CITRIC ACID
A Dictionary of Arts, Manufactures and Mines · 1840 · p. 304
( Acide citrique , Fr.; Citronensäure , Germ.) Scheele first procured this acid in its pure state from lemon juice, by the following proce . The juice put into a large tub, is to be saturated with dry chalk in fine powder, noting carefully the quantity employed. The citrate of lime which precipitates being freed from the supernatant foul liquor, is to be well washed with repeated affusion and decantation of water. For every 10 pounds of chalk employed, nine and a half pounds of sulphuric acid, diluted with six times its weight of water, are to be poured while warm upon the citrate of lime, and well mixed with it. At the end of twelve hours, or even sooner, the citrate will be all decomposed, dilute citric acid will float above, and sulphate of lime will be found at the bottom. The acid being drawn off, the calcareous sulphate must be thrown on a canva filter, drained, and then washed with water to abstract the whole acid. The citric acid thus obtained may be evaporated in leaden pans, over a naked fire till it acquires the specific gravity 1·13; after which it must be transferred into another ve el, evaporated by a steam or water bath till it a umes a syrupy aspect, when a pellicle appears first in patches, and then over the whole surface. This point must be watched with great circumspection, for if it be pa ed, the whole acid runs a risk of being spoiled by carbonization. The steam or hot water must be instantly withdrawn, and the concentrated acid put into a crystallizing ve el in a dry, but not very cold apartment. At the end of four days, the crystallization will be complete. The crystals must be drained, re-di olved in a small portion of water, the solution set aside to settle its impurities, then decanted, re-evaporated, and re-crystallized. A third or fourth crystallization may be nece ary to obtain a colourle acid. If any citrate of lime be left undecomposed by the sulphuric acid, it will di olve in the citric acid, and obstruct its crystallization, and hence it will be safer to use the slightest exce of sulphuric acid, than to leave any citrate undecomposed. There should not however be any great exce of sulphuric acid. If there be, it is easily detected by nitrate of barytes, but not by the acetate of lead as prescribed by some chemical authors; because the citrate of lead is not very soluble in the nitric acid, and might thus be confounded with the sulphate, whereas citrate of barytes is perfectly soluble in that test acid. Sometimes a little nitric acid is added with advantage to the solution of the coloured crystals, with the effect of whitening them. Twenty gallons of good lemon juice will afford fully ten pounds of white crystals of citric acid. Attempts were made both in the West Indies and Sicily, to convert the lime and lemon juice into citrate of lime, but they seem to have failed through the difficulty of drying the citrate for shipment. The crystals of citric acid are oblique prisms with four faces, terminated by dihedral summits, inclined at acute angles. Their specific gravity is 1·617. They are unalterable in the air. When heated, they melt in their water of crystallization; and at a higher heat, they are decomposed. They contain 18 per cent. of water, of which one half may be separated in a dry atmosphere, at about 100° F., when the crystals fall into a white powder. Citric acid in crystals is composed by my analysis of carbon, 35·8, oxygen 59·7, and hydrogen 45; results which differ very little from those of Dr. Prout, subsequently obtained. I found its atomic weight to be 8·375, compared to oxygen 1,000. I cannot account for Berzelius’s statements relative to the composition of this acid. Citric acid in somewhat crude crystals is employed with much advantage in calico-printing. If adulterated with tartaric acid, the fraud may be detected by adding potash to the solution of the acid, which will occasion a precipitate of cream of tartar.
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