wide, and for this reason the determina- tion of the iodin value is liy itself of little value as a means of detect- ing adulteration. Onl}' in cases of gross adulteration could it be conclusive. By a careful selection of the oils to be used in making the mixture, large proportions of either lai'd or peanut oil could be used without producing an abnormal iodin value. As is shown in Table XVII, page 26, the iodin value increases as the solid fatty acids and the melting point of the fatty acids decrease. It is only when this factor is determined, in connection with these other factors and with the iodin value of the liquid fatty acids, that it may serve as a valuable indication of the purity of an oil. Table XI. — The. Hubl number of various oils. Kind of oil. Result.s ob- tained in the Bureau of Chemistry. Compiled results. Kind of oil. Results ob- tained in the Bureau of chemistry. Compiled results. California olive - . Italian olive 78. 5 to 89. 8 79. 2 to 86. 1 77. 7 to 93.5 79.0 to 89.8 84.1 to 84.5 79. 3 to 89.5 60.0 to 82.0 93. to 102. 85.6to 105.0 Cotton-seed Sesame 103. 8 to 110. 9 106.6 92. 5 to 101. 2 98.4 to 113.0 116. 7 to 123. 3 104. 1 to lO.**. 3 133.2 to 134.9 106. 5 to 110. 7 102.0 to 112.0 94.1 to 106. 2 Ajgerian olive Mustard 92. 1 to 106. 5 Lard 69. 7 to 77. 2 96.2 87.8to96.3 111.1 to 123.9 Sunflower 119.0 to 135.0 130. 5 to 141.0 The Hiibl method has never been considered entirely satisfactory, owing to the poor keeping quality and the slowness of reaction of the iodin solution used. Recently two new .solutions have been proposed as substitutes, both of which, it is claimed, remain practically unchanged for several months" and are more rajjid in thtMr reaction than the Hiibl solution. The Wijs* solution consists of iodin mono-chlorid dis- solved in glacial acetic acid; the other, proposed later by Hanus," is a solution of iodin mono-bromid in glacial acetic acid. Comparative tests of these two solutions with the Hiibl solution, made upon a large number of olive and other oils, verify the claims made for these new solutions both as regards their keeping qualities and their raijidity of action. A comparison of these methods is given in Table XTI. «Tolman and Munson, Jour. Amer. Chem. Snc, 1903, 25: 244. 6Ber. 1898, 31: 752. «Ztschr. Nahr. u. Genussm., 1901, i: 913. 22 OLIVE OIL AND ITS SUBSTITUTES. Table XII. — lodin numbers of olive oik. Laboratory No. Hiihl ' Wijs Hanus niTmhpr ' number number fShmrs) (SOmin-UsOmin- 1 Difler- ence be- tween Wijs and Hiibl numbers. Difler- ence be- tween Hanus and Hubl numbers. 795 .... 89. 7 90. 9 90. 4 89.7 1 90.6 90.0 89.8 914 ' 90.0 +1.2 + .9 +1.6 + 1.4 +1.6 +1,9 +1,5 +1,6 + 1,6 +1,0 +1.0 + .4 + .3 +1.0 + .9 + 1.5 + .4 + .7 + 1.3 +2.0 +1.6 +L3 +1.4 +L6 +L6 +1.7 +L6 +1.8 +2,3 +0 7 796 , 797 + .3 + 2 798. . . 89.7 80.9 84.8 91.1 90.4 82. 5 81 - 7 + .7 + .8 960 : 833 ... . 86.7 86.7 86.5 86. 1 82.8 81.6 83.1 81.5 83.6 82.2 87.8 80.9 79.9 83.1 83.4 87.7 82 4 86,5 85.9 85.9 86.1 82.8 81.1 82.6 80.9 83.1 81.8 86.7 81,6 80,0 81.8 81.9 86. 3 m s +1 7 831 832 834 936 933 835 962 955 952 840 935 953 958 959 9.54 . . 85.2 84.9 84.6 81.8 80.6 82.7 81.2 82.6 81.3 86.3 80.6 79.2 81.8 81.4 86.1 + .7 +1.0 + .6 +1.0 + .5 - .1 - .3 + .5 + .5 + .4 +L1 +1.4 0.0 + .5 + .2 81.1 84.5 80.5 80.8 80. 80.7 86.1 89.0 81.0 83.3 86.9 87.2 85.1 84.2 81.9 +1 1 956 85. 9 Rfi- 6 +1.1 82.0 82.3 87.7 82.2 87.9 9L3 81.4 81.1 86.6 81.5 87,1 89,9 84,9 82,6 87.3 87.1 .85.6 84.2 82.0 + .9 961 + .3 836 + .6 931 + .8 +1.0 838 839 + .9 837 + .9 673 84.1 88.0 88.1 86:6 85.0 83.4 + .8 + 1.1 + .9 +1.5 + .8 + 1.5 1-1. .1 . .- _ .7 841 + .4 842 + .1 843 + .5 .S44 0.0 1091... -t- 1 Average (36 samples) + 1.3 2.3 0.3 +0.60 1.7 0.0 Table XII gives the ro.sults obtiiiiied upon olive oils and TaljJe XIII the results obtained upon other nondrying- oils, semidr3inii-, and dry- ing oils. The values obtained with olive oils are slightlj- higher when the Wijs or the Hanus solution is used, but the difference is not suffi- cient to materially change the standard already' existing for this oil. With other oils having a low iodiii value closely agreeing results were obtained by the three nietliods, as shown in the values olitaincd for oleo oil, butter, and lard. With mustard and rape oil of the iiondiy- ing oils, and linsee'd oil of the drying oils, much higher results were obtained by the Wijs and the Hanus methods, and the use of either of these will necessitate the establi.shment of new standard.s. METHODS OF ANALYSIS. Table XIII. — lod'm numhers of various oils and fats. 23 Labo- ratory No. ' tils and fats. Hubl number (3 hours). Wijs number (30 min- utes) . Hanus number (30 min- utes) . Differ- ence be- tween Wijs and Htibl numbers. Differ- ence be- tween Hanus and Hubl numbers. FATS. 8.93 G.09 35.3 34.8 42.0 .53.6 .52.8 B2..5 m. 3 69.3 73.7 81.7 76.1 96.3 94.5 107.7 110.4 113.0 98.4 103.5 106.4 101.3 100.2 106.4 103.8 106.2 104.8 106.4 119.0 119.0 123.3 133.4 131.9 169.8 179.5 9.05 6.43 36.2 35.9 43.5 53.5 53.7 52.9 66: 70.5 74.6 79.4 75.6 99.0 95.2 109.5 118.5 118.2 104.3 112.0 117.3 10.5.7 104.1 109.2 105.3 107.3 106.2 107.0 123.2 122.2 129.2 135.2 139.1 186. 5 188.7 8.60 6.40 35.3 35.4 43.3 52.3 52.2 52.0 64.8 69.8 73.9 78.9 74.0 97.4 94.1 107.7 115.5 116.8 103.8 110.2 114.8 105.2 102.8 107.7 105. 2 107.8 106.7 106. 5 120.2 119.6 126.0 132. 9 138.4 184.5 183.7 -1- 0. 12 + .34 + .90 -1- 1.10 -t- .90 - .10 -1- .90 + .40 - .30 + 1.20 + .70 - 2.30 - .50 -1-3.00 -1- .70 -1- 1.80 + 8.10 + 5.20 + 5.90 + 9.00 -1-10.90 + 4.40 -1- 3.90 + 2.80 -1- 1.50 + 1.10 -1- 1.40 + .60 -1- 4.20 + 3.00 -1- 6.80 -f 1.80 + 4.20 fl6.70 -1- 9.20 - 0.33 -1- .31 1170... 1168 -1- .00 do -1- .60 Oleo + .70 - 1.30 . do . - .60 do - .50 ....do - 1.50 23606 NONDRYING OILS. Lard + .50 487 .. + .20 1181 - 2.80 1182 .. - 2.10 772 -1- 1.10 1149. ...do - .10 492. . . do.h + .00 770 Mustard -f 5.10 771 do + 3.80 776 . do -t- 5.40 486 + 6.70 495 -t- 8.40 775 -1- 3.80 490.. + 2.60 SEMIDRYING AND DRYING OILS. + .80 1159... 1160. . . + 1.40 do -f 1.60 1161 do + 1.90 489 + .10 444 -1- 1.20 491 .. -f .40 777 + 2.70 493 - ..50 774 -1- 3. .50 1162 -fl4.70 1188 do. 1- -1- 4.20 a Commercial oils. & Adulterated with cotton-seed oil. c' Four hours for Hiibl determination. As will be seen from Table XIV, the leno-th of time involved in the determination is greatly lessened liy the use of the Wijs and the Hanus solutions. In case of olive oils the reaction is complete in tifteen minutes; cotton seed, sesame, mustard, and other nondrying and .semi- drying oils require thirtj" minutes; while rape and linseed oils require one hour for complete absorption. 24 OIIVE OIL AND ITS SUBSTITUTES. Tablk XIV. — Time necessary for absorption of iodin. Labo- ratory No. Kind of oil or fat. Iodin numbers by Hanus method. Iodin numbers method. by Wijs 15 min- utes. 30 min- utes. 1 hour. 15 min- utes. 30 min- utes. 1 hour. 773 8.7 6.4 35.2 35.4 43.2 62.4 51.9 64.6 52.2 80.4 70.0 90.1 82.1 86.5 96.0 125.0 8.6 6.4 35.4 35.5 43.4 51.8 52.1 65.1 62.4 80.6 69.7 90.4 81.7 86.5 97.4 126.0 119.4 106. 107.4 116.8 137.4 18B.3 22077 Konut 1170 Butter 1168 do 35.8 35.9 Oleo 52.9 do do do 23606 798 90.3 82.2 86.5 97.7 126.0 120.0 105.0 107.5 117.6 138.4 186.2 90.0 82.6 86.5 98.8 126.5 91.2 82.6 86.7 99.0 126.5 118.0 104.3 105.8 116.1 138.9 190.2 960 .... do 82 5 833 do 772 Peanut 99 777 128 771 do 776 ...do 104 6 775 770 Maize 117.1 138.8 183.8 118 5 774 136.8 139.1 1162 These results show but little choice between the two new solutions, the Hanus solution giving results slightly closer to the figures obtained bv the Hi'ibl method. The Wijs solution is prepared by dissolving 13 grams of pure iodin in a liter of glacial acetic acid which does not reduce a solution of l)ichroniate of potash in sulphuric acid; a current of pure chlorin gas is run into the solution until the halogen content is doubled. A slight excess of iodin is recommended. The change of color in the solution as the end point is approached is quite marked. The Hanus solution used is made l)y dissolving 13 grams of iodin in a liter of glacial acetic acid and then adding sufficient bromin to double the halogen content; about 3 cc are sufiicient. Tlie method of using these solutions is the same as with the Hiibl solution except that an excess of unabsorbed iodin of at least TO per cent of the total titer is necessary; and only 10 cc of the 20 per cent potassium iodid solution are used, the solution being thoroughly mixed before the water is added. In the above work the absorption *was allowed to continue thirty minutes, as .some of the adulterants of olive oil require a slightlj^ longer time than the oil itself to complete the absorption. Great care must be taken that no change of temperature occurs while measuring the solutions. The high coefficient of expansion of acetic acid (0.00115 for 1° C.) will cau.se an appreciable error if even a slight change of temperature takes place. If 40 cc of these solutions are measured, a change in temperature of zh 1° C. wil] give a change of =F 0.11 cc in the amount of N 10 thiosulphate used to neutralize them. Table XV shows how great the variation in titer mav be in a change of temperature of 11^ C. METHODS OF ANALYSIS. Table XV. — Influence of temperature on tite.r. 25 Tempera- ture. 40 CO iodin- mono- broraid in N.aO thio-sul- rc. 92.05 91.85 91.80 91.35 91.10 90.80 "C. 16 17.6 18.5 21.5 24.5 27 +11 —1.25 The results of this investigation show that either of the two new methods gives satisfactory results and that both solutions are decided improvements over the Hiibl solution, not only in possessing much better keeping qualities, but also in rapidity of action. The Haiius solution gives results somewhat closer to those obtained b}' the Hubl method, and is much more easily prepared than the Wijs solution. Saponification or Koettstorfer Number. The saponification number, or number of milliyranis of potassium hydroxid needed to saponify 1 gram of fat, was determined as directed l)y the Association of Official Agricultural Chemists." The determination has little value in detecting adulteration of olive oil with any of the animal or vegetalile oils except rape or mustard. Its chief value is in the detection of mineral oils. Table XVI, giving the limits on various oils, shows the uniformity of the Koettstorfer number of the ordinary salad oils, except rape and mustard oil. The variation on the oils other than rape and mu.stard is from 185.0 to 197.7, while the variation on olive oils is from 185.0 to 194.6. Table XVI. — Saponification or Koettstorfer number of various oils. Kind of oil. Results ob- tained in Bu- reau of Chemistry. Compiled re- sults. Kind of oil. Results ob- tained in Bu- reau of Chemistry. Compiled re- sults. California olive . . 189. 3 to 194. 6 189. 7 to 192.0 195. 3 to 197. 7 174.1tol7G.6 173. to 182. 8 192.5 187.0 to 193. 5 185.0 to 192. 3 189. 5 to 196. 167.71O1K3.0 170. 2 to 174. 7 183.0 to 191.7 188. 8 to 196.0 196.0 to 198. 5 190.7 1.89. 9 to 193. 4 191. 2 to 192. 3 190. 2 to 193. 8 189. 3 to 196 Italian olive Lard . . Cotton seed Sesame 191.0 to 196. 6 188 4 to 394 6 Rape Maize Sunflower Poppy seed 188 to 193 i 188.0 to 197 6 Almond 192. 8 to 194 Melting Point of Fatty Acids. The method u.sed for this determination was that described in the Provisional Methods for Food Analysis.* A variation was fomid on «U. S. Dept. Agr., Division of Chemistry BuL 46, p. 48. 6U. S. Dept. Agr., Bureau of Chemistry Bui. 65, p. 31. 20128— No. 77—05 4 26 OLIVE OIL AND ITS SUBSTITUTES. California oils of known purity of from 19.2° to 31^' with an aver- age of 22.5''. Blasdale" found the variation on eleven samples of California oils to be from 21'^' to 26". and Colby* gives a range of from 21^^ to 28°. On Italian oils the writers found a variation of from 21° to 29.3°. Other published results give a variation of 23.7° to 29°. Milliau'- reports on French oils 24° to 26°, but on Algerian'' oils gives a range of from 24.8° to 38°. This shows that Algerian oils are quite different from the European and Californian products. Table XVII, prepared from Table XXXV, .shows the relation be- tween the Hiibl number, percentage of solid fatty acids, and melting point of fatty acids in California olive oils. The writers found that in a general way the same relation held good for Italian oils. Milliau'' did not tind this relation to hold on oils from Tunis. He found oils with a Hiibl number of SS and a melting point of fatty acids of 37° C, and concluded from this that there were fatty acids present more unsaturated than oleic acid. Table XVII. — Kelation bi'lween Hiibl number, solid fall)/ acirh, mul melting point of faity acids {California oiVji). Serial No. Hiibl number. Solid fatty acids. Melting- point of fatty acids. Serial No. Hiibl number. Solid fatty acids. Meltinff point of tatty acids. 