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Contribution from the Bureau of Chemistry CARL L. ALSBERG, Chief

Washington, D. C. Vv January 24, 1920


By R. W. Hits, Chief of Western Food and Drug Inspection District, and R. S. HoLtinesHeaD, Junior Chemist, San Francisco Station.*

CONTENTS. Page. Page Olive culture in California___._____ 1 | Purpose of investigation-_-_-_---_- 7 Varieties of the olive grown in Cali- Plan of investization——*— =" —- 2 ee 8 VC TEEN ears ee SRNR nga Tees Nea eet, 2 | Methods of examination___________ 9 Olive-picking season ______________ 3 | Results of examination of fresh olives_ 13 Changes in composition during ripen- Results of examination of pickled TIP SSE 2s SL AVN a ee ia eee 3 CON 2; < el nee a te Shc 19 The pickling’ of olives... = Sit} ASU Marie | es eS es See er eee 24


With the single exception of Arizona, olive culture in this country is limited to California, where the tree was introduced in the early days by Spanish priests, the first grove being planted in San Diego in 1769.2. This origin is recorded in the name of what is to-day the most popular variety, the Mission olive, a descendant of the early plantings. The culture of the olive has extended until there are trees in 38 counties, the important counties being Riverside, Tulare, Te- hama, Los Angeles, Butte, Fresno, San Bernardino, and Shasta. In the spring of 1916 a State census showed 834,939 bearing and 515,221 nonbearing trees. In general, the olive-growing sections may be roughly grouped into three districts. The northern district, in the Sacramento Valley, centers in Butte County, with some groves as far south as Sacramento, and many fresh plantings in southern Shasta County, the farthest north. This district is one of the most im- portant, and contains an enormous number of trees not yet bearing. The central district is in the San Joaquin Valley, principally in

1The authors wish to acknowledge their indebtedness to V. B. Bonney for a portion of the analytical work done in 1916, and to W. W. Karnan for a part of that conducted in 1914.

2 Ann. Rept. Calif. Development Board for 1916. San Francisco, 1917.



Tulare and Fresno counties, centering at Lindsay and Fresno. Re- cently some very extensive planting has been done in Tulare County. The southern district lies in the territory centering around Los Angeles and San Diego. Although the oldest, it is, or soon will be, surpassed in production by both of the other districts. There are some groves also in a few sheltered valleys along the southern coast, and elsewhere, but they have little commercial importance. Planting is being done in the Imperial Valley. In 1916 the State’s estimated yearly production was 1,000,000 gallons of olive oil and 300,000 6-gal- lon cases of pickled olives.t. The rapidly growing popularity of the pickled ripe olives and the protection afforded to olive oil by food legislation have given a great impetus to the industry.


The varieties of olives that have been grown in California are very numerous. The California Agricultural Experiment Station has reported analyses of 57 varieties.2, The important ones, however, are limited in number, the favorite varieties being, in approximate order of importance, the Mission, Manzanillo, Ascolano, Sevillano, and Nevadillo Blanco.* Since the Nevadillo Blanco is more important as an oil olive than for pickling, the observations reported in this bulle- tin have been limited to the first four named. The Oblitza olive, a large Dalmatian variety, is also used for pickling. The olive was originally grown largely for oil, but more recently the pickling varieties have been in greater demand. The following descriptions of the five varieties are based in part upon material recognized by the industry under the respective names and in part on publications of the University of California.*

Mission—This name denotes the variety derived from the old mission groves, and possibly covers several subvarieties. Of these _the common or broad-leaved Mission is the one generally known as Mission. The fruit is of medium to large size, about ten-sixteenths to twelve-sixteenths inch in diameter; ovate, oblique—sometimes very much so—tip rather pointed; fruit variable in size; pit straight or somewhat curved, usually with a sharp point. (PI. L)

Manzanillo—tThis variety was imported from Spain. It is a medium to large-sized olive, about the same as the Mission, approxi- mately ten-sixteenths to twelve-sixteenths inch in diameter; quite regular, rounded oval, more nearly globular than the Mission, and

1 Ann. Rept. Calif. Development Board for 1916. San Francisco, 1917.

2 Rept. of Work of Agr. Exp. Sta., Univ. Calif., 1898-1901, pp. 263-307. Sacramento, 1902.

$B. J. Wickson. The California Fruits and How to Grow Them, pp. 335-350. San Francisco, 1914.

