NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.

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Designation: D1426 − 08

StandardTest Methods for

Ammonia Nitrogen In Water1
This standard is issued under the fixed designation D1426; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.

1. Scope 2. Referenced Documents

1.1 These test methods cover the determination of ammonia 2.1 ASTM Standards:2
nitrogen, exclusive of organic nitrogen, in water. Two test D1066 Practice for Sampling Steam
methods are included as follows: D1129 Terminology Relating to Water
D1192 Guide for Equipment for Sampling Water and Steam
Sections
Test Method A—Direct Nesslerization 7 to 15 in Closed Conduits (Withdrawn 2003)3
Test Method B—Ion Selective Electrode 16 to 24 D1193 Specification for Reagent Water
1.2 Test Method A is used for the routine determination of D2777 Practice for Determination of Precision and Bias of
ammonia in steam condensates and demineralizer effluents. Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
1.3 Test Method B is applicable to the determination of D5810 Guide for Spiking into Aqueous Samples
ammonia nitrogen in the range from 0.5 to 1000 mg NH3N/L D5847 Practice for Writing Quality Control Specifications
iTeh Standards
directly in reagent and effluent waters. Higher concentrations
can be determined following dilution. The reported lower
for Standard Test Methods for Water Analysis
E60 Practice for Analysis of Metals, Ores, and Related

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range is based on multiple-operator precision. Lower limits
have been obtained by two of the twelve laboratories partici-
Materials by Spectrophotometry
E275 Practice for Describing and Measuring Performance of
Ultraviolet and Visible Spectrophotometers
1.4 Both test methods A and B are Document
applicable to surface and Preview
pating in the round robin.
2.2 APHA Standard4:
Standard Methods for the Examination of Water and Waste
industrial waters and wastewaters following distillation. The Water
test method for distillation given in Appendix X1 has been
ASTM D1426-08
used in the past to meet requirements for predistillation of 3. Terminology
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samples being analyzed for ammonia. 3.1 Definitions—For definitions of terms used in these test
1.5 The values stated in SI units are to be regarded as methods, refer to Terminology D1129.
standard. No other units of measurement are included in this
4. Significance and Use
standard.
4.1 Nitrogen is a nutrient in the environment and is neces-
1.6 This standard does not purport to address all of the sary to sustain growth of most organisms. It exists in several
safety concerns, if any, associated with its use. It is the forms such as nitrate, nitrite, organic nitrogen such as proteins
responsibility of the user of this standard to establish appro- or amino acids, and ammonia.
priate safety and health practices and determine the applica-
4.2 Ammonia is a colorless, gaseous compound with a sharp
bility of regulatory limitations prior to use.
distinctive odor. It is highly soluble in water where it exists in
1.7 The distillation method now appears as Appendix X1 a molecular form associated with water and in an ionized form
and is provided as nonmandatory information only. The auto- as NH4+. The extent of association or ionization is dependent
mated colorimetric phenate method has been discontinued.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
1
These test methods are under the jurisdiction of ASTM Committee D19 on Standards volume information, refer to the standard’s Document Summary page on
Water and are the direct responsibility of Subcommittee D19.05 on Inorganic the ASTM website.
3
Constituents in Water. The last approved version of this historical standard is referenced on
Current edition approved Aug. 15, 2008. Published September 2008. Originally www.astm.org.
4
approved in 1956. Last previous edition approved in 2003 as D1426 – 03. DOI: Available from American Public Health Association, 800 I St. N.W.,
10.1520/D1426-08. Washington, DC 20001, http://www.apha.org.