23462 23461 23459 23466 23692 79.9 83.0 82.9 84.3 85.6 Percent. 10.91 7.62 5.70 7.23 5.12 °a 31.0 28.0 25.0 23.4 22.6 23463 23460 23457 2.34.58 23605 85.6 85.7 86.2 88.2 88.5 rer cent. 4.92 6.27 3.39 4.42 2.43 21.3 23.4 21.1 23.6 20.2 The melting points of the fatty acids of peanut oil, cotton-seed oil, and lard oil are so much higher than tho.se of the mixed acids of olive oil that any considerable addition of any one of these oils to olive oil would produce an abnormal melting point. This is especially true of lard oil and cotton-seed oil. Sesame oil varies but little from olive oil in respect to the melting point of its fatty acids, l)ut oils of rape seed, mustard seed, sunflower, poppy seed, and maize are appreciably lower. Since, however, none of the.se would proba1)ly be mixed with anj'^ but olive oil or some one of the oils having a higher melting point than olive oil, this difference would be of little value in the detection of their sukstitution for olive oil. The determination of the melting point in itself has little value in the detection of adulteration, but is of decided value when taken in connection with other factors in judging whether or not the oil is normal. The melting points of the fatty "Jour. Amer. Chem. Soc, 1895, 17; 935. '' California Agr. Expt. Sta. Rept., 1897-98, p. 169. <^Bul. (Ill Ministore de I'Agriculture, 1S95, p. 139. <* Milliau, Bertainchand, andMalet, Rapport sur les huilesd'olivede Tunisie, 1900. METHODS OF ANALYSIS. 27 acids of variou.s oils as determined in this laboratory and as found in the literature on the subject are given in Table XVIII. Table XVIII. — Melting point of fatty acids of various oils. Kind of oil. Results ob- tained in Bu- reau of Chemistry. Compiled re- sults. Kind of oil. Results ob- tained in Bu- reau of Chemistry. Compiled re- sults. California olive .. Italian olive 19. 2 to 31.0 21. 6 to 29. 3 21.0 to 28.0 23. 7 to 29. 24.0 to 26.0 24.8to3«.0 12. to 14. 15. to 21. B 15. 5 to 22. Sunflower Maize 21.0 21.6 to 23.0 2.5. 4 to 2.5. 8 27.4 33. 2 to 37. 6 33.2 to 38. 4 35. 5 to 39. 6 °C. 17.0 to 24.0 16 to 22 4 Algerian olive. Sesame Peanut Lard . . . 21 to 40 I) 23.2 20. 8 to 21 5 20. etc 21. 9 Mustard 33 to 38 4 Cotton seed 32. to 43. Solid Fatty Acids. By solid fatty acids are meant those whose lead salts are insoluble in ether. The method of determination used was that described in the Provisional Methods for Food Analysis." From these results, calcula- ting the average total fatty acids present as 95.5 per cent/' the percent- age of liquid fatty acids can be obtained. As the latter ai'c the unsatu- rated fatty acids and alone absorb the iodin, the percentage of these acids and their iodin value gives a fair idea of the nature of the oil under consideration. Some of the oils of Tunis must contain fatty acids more unsaturated than oleic to give the high iodin number, and also the high per cent of solid fatty acids found by Milliau, Bertain- chand, and Malet.* The iodin number of the oil multiplied by 100 and divided b}' the per cent of liquid fatty acids will give their iodin number, providing the solid fatty acids are saturated. The calculated results agree fairly well with those obtained by experiment. These results show that in olive oils the unsaturated fatty acids are variable in their composition and can not be considered as pure oleic acid. From Table XXXIII it is seen that in lard oil the un.saturated fatt}^ acids have practically the same iodin number as the unsaturated acids of olive oil. Rape-seed oil does not differ much in this respect from olive oil. Mixtures of lard and cotton-seed oils which would give a normal iodin number for olive oil would have a much higher iodin num- ber for the liquid acids. The relations between the .solid fatty acids, the iodin number of the oil, and the liquid fatty acids, are of great value in identifying an oil of unknown origin. These factors for vari- ous oils are given in Table XIX. It can be seen from this table that the mixing of these oils with olive oil will change the figures on the mixture in a number of ways. An addition of maize oil would increase the iodin number of both the oil and the liquid fatty acids, but «V. S. Dept. Agr., Bureau of Chemistry Bui. 65, p. 28. «Bapport sur les huiles d'olive de Tunisie, 1900. 28 OLIVE OIL AND ITS SUBSTITUTES. would not affect the solid fatty acids. Cotton-seed oil would iucrcaae all of these figures. Table XIX. — The lodin numbers and the per cent of solid fatty acids ofvarioxis oils. Kind of oil. Hflbl number. lodin number of liquid fatty acids. Solid fatty acids. Kind of oil. Hiibl number. lodin number of liquid fatty acids. Solid fatty acids. 134.9 123.3 119.7 119.2 113.0 110.4 98.4 108.3 10.5. 8 151.7 139.8 134.8 134.5 121. 1 116.8 103.0 141.5 136.3 Per cent. 6.67 7.44 6.70 6.98 2.32 1.06 Trace. 19.04 17.87 Sunflower 108.3 104.1 92.5 101.2 97.9 75.9 69.7 72.5 77.2 117.8 113.8 96.9 107.5 115. 4 98.9 101.3 97.9 101.3 Per cent. 3 67 Maize Do Rape 4.12 Do .12 Do Do 1.43 10. '70 Do Lard . 18 90 Do Do 26.68 Do 21.43 Do Do 19.30 The addition of mustard oil would increase the iodin number.s, but decrease the solid fatty acids. Lard oil would decrease the Hiibl number and increase the solid fatty acids, but would not affect the iodin number of the liquid fatty acids. In many cases, however, especially if buc .small amounts were added to olive oil, the changes in the factors would be so slight as to give no indication of any adulteration. Frek Fatty Acids. The free fatty acids were determined by the method described in the Provisional Methods for Food Analysis" and the results calculated as oleic acid. One cubic centimeter of deci-normal alkali is ecjual to 0.0282 gram of oleic acid. This determination is of considerable value, in that it gives some idea of the condition of the oil. As a rule this figure increases with age and may be to some extent an index of the rancidity of the oil. The amount of free acid greatly affects the physical constants of oils as has alrcad}' been shown. All oils have some free acid present, even when freshly pressed. Its amount prob- ably depends on the condition of the fruit or seed and the processes of manufacture. Milliau, Bertainchand, and Malet* found a,s high as 3.9 per cent of free acid in freshl}- pressed olive oil, probablj^ due to the overripe or decayed condition of the olives. With a nunilior < .\ cold-prossed seed oils manufactured in this laboratorj' the determination of free fattj' acids was made within three days after the oils were pressed, with the following results: Sunflower oils, 0.18 and 1.72 per cent; peanut oil, 0.04 per cent; mustard-seed oil, 1.13 per cent; and rape-seed oil, 0.63 per cent. These figures show the presence of considerable amounts of free acids in the seeds. In Table XX are given the data showing the quantity of free acid in "U. S. Dept. Agr., Bureau of Chemistry Bvil. 6.5, p. 27. ftRapport sur les huiles d'olive de Tuuisie, 1900. METHODS OF ANALYSTS. 29 a number of sillrlple.•^ of olive oil of known history. Nos. 22617, 22714:, and 23126 all show an acidity that might be considered normal for fresh oils, although eight and ten years old. On the other hand Nos. 22618 and 22619, which were three years and one year old, respec- tively, show an excessive amount of free acid. It therefore follows that the time factor has but little influence upon the acidity, while No. 22619 indicates that high temperature favors the formation of the free acids. Table XX. — i'Vtc acids in. olive ails. Serial No. Free fatty acids as oleic. History of sample. 22617 Per cent 0.36 8.21 44.40 1.26 2.73 1.40 4.33 Made in 1893 from Redding Picholine olives. 22618 Made In 1898 from mixed varieties of olives. 22619 Made in 1900 from Manzanillo olives bv stronglv heating the fruit. 22714 Second pressing. 10 years old. 22715 Poor quality of oil, not an edible oil. 22126 Isouth American oils exhibited at Chicago in 1893. 22127 Eleven samples of pure California olive oils, all of which were con- sidered fresh oils, gave an average content of free acid of 1.16 per cent, and the extremes were 0..59 per cent and 2.2'4 per cent. Twelve samples of commercial California olive oils in which no added oil was detected contained an average of 2.40 per cent free acids, and this figure is more nearly in accord with the averages of the French and Italian commercial oils than is the average given for the California oils of known purity. This is undoubtedl}- due to the fact that previous to leaving the storeroom of the manufacturer the oil is kept under more favorable conditions of light and temperature than it receives after entering the retail stores. By reference to Table XXXII I it is seen that lard oil, peanut oil, and the various seed oils show an appreciable content of free acids, difl'ering in this respect but little from olive oils. Cotton-seed oil alone is an exception. This oil is refined by use of alkali, and so shows but small amounts of acidit}' and yields but little upon long standing. The rancidity of oils and fats has been the subject of extensive study by various investigators, and opinions regarding its causes are extremely varied. Lewkowitsch" states that pure, nondiying oils when protected from air and light remain unchanged at ordinary tem- peratures; on exposure to light and air they undergo change, consist- ing of the development of butyric, isobutylacetic, and other volatile acids in small quantities, an increase in free acids, and the acquire- ment of a disagreeable smell and acrid taste. These changes the author considers due to direct oxidation bj' the oxygen of the air, this action being intensified b}' sunlight. "Chem. anal, oils, fats, and waxes, 2d ed., p. 10. 30 OLIVE OIL AND ITS SUBSTITUTES. Ballantyne " has shown that in many instances rancidity exists long before the formation of free acids, and that on the other hand free acids may be liberated long before the oil becomes rancid. A. Schmidt'' states that an oil may have a high acidity without being rancid, and that the oil becomes rancid upon partial or complete oxidation of the free glycerin to aldehydes and ketones. Scale ''found that olive oil and lard contained no water soluble volatile acids in a fresh condition, but these acids developed with age and consequent rancidity of the oil and fat. Browne'' has made a study of the changes incident to the development of rancidity in butter fat and records some interesting results. Table XXI, taken from his work, shows the effect of the development of rancidity upon the various values of the oil. As the rancidity develops there is a decided increase in the acid, saponification, ether, and Reichert values, a mark(>d decrease in the iodin value and the percentage of insoluble acids, and a slight decrease in the per- centage of glycerin. Table XXI. — Effect of development of rancidity upon butter fat (Browne). No. of sample. Condition. Acid value. Saponifi- cation number. Ether num- ber. Reichert number. Hubl num- ber. Oleic acid (cal- culated). Insoluble acids. Glycerol. 0.48 1.28 10.90 28.84 30.00 3.5. 38 .45 1.22 ..50 7.09 ..5.5 11.73 ..51 14.80 228.1 230.3 241.0 260.0 262. 1 269.3 229. 9 232.3 223.9 233.7 232. 6 247.7 226.6 245. 3 227.6 229. 230. 1 231.2 232. 1 233. 9 229.5 231.1 223. 4 226.6 232.1 236.0 22.5.1 230. 15.63 15.80 17.00 18.75 19.80 21.13 34.95 34.56 28.40 14.35 11.15 8.55 33.93 29. 96 34.49 28.69 29.66 19.76 34.92 22.55 Per cent. 38.79 38.35 31.52 15.93 12. 38 9.49 37.66 33.26 38.28 31.85 32.81 21.93 38.76 25.03 Per cent. Per cent. 1 week old 1 month old 2 months old 4 months old 8 months old Fresh la 87.20 86.80 S8.96 8.5.06 86.41 80. 42 88.46 SI. 15 12.54 lb Rancid 12.40 12.21 2b Rancid, 1 month old 12 02 3a Fresh 12 69 3b Rancid. 2 months old 12,35 4a Fresh 12.33 4b Rancid. 3 months old 11.67 Rancidity maj' affect the physical and chemical values of oils and fats in several ways. If large amounts of free acid are formed and little oxidation takes place the .specific gravity and index of refraction may be lowered and the iodin number very little affected. If oxida- tion has taken place there will be an increase in the specific gravity, index of refraction, and saponification number, and a decrease in the iodin number. From the foregoing it is apparent that oils are extremely susceptible to change under the influence of light, air. and heat, and that dete- rioration is in a large measure prevented b}' the exclusion of air and o Jour. Soc. Chem. Ind., 1891, 10: 29. i-Ztschr. Anal. Chem., 1898, 37: 301. 