Rept. of Work of Agr. Exp. Sta., Univ. Calif., 1898-1901. Acknowledgments are due F. T. Bioletti for reviewing these descriptions.

Bul. 803, U. S. Dept. of Agriculture. PLATE I.



Bul. 803, U. S. Dept. of Agriculture. PLATE I]




more rounded on the outer end, and with little indication of a point; pit straight, shorter than the Mission, and with the greatest diameter nearer the apex, often with a short, sharp point at the apex. (Pl. II.)

Ascolano.—This is a very large olive, twelve-sixteenths to eigh- teen-sixteenths inch in diameter; shape a rounded oval with some in- dication of a point, resembling an exaggerated Manzanillo; very soft and tender when ripe; pit with a short, sharp point at the apex. (Pl. ITT.)

Sevillano.—This is also a very large fruit, the largest of the Span-

_ ish varieties, and supposed to represent the one exported from Spain

as “Queen olives, from fourteen-sixteenths to eighteen-sixteenths inch in diameter; shape ovate, oblique, resembling a large Mission; very soft and tender when ripe; pit pointed and exceedingly rough, | and sometimes with very sharp-pointed projections along its sides. (Pl. IV.)

Nevadillo Blanco.—This variety is small to medium in size, from eight-sixteenths to eleven-sixteenths inch in diameter; relatively long compared to diameter; pit comparatively large, quite curved, distinct veins on surface, and with a short, sharp point at apex.

The size statements in these descriptions refer only to the average run on the tree. Commercially all olives are separated into grades

of different sizes. OLIVE-PICKING SEASON.

The picking season for the olive varies greatly. It is influenced somewhat by variety, but more by locality. In the warm inland val- ley of the northern district the fruit matures earlier than in the southern portion of the State. The Manzanillo matures somewhat. earlier than the Mission. In Butte County, in the northern district, Manzanillos are often picked about the middle of October, Missions late in October or about the first of November, and all varieties are gathered by January 1. In fact, there is danger from frost during December. In the southern district Manzanillos may be picked about November 1 and Missions about November 10. Ascolanos are picked about November 1. All olives are off the trees by February 1 to 15. In some exposed places nearer the coast the seasons may be still later.


Any study of the ripening of the olive must be preceded by a con- sideration of its constituents. The following are known or have been reported: Fixed oil, protein, mineral matter, mannit (in the immature fruit only), an oxidizing enzyme acting on the oil, the enzyme emulsine and a glucoside “oleuropein,” wax, reducing sugar probably dextrose.2, De Luca? and others? claim to have iso-

1C,. Wehmer. Die Pflanzenstoffe, p. 600. Jena, 1911. 2 Arch. Pharm. (1902), vol. 240, p. 475. 3 Rend. accad. sci. Napoli (1865), p. 79.


lated mannit from the immature olives, but more recently Hart- wich and Uhlmann? declared that its presence had not been con- clusively shown, and stated that they could not detect it. These authors, who followed microscopically the development from bud to fruit, state that there is no starch in the olive at any stage, with the exception of cells adjoining the stomata. These writers also re- ported that glucose was present in almost all stages of developmertt, and they believed it to be the substance from which the oil is formed. Of interest is the glucoside discovered by Bourquelot and Vintilesco ? and named by them “oleuropein.” Subsequently * they isolated it in a state of comparative purity, finding it powerfully levorotatory and yielding d-glucose on hydrolysis by dilute acid or emulsine. They reported it as possessing a strongly bitter taste, which is of special interest, since it thus appears probable that this is the sub- stance, or at least one of the substances, which gives to fresh olives, both in their green and ripe state, their intensely bitter flavor, mak- ing it impossible to eat them until the bitter principle has been re- moved by the pickling process. Also Bourquelot and Vintilesco,* by the use of invertine, claim to have demonstrated the probable presence of very small amounts of sucrose in the olive.