*A Summary of Changes section appears at the end of this standard

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 D1426 − 08
on the temperature and pH. It may also be toxic to aquatic life. Nessler’s reagent to give the characteristic yellow color in the
The extent of toxicity is dependent upon species and extent of time required for the test. Similarly, volatile alkaline com-
dissociation.5 Ammonia may occur in water as a product of pounds such as hydrazine and the amines will influence
anaerobic decomposition of nitrogen containing compounds or titrimetric results. Some organic compounds such as ketones,
from waste streams containing ammonia. aldehydes, alcohols, and some amines may cause an off color
on Nesslerization. Some of these, such as formaldehyde may
5. Purity of Reagents be eliminated by boiling off at a low pH prior to Nesslerization.
5.1 Reagent grade chemicals shall be used in all tests. Residual chlorine must be removed prior to the ammonia
Unless otherwise indicated, it is intended that all reagents shall determination by pretreatment of the sample.
conform to the specifications of the Committee on Analytical 9.2 Turbid samples may be clarified with ZnSO4 and NaOH
Reagents of the American Chemical Society, where such solution; the precipitated Zn(OH)2 is filtered off, discarding the
specifications are available.6 Other grades may be used, pro- first 25 mL of filtrate, and the ammonia is determined on an
vided it is first ascertained that the reagent is of sufficiently aliquot of the remaining clear filtrate by direct Nesslerization.
high purity to permit its use without lessening the accuracy of Ammonia can be lost in basic conditions. Check procedure
the determination. with a standard solution.
5.2 Unless otherwise indicated, references to water shall be
understood to mean reagent water conforming to Specification 10. Apparatus
D1193, Type I. In addition, this water shall be free of ammonia 10.1 Nessler Tubes— Matched Nessler tubes4 about 300
nitrogen. Such water is best prepared by the passage of distilled mm long, 17-mm inside diameter, and marked for 50 mL at 225
water through an ion-exchange resin. These resins should also 6 1.5 mm from inside the bottom.
be selected so that organic compounds which might subse-
10.2 Photometer—Filter photometer or spectrophotometer
quently interfere with the ammonia determination will be
suitable for absorbance measurements at 425 nm. Filter pho-
removed. Regeneration of the ion-exchange materials should
tometers and photometric practices used in this test method
be carried out in accordance with the instructions of the
shall conform to Practice E60. Spectrophotometers shall con-
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manufacturer.
form to Practice E275.
6. Sampling 10.3 Stoppers—Rubber, size No. 2, to fit Nessler tubes.
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6.1 Collect the sample in accordance with Practice D1066,
Specification D1192, and Practices D3370, as applicable.
These stoppers shall be boiled in H SO (1 + 99), rinsed,
boiled in NaOH solution (1 g/L), rinsed, allowed to stand in
2 4

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dilute Nessler reagent for 30 min, and then rinsed again.
6.2 Preserve the samples by the addition of 1 mL of
concentrated sulfuric acid per litre and store at 4°C. The pH 11. Reagents
should be 2.0 or less. Analyze the samples within 24 h of
sampling. Do not use mercuric chloride as a preservative. 11.1 Ammonia Nitrogen Solution, Standard (1 mL = 0.01
ASTM D1426-08mg N)—Dry reagent grade ammonium sulfate ((NH4)2SO–4)
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TEST METHOD A—DIRECT NESSLERIZATION for 1 h at 100°C. Accurately weigh 4.718 g and dissolve in
water. Dilute to 1 L in a volumetric flask. Pipet 10 mL of this
7. Scope stock solution to a 1-L volumetric flask and dilute to volume
7.1 This test method is suitable for the rapid routine with water.
determination of ammonia nitrogen in steam condensates and 11.2 Disodium Dihydrogen Ethylenediamine Tetraacetate
demineralized water. See Appendix X1 for the distillation test Solution (500 g/L)—Dissolve 500 g of disodium dihydrogen
method. ethylenediamine tetraacetate dihydrate in water containing 100
8. Summary of Test Method g of NaOH. Gently heat to complete dissolution. Cool and
dilute to 1 L.
8.1 A sample aliquot is Nesslerized directly and the ammo-
nia content determined colorimetrically. 11.3 Nessler Reagent—Dissolve 100 g of anhydrous mercu-
ric iodide (HgI2) and 70 g of anhydrous potassium iodide (KI)
9. Interferences in a small volume of water. Add this mixture slowly, with
stirring, to a cooled solution of 160 g of sodium hydroxide
9.1 Glycine, urea, glutamic acid, cyanates, and acetamide
(NaOH) in 500 mL of water. Dilute the mixture to 1 L. Store
hydrolyze very slowly in solution on standing, but, of these,
the solution in the dark for five days and filter twice, either
only urea and cyanates will hydrolyze on distillation at a pH of
through a fritted glass crucible or glass fiber filter before using.
9.5. Glycine, hydrazine, and some amines will react with
If this reagent is stored in a chemically resistant bottle out of
direct sunlight, it will remain stable up to a period of 1 year.
5
Quality Criteria for Water, USEPA-440/9-76-023, July 26, 1976, pp. 16–24.
6
Reagent Chemicals, American Chemical Society Specifications, American NOTE 1—This reagent should give the characteristic color with ammo-
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not nia within 10 min after addition, and should not produce a precipitate with
listed by the American Chemical Society, see Annual Standards for Laboratory small amounts of ammonia (0.04 mg in a 50-mL volume). The solution
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia may be used without 5-day storage if it is filtered through a 0.45 µm
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, membrane (previously rinsed with reagent water Type I (see Specification
MD. D1193)) shortly before use.