'Ztschr. Nahr.-Unt. Hyg. u. Waarenk., 1896, 10: 239. ''Jour. Amer. Chem. Soc, 1899, 21: 975. COTTON-SEED OIL. 31 sunlight and b}' proper tenaperature conditions. These facts are of material importance, as the pleasant flavor and agreeable odor of pure, fresh olive oil may be easily destroyed upon the development of rancidity, while if kept under proper conditions the oils will remain practically unchanged for a long time. From the chemist's stand- point rancidity may so affect the values of an oil as to make it abnor- mal in many respects, and in the mterpretation of analytical data this fact nmst be given due consideration. OLIVE OIL SUBSTITUTES. Cotton-Seed Oil. Cotton-seed oil is the chief adulterant of and substitute for olive oil in this country. It is used to a large extent under the name of salad oil, but is also frequently sold as olive oil, with Avhich it is extensively mixed. The well-refined oil has a pleasant though characteristic taste and odor, and is much less inclined to become rancid than are olive oil and other oils used for salad purposes. The cotton-seed oil sold for salads is refined in part by the use of alkali, and this treatment removes all free, fatty acids. The samples of cotton-seed oil found upon the market all showed very low percentages of fi-ee, fatty acids due to the above treatment and to the tendencv of this oil to remain stable. One sample of unpurified, cold pi'essed cotton-seed oil exam- ined had 2.17 per cent of free acids, but practicallv all of this amount existed in the seed at the time of pressing, as free acids wei'e deter- mined within a few days after the oil was pressed. Table XXII. — Collon-seed oil. Determinations. Analysts. as, a Butyro-refrac- tometer read- ing at 16.5" C. H o - 1% II M - a C m ■M c > c 1 ll of faO>. go cS :::o o'al H De Negri and Fabris: a Minimum 0. 9230 .9250 .9226 .9236 .9160 .9300 1 .9250 .9216 .9362 Degrees. 50.0 .53.0 172.4 191.1 163.0 170.0 106.5 110.7 103.8 110.9 102.0 111.0 fl06.0 \108. 104.5 114.0 191.8 194.7 ° a 34.0 39.0 °C. Peret. Mfl.ximnm Tolman and Munson: h Minimum 72.3 75.6 1.4737 1.4757 66.2 73.4 74.0 77.0 7.i.5 55.0 71.0 04 Maximum 2 17 Allen: c 191.0 196.6 |l92.5 191.0 195.0 35.0 40.0 /3.5.0 \43.0 32.0 43.0 32.2 37.6 30.5 35.2 Ariiximiini Lewkowitsch:rf Minimum 1.4747 Twenty-two other anal- ysts: e Minimum Maximum a 10 samples. Annali del Laboratorio ehimlco centrale delle Gabelle, vol. 2, Gli Olii, pt. 2, p. 92. & 4 samples. fCom. Org. Anal., 3d ed., vol. 2, pt. 1, p. 140. d Oils, Fats, and Wa.xes, p. 374. c Annali del Laboratorio chimico centrale delle Gabelle, vol. 2, Gli Olii, pt. 2, p. 92, 32 OLIVE OIL AND ITS SUBSTITUTE^. Table XXII is a compilation of the results of a large number of analyses, and gives the limits which have been obtained for this oil. Some of these figures are so extraordinary that the oils from which they were obtained can hardly be considered otherwise than abnormal. In this bulletin the term " normal oils" is used to indicate those which are not so rancid as to be unfit to be eaten or which have not been oxidized by artificial means. On rancid or oxidized oils results can be obtained which are entirely difl^erent from those which would be found on fresh oils, and in this report salad oils only are considered. Cotton-seed oils with a specific gravity as low as 0.9160 and as high as 0.03CO are most likely abnormal. Such figures can hardly be consid- ered of any value unless further data as to free acids and condition of the oils are known. In this connection samples Nos. 1.3235 and 2.3656 of peanut oil in Table XXXIII serve as examples. The first oil was what is called a "blown" oil, and the results obtained with it are entirel}^ abnormal. It has a specific gravity of 0.936'4, an iodin number of 77, and saponification number of 199. The second has a specific gravity of 0.9155, but has 13.51 per cent of free acid. Such an oil could not be used under any circumstances as salad oil, and cei'- tainly should not be considered in establishing limits for peanut oil. When added in any considerable amounts to olive oil, cotton-seed oil is not difl]cult to detect, on account of its high specific gravity, iodin immber, Maumene figui'e, and index of refraction. Moreover, there are the qualitative tests of Bechi, Halphen, and the nitric acid reaction to detect it in small amounts. The Halphen test" is extremely delicate, detecting 1 per cent or less of the unheated oil. This test is characteristic of cotton-seed oil, and if obtained in an olive oil is proof of its presence. But Holde and Pelgry* have shown that cotton-seed oil if heated for ten minutes to 250- C. loses the power of giving both the Halphen and Bechi tests. The writers found that it took twenty minutes to completely destro}^ the power to give the Halphen test, but the reaction was greatly weakened on oils heated a much shorter time. This heated oil if refined would lose the taste and odor due to heating and could be mixed with olive oil in small amounts without giving the Halphen, Bechi, or Milliau test. But the nitric acid reaction is apparently not affected in any waj' by this heating. Tortelli and Ruggeri'' have made an extensive study of heated cotton-seed oil in order to discover means of detecting it in olive oil. They found that it was nece.ssary to heat the cotton-seed oil twenty minutes at 250° C. in order to completely destroy its power of reacting with Halphen or Bechi reagents. The values of the oil are not «U. S. Dept. Agr., Bureau of Chemistry Bui. 65, p. 32. ftChem. Rev. Fett. u. Hartz. Ind., 1899, 0: 67; Jour. See. Chem. Intl., 1899, 18: 711. fAnnali ilel Lab. chira. cent, delle Gabelle, 1900, p. 249. COTTON-SEED OIL. 33 affected to any great extent by this heating, as is shown in Table XXIII, talien from their work. Table XXIII. — Values of heated cotton-seed oil {Tortelli and Ruggeri). Temperature and time of heating. Specific gravity at 15.5° C. Butyro- reffac- tometer reading at 15.6° C. Mau- menS number. Hub! number. lodin number of liquid fatty acids. Melting point of fatty acids. Solidify- iTis point ul fatty acids. Oriffinal oil .. ... 0. 9240 Degree/!. 56.0 67.0 108.6 104.0 103.8 109.9 108.3 107.5 106.9 147.0 140.2 138.3 147.7 142.7 141.5 140.7 °C. 35.8 °C. ''50° C for ] minutes Original oil .9240 .9230 .9244 .9243 56.0 56.5 56.5 57.6 67.0 07.0 06.0 65.0 35.8 36.9 36.0 36.2 32.2 200° C. for 10 minutes 250° C. for 10 minutes 250° C. for 20 minutes 32.4 32.5 32.5 The iodin number of the liquid fatty acids is affected ))y heating to a greater degree than any other value, Itoing considerably lowered. Tortelli and Ruggeri propose the following method for the detection of the heated oil which depends on the fact that Avhile such an oil will not give the Halphen or Bechi test, the reacting substance is not entirely destroyed, and by concentrating this a reduction of silver is obtainable. The liquid fatty acids are separated as described under Muter's method." The liquid fatty acids are treated in a test tube with a mix- ture of 1 cc of a 5 per cent aqueous solution of silver nitrate and 10 cc of 90 per cent alcohol, and heated to from 70'^ to 80-' for several hours if necessary, in order to get a reduction of silver. By this method small quantities of heated cotton-seed oil in olive oil may be detected. Other reactions which'will show the presence of heated cotton-seed oil are the nitric-acid test, using acid of specific gravity 1.375, and the Brulle* test, with nitric acid and egg albumen. The former was tried on some heated cotton-seed oil which would not react with the Hal- phen reagent, and a sti'ong reaction was. obtained with a mixture of 10 per cent of heated cotton-seed oil and 90 per cent of olive oil. Smaller amounts could easily be detected. The test is not as sensitive as the Halphen or Bechi test on unti'eated oils, but it is of great value forusewith heatedoils. It may also be of value in determining whether a weak test with the Halphen reagent is due to a small amount of unheated cotton-seed oil or a larger amount which has been heated enough to weaken the Halphen reaction. Some of the other oils react, however, with nitric acid. Sunflower oil, treated bj^ this method, gives a deep brown color which can not be distinguished from the color obtained with cotton-seed oil. Peanut oil gives only a very slight test. Maize oil reacts very strongly, giving a peculiar reddish color that might be mistaken at first for the cotton-seed oil test. "IT. S. Dept. Agr., Bureau of Chemistry Bui. firi, p. 28. f-R. Brulle, Comp. rend., 1893, 106: loi;. 34 OLIVE OIL AND ITS SUBSTITUTES. The Brulle" test for cotton-seed oil is also effective on oils heated to' 250° C. It is conducted as follows: Place in a test tube 0.1 gvum of dry albumen finely powdered and 2 cc of nitric acid (3 parts nitric acid. 1.40 specific gravity and 1 part water) and 10 cc of oil. Heat without stirring until the acid begins to boil, then cautiously agitate until the albumen is dissolved. Under this treatment olive oil will not show an^' change of color, while cotton-seed oil can be detected by the red coloration. Other oils, such as peanut, sunflower, and rape, are also colored by this process. Olive oil forms an elaidin after this treat- ment, which is very different from that given by the other oils, except lard oil, which, because of its content of oleic acid, acts very similarly. Peanut Oil. Peanut oil is probably used as an adulterant of olive oil more exten- sively in Europe than in this country where cotton-seed oil is so com- mon. The oil has a pleasant, nutty flavor, and makes a good salad oil, for which purpose it is quite extensively used in Europe under its own name. The values of peanut oil are so little different from olive oil that consideral)le quantities of it could be mixed with olive oil without being dctei ted l)y tliese figures. Ta))le XXIV gives the results compiled from published data on peanut oil. Table XXIV.— Peanut oil. Determinations. Analysts. >> Us m k a c i a ao *- CO Q.- CO »i a c 3 ■■3 a a CO a? si oai CO § Si •t-. Eft O as Miintz, Durand, and Mil- liau:ii Minimum 0. 9n.'i\ . 9210J .9U0 .9200 . 9165 .9200 .9155 .9188 . 9160 .9220 Degrees. 46.0 49.0 56.7 45.0 51.0 46.5 63.2 44.0 G7.0 127.0 129.1 154.2 97.0 85.6 95.0 9^0 100.0 .87.8 96.3 85. 6 105. 190.0 194.0 189.4 193.0 188.8 191.8 189.3 196.0 31.0 29.0 34.0 27.0 81.0 33.2 S6.4 26.0 35.0 °C. 28.0 25.0 32.0 22.0 25.0 23.0 31.0 Perct. S. P. Sadtler:b Maximum 79 De Nes:ri and Fabris: c Minimum Tolman and Munson: d Minimum. 67.5 n.3 1.4707 1.4731 24 13 51 Twenty-one other ana- ly.sts: e Minimum ^r^)■v^mnm Maximum .9220 .9110 67.0 44.0 154. 2 127.0 105.0 85.6 196.0 188.8 36.4 26.0 32.0 23.0 13 61 Minimnm 24 aBulletin duMini.sWre de rAgrioulture, 1895, p. 139. 6 4 samples. Amer. Druggist and Pharm. Rec. 1897, vol. 31, no. 5. c8 siimples. Annali del Laboratorio chimico centrale delle Gabelle, vol. 2, Gli Olii, pt. 2, p. 12. d 5 samples. e Annali del Laboratorio chimico centrale delle Gabelle, vol. 2, Gli Olii, pt. 2, p. 12. From this table it can be seen that oils could be selected for admix- ture which would not affect the values of olive oils to any degree except a Chem. Ztg. Eep. 1888, 12: 107. PEANUT OIL SESAME OIL. 35 in case of very gross adulteration. Sample 499, Table XXXIII. a cold pressed oil prepared in this laborator}-, is an example of this. It has a specific gravity' of t).91S6, a Hiibl number of 87.8 and O.