A number of studies on the ripening of the olive in Europe are given in the literature on this subject. De Luca seems to have been the first investigator,> beginning in 1861. He showed the increase ‘in the volume and weight of the fruit and that the oil increased gradu- ally from the time the pit was formed. In 1878, Roussille® pub- lished analyses following the ripening and showing an increase of oil in the fruit fiesh from about 1 per centin July to 34 per cent at the end of November. Funaro published similar analyses,’ tracing the oil in the fruit flesh from a very low figure in the latter part of July to 27 per cent in late February. Hartwich and Uhlmann, studying fruit from San Remo; distinguished three periods of development. In the first, covering approximately July and August, the pit was forming, and the oil content, on a basis of the whole fruit, increased from about 0.5 per cent to 5 per cent. In the second period, Septem- ber and October, the pit increased little, while the flesh and oil in- creased rapidly. In the third period, from October to January, the oil increased slowly until there was 30 per cent in the fruit flesh, which finally declined to nearly 25 per cent in the middle of Feb- ruary. De Luca had noted a similar decrease in oil at the end of the

i Arch. Pharm. (1902), vol. 240, p. 475.

2J. pharm. chim. (6th ser.) (1908), vol. 28, p. 303. Compt rend. (1908), vol. 147, p. 533.

2J,. pharm. chim. (7th ser.) (1910), vol. 1, p. 292.

4J. pharm. chim. (6th ser.) (1908), vol. 28, p. 303 (7th ser.) (1910), vol. 1, p. 292.

5 Rend. accad. sci. Napoli, for 1861 and following years (original source not available).

6Compt. rend. (1878). vol. 86, p. 610. 2

7 Landw. Vers-Sta. (1880), vol. 25, p. 52.

Bul. 803, U. S. Dept. of Agriculture. PLATE III.



Bul. 803, U. S. Dept. of Agriculture. PLATE IV.



season. Altogether it is evident that the increase in oil is the strik- ing feature in the development of the fruit.


There are two methods for rendering edible the fruit of the olive tree, only one of which is commercially valuable. By allowing the olives to soak in brine or fresh water, which is frequently changed, for from 6 weeks to 2 months, the bitter principle is decomposed or removed, and a very palatable article is produced. This method, however, consumes too much time, and the losses due to mold and softening of the fruit bar its general use on a large scale.

Although there are, of course, minor differences in various plants, the general commercial method of pickling ripe olives is as follows: The olives are picked by hand. The buyer gives instructions to the pickers as to the color desired, which varies from yellow” to red or tinges of red. Usually at least three pickings are necessary to obtain the maximum amount of olives of the desired color. Some- times the fruit is sent 500 miles to the factory, as from Butte County to San Diego. Such long shipments are made in barrels or wooden vats, the fruit being covered with a weak brine to which is sometimes ~ added a small amount of caustic soda, about one-fourth pound to the gallon.

In the factory the first operation is grading to size, for which purpose several. machines have been designed. The most common type of grader consists of a series of vibrating screens with circular holes of gradually increasing size. This gives grades of three or four sizes, the olives smaller than nine-sixteenths inch being gen- erally used for oil. In another common modification the screen bot- toms are made of narrow tin strips, the distances between which cor- respond to the diameter of the holes in the other machine. Both of these machines tend to bruise the fruit somewhat. To avoid such bruising another very simple and satisfactory machine, consisting of a series of rubber-covered rolls which are set at slight angles to each other and inclined, is used. The opening between the rolls is smallest at the top of the incline, and largest at the bottom. The rolls rotate in pairs in opposite directions, so that the inside sur- faces turn upward. The olive rolls down the incline, and there is no tendency to mash the olive or bruise it by sudden contact with any sharp edges. When the opening between the rolls becomes greater than the short diameter of the olive it drops through into boxes below, according to its size. The size graduations are usually made on the basis of a difference of about two-sixteenths inch in diameter. There are no recognized trade standards for the size erades or for their commercial designations. Each packer has his


own system. The standards in Table 1, based on the best com- mercial practice, have been suggested by Bioletti.t

TABLE 1.—Standards for size grades.

