Weigh the sample accurately into 500 mL flask or bottle to which has been added 20 mL of CCl4. The weight of sample must be such that there will be an excess of Wijs solution of 50-60% of the amount added, i.e., 100-150% of the amount absorbed. Table 1 is a convenient guide to the size of sample to be used.
Make certain that the sample is completely dissolved and then pipet 25 mL of the Wijs solution into the flask containing the sample and swirl to ensure an intimate mixture.
4. Prepare and conduct at least two blank determinations with each group of samples simultaneously and similar in all respects.
5. Store the flask in a dark place for exactly 30 min (see Notes, 1) at a temperature of 25 ± 5°C.
6. Remove the flask from storage and immediately add 20 mL of KI solution, followed by 100 mL of distilled water.
7. Immediately titrate with 0.1 N Na2S2O3 solution, adding it gradually and with constant and vigorous shaking (see Notes, 2). Continue the titration until the yellow color has almost disappeared. Add 0.5 mL of starch indicator solution and continue the titration until the blue color has just disappeared.