The sodium arsenite may be prepared from pure arsenious oxide, as described below, and is stable for considerable periods; but commercial oxide requires resublimation to remove arsenic sulphide, which may be present in small quantity. To prepare the solution, dissolve about 5 grams of the powdered oxide, accurately weighed, in 10 cc. of a concentrated sodium hydroxide solution, dilute the solution to 300 cc., and make it faintly acid with dilute hydrochloric acid. Add 30 grams of sodium bicarbonate dissolved in a little water, and dilute the solution to exactly 1000 cc. in a measuring flask. Transfer the solution to a dry liter bottle and mix thoroughly.
It is possible to dissolve the arsenious oxide directly in a solution of sodium bicarbonate, with gentle warming, but solution in sodium hydroxide takes place much more rapidly, and the excess of the hydroxide is readily neutralized by hydrochloric acid, with subsequent addition of the bicarbonate to maintain neutrality during the titration.
The indicator required for this process is made by dipping strips of filter paper in a starch solution prepared as described on page 76, to which 1 gram of potassium iodide has been added. These strips are allowed to drain and spread upon a watch-glass until dry. When touched by a drop of the solution the paper turns blue until the hypochlorite has all been reduced and an excess of the arsenite has been added.
DETERMINATION OF THE AVAILABLE CHLORINE IN BLEACHING POWDER
Bleaching powder consists mainly of a calcium compound which is a derivative of both hydrochloric and hypochlorous acids. Its formula is CaClOCl. Its use as a bleaching or disinfecting agent, or as a source of chlorine, depends upon the amount of hypochlorous acid which it yields when treated with a stronger acid. It is customary to express the value of bleaching powder in terms of “available chlorine,” by which is meant the chlorine present as hypochlorite, but not the chlorine present as chloride.
Procedure.—Weigh out from a stoppered test tube into a porcelain mortar about 3.5 grams of bleaching powder (Note 1). Triturate the powder in the mortar with successive portions of water until it is well ground and wash the contents into a 500 cc. measuring flask (Note 2). Fill the flask to the mark with water and shake thoroughly. Measure off 25 cc. of this semi-solution in a measuring flask, or pipette, observing the precaution that the liquid removed shall contain approximately its proportion of suspended matter.
Empty the flask or pipette into a beaker and wash it out. Run in the arsenite solution from a burette until no further reaction takes place on the starch-iodide paper when touched by a drop of the solution of bleaching powder. Repeat the titration, using a second 25 cc. portion.
From the volume of solution required to react with the bleaching powder, calculate the percentage of available chlorine in the latter, assuming the titration reaction to be that between chlorine and arsenious oxide: