Part 15

Reagents.—1. Nitric acid. Dilute 1 part of concentrated nitric acid with 4 parts of distilled water. Free the dilute acid from brown oxides of nitrogen by aeration.

2. Sulfuric acid. Dilute 1 part of concentrated sulfuric acid with 3 parts of distilled water.

3. Dilute sulfuric acid. Dilute 25 cc. of concentrated acid to 1 liter with distilled water. Add enough permanganate solution to color faintly the dilute acid.

4. Standard manganous sulfate. The standard solution of manganous sulfate prepared as described under persulfate method (p. 48) should be used and the standards should be prepared by following the same procedure as is used for the sample. This solution is more permanent than a solution of potassium permanganate, which may, however, be used. To prepare it dissolve 0.288 gram of potassium permanganate in distilled water and dilute the solution to 1 liter.

5. Sodium bismuthate. Purest dry salt.

Procedure.—Use an amount of the sample that contains not more than 0.2 mg. of manganese. Add 0.5 cc. of sulfuric acid and evaporate to dryness. Heat until the sulfuric acid is volatilized and ignite the residue. Dissolve in 40 cc. of nitric acid, add about 0.5 gram of sodium bismuthate, and heat until the permanganate color disappears. Add a few drops of a solution of ammonium or sodium bisulfate to clear the solution and again boil to expel oxides of nitrogen. Remove from the source of heat, cool to 20° C., again add 0.5 gram of sodium bismuthate, and stir. When the maximum permanganate color has developed, filter through an alundum or Gooch crucible containing an asbestos mat ignited and washed with potassium permanganate. Wash the precipitate with dilute sulfuric acid until the washings are colorless. Transfer the filtrate to a 50 cc. Nessler tube and compare the color of it with that of standards prepared from the potassium permanganate solution. To prepare the standards, dilute portions of 0.2, 0.4, 0.6 cc., etc. of the permanganate solution to 50 cc. with dilute sulfuric acid. The content of manganese is calculated as described under persulfate method (p. 49).

LEAD, ZINC, COPPER, AND TIN.

Determinations of lead, zinc, copper, and tin are important in certain mining regions and in places where the water has a solvent action on pipes and other containers. The use of certain “germicides” also makes it necessary to test for some of these metals.

Lead, zinc, and copper may be determined colorimetrically or electrolytically. The colorimetric methods are not so accurate as a combination of both, and are chiefly of value as qualitative tests.

It is possible to make a rough estimation of the amount of lead in clear waters by acidifying with acetic acid, saturating with hydrogen sulfide, and comparing the color produced with that produced by standard lead solutions in Nessler tubes, treated in similar manner. This method, however, is not applicable if the water is colored or contains iron.

Reagents.—1. Standard lead solution. Dissolve 1.60 grams of lead nitrate (Pb(NO{3}){2}) in 1 liter of distilled water. One cc. of this solution contains 1 mg. of lead (Pb). As a check it is desirable to determine lead as sulfate in a measured portion of this solution.

2. Standard copper solution. Dissolve about 0.8 gram of copper sulfate crystals (CuSO{4}.5H{2}O) in water and, after the addition of 1 cc. of concentrated sulfuric acid, dilute the solution to 1 liter. Determine the copper in 100 cc. of this solution in the usual way by electrolytic deposition. Dilute the solution so that 1 cc. contains 0.2 milligram copper (Cu). This solution is permanent.

3. Ammonium chloride. Twenty-five per cent solution.

4. Ammonium acetate. Fifty per cent solution.

5. Ammonium hydroxide. (Sp. gr. 0.96.)

6. Hydrogen sulfide. Saturated solution.

7. Potassium sulfide. An alkaline solution of potassium sulfide made by mixing equal volumes of 10 per cent potassium hydroxide and a saturated aqueous solution of hydrogen sulfide.

8. Potassium oxalate. Crystals.

9. Potassium sulfate. Crystals.

10. Alcohol. Ninety-five per cent.

11. Alcohol. Fifty per cent.

12. Acetic acid. Fifty per cent.

13. Nitric acid. Concentrated acid (Sp. gr. 1.42).

14. Nitric acid. Dilute 1 part of the concentrated acid to 10 parts with distilled water.

15. Hydrochloric acid. (Sp. gr. 1.20.)

16. Sulfuric acid. Concentrated acid (Sp. gr. 1.84).

17. Sulfuric acid. Dilute the concentrated acid with an equal volume of distilled water.

18. Urea. Crystals.