-iO per cent of free a(-id. Such an oil could be mixed in almost any proportion with an olive oil of low iodin number and not give even a hint from the physical and chemical values of its presence. Practicallj' the onlj^ test that is positive is the isolation of ai'achidic acid, which is present in peanut oil to the extent of from 3 to .5 per cent. In four samples of peanut oil examined in this laboratory from 3.41 to 4.24 per cent of the acid was found, having a melting point of from 72° to 73°. Allen " gives an average of 5 per cent. In Table XXXIII results are given on two samples of peanut oil, Nos. 13234 and 13235, which were exam- ined to determine the effect of age. Both had been kept in stoppered bottles for eight years; No. 1323.5 was a heated oil. Both were exceed- ingly rancid to taste and smell, but No. 13234 had only 2.93 per cent of free acid, showing that acidity is not an index of rancidity. No. 13235 shows that great changes have been brought about in the oil in the process of heating. Renard's* test is as satisfactorj- as any of the methods for detecting arachidic acid. Twenty grams of the oil to be tested should be taken so that enough of the arachidic acid can be separated to make the melt- ing point which should be determined in every case, as some oils, such as cotton-seed and lard, will give a precipitate wdiich resembles ara- chidic acid except that it has a lower melting point. Sesamk Oil. Like peanut oil, sesame oil has a pleasant tlavor and is well adapted . to the adulteration of olive oil. However, it is not extensively used in this country, as the analyses of commercial samples show. Table XXV gives the results compiled fi-om published data on sesame oil. "Com Org. Anal., 3d ed., vol. 2, pt. 1, p. 134. * Comp. Rend. 1871, 73: 1330. U.S. Dept. Agr., Bureau of Clieuiistry, Bui. (i.5, p. 33. 36 OLIVE OIL AND ITS SUBSTITUTES. Table XXV. — Sesame oil. Determinations. Analysts. aJ 2*0 6 11 nS III 0) Q ■So s e 1 a? og 1 a .2 S-3 i .... « □Q So De Negri and Fabris:a 0. 9230 .9237 .9218 .9230 .9200 .9250 Degrees. 63.0 64.0 61.3 54.0 65.0 68.5 "ma' 150.0 106.8 107.7 97.9 104.0 102.0 112.0 188.4 190.4 190.7 190.0 194.6 23.0 26.0 27.4 26.0 21.0 40.0 °C. 20.0 22.0 22.0 21.0 34.0 Perct. Maximum Tolman and Munson & Mlintz, Durand, and Mil- 73.3 i.4742 0.44 Tweiity-tive other ana- lysts: rf \r«-in"Trmm 1 "6 sample.';. Annali del LaboYatorio chimico oentrale delle Gabelle. vol. 2, Oli Olii, pt. 2, p. 82. ''1 sample. c Bulletin du Ministi^re de 1' Agriculture. 1.S95, p. 139. rfAnnali del Laboratorio ehimicn oentrale dclle Gabelle, vol. 2, Gli Olii, pt. 2, p. s-z. The specitic gravity, iiide.x of refraction, Maumene iiuniber, and iodiu number of thi.s oil are till materiallj' liigher than for olive oil, and serve as an indication of adulteration. The qualitative test of Baiidouin and VillavecehiaV nioditication of the .same, are character- istic of sesame oil and permit of the certain detection of amounts as small as 2 per cent. It must alwa_ys he remembered, however, that there are some olive oils from Italy and Tunis which give a reaction with this test which is difficult to difl'erentiate unless comparative tests are carried on with sesame oil, when they can be readily distinguished. Milliau " states that when the fatty acids were u.sed in making this test .0 1 Tuuis'oils the red coloration found with the oils themselves was not obtained. Maize Oil. Maize oil is produced in large amounts in the United States, and, owing to its cheapness, may lind use as a substitute for olive oil. This product, which is a semidrying oil similar to cotton-seed oil, has thus far been used but little for salad purposes, only one sample being found upon the market. It possesses the flavor and odor characteristic of maize, uiul these qualities aid in its detection when not mixed with other oils. The results of the analysis of a number of maize oils are given in Table XXVI. "Milliau, Bertainchaiid, and Malet, Hajiiairt siir lea huilea d' olive deTunisie, 1900, p. 33. MAIZE OIL MUSTARD-SEED OIL. Table XXVI. — Maize oil. 37 Determinations. Analysts. boo ¥ 02 S2.S IS .SO 1-2 II M OS s a w B o ■a? 1! 1 CO Id P4 De Negri and Fabris:a 0.9215 .9220 .9233 .9253 .9243 .9213 .9215 .9255 Degrees. 84.0 86.0 75.2 89.2 81.6 74.0 56.0 89.0 190.2 212. 5 ne.'o" 111.1 112. 6 116.7 123.3 122.7 118.6 119.6 123.9 190.0 190.8 189.9 193.4 189.7 192.6 188.0 193.4 °(7. 17.0 20.0 21.6 23.0 13.0 16.0 Perc(. Maximum Tolman and Munson:& Minimum 76.2 77.5 1.4760 1.4768 1 80 Archbutt <" . . 2 40 1.4766 22.4 16.0 20.0 13.0 14.0 Six other analysts: « 3 12 Maximum 3 50 "3 samples. Annali del Laboratorio chimieo centrale delle Gabelle, vol. 2. Gli Olu, pt. 2. p. 122. bi sample.s. rjour. Soc. Chem. Ind., 1899, 18: 346. dJour. Amer. Chem. Soc, 1900, 22: 453. e Annali del Laboratorio chimieo centrale delle Gabelle, vol. 2, Gli Olii, pt. 2, p. 122. The specific gravity, rise of temperature with sulphuric acid, index of refraction, and iodin absorption are much higher for maize than for olive oil, and the last three values are considerably higher than for cotton-seed oil. The high Maumene number and iodin absorption of this oil would materially iniiuence the values of olive oil even when added in amounts as small as 10 or 15 per cent. The content of solid fatty acids of maize oil is rather low, hence the iodin number of the liquid fatty acids is not so charactei'istic as with cotton-seed oil. Maize oil gives a peculiar red color when shaken with nitric acid (specitic gravity, 1.37), which is quite different from the color obtained with cotton-seed oil, and would sei've to differentiate them. Mustard-seed Oil. This oil belongs to the I'ape-seed oil group, and in general charac- teristics it differs but slightly from rape-seed oil, as is apparent from Table XXVII. 38 OLIVE OIL AND ITS SUBSTITUTES. Table XXVII. — Mustard-seed oil. Determinations. Analysts. 1 Butyro-refrac- tometer read- ing at 16.5° C. 1-2 a V a; C II 1 c 3 W c o '■So 1? CO ■a 1 De Negri and Fabris:n Minimum 0.9125 .9175 .9147 .9193 .9151 .9161 .9142 .9155 .9180 .9142 .9183 Degrees. 42.0 46.0 61.4 79.4 130.9 190.3 92.1 106.5 98.4 113.0 98.4 103.6 r 96.8 \98.8 96.0 96.0 170.2 174.6 173.0 182.8 173.9 174.7 171.2 173.3 °a 16.0 18.0 20.8 21.5 16.0 16.0 °C. Perc(. Tolman and Munson: b Minimum 74.5 76.5 1.4750 1. 4762 1.4761 1.4760 1.4740 13 Blasdale: <- Maximum . Crosseley and Le Sueur: d I .. .. J 39.0 44.0 108.0 Miintz, Durand and Mil- liau: *■ 16.0 16.0 15.0 Seven other analysts:/ Minimum \ Maximum ( a 6 samples. Annali del Laboratorio ehimico centrale delle Gabelle, vol. 2, Gli Olii, pt. 2, p. 37. b 5 samples. c2samples. Jour. Amer. Cliem. Sue., 1895, 17: 935. d2 samples. Jour. Soc. Chcm. Ind.. 189S, 17: 989. el sample. Bulletin du Minist^re de 1' Agriculture, 1895. p. 139. /Annali del Laboratorio chimico centrale delle Gabelle, vol. 2, Gli Olii, pt. 2, p. 37. It is probable that thi.s oil is seldom if ever used as an adulterant of olive oils, although it is frequently added to rape oil, and this may find its way into olive oil. Means of detecting it in small quantities are as unsatisfactory as for rape oil, and the analyst will scarcely be able to distinguish between the oils of this group. The presence of sulphur compounds in the oils of the Crucifei'se gives a means for their detection. If the oils are saponified with alco- holic potash and stirred with a silver spatula, the silver will become blackened by the formation of sulphid. Rape-seed and Colza Oils. Rape-seed and colza oils may be considered practicall_y identical as regards source and composition, and for convenience the terms are considered here as being synonymous. This oil is derived from vari- ous species of Brassjica of the family' Vruc'iferx., and according to Allen" is used as an adulterant for olive oil. According to the Codex Alimentarius Au.striacus rape oil or colza oil is the oil from the field cabbage {Brassicn campe^triH)., but all the following oils are sold under the name of rape oil: Colza oil from Brasslca campestria; rape oil from Brassiat carnpestris, variety najius; rape oil from Brmsica caiiipestris., variety rapa; Hederich oil from Bap/iaiiua Raphanistrwn or field radish, and radish oil from Raphmms satmus. Although the a Com. Org. Anal., 3d ed., vol. 2, pt. 1, p. 92. RAPE-SEED OIL. 39 values of thi.s oil would make small additions of it difficult of detec- tion, it is not so well adapted as a substitute for olive oil as the products previously mentioned under this class, owing to the acrid taste of even the well-refined oil. Analj'ses of rape and colza oils are given in Table XXVIIl. Table XXVIII. — Rape-seed and colza oih. Determinations . Analysts. >> Win 0. CO 6 aj s til s i 11 11 1 3 K 1 oj 32 Co S3 Si- 60 >. 2.22 O P-33 m 'id a a 1 Crosseley and Le Sueur: « 0, 9142 .9171 .9143 .9163 .9145 .9150 .9150 .9170 .9112 .9184 Degrees. 1.4744 1.4748 1.47.52 f 94.1 tl04.8 92.5 101.2 99.0 103.0 97.2 102.1 97.0 106.2 167.7 173.0 174.1 176.6 17.5.0 177.0 170.0 1S3.0 °c. °C. Perot. 1 74.1 74.8 54.5 67.8 48.0 56.0 49.0 51.0 50.0 59.0 13.5.0 152.5 133.0 155.0 Tolman and Munson: & Minimum 20.0 21.9 16.5 17.0 16.0 19.0 15.5 22.0 15.0 16.0 63 Miintz. Durand, and Mil- liau:c Minimum De Negri and Fabris:'' Twenty-one other ana- lysts: e Minimum i n7 samples. Jour. Soc. Chem. Ind., 189.S, 17: 989. '»4 pample.s. <*2 samples. Bulletin du Ministi^re de I'Agrifulture, 1895, p. 139. ^14 samples, .\nnali del Laboratorio ehimico centrale delle Gabelle, vol. 2, Gli Olii, pt. 2, p. 2l>. e Annali del Laboratorio ehimico centrale delle Gabelle, vol. 2, Gli Olii, pt. 2, p. 26. The specific g-ravities of these oils are practicallj' identical with that of the olive; the index of refraction, iodin number, and rise of tempera- tui-e with sulphuric acid are considerably higher. The saponification number is much lower than for olive oil or for any of the oils used to adulterate it, with the exception of the other members of the rape-oil group. The average saponification value given for rape oil is about 173, while the average value for olive oil is about 193, and an olive oil having a saponification value much below 190 should be looked upon with suspicion. An addition of less than 30 per cent of rape oil would probably be difficult to detect, Vmt this amount should be sufficient to materially afiect the values of a normal olive oil. Low specific gi'avity accompanied by a high index of refraction is one of the marked char- acteristics of rape oil, wherein it differs from most oils which with a low specific gravity have a low refractive index. Valenta" has suggested the difi'erentiation of oils by their solubility in glacial acetic acid of 1.0562 specific gravity, and states that rape and mustard oils are the only common oils not completely soluble in this "Dingier, 1884, 252: 296; Jour. Chem. Soc, 1884, 46: 1078. 40 OLIVE OIL AND ITS SUBSIITUTES. acid. Allen " coufirms the statement of Valenta, but suggests that the solubilitj" of an oil is greatly increased bj' a high percentage of free acids. The strength of acetic acid used, according to this author, maj' vary considerably without greatly affecting the solubility. Hurst,* on the other hand, finds that rape and colza oils are completely dissolved by glacial acetic acid and gives the temperature turbidity of from 73° to 99°. Thomson and Ballantyne " have also studied this question and find that Valenta's statement liolds good only when acetic acid of spe- cific gravity 1.0562 is employed; if an acid of specific gravity 1.0542 is used rape oil is completely soluble. In working in this laboratt)r3' upon Valenta's test with acid of 99.5 per cent strength it was found that rape oil and mustard oil both dis- solve completely at a temperature of 120° C, although at a very slightly reduced temperature the oils are again partly precipitated. Olive oil is readily solulile at 120°, but precipitates again upon a slight reduction of temperature. Mixtures composed of 20 per cent and 40 per cent of rape oil with olive oil and similar mixtures of mustard oil showed no distinction from pure olive oil in respect to solubility. Hence as a means of detecting rape oil, and especially mixtures of the same -with olive oils, this test must be considered of little value. Sunflower Oil. Sunflower oil has a mild taste and pleasant odor, and the cold drawn oil is said to be used in some sections of Europe for culinary purposes. '* The physical and chemical characteristics of this oil are so widely dif- fei-ent from those of olive oil that additions of even relatively small amounts to olive oil would lie sufiicient to make the values of the hitter abnormal. The compiled results of the analyses of sunflower oil are given in Table XXIX. ajour. Soc. Chem. Ind., 1886, 5: 69, 282. 6 Jour. Soc. Chem. Ind., 1887, G: 22. <;Jour. Soc. Chem. Ind., 1891, 10: 233. rfjour. Soc. Chem. Ind., 1892, 11: p. 470. SUNFLOWEK OIL POPPY-SEED OIL. Table XXIX. — SimHoirer nil. 41 Determinations. Analysts. CO Butyro-refrac- tometer read- ing at 15.5° C. §0 1-2 a a i s |i S a) Qj a 0.-S 1 a 3 w a o r .S.S 32 MIS' 1 = 1 De Negri and Fabris* « |o.9260 .9201 .9205 .9240 .9262 .9240 .9260 .9260 .9520 Degrees. /72.0 \75.0 jeo.o f67.5 173.0 167.0 119.7 120.1 fl04.1 tl08. 