A practical treatise on the manufacture of perfumery

by C. Deite

Expression.—This is only practicable when the substances are especially rich in oil and of sufficient softness, as in the case with the peel of the orange, citron, lemon, etc. In such instances the material is simply placed in a linen cloth and subjected to a strong pressure until it ceases to yield oil. The press may be of any size according to the quantity to be expressed. For small quantities it generally consists of an iron vessel, having a small opening at the bottom so that the oil may flow out. The material is placed upon a perforated bottom inside of the vessel and covered with a well-fitting iron plate, that can be pressed down by means of a screw. Though the material is fairly exhausted by such a press, for large operations it is advisable to make use of a hydraulic press, which is constructed and managed in exactly the same manner as those used for the expression of fixed oils.

By expression a turbid milky fluid is obtained, which consists of the volatile oil and aqueous substances. The latter are a solution of various extractive substances and salts in water. This fluid, as it runs from the press, is received in tall, narrow, glass vessels and brought into a cool place for clarification. This frequently requires several days, three distinct layers being generally distinguished. On the bottom is a mucous layer consisting of cell substances carried along by the liquid bodies. Over this is a clear fluid consisting of a solution of extractive substances, vegetable albumen, and salts, and upon this floats the volatile oil, being specifically the lightest body, which, by its greater refractive power, can be clearly distinguished from the aqueous fluid.

The oil is separated by bringing all that has been expressed into a bottle provided near the bottom with a lateral neck closed by a cock. After separating the oil from the aqueous fluid, the latter is allowed to escape by opening the cock.

The oil obtained in this manner is still impure, and requires further treatment to remove small vegetable fibres, invisible to the naked eye, which float in them, and cause them to be somewhat opaque and slightly opalescent. By their subsequent decomposition they would also give the oil a disagreeable odor.

There are two methods of obtaining the oil entirely clear, viz., filtration and distillation. Filtration is the cheaper process, but requires special precautions to exclude the air as much as possible to prevent the oil from undergoing injurious changes. By arranging the filtering apparatus so that the oil always comes in contact with only the same quantity of air, the injurious action of the oxygen is reduced to a minimum. It is self-evident that the apparatus should not be placed in the sun, but in a semi-dark, cool place.

Fig. 1.

A filter of simple construction, and performing excellent service, is shown in Fig. 1. It consists of a large glass bottle, F, hermetically closed by a doubly-perforated cork. The neck of the glass funnel T, the upper rim of which is ground smooth, is placed in one of the holes, and a glass tube, r, bent at a right angle, is fitted into the second hole. A thick wooden lid, with a rubber ring on the lower side, is placed upon the funnel, thus closing it air-tight. In the centre of the lid is fitted a glass tube, r´, also bent at a right angle, which is connected with the tube r, by a rubber hose, k. After the funnel has been provided with filtering paper and the oil to be filtered, the lid is placed upon it, and must not be removed, except for the purpose of pouring more oil into the funnel. The air in the bottle F is displaced by the oil dropping into it, and escapes through r, k and r´ into the funnel, and thus only the air in the bottle and funnel can act upon the oil.

The other method for the complete purification of expressed oil is by rectification or distillation with water. For this purpose the oil, together with a little water, is brought into one of the stills described later on, and the oil distilled over. It is sometimes difficult to obtain the last portion of the oil, especially with a still heated by direct fire, and it is therefore preferable to combine it with a fresh quantity of the same oil to be distilled.

Distillation.—There are at present two methods in use. The one is founded upon the direct action of the heat, the other upon the use of steam. The first was formerly in general practice, and is still largely employed in France and England, and to a limited extent in this country. It is, however, very deficient in many respects. As the stills must necessarily be of small capacity, only small quantities can be distilled at one time, and the oils very rarely possess the peculiar odor due to them, and sometimes the odor is even altered. In mixing too little water with the materials to be extracted, there is danger that empyreumatic oils will be formed; a large quantity of water, on the other hand, is of disadvantage, in so far as in case the perfume-materials contain little oil, only a perfumed water, but no oil, will be obtained. In order to avoid these inconveniences, or, at least, to do away with some of them, another plan was devised. The materials to be distilled were spread upon sieves, which were suspended in the upper part of a still, so that they might be penetrated from below. It is true no scorching is possible in this case, as was in the other process when the heating was continued after all the water had evaporated, and the oil retains its proper color, but by this method only small quantities can be extracted at a time. The still generally used for distillation with direct heat resembles so much an ordinary whiskey still as to need no further description here.