Part 21

If the material does not flow readily fill the weighed flask as completely as possible without exerting pressure during the procedure. Weigh and then fill the flask to the brim with distilled water. Let it stand for a few minutes, until trapped air has escaped, then add more water if necessary and weigh. Subtract the weight of the added water from the weight of the water that completely fills the flask; the specific gravity is equal to the weight of the material divided by this difference. Record the specific gravity only to the second decimal place.

MOISTURE.

Heat approximately 25 grams of sludge or mud in a weighed nickel dish on the water bath until it is fairly dry. Dry the residue in an oven at 100° C., cool, and weigh. Repeat to approximate constant weight. The loss in weight is moisture.

VOLATILE AND FIXED MATTER.

Ignite, at dull red heat in a hood, the residue from the determination of moisture until all the carbon has disappeared. Cool the residue in a desiccator and weigh it. The residue is the fixed matter. The volatile matter is the difference in weight between the original dried sludge and the ignited sludge.

TOTAL ORGANIC NITROGEN.

Preparation of sample.—For the determination of organic nitrogen and fats dry approximately 50 to 75 grams of the sludge or mud in a porcelain dish first on the water bath and finally in the hot-water oven until all the moisture has disappeared. Grind the dry material to a fine powder and keep it in a glass-stoppered bottle.

Reagents.—1. Sulfuric acid. Concentrated, nitrogen-free. 2. Copper sulfate solution. Ten per cent. 3. Potassium permanganate. Crystals.

First procedure.—Weigh accurately 0.5 gram of dried sludge or 5.0 grams of dried mud and put it into a 500 cc. Kjeldahl flask. Digest it with 20 cc. of sulfuric acid, or more if necessary, and 1 cc. of copper sulfate solution to assist the oxidation. Boil for several hours until the liquid becomes colorless or slightly yellow. Oxidize the residue with 0.5 gram of potassium permanganate, and follow the “Procedure for Sewage” (pp. 21–22).

Second procedure.—The following method is convenient for routine work at sewage disposal plants. After digestion as described in the first procedure, cool, transfer to a glass-stoppered 100 cc. flask, dilute with distilled water to 100 cc., and mix well. Transfer 50 cc. with a pipette into another 100 cc. volumetric flask, and make this portion alkaline with 50 per cent sodium hydroxide, testing a drop of the liquid on a porcelain plate with phenolphthalein to insure neutralization. The formation of a floc usually indicates that neutralization is complete. Dilute the solution to 100 cc., pour it into a small glass-stoppered bottle and permit it to stand until the next day. Nesslerize an aliquot portion of the clear supernatant liquid, and calculate the percentage of nitrogen in the material.

ETHER-SOLUBLE MATTER.

Fats are usually determined only on sewage sludge, but some mud deposits contain small quantities due to the presence of trade wastes.

Procedure.—Weigh 0.5 to 25 grams of dry material according to the quality of the sludge or mud. Add water to the weighed portion in a porcelain dish and acidify the mixture with N/50 sulfuric acid in the presence of litmus tincture or azolitmin solution as indicator. Avoid adding too much acid as an excess gives too high results on account of fatty acid residues. Evaporate the acidified mixture to dryness on the water bath, and heat it in the hot air oven at 100° C. two to three hours. Extract the dry residue with boiling ether, rubbing the sides and bottom of the dish to insure complete solution of the fat. Three extractions with ether are usually sufficient. Filter the ether solution through a 5 cm. filter paper into a small flask. Evaporate the ether slowly, dry the fatty extract for half an hour at 100° C., cool in a desiccator, and weigh. If it is desirable, particularly with certain industrial wastes, to determine the quantity of saponified fat determine the fats with and without the addition of acid. The difference between the quantities found by the two determinations is the content of saponified fat.

FERROUS SULFIDE.

The liberation of hydrogen sulfide on adding dilute hydrochloric acid to a sludge indicates the presence of ferrous sulfide. As ferrous sulfide quickly oxidizes on exposure to air a quantitative determination of this constituent must be made immediately after collection of the sample.

Procedure.—Heat a definite portion of the sludge with hydrochloric acid in a flask. Pass the liberated gas through bromine water or hydrogen peroxide. Determine gravimetrically the sulfate in the oxidizing solution, and calculate the equivalent of ferrous sulfide by multiplying the weight of barium sulfate by 0.376.

BIOCHEMICAL OXYGEN DEMAND.

The quantity of river mud most suitable for the determination of the biochemical oxygen demand ranges within certain limits, largely according to the amount of oxidizable matter present. For examinations of river mud prepare a 1 per cent stock suspension in distilled water or tap water saturated with oxygen and free from nitrate; use in the test a dilution of this stock suspension equivalent to a concentration of 1 to 10 grams per liter of mud. For examinations of fresh sewage sludge prepare a 1 per cent stock suspension in a similar manner, but use in the test a dilution equivalent to only 0.1 to 1.0 gram per liter of wet material. For examinations of dried sludges, which have undergone more or less oxidation higher concentrations may be required.

Procedure.—Place a measured portion of the sample, or the proper amount of the 1 per cent stock suspension of the sample, in a 300 cc. narrow-mouth glass-stoppered bottle, and dilute it to the desired concentration with water saturated with oxygen. Determine the oxygen content at 20° C. of the waters that are used for dilution. This determination must be made before the mud or sludge is added because iron sulfide in the mud or sludge rapidly consumes part of the dissolved oxygen. Incubate at 20° C. for five days.

Shortly before the determination of the oxygen remaining in solution at the end of five days rotate the bottle once or twice to mix its contents and allow sedimentation for about 30 minutes. Siphon the greater part of the liquid through a narrow-bore siphon into a 150 cc. bottle, which has been filled with carbon dioxide. Reject the first 25 cc. of the siphoned liquid and allow a little to overflow at the end of siphoning. Determine the oxygen content of the solution in the bottle in the usual way (pp. 65–68). Report the oxygen demand in percentage of the dried mud or sludge.

ANALYSIS OF CHEMICALS.

The following sections describe the accepted methods for the analysis of the chemicals commonly used in the treatment of water.

REAGENTS.

1. Distilled water. In practically all the tests of chemicals it is necessary to use exclusively distilled water that has been freshly boiled to free it from carbon dioxide and oxygen.

2. Concentrated hydrochloric acid. Sp. gr. 1.20.

3. Hydrochloric acid, N/2.

4. Hydrochloric acid, N/10.

5. Ammonium hydroxide. Redistilled; sp. gr. 0.90.