3 119.7 135. 122.0 135.0 129.0 133.2 188.0 189.3 191.2 192.3 188.0 194.0 188.4 197.6 192.0 194.0 °a 22.0 24.0 }21.0 }23.0 } 18.0 17.0 PCT-rf. Maximum 72.1 T2.1 \ 1.4736 1. 4739 1. 4769 Tolmau and Miinson: f> Minimum r IS \1.72 Lewkowitsehic J Allen: rf Minimum . . Seven other analysts: Minimum 17.0 23.0 "3 samples. Annali del Laboratorio chimico centrale delle Gabelle, vol. 2, Gli Olii. pt. ; 6 2 samples. I- Oils, Fats, and Waxes, p. 356. ((Com. Org. Anal., 3d ed.. vol 2, pt. 1, p. 93. p. 106. Poppt-Seed Oil. According to Allen" and Lewkowitsch,* this oil is quite largely used in Europe as a salad oil and for culinary purposes, and is used some- what as an adulterant for olive oil. In this countiy, however, it is not used either as a salad or cooking oil to any extent, and it is doubt- ful whether it is ever used as an olive-oil adulterant. Fi"om Table XXX it is seen that the specitic gravitj-, index of refraction, Maumene number, and iodin absorption of poppy oil are exceptionally high, and these characteristics are sufficient to indicate its addition to an olive oil, although, in the absence of distinct qualitative tests, the difficulty of definitely distinguishing between this oil and some of the others already mentioned, when added in small proportions, is apparent. » Com. Org. Anal., 3d ed., vol. 2, pt. 1, p. 94. * Oils, Fats, and Waxes, 2d ed., p. 352. 42 OLIVE OIL AND ITS SUBSTITUTES. Table XXX. — Poppy-seed oil. Determinations. Analysts. Butyrorefrae- tometer read- ing at 15.5° C. Index of refrac- tion at 15.5° C. a ii DO « 1 a 3 W o if 1 Solidifying point of fatty acids. De Negri and Fabris: « lo. 9270 .9239 .9244 .92.% .9240 .9370 Degrees. 88.5 75.8 85.5 80.0 71.0 86.4 1136.8 \137.5 213.0 237.0 222.0 133.2 134.9 133.0 130.5 141.0 193.4 193.8 190.2 193.8 192.8 194.0 °c. 20.0 21.0 28. 4 25.8 20.5 |20. ft °f. Pad. 77.1 77.8 1.4760 1.4770 Tolman and Munson: b Minimum 16.0 0.90 2.31 Mlintz. Durand, and Mil- Sixteen other analysts: 1 a 3 samples. Armali del Laboratorio chimico centrale delle Gabelle, vol. 2, Gli Olii, pt. 2, p. 114. b 2 samples. 1 sample. Bulletin du Ministjre de I'Agriculture, 1895, p. 139. Lakd Oil. This oil i.s so manufactured that it remains liquid at ordinarj' tem- peratures, and when well retined is entirelj^ free from the taste and odor of lard. When heated, however, this odor is developed, and may .serve as a means of distinguishing lard oil when not mixed with other oils. If so mixed, however, even though the lard oil be largel_y in excess, this odor is sufficiently masked to make the test of little value. The following table gives a nunilier of analyses of lard oil: Table XXXI. — Lard oil. Determinations. Analysts. to Butyro-refrae- tometer read- ing at 15.5° C. Index of refrac- tion at 15..5° C. B 3 C Is § 11 S3 1 a 3 B c o OS oi V p. ii bL'C en o . Tolman and Munson; « 0.914S .9175 } .9154 \ .9160 [ .9160 Degrees. 66.8 69.5 65.2 1.4702 1.4720 1.4692 39.9 47.8 103.3 110.8 69.7 77.2 73.0 f 67.0 t 82.0 60.0 19.5.3 197.7 193.0 189.5 196.0 °C. 33.2 38.4 3,5.0 > °C. 31.0 Pern. 0.2H 1.28 Diiyk:/> Maximum 41.0 33.0 91.0 Allen:*- Minimum 1 35.0 34.0 Muntz, Durand. and Mil- liaujrf a 4 samples. ire de I'Agriculture, 1895, p. 139. LARD OIL — MISCELLANEOUS OILS. 43 The specific gravity, refractive index, rise of temperature with sulphuric acid, and saponification number of this oil are practicallj' identical with the same values of olive oils. The iodin number is much lower, and the melting point of fatty acids much higher than for olive oils, but when mixed, for example, with an olive oil having a high iodin number and a consequently low melting point for its fatty acids as much as 50 to GO per cent of the lard oil could be used without ren- dering these values abnormal for pure oils. The lard oils have a high content of solid fatty acids, but this factor is rendered of little value when the oil is mixed with an olive oil having a high iodin number, since such an olive oil will prol)ably have a correspondingly low con- tent of solid fatty acids as is shown by Table XXXIII. Miscellaneous Oils. The oils named ir. tables XXXll and XXXIII were analyzed to obtain further data regarding their values, and also for the purpose of studying their use in the adulteration of olive oil. Through thfs. kindness of the V. D. Anderson Company, of Cleveland, a number of cold-pressed oils were prepared from seeds which were identified in the seed laboratory of the Department of Agriculture. They are as follows: Brown niUMturi 1 Brassica anensis (cliarlock ) . Black luustaril Brassica juncea (Indian mustard). Yellow nuistard _ Sinapis alba (yellow mustard). Rape Brassica napus. Poppy - Papaver somnifera ( iipiiim poppy ). The cocoanut oil was pressed from the flesh of cocoanuts. The pea- nuts used were from Virginia. The almond, cotton-seed, and linseed oils were prepared from commercial seed. Other oils were prepared in the laboratory. There are a number of commercial oils included in these tables, l)ut as there was no way of being assured of their purity the results obtained are not of great viilue. Sample No. 23606 was sent by Armour & Co. as a pure neutral lard oil and it had practically no lard odor or taste except when heated. The.se samples were discussed under the headings of the various oils. Table XXXII. — Description of miscellaneous oils. ^™-^ i Kind of oil. Source. Description. 22077 773 494 Cocoanut do Palm India Refining Co., Philadelphia, Pa. V. D. Anderson Co., Cleveland, Ohio. Schiefflein & Co., New York City Konut — cocoanut oil, lard substitute. Cold-drawn oil. Commercial oil 22433 Lard 22434 23606 487 1181 1182 do do do Magnolia do Z. D. Oilman, Washington, D. C Armour & Co., Chicago, 111 Schiefflein & Co., New York City James Brody, Biloxi, Miss ... .do Neutral lard oil. Commercial oil. Oil from pulj) ol" magnolia seed. Fat from pulp of magnolia seed. Oil from pulp of magnolia seed. 1160 do do 44 OLIVE OIL AND ITS SUBSTITUTES. Table XXXII. — Description of miscellaneoutt oils — Continued. Serial No. Kind of oil. Source. Description. 23666 499 Peanut do ....do Z. D. Oilman, Washington, D. C Prepared In laboratory Commercial oil. Cold-drawn oil 13234 13235 do 8 years old; cooked oil. Cold-drawn oil. 772 -1149 do do Mustard do do . . do ... V. D. Anderson Co., Cleveland, Ohio. 480 495 .Scliiefflein & Co., New York City Commercial oil. 770 771 V. D. Anderson Co., Cleveland, Ohio. . ...do Cold-drawn oil; brown nuistard. 776 do do 490 SchiefRein & Co., New York City Prepared in laboratory. 496 do do do Almond Sesame Sunflower do 775 937 v. D. .\nderson Co., Cleveland, Ohio. V. Villavecchia Rome, Italy Do. Colza oil di Vercelli (Picimente). Cold-drawn oil. Commercial oil. 1187 489 23624 V. 1). .\nderson Co., Cleveland. Ohio. Schiefflein & Co., New York City 498 do ". Do. 491 444 497 777 1159 1160 Maize do do do Cotton-seed .. do Schiefflein & Co., New York City Glucose Sugar Refining Co. , Chicago, Indianapolis Hominy Mills, Indiana. V. D. Anderson Co.. Cleveland, Ohio. American Cotton Oil Co., New Y'ork City. Commercial oil. Do. Cold-drawn oil. Commercial oil—" Butter Oil." 1161 do do Commercial oil — "Cooking Oil." 1186 493 774 1188 do Poppy V. D. Anderson Co., Cleveland. Ohio. Schiefflein & Co., New York City V. D. Anderson Co., Cleveland. t)hio. do .*. Cold-drawn oil. Do. Do. Table XXXIII. — Analt/seK of mtscfllaneoii!! oils. COCOANUT OIL. Serial No. Specific gravity at 15.5° C. Butyro- refrac- tomc- ter reading at 15.5° C. Index of re- frac- tion at 15.5° n. Man- Spe- cific tem- Hiibl num- ber. lodin num- ber of liquid fatty acids. Sapon- ifica- tion value. Melt- ing point of fatty acids. ''""'J fattv fatty '^i'y '"^Z acids as '''^""'- oleic. num- ber, pera- ture reac- tion. 6s 22077 0.9269 .9259 Degrees. 7.90 8.58 °C. Per el. Per et. 773 49.1 1.4587 21.0 44.0 31.9 259.5 25.2 66.90 0.11 PALM OIL, 494 0.9128 53.0 99.0 201.0 22433 0.9148 67.4 1.4706 47.8 106.2 76.9 94.0 98.9 195.7 33.2 18.90 0.75 23434 . 9145 67.4 1.4706 46.8 104.0 77.2 101.3 195.3 34.2 19.30 .78 23606 .9160 69.5 1.4720 46.5 103.3 69.7 9.5.8 101.3 197.7 38.4 26.68 .28 487 .9175 66.8 1.4702 39.9 110.8 72. 6 93.9 97.9 196.2 35.8 21.43 1.28 MAGNOLIA OIL. 1181 0. 9128 64.5 81.7 76.1 80.4 106.2 106.7 100.3 189.5 189.2 34.3 38.2 18.32 24.24 15.48 38.07 1182 48.28 .9130 65.0 1 MISCELLANEOUS OILS. 45 T.\Bi.E XXXIII. — Analyses of miscellaneous oils — Continued. PEANUT OIL. Serial No. Specific gravity at 15.5° C. Butyro- refrac- tome- ter reading at 15.5° C. Index of re- frac- tion at 15.5° C. Man- mene num- ber. spf- CltlC tem- pera- ture reac- tion. Hiibl num- ber. lodin num- ber of liquid fatty acids. 11 it Sapon- ifica- tion value. Melt- ing point of fatty acids. Solid fatty acids. Free fatty acids as oleic. 23656 499 13234 <■ 1323T 772 1149 0.9155 .9186 .9188 .9364 .9188 Degrees. 67.5 70.0 71.0 75.0 71.3 70.5 1.4707 1.4723 1.4729 1.4763 1.4731 1.4726 61.0 46.5 65.6 67.3 63.2 135. 5 129.1 154.2 186.9 136.3 89.1 87.8 191.4 191.8 190.7 °C. 33.2 34.3 36.0 37.6 36.4 33.6 Perct. Perd. 13.51 a .40 f.2.93 77.0 96.3 94 3 199.0 189.9 1SS 8 f5.96 114.0 d .24 MU.STARn OIL. 486 0.9178 .9170 .9184 .9193 .9147 76.1 76.5 76.2 76.5 74.5 1.4759 1.4762 1.4760 1. 4762 1.4750 68.5 68.2 77.6 79.4 61.4 190.3 189.4 165.4 169.3 130.9 103.0 105. 8 110.4 113.0 98.4 175.9 176.0 178. 5 182.8 173.0 21.0 21.8 20. S 20.8 21.1 4.05 1.06 2.32 Trace. 1.13 495 770 771 776 114.2 119.8 103.1 115.7 116.8 121.1 103.0 .38 .48 .34 .13 RAPE OIL. 490 0. 9161 74.3 1. 4749 .54.5 151.4 92. 5 100.5 96.9 175.7 20.0 0.12 3.67 496 .9143 74.3 1.4749 54.9 152.5 92.7 101.5 98.0 174.7 21.9 1.02 .63 775 .9163 74.1 1.4748 63.6 136.6 101.3 105.1 106.0 176.6 20.5 Trace. 1.26 937 .9158 74.8 1 1.4752 67.8 144.5 101.2 107.5 174.1 20.4 1.43 1.62 ALMOND OIL. 0.9186 1 70.9 4.5.3 117.6 96.2 192.5 i 23. 489 0.9218 73.3 SESAME OIL. 170.3 106.6 U.5.4 190.7 27.4 0.44 SUNFLOWER OIL. 23624 498 0.9201 .9205 72.7 72.1 1.4739 1.4736 60.0 166.7 108.3 104.1 113.8 105. S 117.8 113.8 MAIZE OIL. 491 444 497 777 0.9233 .9256 76.2 77.3 75.6 77.6 1. 4760 1.4767 1. 4757 1. 4768 75.2 76.5 9.2 208.9 212.5 119.2 119.7 116.7 123.3 133.3 126.6 129.4 134.5 134.5 134.8 132. 1 139.8 COTTON-SEED OIL. 193.4 ; 191.5 191.7 189.9 22.0 23.0 1159 1160 1161 1186 0.9226 . 9226 . 9226 .9236 72.5 72.3 72.3 75.6 L4738 1 1.4737 ! 1.4737 1.4757 66.4 73.4 66.2 67.1 172.9 191.1 172.4 174.3 103.8 106.2 104.8 110.9 I 197.1 3-5.5 196.9 39.0 196.0 39.6 198.5 I 38.0 6.98 6.70 7.07 7.44 3.12 1.80 ""'3.' 66 22.90 22.43 23.60 0.07 .07 .04 2.17 a3.41 per cent arachidic acid; melting point 72.5°; cold pressed oil. 63.78 per cent arachidic acid: melting point 72.8°. el. 24 per cent arachidic acid: melting point 73°. rf4.12 per cent arachidic acid; melting point 72°: cold pressed oil. « Cooked oil. 46 OLIVE OIL AND ITS SUBSTITUTES. Table XXXIII. — AnahiKef of miscellaneous oils — Continued. POPPY OIL. Serial No. Specific gravity at 15.6° C. Butyro- retrac- tome- Index of re- Mau- men^ num- ber. Spe- cific tem- pera- ture reac- tion. Hiibl num- ber. lodin num- ber of liquid fatty acids. Sapon- ifica- tion value. Melt- ing point of fatty acids. Solid fatty acids. Free fattv reading! "°"-g* at 15.6° ^^a" c. ^■ i.-6 313 o to 6^ acids as oleic. 0.9239 .9244 Degrees. 1.4"6(i 1.4770 85.5 75.8 237.6 213.0 133.2 134.9 190.2 193.8 °C. 25.4 25.8 Per. ct. "'e'.hi' Pei-ct. 2.31 774 142.0 151.7 .90 LINSEED OIL. 1188 0.9318 88.8 1.4831 179.5 191.7 19.2 3.88 0.40 OLIVE OILS OF KNOWN ORIGIN. California Oils. The oils in Tables XXXIV aud XXXV were obtained principally from producers of e.stablished reputations and were accompanied by affidavits as to purity. Three samples, made at the station, were obtained from G. E. Colby, of the California Agricultural B^xperi- nient Station. The oils reported on are from all parts of the State devoted to olive culture and represent practically all the ditierent existing soils and climatic conditions, which undoubtedly exert a great influence on the chemical and physical characteristics of the samples. The results give a good idea of the variability of California oils. The analyses are more complete than any previoush' published data on this subject, which gives them added value in determining the limits of the various values. The per cent of free fatty acids eliminates two oils which would otherwise give an extraordinary variation to the spe- cific gravity and index of refraction figures, a variation that is certainly not legitimate for the grade of oils considered here. Oils such as Nos. 22619 and 673 are not fit for use as salad oils, as they contain 44 and 12 per cent of free acid respectively. This factor should always be taken into consideration in reporting low results on specific gravit}' and refrac- tive index. The variety of olive and the climate and soil may greatly affect the oil ; how much these factors affect the produt't must be decided by further study. Six samples of oil (Nos. 23456, 831, 833, 23457, 832, and 834) show the uniformity of oils produced from different varieties of olive where the soil and climatic conditions are the same and the same process of manufacture is used. The fir.st three were made from Ital- ian varieties and the last three from the Mission olive. The Mission olive, introduced into California by the old Mission fathers, is the variety generally grown in the State, and most of the oil made comes from it. Table XXXVI gives the compiled results of analyses of California oils. CALIFORNIA OILS. Tablk XXXI \'. — rkscription of Cnlifornia olive oiln of tvoinr origin. 