Contributions to the Analysis of Rubber. I. Determination of the Water-Soluble Components of Rubber

1. It is shown that the methods which are ordinarily used for determining water-soluble substances in raw rubber give low results, and are quite useless for vulcanized rubber. 2. New analytical procedures are developed for determining the water-soluble substances in raw rubber and in vulcanized rubber. These procedures are carried out in the following manner. (a) Raw Rubber.—Heat 2 grams of rubber in 80 cc. of xylene and 5 cc. of acetic acid on a water bath until the rubber is completely dissolved, add 5 cc. of acetic acid and 10 cc. of water, heat for 3–4 hours on the water bath with frequent agitation, transfer to a distilling flask (rinsing the first flask with 50 cc. of hot water), distill the xylene with steam, filter the residual solution, evaporate the filtrate on a water bath; and dry at 100° C. (b) Vulcanized Rubber and Rubber Mixtures.—First extract the sample with acetone, heat 2 grams of the acetone-extracted sample with 80 cc. of xylene on a water bath, add 5 cc. of acetic acid, reflux the mixture on an oil bath, after complete dissolution add 5 cc. of acetic acid and 10 cc. of water, heat the solution for 2 hours on an oil bath at 110–120° C., distill the xylene, as in the determination with raw rubber, filter the residue, evaporate the filtrate to dryness, take up the residue in 50 cc. of water, pass a current of hydrogen sulfide through the solution for 10 minutes to precipitate zinc as sulfide, filter, evaporate the filtrate, and dry the residue at 100° C. 3. In the presence of calcium compounds, magnesium compounds, glue and textiles, the method gives false results. Modifications of the method are therefore recommended, whereby these substances are eliminated.