5. A sample of pig iron contains 1.43 per cent. of "combined" and 2.02 per cent. of "free" carbon. Taking 2 grams of it for each determination, what weight of CO2 will be got on burning the residue from solution in ammonium cupric chloride, and what from the residue after solution in hydrochloric acid?
BORON AND BORATES.
Boron occurs in nature as boric acid or sassoline (H3BO3); borax or tincal (Na2B4O7.10H2O); ulexite or boronatrocalcite (2CaB4O7.Na2B4O7); borocalcite (CaB4O7.4H2O); boracite, 2Mg3B8O15.MgCl2, and some other minerals. Boric acid is also a constituent of certain silicates, such as tourmaline, axinite, and datholite.
The natural borates are used in the preparation of borax, which is largely employed as a preservative agent, for fluxing, and for other purposes.
There is only one series of boron compounds which have any importance. These are the borates in which the trioxide (B2O3) acts the part of a weak acid. The addition of any acid liberates boric acid, which separates out in cold solutions as a crystalline precipitate. Boric acid is soluble in alcohol and in hot water. On evaporating these solutions it is volatilised, although the anhydrous oxide is "fixed" at a red heat. The borates are mostly fusible compounds, and are soluble in acids and in solutions of ammonic salts.
Detection.—Boron in small quantities will escape detection unless specially looked for, but there is no difficulty in detecting its presence. Heated in the Bunsen-burner flame with "Turner's test," it gives an evanescent yellowish-green colour, due to fluoride of boron (BF3). "Turner's test" is a mixture of 5 parts of bisulphate of potash and 1 part of fluor spar. Boric acid itself imparts a characteristic green colour to the flame, which gives a spectrum made up of four well-marked and equidistant lines, three in the green and one in the blue. Solutions of boric acid give with "turmeric paper," which has been dipped into it and dried, a characteristic red tint. This is a very delicate test, but in trying it a blank experiment should be carried out alongside with a solution made up of the same re-agents which have been used in liberating the boric acid in the sample.
Solution and Separation.—The solution presents no difficulty, but the separation is troublesome. The best method is that of Gooch; who, if necessary, first fuses with carbonate of soda, and after the removal of chlorides and fluorides (by nitrate of silver or a lime salt), evaporates the aqueous extract with nitric or acetic acid to dryness in a retort and, subsequently, with repeated doses of 10 c.c. each of methyl alcohol. The distillate contains the boron as boric acid. Half a gram of the trioxide (B2O3) is completely carried over by two evaporations, each with 10 c.c. of the alcohol; but if water or foreign salts are present, more than this is required. In ordinary cases six such evaporations are sufficient for 0.2 gram of the oxide.[123]
GRAVIMETRIC DETERMINATION.
Before the introduction of Gooch's process it was usual to determine the boron trioxide "by difference." If the alcoholic distillate containing the boric acid is digested with about 1 gram (a known weight) of lime for ten or fifteen minutes, the alcohol can be evaporated off without danger of loss. Either calcium nitrate or acetate (which will be formed at the same time) yields lime upon subsequent ignition. Consequently, the increase in weight, after ignition, upon that of the lime taken gives the amount of boron trioxide present. The trioxide contains 31.4 per cent. of boron (B). Since magnesia does not form a soluble hydrate it cannot satisfactorily be used instead of lime.