47 Serial No. Description. 23692 23463 22617 22618 22619 John Bidwell estate, Ghico. Fred Busby, Concord G. E. Colby, Berkeley. do do 22713 Elwood Cooper, Santa Barbara. 22714 do 22715 do. 234oS 23649 844 838 839 840 234.56 831 833 23487 832 834 23462 50S 836 837 835 1091 23605 798 795 796 797 23460 23461 23124 841 842 843 23459 673 do Ehmann Olive Co., Oroville do C. M. Gilford, San Uiego do do Edward E.Goodrich, Santa Clara . do do do do do J. C. Gray, Oroville James Hill & Sons, Lus Angeles . do : do do J. A. Kleiser, Cloverdale Peveril Meigs, Santa Barbara do do do do Morris tt Smith, Yolo Pr. Prosek, (iuerneville J.O. Riddell.Kedlands do do do Vincent C.Smith, Napa do " Rancho Chico " pure olive oil: made from Mission olives. Pure olive oil from Busby'.s olive grove; made from Mission olives. Oil from Redding Picholine olives; made in 1M93. Oil from mixed varieties; made in 1898. Oil from Manzanillo olives (poor quality); made in 1900. Highest grade olive oil; raade from Mi.ssiou olives. Second pressing olive oil, 10 years old; made from Mission olives. Common grade olive oil (for lubricating and similar piuposes); made from Mission olives. Pure oUve oil, highest grade; made from Mission olives. Pure olive oil. Do. "Gifford's Best" olive oil; made from Mission olives. Olive oil just from separator; made from Mission olives. Oliveoil 6 weeks old; made from .Mission olives. El Quito olive oil, Italian variety. El Quito olive oil, Italian variety, 1901. El Quito olive oil, Italian variety, 1902. El Quito olive oil. Mission variety. El Quito olive oil. Mission variety, 1901. El Quito olive oil. Mission variety, 1902. Pure olive oil from Mount Ida olive grove; made from Pieholine olives. Hill's pure olive oil. Hill's pure olive oil; sea.son 1901. Olive oil, first pressing, 1902. Olive oil, second pressing, 190'-'. Pure olive oil. Meigs's pure olive oil; made from Mission olives. Oliveoil; made from Mission olives. Olive oil; sample taken from top of barrel. Olive oil; sample taken from middle of barrel. Olive oil; sample taken from bottom of barrel. Pure olive oil. Do. Riddell'spure olive oil. Oil from ripe olives, 1901. Oil from ripe olives, 1902. Oil from green olives. 1902. Pure olive c»il; from "Glen Olive" farm. Second pressing olive oil; from "Glen Olive " farm. Table XXXV. — Analyses of California olive oils of known origin. h c '4 3 H (d 1? II c oi g d 3 lodin num- ber of liquid fatty acids. Saponification value. o •11 ii CD — S 2 1 'So 1 "a id «^ 94.3 94.4 1° 23692 .... 0.9168 .9164 Degrees. 68.5 68.4 67.3 67.5 62.0 68.7 68.5 68.2 68.7 68.0 68.5 69.2 69.2 68.9 68.3 68.8 68.8 68.3 68.8 68.8 1. 4713 1.4712 1.4706 1.4707 1.4672 1,4715 1. 4713 1.4711 1.4715 1.4710 1. 4713 1.4718 1.4718 1. 4716 1.4711 1.4715 1.4715 1.4711 1. 4715 1. 4715 86.6 85; 6 78.5 83.7 79.6 8.5.3 84.6 84.7 88.2 83.4 84.2 86.2 89.0 86.3 84.3 85.2 84.8 86.2 84.9 84.5 96.6 91.5 191.2 191.9 194.4 192. 6 191.8 191.1 191.5 191.3 191.4 192. 1 189.7 190.6 189.9 189.4 191.9 189.3 189.8 191.6 189.3 189.3 °c. 22.6 21.3 30.2 20.7 24.5 2'2'4 20.5 23.5 ■2-2.6 2.5.8 '24.0 ■21.2 24.0 23.4 ■20.6 20.2 21.1 •20. 5 19.4 Feret. 5.12 4.92 "h'.'n 3.87 '"h'.ib 4.94 6.94 7.23 ""6.'55' 3.39 5.40 6.03 Per ct. 0.95 23463-..- '22617 48.0 106.6 .79 .36 22618 ^ 8.21 2'2619a 44.40 22713 . 94.9 "gi.'g' 88.9 94.3 92.2 90.5 96.8 .73 22714. 1.26 22715 2. 7f, 23158 . - - - 23649...- 844 .9169 .9164 .9180 .9169 .9171 .9169 .9169 .9168 .9170 .9166 .9173 .9168 48.4 43.5 46.9 49.5 48.4 48.2 47.7 46.6 48.0 47.0 47,6 46.2 107.6 96.6 97.9 108.5 106.0 105.7 106.0 98.1 101.0 104.4 100.1 97.2 .73 1.43 .35 838.... 839.... 840.... 23456.... 831 ""93.'4' 96.4 98.2 96.3 95.4 1.07 3.51 1.09 .63 .61 833.... 23457.... 832.... 834...: "9i.'2' 95.2 93.5 93.2 94.4 .65 .97 .86 .34 "Not included in average on account of high percentage of free acid. 48 OLIVE OIL AND ITS SUBSTITUTES; T.tBLE XXXV. — Analyses of California olive oils of known origin — Continued. 1 GO 1.2 a a d ■a o B c ll 1 a 5 3 lodin num- ber of liquid fatty acids. 5 ^ r 1 *^ ■3.5- 23462.... .506 .... .9162 .9174 .9174 .9167 .9167 .9167 .9171 .9177 .9177 .9177 .9177 .9167 .9162 .9171 .9168 .9168 .9169 .9162 .9149 Degrees. 66.9 68.6 68.8 68.4 68.2 68.8 68.5 68.8 69.0 68.8 68.8 68.2 67.5 68.2 68.8 68.7 68.6 67.7 66.4 1.4703 1.4713 1. 4715 1.4713 1.4711 1.4715 1.4713 1.4715 1.4717 1. 4715 1.4716 1.4711 1.4707 1.4711 1. 4715 1.4715 1.4714 1.4709 1.4699 43.0 38.0 48.2 45.0 44.8 45.3 47.1 51.0 60.0 .52. 1 50.2 47.0 45.0 4.5. 5 47.1 4G.8 45. 6 45. o 4.5.0 96.5 98.9 106.7 98.6 98.2 94.5 104.2 107.3 106.2 109.7 106. 6 104.0 100.0 "gs.'s' 97.7 96.2 101.2 96.0 79.9 84.4 86.0 84.2 82.7 81.9 88.5 89.7 89.7 89.8 89.8 86.7 83.0 83.7 86.9 87.2 86.1 82.9 83.3 91.7 94.4 192.2 193.1 190.7 190.3 190.4 190.0 191.6 190.0 1.89.8 189.9 189.7 190.4 192.0 193.3 189.4 189.5 189.6 191.6 189.5 °a 31.0 22.4 24.8 23.6 26.0 26.6 20.2 19.2 19.8 19.2 19.6 23.4 28.0 25.4 21.6 21.4 22.8 25.0 21.6 Per el. 10.91 ""b'.ih' 6.19 12.96 2.43 ""4.' 73' 4.69 5.44 0.24 7.62 6.20 8.61 7.52 4.33 5.69 7.58 Per d. .79 71 836 ... . 2.51 837.... 835.... 1091 .... 93.1 92.6 .51 .96 1.42 23605.... 798.... 94.6 95.0 1.54 .63 796.... 796.... 797.... 23460 .... 23461 .... 23124.... 841 .... ' '93."8' 92.4 92.8 98.7 98.8 98.6 95.8 95.4 93.7 .75 .61 .63 2.24 1.07 .47 .20 842 .... .21 843 ... . .28 234.59.... 673o... 90.3 93.3 1.72 12.11 Average Max .... Min .9170 .9180 .9162 68.4 69.2 62.0 1.4713 1.4718 1.4703 46.9 52.1 38.0 101.8 109.7 94.5 85.3 89.8 78.5 92.8 96.6 88.9 96.0 98.8 90.5 190.9 194.4 189.3 22.9 31.0 19.2 5.86 12.96 2.02 1.20 44.40 .20 f'Not included in averaiEre on account of high percentage of free acid. Table XXXVI. — Analyses of California olive oils. (Compiled. ) Determinations. Analysts. V Sits 1 ^ GO'S S2.S n ^0 ^& <2 ■o g go a-s || 00 = 0) .a a H 1 u M c > 1 h: 03 her:- -a t Blasdale:n 0. 9161 .9174 .9162 .9180 .9140 .9185 Degrees. 1.4710 1.4716 1.4703 1.4718 1.4689 1.4717 45.0 47.0 38.0 82.1 94.5 109.7 80.0 86.5 78.5 89.9 77.7 93.8 190.5 193. 5 189.3 194.6 187.0 193.5 21.0 26.0 19.2 31.0 21.0 26.0 Perd. Maximum Tolman and Munsonib Minimum Maximum 66.9 69.2 0.20 44.40 Colby :■-■ ATinimiim Maximum. n 11 samples. Jour. Amer. Chem. Soc., 1895, 17: 935. 6 42 samples. <; California Agr. Expt. Sta. Kept., 1897-98. p. 166. Italian Olive Oils. These oils, re.sults upon which are given in Tables XXXVIl and XXXVIII, were obtained throug-h V. Villavecchia, chemist of the custom-house at Home, and Giacomo Dellapiane f u Andrea, of Genoa. The oils repi'esent all the large oil-producing districts of Italy. It is impossible to give the variety of olive used on account of the great number of varieties in Italy; each small district may have a distinct variety of olives. The Italian olive oils are not materially different ITALIAN OLIVE OILS. 49 from the California oils. The}' have a somewhat lower Hiibl iium- ber, and the percentage of solid fatty acids and the melting point of the free fatty acids are on the average considerably higher. One noticeable difference between the two oils was observed after they had stood in an ice box for several weeks. Many of the California oils showed no separation of solid fats and none of them l)ecame solid, while nearly all the Italian oils did become solid. This characteristic also held with the commercial oils. The French oils resembled in this respect the Italian oils. Tables XXXIX and XL give the com- piled results of analyses of Italian and miscellaneous olive oils, respectively. Table XXXVII. — Description of Italian olive, oils of hicwn origin. Serial No. 680.. 933.. 960.. 961.. 936.. 986.. 962 931.. 932.. 958.. 969.. 934.. 952.. 953.. 954.. 955.. 957.. 966.. Source. Fred Bailer & Co., Messina V. Villavecehia, Rome Giacomo Dellepiane fii Andrea, Genoa. do V. Villavecehia, Rome do Giacomo Dellepiane fu Andrea, Genoa. v. Villavecehia, Rome do Giacomo Dellepiane fu Andrea, Genoa. do V. Villavecehia, Rome Giacomo Dellepiane fu Andrea, Genoa. ....do ....do ....do do ....do Description. Pure olive oil (Bari). Olio di oliva di Bari (Puglie). Bari, first quality. Bitonto. Olio di oliva di Bitonto (Puglie). Olio di oliva 'ees. 67.9 67.7 67.6 67.6 (-.7. 7 07.7 67. 67.6 67.5 68.0 68.0 67.6 68.0 67.3 68.5 67.8 68.0 68.3 67.8 68.5 67.3 S a a u-> r-i ■J u i.9160 .9180 Degreee. 32.0 36.5 33.0 36.6 32.0 37.0 ;;;;;;; 79.1 88.3 81.1 89.8 79.0 87.1 187.9 192.2 185.0 192.0 188.8 192.3 "C. °a ft'. c(. De Negri and Fabris: a De Negri and Fabris: « Maximum .9166 i 83.7 ! Miintz, Durand and Mil- Han: e .91.'>8 .9163 .9169 .9156 .9180 30.0 35.0 37.0 39.6 49.1 83.3 97.2 83.7 84.0 24.0 24.5 23.7 21.6 29.3 22.0 23.0 Tortelli and Ruggeri / Tolman and Munson: if 67.3 68.5 1.4703 1.4713 95.6 104.7 79.2 86.1 189.7 192.0 O.Gl 2.79 .9180 .9145 104.7 83.3 89. 8 79.0 192.0 185.0 29.3 24.0 1 a Annali del Laboratorio chimico centrale delle Gabelle, vol. 2, Gli Olii, pt. 2, p. 114. bl8 samples. Oil from green olives. c 17 samples. Oil from ripe olives. 0. 53 Rjimples. Pure oils from various sources. e4 sampk's. Bulletin du Minist6re de P Agriculture. 1895. /Annali del Laboratorio chimico centrale delle Gabelle, 1900. vol. 4, p. 249. g 18 samples. Table XL. — Miscellaneous olive oils. [Compiled.) Analysts. Miintz, Durand and Mil- liau (oils from Africa}:" Minimum Maximum Muntz, Durand and Mil- liau foils from Spain): ft Minimum Maximum Miintz, Durand and Mil- liau ( nils from Portugal } :b Minimum Maximum Miintz, Durand and Mil- liau (oils from Greece):'' Minimum Maximum Miintz, Durand and Mil- liau (oils from Turkey )&: Minimum Maximum Miintz, Durand and Mil- liau (oils from the Le- vant):'' Minimum Maximum Determinations. 5u 0.9169 .9172 I .9160 I .9167 £3 c . 9165 Degrees. 30.0 35.0 fSO.O 136.0 (30.0 t35.0 (30.0 \35.0 (30.0 136.0 ao Is CO * 83. 3 84. 1 97.2 84.5 83.3 97, .2 ;' 83.3 I 84.1 83.3 97.2 « 4 samples. Bulletin du Ministt^re de 1' Agriculture, 1895, i> Bulletin du Ministire de 1' Agriculture, 1896, p. 139. 83.3 97.2 83.3 97.2 p. 139. 83.6 c > c p. 03 6X1 >. 1 Bolidi point acids. °c. 24.0 26.0 "C. 22.5 24.5 24.0 22.0 24.5 23.5 26. 23.5 24.6 23.0 24.5 23.0 Perct. COMMERCIAL OLIVE OILS. Table XL. — Miscellaneous olive oils — Continued. 51 a 15 samples. Bulletin du Minlst6re de rAgriculture. 1895. p. 139. b-i9 samples. Bulletin de rA^rit^ulture et Comnicrcf dc Tunis, f? samples. Bulletin du Ministere de rAgricultun-, is'.i.'i, p. 139. dThese t\v(> South American oils were exhibited at ilie World's Fair, Chicago. From W. C. Blasdale, Berkeley, Cal. COMMERCIAL OLIVE OILS. One hundred and tift3--seven samples of commercial olive oils were examined, of which 72 were labeled French oils, 67 were Italian oils, 15 were California oils, and the remainino* 8 were of miscellaneous origin. Sixt^^-oue samples were furnished by the Treasury Depart- ment and came from the appraisers' stores at New York and Philadel- phia; 96 samples were bought upon the markets at Boston, Buffalo, Chicago, New Haven, New Orleans, 8t, Louis, San Francisco, Oakland, and Washington. The following table summarizes the results obtained on these commercial oils: Table XLI. — Summary of commercial oils. Kind and source. Total num- ber of samples. Samples containing oils other than olive. Samples containing cotton-seed oil. French oils: From appraiser's stores Puroha.sed in market Italian oils: From apprai.'ser'.s stores Purchased in market Total imported oils: From appraistT's stores Purchased in market California oils, purchased in market Miscellaneous oils/t purchased in mark 5 6 11 2 2 aOne sample sold as "superior to any olive oil" was maize oil. Descriptions of the commercial samples are given in Tables XLIl, XLIV, XLVI, and XLVIII, and the results of the analyses are given 52 OLIVE OIL AND ITS SUBSTITUTES. in Tables XLIIT. XLV, XLVII, and XLIX. Table XLIII gives the results obtained on the fommercial samples of California oils. These oils agree very closely with the California oils of known puritj^ given in Table XXXV. The melting point of the fatty acids of No. 23114 is rather high, but the percentage of solid fatty acids is also high, and the iodiii number is correspondingly low. Table XLII. — Description uf commercial California oils not found iidulterated. Serial No. Source. Ca- pacity of recep- tacle. Price. Price of 10 ounces. Label. 22432 22616 C. C. Bryan, Washing- ton, D. 0. F. J. Lea & Co., Oak- land. Cal. Alameda Co., Boston, Mas.«. Sunset Grocery Co., Oakland, Cal. Torrey & Gardiner, Oakland, Cal. A. Simon, San Fran- cisco, Cal. John Schloen, San Francisco, Cal. L. Lehenbaiuu & Co.. San Francisco, Cal. J. Caire Co., San Fran- cisco, Cal. do Ounces. 20.3 Dollars. 1.00 Dollars. 0.49 California Olive Oil, Olivina. .luliiis Paul Smith, Livermore, Cal. 23069 23099 23101 23109 23112 23114 23116 23117 15.5 26.3 19.6 19.2 20.3 22.0 20.9 19.6 .60 1.00 1.00 .90 1.00 1.85 1.00 1.00 1.00 ..38 .39 .61 ..52 .45 .41 .47 .61 California Olive Oil. Alameda Co., Boston, Mass. Absolutely Pure, Absolutely Pure. "San Pedro." Old Mission Olive Oil. Akerman & Tuffley, San Diego, Cal. Coburn's Olive Oil. Coburn, Tevis & Co., San Francisco, Cal. Gifford's Best California Olive Oil. Abso- lutely Pure. C. M.Gifford, Jamacha Val- lev, San Diego Co., Cal. Santa Ana, California, Olive Oil. First Press- ing. Pure Olive Oil. Quito Olive Farm, Santa Clara Co., Cal. 23118 do Jose, Cal. 23124 J. 0. Riddel. Red- lands, Cal. do Mrs. Emilv Rober.son. Riddel's Olive Oil. First Pressing. J. 0. Rid- del, Redlands, Cal. Pure Olive Oil. F. M. Hunt, Redlands, Cal. 23126 Table XLIII. — Analyses of commercial California oils not found adulterated. Serial No. Specific gravity at 15.5° C. Butyro- refrac- to- meter reading at 15.5° C. |d ■ s a 1 a a 3 iS lodin number of liquid fatty acids. C o h — «j G > 1 Melt- ing point of fatty acids. Solid fatty acids. Free fatty acids as oleic. 22432 0.9162 Degrees. 68.7 67.4 67.1 67. 7 67.9 67.9 68.1 67.4 68.9 08.6 68.0 68.2 67.9 1.4715 1.4707 1.4705 1.470.S 1.4710 1.4710 1.4711 1.4707 1. 4717 1.4714 1.4710 1.4711 1.4710 41.0 ■ '43."6" 43.5 .61.0 44.5 46.3 49.6 45.0 43. S 45.2 46.5 48.0 84.6 81.0 79.0 81.6 83.8 80.3 79.9 79.9 83.4 83.7 81.0 83.7 86.5 91.5 191.6 192.6 193.4 190.5 192.9 193.2 192.4 194.9 191.9 192.2 193.1 193.3 193.2 °a 22.6 26.0 26.2 21.9 26.1 25.8 25.2 33.4 22.4 20.7 23.1 25.4 23.2 Perct. 3.22 ""7.' 45" 4.01 7.18 8.32 7.96 13.20 6.47 3.62 6.62 6.20 6.42 Per ct. 1.27 22616 3.49 23069 23099 23101 23109 23112 .9167 .9163 .9177 .9163 "88.'4' 93.9 88.5 "'ji.'g' 90.9 89.4 88.7 92.5 93.2 89.8 85.9 94.9 92.0 93.3 97.0 94.1 92.1 90.1 93.7 95.0 .'29 3.96 1.18 23114 .9167 .9171 .9167 .9164 .9171 .76 231111 23117. .69 .80 23118 1.24 23124 .47 231''6 7.26 Average . . . Maximum. Minimum . .9165 .9177 .9162 68.0 68.9 67.1 1.4710 1.4717 1.4705 45.5 51.0 41.0 82.2 86.5- 79.0 91.2 94.9 88.4 92.5 97.0 86.9 192.7 194.9 190.5 24.7 33.4 20.7 6.47 13.20 3.22 1.95 3.96 .29 C'OMMEBCIAL OLIVE OILS. 53 The following letter was received in regard to the analytical results obtained on sample No. 23117: Oakland, Cal., April S8, 1903. In returning the accompanying statement of the chemical analysis of Pala Grove oil I would like to make one change. Jn.st before receiving the paper from Wash- ington 1 had a test made of this year's product by F. M. Curtis & Son, analytical chemists in San Francisco. They returned me the following: ■ Specific gravity at 15.5° C 0. 9147 Free fatty acids (in terms of oleic) per cent. . 0. 36 lodin number (Hiibl) - 83.9 Cotton-seed oil None. You will note the difference in the percentage of free fatty acids, your analysis calling for 0.80 per cent. I was at a loss to account for the great difference until I recalled the age of the oil you had tested. The .Tustinian Caire Company have had no oil of ours since the 1901 crop, and when that was put in still had some of the 1900 crop on hand, so that what j'ou bought from them was at least 2 years old. Thanking you for your courtesy, I am, very respectfully, Caekie Cutler JIcLenegan. Pala Olive Grove, » a ^ A lodin number B ■2^ n ■0 56 as. ?!^ S!=i t. o£ liquid fat- .S.S •3 CJ QJlO Si .Q ty acids. Is >. =3d •E Is p. O Q> 33 r 1 CO " a w ^13 CO O 1° 1 1 Dcqrees. °c. Per a. JPer ct. 7049 .... 0. 9183 67.5 1.4707 85.0 20943.... .9180 68.1 1.4711 43.2 96.0 80.3 91.6 195.2 30.2 1.32 20955.... .9157 68.2 1.4711 42.0 93.2 79.8 90.6 193.4 26.2 1.32 20956 .... .9165 67.4 1.4707 45.2 100.3 83.0 97.4 192.6 30.6 1.56 20957.... .9173 67. 9 1. 4709 48.8 108.4 81.4 98.3 193.2 27.8 12.69 1.02 21003.... .9164 68.0 1.4710 41.8 92.8 79.8 91.5 192.7 25.2 1.32 21063 67.4 67.8 1.4707 1. 4709 40.7 43.6 90.4 96.9 80.6 79.0 95.6 92.2 192.3 194.1 25.2 26.0 8.2i 2.62 21071 .... .9161 1.91 21072 67.5 67.8 67.3 1.4707 1.4709 1. 4706 42.0 47.2 42.0 93.3 104.9 93.2 80.9 81.2 81.3 89.6 90.0 93.2 8.8.1 192.3 193.5 192.8 25.2 30.6 25.0 3.74 "io.'ii' .76 21112 1.56 21397.... .9163 1.52 21398 . . . . .9167 67.0 1.4704 43.8 97.3 80.8 94.1 98.5 193. 1 29.4 13.56 1.20 21399.... .9169 67.5 1.4707 43.8 97.3 81.4 93.9 97.7 193.0 25.8 12.20 2.16 21870 . . . . .9164 67.6 1.4707 45.2 100.3 80.7 91.2 192.8 29.0 2.29 21871.... .9163 68.0 1.4710 43.8 97.3 79.5 91.6 94.7 194.4 11.62 3.63 21872.... .9165 67.3 1.4706 43.0 9.5.5 79.9 93.2 93.8 192.6 27.0 10.44 .92 21873.... .9167 68.0 1.4710 46.5 103.3 81.8 99.4 97.8 193.5 27.0 11.94 .66 21874.... .9166 67.6 1.4708 47.2 104.9 82.9 94.6 195.0 28.2 1.55 21875.... .9163 67.8 1.4709 44.4 98.6 81.4 92.0 93.9 191.6 26.7 8.92 .96 21876.... .9163 67.5 1.4707 44.4 98.6 79.7 91.9 96.0 192.8 12.50 2.75 21877.... .9166 68.1 1.4711 44.6 99.1 80.0 96.0 194.8 29.4 2.00 21878.... .9166 67.8 1.4709 45.0 100.0 79.0 97.4 196.3 28.0 14.46 2.39 21879 . . . 68.0 68.5 1.4711 1.4713 47.6 47.4 105. 8 105.3 84.2 83.1 100.0 98.4 97.6 100.0 192.6 193.5 28.4 27.0 9.26 12.38 1.65 21880.... .9172 .45 21881.... .9165 68.0 1.4710 41.4 92.0 80.1 96.3 194. 5 28.2 12.36 .71 21882.... .9174 68.0 1.4710 47.4 10.5.3 80.8 92.7 99.7 194.0 30.4 14.45 .90 21883.... .9167 68.2 1.4711 47.4 10,5.3 83.8 99.7 192.1 25.2 11.56 .52 21884.... .9170 68.1 1.4710 42.4 94.2 83.7 93.1 93.8 193.5 27.2 6.33 1.76 21885 68.2 67.8 1.4711 1.4709 44.4 42.8 98.6 9.5.1 80.2 80.9 95.7 95.7 94.1 193.6 194.2 28.0 27.2 11.93 9.68 .66 21886.... .9165 .89 21887.... . 9153 67.6 1. 4707 45.5 101. 1 81.2 92.6 192. 1 28.8 7.89 1.34 2IS88.... .9173 67.5 1.4707 42.4 94.2 80.1 98.1 194.3 24.6 13.95 1.09 21889.... .9163 67.7 1.4707 42.1 93.5 80.8 96.0 94.3 196.3 26.7 9.92 .47 21890.... 68.0 67.8 68.0 1.4711 1.4709 1. 4710 44.0 43.7 40.7 97.8 97.1 90.4 82.8 82.6 79.8 93.7 93.2 91.3 94.3 94.6 193.6 192.7 196.1 26.9 27.4 28.0 7.73 8.34 .89 21891 . . . .84 21892.... .9i63 2.14 21893.... .9163 67.5 1. 4707 41.4 92.0 81.6 91.1 191.7 23.7 6.i7 .48 21894 67.5 68.7 67.2 67.3 1.4707 1.4709 1.4704 1.4705 42.6 42.2 42.8 45.5 94.6 93.7 95.5 101.1 81.1 80.9 80.2 83.6 194.2 193.5 193.2 193.1 24.7 24.2 25.2 27.6 "e.'si' 6.11 3.44 22908 . . . "90.' 6' 91.2 89.7 3.18 22913 1.83 2-2914 .9153 2.58 22918 . . . . .9152 67.8 1.4709 42.4 94.2 80.9 191.2 26.3 2.28 22919 .... .9157 68.0 1.4711 42.5 94.4 81.9 93.1 94.6 193.6 27.2 9.06 1.98 22920.... .9167 66.4 1.4699 51.5 114.4 83.6 92.1 191.7 27.2 1.82 23066 . . . . .9161 67.2 1.4705 48.8 108. 4 82.5 94.8 192.6 25.0 8.56 1.06 23071.... .9170 67.1 1.4705 47.2 104.9 80.6 91.1 191.7 27.5 7.11 2.93 23088.... .9167 67.6 1.4708 44.0 97.8 .HO. 6 .89. 5 192.8 25.0 5.53 1.73 23092 . . . . .9177 67.4 1.4706 51.4 114.2 80.5 96.2 194.2 30.0 15.95 1.07 23103.... .9196 67.4 1.4706 47.6 10.5.8 82.5 91.1 97.9 193.0 29.6 11.37 2.06 23105.... .9168 67.8 1.4708 48.2 107.1 80.8 93.4 94.2 191.3 28.6 9.87 1.38 23110.... .9168 67.7 1. 4709 49.4 109.7 .84.2 101.8 193.0 30.8 12.81 1.66 23111 .... .9173 67.8 1.4708 50.0 Ul.l 80.4 94.7 97.3 193.1 29.4 12.90 .81 23128.... .9166 67.6 1.4707 48. 2 107. 1 81.4 92.8 93.5 192.2 27.2 8.50 1.62 23129 . . . . .9160 67.8 1. 4709 46.0 102. 2 82.2 92.8 192.1 29.0 6.99 .95 23133.... .9177 67.5 1.4707 44.0 97.8 80. 5 89.1 190. 5 23.8 5.26 .90 23135.... .9170 67.7 1.4708 46.0 102.4 81.0 95.7 191.5 28.0 10.90 .99 23136.... .9168 67.2 1.4705 45.4 100.8 79.4 91.3 192.3 27.8 8.59 2.27 23138.... .9150 67.6 1.4707 4.5.4 100.8 82.2 193.3 26.3 1.69 23139.... .9165 67.6 1.4707 49.5 llO.t) 81.4 97.9 97.1 192.0 29.6 ii.76 1.71 23140.... .9164 67.6 1.4707 46.5 103.3 80.5 94.7 93.0 191.3 28.1 8.98 2.22 23141 . . - . .9172 67.2 1. 4705 48.0 106. f 80.1 92.3 93.7 191.3 27.7 10.00 3.31 Av .. .9166 67.7 1.4708 45.1 100.1 81.3 93.7 94.9 193.0 27.3 9.98 1..59 Max. .9196 68.7 1.4713 51.5 114.4 85.0 100.0 101.8 195. 3 30.8 1.5.95 3.63 Min. .9150 66.4 1.4699 40.7 90.4 79.0 89.5 88.1 190.6 23.7 3.74 .45 56 OLIVE OIL AND ITS SUBSTITUTES. Table XL VI. — Description of Italian olive oils not found adulterated. Serial No. Source. Capac- ity of recep- tacle. Price. Price of 10 ounces. Label. Ounces. Dollars. Dollars. 21907... Appraiser's office, Port of New York. Bari. 21911... do Bari. 22910... John A. Seel, Roches- ter, N. Y. '"iai.'o' "'2.'50' '"'o.'io' Olio d'Oliva Finissimo, Garantito Genuino, A. Nicolini, Bari. 21895... Appraiser's office. Port of New York. Sorrento. 21908. . . do Naples. Naples. Olio d'Oliva Fini-ssimo, Faicchio & S. Loreu- 21915... do 23082... Santo Capasso, New- '"n.o "'i.'oo' ....... Haven, Conn. zello, Prov. di Benevento. 20958... A.M.&J.Solari,New Orleans, La. 16.2 .65 .34 Olio d'Oliva di Lucca, F. Bertolli. 21111... Appraiser's office, Port of Philadel- Olio d'Oliva Suprafino, F. Bertolli, Lucca. phia. 21199. . . do 8.4 Lucca Finest Cream Salad Oil, Warranted Pure Olive Oil, Smith, Kline & French Co,, Philadelphia, 21896... Appraiser's office. Lucca. Port of New York. 21897... do , Lucca. 21898... do Lucca. 21899. . . do '.'.'.'.'.'.'.'. Lucca. 21902... do Lucca. 21909... do Lucca. 23068... S. S. Pierce, Boston, Mass. ■"'io.'i' "'".'35' " ".'34' Pure and Best Cream Olive Oil. 23093... Booth Meat Co., New Haven, Conn. 1.S.6 .75 .40 Cream Olive Oil, Made in Leghorn for W. A. Castle, SpringSeld, Mass. 23095... Bronson & Piatt Co., New Haven, Conn. 8.7 .35 .40 Huile d'Olive Excelsior, Toscana Excelsior, Lucca. 23097... H.Olson, Oakland, Cal. 23.6 .65 .27 Pure Lucca Oil, Crosse& Blackwell, London. 23100... .\eard& Russell, Oak- land, Cal. 24.7 .85 ,34 Extra Sublime Cream Lucca Olive Oil. 23106... John Bnlotti, San Francisco, Cal. 25. -1 .65 .25 Fine Lucca Oil, Imported by John Bulotti, San Francisco, Cal 23107... H.Weedcn. San Fran- cisco, Cal. 13.5 .50 .37 The Best Lucca Olive Oil, G. Fontana & Co., S:in Fr;uicisco. Cal. 23113... Goldberg, Bowen & Co., San Francisco, Cal. Mrs. C. Goessel, San 19.9 .60 .30 Sultlinu' Lucca Oil, Goldberg, Bowen & Co., San Francisco, Cal. 231L'-2. . . 21.3 .65 .30 Genuine Italian Olive Oil, M. Ricci o ai m " o to wO ^o O H o o H H O Bui, 77, Bureau of Chemistry U S. Dept. of Agr. Plate II. ^^^^ EXTRA fl^V P!i BORDEAUX -FRANCE SVKCTALLY BOTTLED FOK / and imp.T3 -^ a 23074 .... 23073.... 21903 .... 21904 .... 21913 . - . . 21916.... 21919.-.. 23119.... 22e09.... 230U7.... 23084 .... 23137.... 21029 .9165 .9175 .9160 .9102 .9103 .9179 . 9157 .9156 .9151 . 9159 .9165 .9154 Degrees. 66.8 67.1 67.3 67.8 67.2 07.6 es.o 66.9 66.8 66.9 67.4 68.0 66.3 67.3 1.4701 1.4705 1.4705 1.4709 1.4704 1.4707 1.4711 1.4703 1.4701 1.4702 1.4706 1.4710 1. 4699 1.4705 45.9 41.4 41.4 44.2 42.8 44.7 42.5 47.5 44.0 44.4 48.4 44.2 40.8 45.5 102. 92.0 92.0 98.2 95,1 99.3 94.4 105.5 97.8 98.6 107. 5 98.2 90.7 101.1 81.2 78.5 80.6 81.6 80.2 81.6 84.6 82.6 82.7 80.8 83.3 82.5 77.6 83.6 ' 'go.'e' 92.7 99.7 93.3 "gi.'g' 94.6 88.4 90.0 95.1 94.8 9.% 2 98.5 100.2 "go.'s' 92.8 94.4 90.5 91.9 191.6 191.9 192.5 192.4 193.2 194.6 193.6 193.5 192.7 192.1 192.6 193.7 190.9 193.1 °C. 24.4 21.0 29.4 29.4 25.2 30.4 27.2 28.0 26.0 25.6 26.0 24.2 26.2 30.4 Per ct. 3.70 8.62 10.74 9.47 11.26 12.68 11.21 '4.' 