1. The specimen of “Bismuth Tribromphenolate” sent to the Council of National Defense complies with the New and Nonofficial Remedies description for bismuth tribromphenate, except that it contains considerable amounts (approximately 16 per cent.) of alcohol-soluble, uncombined tribromphenol.
Revision of N. N. R. Standards
The results of the examination of the three specimens were sent to the Heyden Chemical Works and to Merck and Co. (in each case disclosing the identity of the particular firm’s product), asking aid in the standardization of the product. After Merck and Co. had submitted valuable advice for a revision of the somewhat loosely drawn standards for bismuth tribromphenate in N. N. R., 1918, the inquiry whether the following proposed revision of the description of bismuth tribromphenate in New and Nonofficial Remedies was acceptable, was submitted to both firms:
BISMUTH TRIBROMPHENATE.—Bismuthi Tribromphenas.—Bismuth Tribromphenol.—Xeroform.—A basic bismuth tribromphenate of variable composition.
An amorphous, yellow, nearly odorless and tasteless powder, neutral to moistened litmus paper.
It is only slightly soluble in water, alcohol, chloroform, liquid petrolatum and vegetable oils. Alkalies and strong acids decompose it. It is stable at temperatures below 120 C.
When about 1 gm. of the salt is boiled with 10 c.c. of sodium hydroxide test solution, the liquid filtered, and the filtrate acidulated with sulphuric acid, the white curdy precipitate produced, when washed and dried, melts at 90 to 95 C. (tribromphenol). The contents of the filter dissolve completely in dilute hydrochloric acid (insoluble inert material).
Boil 1 gm. of bismuth tribromphenate with 20 c.c. of a mixture of equal parts of acetic acid and distilled water, cool the solution and filter. Free the filtrate from bismuth by the addition of hydrogen sulphide, boil the mixture and again filter. The latter filtrate leaves not more than 0.005 gm. of residue on evaporation and gentle ignition (alkalies and alkali earths).
Shake for one minute in a separatory funnel, 2 gm. of bismuth tribromphenate, 20 c.c. of ether, and 20 c.c. of a mixture of equal volumes of hydrochloric acid and distilled water. Draw off the aqueous portion and concentrate to about 4 c.c.; pour it into 100 c.c. distilled water, filter, evaporate the filtrate on the water bath to 30 c.c., again filter and divide this filtrate into portions of 5 c.c. each. Mix one portion with an equal volume of dilute sulphuric acid; it does not become cloudy (lead). Treat another portion with a slight excess of ammonia water; the supernatant liquid does not exhibit a bluish tint (copper). Another portion is not immediately affected by barium nitrate test solution (sulphate).