Average Average number per pound. diameter Designation. Size. in six-

teens Of | Mission. | Sevillano. | Ascolano. | Manzanillo. iimfralance sss Ap abe eee | 1 16 35 33 36 39 LENE Ds lees ae Sew ap i ay aa | 2 14 52 49 54 58 IMediam’s £2 ce Wile ee SE) 5 ae a 3 12 82 78 8 93 Sa roe ao ee ee ee eee 4 10 135 142 148 160 1 Dp:q Witz iS) C07 GR ia eee Vs ee © 5 Below 9 ? ? ?

Many fancy names and symbols are used to designate the various grades. The graded olives are sometimes run over sorting belts to be segregated for color, but this is not common.

After being graded and sorted, the olives are taken to the nicking

vats. In the newer factories, Thess are made of concrete, about 8 by 3 by 2 feet. Similar tanks of redwood are also used, and some- times circular tanks of redwood, about 8 feet in diameter and from 4 to 5 feet deep. Subject to some variation, the following treatment is applied: A quantity of 14 to 2 per cent caustic soda solution, in weight about five times that of the olives, is poured over the fruit, _and allowed to stand for from 6 to 8 hours, with frequent stirring. This liquor is then drained off, and the olives exposed to the air for 24 hours, with occasional stirring. More of the same or a weaker

solution is applied for a similar length of time, and again run off and

the fruit aerated. This operation is performed a third time, or until the caustic reaches the pit, as indicated by a darkening of the flesh. The lye solution is then run off, and fresh water added to the vat. The water is changed about every 12 hours until all the lye is washed out. The pickler determines this by. taste. Tests of all commercial samples analyzed, with phenolphthalein, show the ab- sence of free alkali or normal carbonates. At this point, salting of the olives is begun by soaking them in solutions of brine of gradually increasing strengths, of about 1, 2, and 4 per cent of salt. Factory control is by means of the salometer, a hydrometer graduated in hundredths from zero in distilled water to 100 in saturated salt so- lution. Usually the strongest solution employed is approximately 15° on this scale. The olives are soaked about 2 days in each of these different solutions, after which they are canned in a 3 or 4 per cent brine and processed in a water bath. Recently Bioletti and Cruess have proposed preserving in lacquered cans or glass jars with- out any liquid.? It is claimed that the olives thus treated keep their black color better than when brine is used.

1Calif. Agr. Exp. Sta. Bul. 263. EEE California Olive Association recently has adopted

a set of size standards. 2 Calif. Agr. Exp. Sta. Bul. 289.

tie bey old

: 4 : = :

rat es i,

Bul. 803, U. S. Dept. of Agriculture. PLATE V.



In most factories, after salting, the olives aré run over sorting belts, where they are sorted into two or three color grades, and all bruised or injured fruit removed before canning. Patents for as- signment to the public have been applied for by Bioletti and Cruess of the California Agricultural Experiment Station at Berkeley, for improvements in olive pickling, which involve the use of heated solutions, with aeration and constant circulation of the solutions.* These conditions are obtained in various ways, and it is claimed that the time required is very much shorter, and that a more satisfactory product is obtained. Further details can be had from their de- scriptions. A point of special interest in pickling the black or ripe olives is that the black color is formed or set by aeration accompany- ing the alkali treatment.

The pickling of green olives for sale as such is very similar. The olives are picked before any yellow color shows, and they are treated with similar solutions, except that usually only two caustic solu- tions are used, and the greatest care is taken to protect the olives from exposure to the air, which tends to cause a darkening of the color. The green olive is given an after fermentation under 7 per cent brine which develops its peculiar piquancy.


