4. Starch. A freshly prepared solution for use as indicator.
Procedure.—Add 500 cc. of the sample to 10 cc. of the standard iodine solution and 1 gram of potassium iodide in a large glass-stoppered bottle or flask. If the sample is to be collected from a tap lead the water into the bottle through a rubber tube extending to the bottom of the bottle so as to eliminate errors due to aeration. Shake the bottle, allow it to stand for a few minutes, and then titrate the excess of iodine with sodium thiosulfate in the presence of starch indicator. Hydrogen sulfide (H2S) in parts per million is equal to 0.34 times the difference in cubic centimeters between the amount of iodine solution added and the amount of N/100 thiosulfate used in the titration.
CHLORINE.
In waters that have been treated with calcium hypochlorite or liquid chlorine it is frequently advisable to ascertain the presence or absence of chlorine. As the reagents which have been proposed for its detection are not specific for chlorine but give similar or identical reactions with oxidizing agents or reducible substances care must be exercised in interpreting the results of such tests: nitrites and ferric salts are of common occurrence, and chlorates also may lead to misinterpretation in waters treated with calcium hypochlorite.
Reagents.—1. Tolidin solution. One gram of o-tolidin, purified by being recrystallized from alcohol, is dissolved in 1 liter of 10 per cent hydrochloric acid.
2. Copper sulfate solution. Dissolve 1.5 grams of copper sulfate and 1 cc. of concentrated sulfuric acid in distilled water and dilute the solution to 100 cc.
3. Potassium bichromate solution. Dissolve 0.025 gram of potassium bichromate and 0.1 cc. of concentrated sulfuric acid in distilled water and dilute the solution to 100 cc.
Procedure.—Mix 1 cc. of the tolidin reagent with 100 cc. of the sample in a Nessler tube and allow the solution to stand at least 5 minutes. Small amounts of free chlorine give a yellow and larger amounts an orange color.
For quantitative determination compare the color with that of standards in similar tubes prepared from the solutions of copper sulfate and potassium bichromate. The amounts of solution for various standards are indicated in Table 13.
| Table 13.—Preparation of permanent standards for content of chlorine. | ||
|---|---|---|
| Chlorine. | Solution of copper sulfate. | Solution of potassium bichromate. |
| Parts per million. | cc. | cc. |
| 0.01 | 0.0 | 0.8 |
| .02 | .0 | 2.1 |
| .03 | .0 | 3.2 |
| .04 | .0 | 4.3 |
| .05 | .4 | 5.5 |
| .06 | .8 | 6.6 |
| .07 | 1.2 | 7.5 |
| .08 | 1.5 | 8.7 |
| .09 | 1.7 | 9.0 |
| .10 | 1.8 | 10.0 |
| .20 | 1.9 | 20.0 |
| .30 | 1.9 | 30.0 |
| .40 | 2.0 | 38.0 |
| .50 | 2.0 | 45.0 |