Standard methods for the examination of water and sewageAmerican Public Health Association. Laboratory Section
Science
Standard methods for the examination of water and sewage
American Public Health Association. Laboratory Section
Sewage -- Analysis; Water -- Analysis
_Second procedure for sewage._—Omit the separation of ammonia nitrogen
and determine the ammonia nitrogen and organic nitrogen together.
Determine the ammonia nitrogen in a separate sample by direct
Nesslerization as described on page 19. The organic nitrogen is equal to
the difference.
NITRITE NITROGEN.[51][63a][64][94c][108]
_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]
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