During the summer and fall of 1914 complaints concerning the pickling of ripe olives in California were received by the Bureau of Chemistry. The charge was made by one or two of the firms en- gaged in this business that it was becoming a very common practice among the picklers of olives to gather the fruit in a green and imma- ture state and so to manipulate it during the pickling that the color was artificially and unnaturally changed from green to black, the finished product being sold as a ripe olive, to the deception of the consumer and the detriment of the industry. The advantages of this alleged fraudulent practice were stated to be that the fruit could be stripped from the trees in one or, at the most, two pickings, whereas if it were left until it had reached a proper stage of ripeness several pickings would be necessary; also that hard, immature fruit requires less care and skill in pickling, and that early picking does away with the danger of frost damage, especially in the northern districts. It was evident that if there were truth in this statement the practice in question would amount to a coloring or staining by which the in- feriority of the immature fruit would be concealed, and that it would be analogous to the coloring of immature oranges by sweating. On examination the question seemed to merit careful study. The in- vestigation here reported was accordingly undertaken to determine whether immature olives were being pickled and sold as ripe, and also whether inferiority was being concealed by a process of coloring.

1Calif. Agr. Exp. Sta. Bull. 289.



As it does not appear that any systematic study has been made of the ripening of olives in California, the plan of this investigation was first to follow the development of the fruit on marked trees, record- ing changes of composition and physical characteristics, especially color, in order to establish, if possible, the differences between im- mature and ripe fruit, and to ascertain how closely the color of the fresh fruit is related to or may indicate maturity. This was done for different varieties and localities, and during successive seasons to show the influence of these factors. In the second place, to make the data applicable to the finished product, different lots of olives were followed through the pickling process to find what changes occur in the composition and color.


When the field work was taken up in 1914, the season was too far advanced to permit of any investigation of composition changes during growth. However, in the middle of December, when the fruit certainly could be considered mature in almost all localities and a large part of the picking was completed, series of samples of the most important varieties of olives were collected from the same or neighboring trees in localities in the northern and southern districts. They were analyzed both to afford data on mature fruit and to show, if possible, the relation of color to composition. Also a number of pickling factories were inspected, and men prominent in the industry interviewed.

In the 1915 season the systematic study of the ripening was under- taken in the northern district. Trees of different varieties in different localities were marked and sampled at intervals of practically three weeks from September 15, when the fruit is well formed, to Decem- ber 15. Since fresh olives are worth from 15 to 20 cents a pound, the value of one tree’s crop is so great that no attempt was made to buy outright the whole crop of the trees under observation. As it was considered desirable to follow the development past the regular har- vest time, arrangements were made with the growers to leave a certain portion of the tree untouched in the picking. Unfortunately, the picking is done by Japanese, Hindus, and Mexicans, and, in spite of the owners’ efforts, many of the trees had been nearly stripped, or at least most of the highly colored fruit had been picked, at the last sampling period. In the northern district the grower generally as- sumes the frost risk up to December 10, and most of the picking is over by the middle of that month.

The plan of operations for the 1916 season was the same as for that of 1915, except that the trees were more numerous and were scat- tered over all the important olive districts.



When received‘at the laboratory the olive samples were immedi- ately examined for color, and, if analysis could not be begun without delay, they were sent to a cold-storage warehouse and stored at about 34° F. until wanted. A slight increase in color was sometimes evi- dent after such storage.

The laboratory methods of examination, as finally adopted, were as follows:


Record the following: Color, flavor (if pickled), and ease of cleav- age of the pulp from the pit; average short diameter in sixteenths of an inch, measuring 50 or 100 olives; number of olives per pound; percentage by weight of pits.


If pickled, pour off the brine and dry the olives with a towel. Reserve the brine for determination of salt. Count out 1 pound of olives, recording the number. Remove the pits with a cherry pitter. Scrub the pits with a brush, dry with a towel, and weigh moist, giv- ing percentage of pits. Pass the flesh of the fruit twice through a meat grinder,’ and receive in an evaporating dish. Weigh out sam- ples immediately, stirring thoroughly with a spoon before removal of each portion. If desired to analyze the pits, air dry them in a warm place, weigh, and grind as fine as possible in a drug mill.


Solids —Weigh out approximately 10 grams in a 2-inch lead cap- sule containing a teaspoonful of recently ignited sand and a short glass stirring rod. Mix intimately and dry in the water oven, which requires from 5 to 7 hours.

