Reagents.—1. Sulfanilic acid solution. Dissolve 8.00 grams of the purest sulfanilic acid in 1,000 cc. of 5 N acetic acid (sp. gr. 1.041) or in 1,000 cc. of water containing 50 cc. of concentrated hydrochloric acid. This is practically a saturated solution.
2. α-naphthylamine acetate or chloride solution. Dissolve 5.00 grams solid α-naphthylamine in 1,000 cc. of 5 N acetic acid or in 1,000 cc. of water containing 8 cc. of concentrated hydrochloric acid. Filter the solution through washed absorbent cotton or an alundum filter.
3. Sodium nitrite stock solution. Dissolve 1.1 gram silver nitrite in nitrite-free water; precipitate the silver with sodium chloride solution and dilute the whole to 1 liter.
4. Standard sodium nitrite solution. Dilute 100 cc. of solution 3 to 1 liter, then dilute 50 cc. of this solution to 1 liter with sterilized nitrite-free water, add 1 cc. of chloroform, and preserve in a sterilized bottle. One cc. = 0.0005 mg. nitrogen.
5. Fuchsine solution. 0.1 gram per liter.
Procedure.—Place in a standard Nessler tube 50 cc. of the sample, decolorized if necessary with nitrite-free aluminium hydroxide (see p. [42]) or a smaller amount diluted to 50 cc. At the same time prepare in Nessler tubes a set of standards, by diluting to 50 cc. with nitrite-free water, various amounts of the standard nitrite solution. The following amounts of standard solution are suggested: 0.0, 0.1, 0.2, 0.4, 0.7, 1.0, 1.4, 1.7, 2.0, and 2.5 cc. Add 1 cc. of the sulfanilic acid solution and 1 cc. of the α-naphthylamine acetate or hydrochloride solution to the sample and to each standard. Mix thoroughly and allow to stand 10 minutes; then compare the sample with the standards. Do not allow the sample to stand more than one-half hour before making the comparison. If the color of the sample is deeper than that of the highest standard repeat the test on a diluted sample. If 50 cc. of the sample is used 0.01 times the number of cc. of the standard matched equals parts per million of nitrite nitrogen. Satisfactory results can be obtained by using either hydrochloric or acetic acid in preparing the test solutions, but the speed of the reaction is more rapid if acetic acid is used.[[112]]
Permanent standards may be prepared by matching the nitrite standards with dilutions of the fuchsine solution. Fuchsine standards have been found to be sufficiently accurate for waters high in nitrite and for sewage. The standards should be checked once a month and kept out of bright sunlight.
NITRATE NITROGEN.[[16]][[36]][[90]][[100]]
Two methods are recommended for the determination of nitrate nitrogen in water, sewage, and sewage effluents.