67' 8.50 7.38 4.40 11.22 Per ct. 2.46 1.22 3.87 1.59 1.83 2.09 1.98 5.30 2.27 2.63 .72 1.60 3.61 2.58 21914.... .9153 Av.. Max. Min. .9161 .9179 .9134 67.3 68.3 66.2 1.4706 1.4712 1.4698 44.0 48.8 39.8 97.8 108.4 88.4 80.9 84.5 77.5 92.4 99.7 90.0 92.61 ' 192.6 100.2 196.6 8S.0 190.1 26.6 30.4 21.0 8.35 13.42 3.70 2.42 15.26 .72 Tables XLVIII iiiul XLIX give the data obtained upon the samples of commercial oils found to be adulterated. The samples containing peanut oil all bore Frencji labels and those containing sesame oil Italian labels. Two California oils contained cotton-seed oil. In all of the above cases the oils were represented to be pure olive oil and in most cases were guaranteed pure and of special grade. One of the most striking facts brouglit out 1)V this examination of imported oils received from the customs officers, and therefore, known to be imported, was that none of them was adulterated with cotton-seed oil. Table XLVIII. — Description of adulterated olive oils. Serial. No. Source. Capac- ity of recep- tacle. Price. Price of 10 ounces. Label. 21027... 21031... 21110 A. L. Biililcr, New Orleans, La. Popovichar.dAbram- ovich , New Orleans, La. Appraiser's oflBce, port of Philadel- phia, do Ounces. 7.4 59.5 Dollars. 0.10 ,90 Dollars. 0.13 .17 Huilc d'Olive Viergc. E. Loubon, Nice, France, Olio d'Oliva, Egisto Dini, Lucca, Italy. Sublime Olive Oil Addisoni Fils Masina, 21113 Italy. Huilc d'Olive, E.Ktra Surfine, Jules Cham. 21395 .. do i bon & Cie., Bordeaux, France. Imported by Chas, W. Longaker, Pottstown, Huile d'Olive. P. M, Loubric, Bordeaux, 21396... do France. Packed for I. K. Bean. 21906 do France. Imported for J. M. Oliver & Sons. Lucca Italy. 22924... 22925. . . Dingens Bros., Buf- falo, N. Y, do 67.0 120.1 1.40 2.25 .36 .20 .19 CUoSopraffino. UmbertoAlbertini,Livorno, Italy. Olio Puro d'Oliva. Restivo & Co., Lucca, 23070... Rice Bros., West New- ton, Mass. (Tiiscana), Italy, Huile d'Oliyc, Vierge. Silas Peirce & Co., Bordeaux, France. COMMERCIAL OILS. 59 Table XLVIII. — Description of adulterated olire oils — Continued. Serial No. Source. Capac- ity of recep- tacle. Price. Price of 10 ounces. Label. Ounces. Dollars. Dollars. 23072... Cobb, Bates, Yer.xa & Co., Boston. Mass." IG 0.55 0.34 Huile d'Olivo Vierge, d'Aix. Dnpont iV: Cie., Bordeaux, France. 23085... E.E. Hall*. Son. New Haven, Conn. 11.5 .59 ..51 Huile d'Olive, Extra Vierge. NaeKely & Pasero, Marseille, France. 28086... do 11.5 • .45 .39 Huile d'Olive. Vierge, d'Aix. .Uex.Eyquem, Bordeaux, France. ■23087... S. Francisconi, New Haven, Conn. 34.1 ,50 .14 Oliod'Oliva. LuigidiCos Matteucci, Lucca, Italy. 23090... G. Savarese, New Ha- ven, Conn. 29.7 .50 .15 Olio d'OIiva, Sopraffino. F. Berio i Co., Lucca, Tu.scana, Italy. 230%... D. M. Welch & Son, New Haven, Conn. 8.7 .30 .34 Huile d'Olive, Extra Surfine. Tisserand & Fils, Bordeaux, France. 23108... F. W. Ruehers&Co., San Frani-isfo, Cal. 18.6 ..50 .26 Olio d'OIiva, Sopraffino. Gaetano Giurlani, Lucca, Italy. 23120... H.C. KUttLTliorn.San Franci.> . . o > O 0) ■ ■ o i> :5^ Zo, s ° ZOh e e H s^l 'I' C _ _ , - _ ;?;fL,DH ;2;pHSi :p-.^o^ an 1> O O CTi o c o 2 _ o o a i- ce «a •2 S t-' aoQOO-i'C^O'i'CJiO-^'^io-^' ciocooocor-otx;t- •OOiiJ'OiC C^eOOiC-lrHt~Or- jiooieococioo^ o S S a,.2 Q) OJ ^ t- +^ OieOOOJCO-^OiiO OiQr M 1/^ >0 CI • O C-1 ifi O O t^ l-- O 3C t^ to O CTi O .C C-1 OT TH01CC»-«000<-*C^l-?"if5-^0 lOdOO'-'CJiOCOtO too— -r Oi -:t< -r *l t^ r- I- t^ 6 -^ ; . ^d CO tiD«S S■XI>^^OtD•^t031O01^nC0Cl ClOiOi-IOC^OOOCO ifll^Or-* ■ r-aj!DotoaicocoicoOin o ■ cc^toiOtocoi--i-'CN — •— r~ 4 ^t 0i Q^ Q3 C^ Q^ G^ O^ G^ O^ O^ O^ t^Oi-iOCOlO-O'^^cOI-^iOO ooor-(^comojCTia>aic7>o rHi-li-l^.-Hi-lf-.r-l(MCJW(MCC (JjOiOvoiCiClOsOOi (N uO CD i^ n o '.c a: o t^ioocaoccoioioc) OOOOOOO — .-H COCCCOCOCOCOCOCOM tc r^ Oi ii^ oi (M c-i a. ■— I OJ CI 1— I Oi O 0> 51 M ?o c^ o 62 OLIVE OIL AND ITS SUBSTITUTES. SUMMARY. (1) The olive oil consumed in this country is largely imported from France and Italy. The amount produced in California is relatively small, although reports warrant the statement that California is capa- ble of supplj'ing the entire home demand. (2) The cost of production of California oil is so much higher than that of the French and Italian oils that it competes with difficulty with the imported oils in the American market, eveu after the latter have paid dut}^ amounting to 50 cents per gallon. (3) The retail prices of the best grade of oil from the three sources are much the same, but the average prices of the imported oils are much less than that of the California oil, owing to the large amount of lower grade foreign oils that is marketed in this country. (4) In the examination of olive oils for adultei-ation, a complete analysis is usually necessary to reveal the real nature of the oil. In cases of gross adulteration the (qualitative tests, specific gra\it_v, and index of refraction will often show the nature of the adulterant and the extent tt) which it is emploj^ed. (.5) The adulteration of foreign oils imported into tliis country is practiced to a much less extent than is popularly supposed. Only .5 of the 01 samples obtained from the customs officers were found to contain other than olive oil. and none of these contained cottonseed oil." On the other hand, oils bought upon the market, bearing labels indicating a foreign origin, were found to be (jnite extensively adul- terated with cotton-seed oil. It seems, therefore, probable that these adulterated oils bearing foreign labels are labeled and modified after leaving th(^ port of entry, neither the domestic nor the foreign pro- ducei' being responsible for them. This practice is equally injurious to the interests of the California, French, or Italian manufacturer of pure olive oil and the consumer. (6) The I'esults of analyses of oils of known purity show that there is a wide range in the various values ordinarily considered of impor- tance in indicating the purity of an oil. This is especially true of the iodin nuinbei', the melting point of fatty acids, and the percentage of solid fatty acids. The California olive oils generally have a higher iodin number, a lower melting point of fattj' acids, and a lower per- centage of solid fatty acids than the French and Italian oils. (7) All samples containing other than olive oil were sold as jnire olive oil. although in one case a careful observation of the label revealed the fact that the oil was an olive oil substitute. " Nine samples out of 250 recently received from the custom-house have contained cotton-seed oil. INDEX OF DEALERS AND MANUFACTURERS. Page, Achiardi. Augustus, Leghorn, Italy .^G Adrlisoni Fils, Jlessina, Italy .78 Agard & Russell, Oakland, Cal 56 Akerman & Tuffley, San Diego, Cal rfl Alameda Co.. Boston. Mass .52 Albertini, Cmberto. Livomo, Italy -iS Allen. W. P., Philadelphia, Pa ,51 Alphonso, Fratelli, Leghorn, Italy 56 .■Vmerican Cotton Oil Co., New York City . . 44 Anable, S. G.. Chicago, III 54 Anderson, V. D., Co., Cleveland, Ohio 43,44 Antonini & Co., Leghorn, Italy 56 Armour i- Co., Chirago, III 43 Baldocchi, Robert, & Co., San Francisco, Cal Bailer, Fred, &Co., Messina, Italy Barton & Guestior, Bordeaux, France Bartuni. G., Leghorn, Italy Bean, I. K Beauraarchand Fils, Bordeaux, France Bebo, Newman & Ikenberg, San Francisco, Cal Berio, F., & Co. , Lucca, Italy Bertolli, F., Lucca, Italy Bidwell (John) Estate, Chico, Cal Billet, Alphonse, Bordeaux, France Blanc, J. E. . Marseilles, France Blasdale, W. C. , Berkeley, Cal Booth Meat Co., New Haven, Conn Bo.'iton .Store. Buffalo, X. Y Boutelleau Fils, France Brandenburg Frdres, Bordeaux, France Brie, J. de, & Co., Bordeau.x, France Brody. James, Biloxi, Miss Bronson & Piatt Co., New Haven, Conn Bryan, C. C, Washington, D. C Buehl, E. M.. Buffalo, N. Y Btihler. A. L.. New Orleans, La Bnlotti. John, San Francisco, Cal Busby, Fred, Concord. N. H Caire. J., Co., San Francisco, Cal Capasso, Santo. New Haven. Conn Castle, W. A., Springfield, Mass Chaffard, Vve. Jardin de la France Chambon, Jules, & Cie., Bordeaux, France. Chapnelle & Cie., Aix, France Clark, S. W., & Son, New Orleans, La Coob, Aldrieh & Co., Boston. Jlass Cobb, Bates, Yerxa & Co., Boston, Mass "In a few cases in which the manufacturer's name 56 49 53,54 66 58 53 54 .59 .56 47 .54 54 5 .56 .59 54 .54 53 43 56 .52 56 .58 56 47 52 66 .56 54 58 54 53 54 53,59 Page. Cnburn, Tevis & Co., San Francisco. Cal ... ,52 Cochrane, E. C. Co., Buffalo, N. Y .54 Cola, Giov. di. Termini. Sicily 57 "Collinflorc Royal Table Olive Oil'V" 57 Connor, E.agan Co.. St. Louis, Mo 54 Conway Co., Boston. Mass ' 56 Cooper. El wood, Santa Barbara, Cal 9, 47 Crosse & Blackwell, London. England .55 Dellepiane, Giacomo, fu Andrea, Genoa. Italy 5, 49 De Martini & Cia.,RivieradiGenova, Italy. 59 De Po.ssel Fils, Marseilles. France 54 DingensBros., Buffalo, X. Y .54..56..58 Dini, Egisto, Lucca, Italy 58 Dove, D., New Haven, Conn 59 Dove Pure Oil Co 59 Dumouron & Cie., Grasse. France .54 Dnpont & Cie., Bordeaux, France 53, .59 Duret, J. L.. & Co.. Bordeaux, France 53 Ehmanu Olive Co., Orovillc, Cal 47 El Montccito Manufacturing Co.. El Monte- cito, Cal 59 Eppling. H. L., Chicago, 111 .54 Eyquem, Alex., Bordeaux, France 59 Faicchio & S. Lorenzello. Italy 56 Faxon. Williams & Faxon, Buffalo, X. Y. . . 5J, 66 Ferrari, B.. tt Co.. Boston, Mass 56 Fontana, G.. & Co.. San Francisco, Cal 56 Fontenelle, A.. Fils ^M. Page. Goodrich, Edward E.. Santa Clara, Cal 12,47 Gray, J. C. OroTiUe. Cal 47 Hall, E. E., & Sons, New Haven, Conn .... 57,59 Hamelsfaler, Chicago, 111 54 Heublein, G. F.. & Bro.. Hartford, Conn... 54 Hill. James, & Sons, Los Angeles, Cal 47 Howland *t Co.. Oakland, Cal 59 Hunt, F. M.. Redlands. Cal 52 Indianapolis Hominy Mills, Ind 44 India Refining Co., Philadelphia, Pa 43 Jevne, C, & Co.. Chicago. Ill 54 KStterhorn, H. C, San Francisco, Cal 69 Kaufman. V.. Chicago, 111 57 Kleiser. J. A., ('loverdale. Cal 47 Koehl, J. .\., New Orleans, La 53 Larroudo Freres, Bordeaux, France 53 Lea, F. J.. A Cn., Oakland, Cal 52 Lebenbaum. L.. res, Bordeaux, France 59 Mattoncci. Luigi di Cos, Lucca, Italy 59 Mayrargue, Joseph, Nice. France 54 McLenegan, Carrie Cutler. San Jose, Cul... 53 ( .See also Pala Grove. ) Meigs, Peveril, Santa Barbara, Cal 13,47 Miller. I. J., Philadelphia, Pa 53 Moro, Pio, fu Comigliano, Liguria, Italy... 57 Morris & Smith. Yolo, Cal 47 Mottet, J., &Cie., Grassc, France 54 Myer, M. P., San Francisco, Cal 54 Naegely ».t Pasero, Marseilles. France 59 Nencioni, Fcrd., Ditta, Pisa, Italy 56 Nesbit, R. N. Co., New Haven, Conn 54 "Nicellc Olive Oil" 53 Nichols, E. E.. New Haven. Conn .54 Newton, Robertson & Co., Hartford, Conn. 53 Nicolini, A., Bari, Italy 56 Olson, H., Oakland. Cal 56 Oliver, J. M., & Sons 58 Pala Olive Grove, San Jose, Cal 52 {See also McLenegan, C. C). Peirce, Silas, & Co.. Bordeaux, France 58 Pierce, S. S. , Boston , Mass 54. 5ii, .57 Page. Pinard, Alphonse, Bordeaux, France 54 Pitito, Nicoli, Leghorn, Italy 56 Plagniol, James, Mar-seilles. France 53,54 Popf, Geo. P., Chicago. Ill 56 Popovich, Abramovich, New Orleans, La. 57, 58,59 Possel, De, fil*, Marseilles, France 54 Price, L. A., Bordeaux, France 54 Prosek, Dr., Guerneville, Cal 47 *- Puget, Adolphe, Marseilles, France 53 Quito Olive Farm, Santa Clara, Cal 62 Rae, S., & Co., Leghorn, Italy 66 "Rancho Chico" 47 Restivo & Co., Lucca, Italv 58 Ricei, M.. &. Co., Lucca, Italy 56 Rice Bros., West Newton, Mass 58 Riddel, J. O., Redlands, Cal 47, 52 Roberson, Mrs. Emily, Olivina Farm, Auburn, Cal 52 Rossetti, D. G., & Co.. Legnorn. Italy 66 Roulan Freres, Bordeaux, France 54 Routh, H. L.,&Sons 56 Ruchers, F. W., & Co., San Francisco. Cal.. 69 "S. Benedictus" 54 ' ' San Pedro " .52 "Santa Ana. California. Olive Oil" .52 Savarese, G.. New Haven, Conn 59 Scatena. S., San Francisco, Cal .59 Schicfflein & Co., New York City 43,44 Schlieswohl & Peterson, Chicago, III .56 Schloen, John, San Francisco, Cal 52 Seel, John A., Rochester, N. Y 54,56 Seville Packing Co., New York, N. V .53 Simon, \.. San Francisco, Cal 52 Smith Cash Store. San Francisco, Cal 57 Smith. Julius Paul, Livermore, Cal 52 Smith, Kline & French Co.. Philadelphia, Pa. 66 Smith, Vincent C, Napa, Cal 47 Soci^te Hygienique Alimentairc 64 Solari, A. M. & J., New Orleans. La 53.56 Stumpf. L.. Grocery Co.^ St. Louis, Mo 54 Sunset Grocery Co., Oakland, Cal 52 Swarbuck. J.(;., New Orleans. La 53 Talbot Fri^res, Bordeaux. France 63 Torrey & Gardiner. Oakland. Cal 52 "Toscana Excelsior" 56 Tisserand .& Fils, Bordeaux, France 59 Vidheau & Cie. Bordeaux, France 53 Villavecchia, V., Rome, Italy 5,44,49 Walter, L. M., San Francisco. Cal 56 Weeden, H., San Francisco, Cal 56 Welch. D. M., &Son. New Haven, Conn... 59 Wheeler, W. P., Oakland, Cal .i9,60 Whiteman & Co., Chicago, III 64 o 1606*08