Ether extract—The material in the lead capsule, including the stir- ring rod, is crushed and brushed into the inner tube of a Knorr fat extractor, prepared with an asbestos mat about 4 inch thick, pre- viously washed with alcohol and ether, and dried. Cut up the cap- sule and add to the tube. Extract for about 12 hours with anhydrous ether. Remove the inner tube, let the ether evaporate, grind up the contents in a mortar, return to the tube, and continue extraction for 4 hours longer. Dry the oil to constant weight in the water oven, avoiding undue heating. Periods of from $ to 1 hour are sufficient.

Protein (NX6.25).—Weigh out about 10 grams into a 9 cm. filter paper, folded into a cone and placed in a wide-mouth weighing bottle. Transfer the paper and sample to the Kjeldahl flask, and determine

1 As the skin of the olive is rather tough, the grinder used must be provided with sharp cutting knives.

130996 °—19——_2


nitrogen by the Gunning method, using 40 to 50 cc. of acid, 10 grams of potassium sulphate, and a small crystal of copper sulphate.

Ash.—Burn a 10-gram sample in a flat-bottomed platinum dish at a moderate temperature. If necessary to get a clean ash, cool, moisten with water, evaporate, and ignite again, repeating until the carbon is gone.

Alkalinity of ash—Add 25 cc. of N/10 sulphuric acid to the ash in the dish, heat under a watch glass for a few minutes, and titrate back with N/10 caustic soda, using methyl orange.

Salt-free ash—In pickled olives, make the solution up to 100 cc., filter, and titrate 25 cc. portions with N/10 silver nitrate and potas- sium chromate indicator. Express as salt, and calculate salt-free ash.


Determine moisture, ether extract, nitrogen, and ash. For mois- ture dry 5 grams in a lead capsule, without sand, to constant weight in the water oven, which requires from four to five hours. Extract this residue with anhydrous ether in the Knorr apparatus. This is completed in from six to eight hours. Use 5-gram portions for nitrogen and ash determinations. Calculate the analysis back from the air-dry basis to that of the original moist pits as removed from the olives.



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The data (Table 2) on the samples collected in December, 1914, at which time practically all olives should be ripe, are interesting. These samples, which were carefully selected and segregated on the color basis, ranged from green to purple. The first four samples in the table were picked from the same or adjacent trees in the same grove, as were all the other pairs of samples bearing the same sample number. Size is recorded as number of olives per pound and also in average short diameter in six- teenths of an inch, as both these methods of designa- oO) tion areused commercially. It may be mentioned that diameter and weight. are not exactly related, ow- ing principally to differ- , so ences in shape. Four col-

K ors are distinguished t

green, yellow, red, and purple. By green is meant “orass” green. Theterm <0 “yellow,” although com- monly used by the grower, is @ misnomer, as it is a yellowish green, which ap-


mae OL INFLE & ~ So = ar ea SOLE = ita mrs, tO

pears just before the first 70) 3 ASTS

the various sets of samples 3k papa cpr]

in Table 2 coming from X x

the same trees or grove N ;

shows that the olives with Fie. 1.—Changes in percentage composition of

the more advanced colors Mission olives occurring during ripening in

1915. usually are larger and

heavier than the others, that they have a lower percentage of pits, and, as a rule, are higher in solids in the fruit flesh and contain more oil in the flesh. The oil in the flesh on the dry basis does not appear to be related closely to the color, being frequently nearly the same for the purple and green olives and sometimes higher in the green sample. The amounts of protein and ash in the flesh are roughly equal, fairly uniform, and do not appear to bear any relation to color. The com- position of the pits also bears no relation to the colors. In general, then, among olives from the same tree or grove, the ones with deeper


color are the largest and have the most oil and solids in the flesh. This does not hold, however, in comparing olives of the same variety from different groves or localities, as in several instances the green colored fruit has the more oil and solids in the flesh (Samples 18208 and 18581; 18582, 18587, and 18591; 18583 and 18588).

Since the complete data on the series of samples taken from marked trees during the seasons of 1915 and 1916, to show the progressive development of the fruit, are too voluminous to be given here, Table 3 has been compiled from the data secured for a single