2
 D1426 − 08
NOTE 2—Mercury and its salts are hazardous materials. They should be TABLE 1 Determination of Precision and Bias for Test Method
stored, handled and dispensed accordingly. Disposal of solutions must be A—Direct Nesslerization Method (Photometric at 425 nm)
made by legally acceptable means. Precision,
Amount Mean
Matrix mg/L Bias,
11.4 Sodium Hydroxide Solution (240 g/L)—Dissolve 240 g Added,
Water
Recovery,
%
mg/L % St So
of NaOH in water and dilute to 1 L.
0.120 Reagent 89 0.011 0.003 −10.8
11.5 Sodium Potassium Tartrate Solution (300 g/L)— 0.200 Reagent 98 0.013 0.002 −2.5
Dissolve 300 g of sodium-potassium tartrate tetrahydrate in 1 0.350 Reagent 98 0.021 0.002 −1.7
1.000 Reagent 101 0.042 0.014 + 1.4
L of water. Boil until ammonia-free and dilute to 1 L.
11.6 Zinc Sulfate Solution (100 g/L)—Dissolve 100 g of
zinc sulfate heptahydrate (ZnSO4·7H2O) in water and dilute to
1 L. Ammonia, mg/L 5 E 3 1.22 (2)

12. Calibration
where:
12.1 Prepare a series of standards containing the following
E = ammonia nitrogen, mg/L.
volumes of standard ammonia nitrogen solution diluted to 50
mL with water: 0.0, 1.0, 3.0, 5.0, 8.0, and 10.0 mL. Mix, add 15. Precision and Bias7
1 mL of Nessler reagent, and remix. After 20 to 30 min, using
a photometer suitable for absorbance measurement at 425 nm 15.1 The precision of this test method was measured with-
and a compensatory blank (Nesslerized ammonia-free water), out the use of any distillation procedure by nine laboratories in
prepare a calibration curve based on a series of these standards. reagent water only at four levels in the range from 30 to 100
mg NH3-N/L, and each concentration was done in triplicate.
12.2 If a visual comparison method is used, prepare a series The test method was tested in reagent water because steam
of 14 Nessler tubes containing the following volumes of condensates and demineralized effluents are similar to reagent
standard ammonia nitrogen solution diluted to 50 mL with water.

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water: 0.0, 0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.4, 1.7, 2.0, 2.5, 3.0, 3.5,
and 4.0 mL. Mix, add 1 mL of Nessler reagent, and remix. 15.2 Analysts using Test Method A in any matrix other than
a steam condensate or demineralized effluent must show the
13. Procedure
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13.1 If the sample contains turbidity, add 1 mL of ZnSO
applicability of this test method to that matrix.
15.3 The precision of Test Method A in reagent water was

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4
solution to a 100-mL aliquot and mix. Add NaOH solution with 0.04 mg/L at 1.0 mg NH -N/L. Other precision data are shown
3

gentle mixing until the pH is about 10.5. Allow to settle and in Table 1.
filter using a water-washed, moderately-retentive filter paper, 15.4 Precision and bias for this test method conforms to
discarding the first 25 mL of the filtrate. Dilute a portion of the Practice D2777–77, which was in place at the time of collab-
ASTM D1426-08
filtrate or clear sample, containing not more than 0.1 mg of orative testing. Under the allowances made in 1.4 of
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ammonia nitrogen, to 50 mL in a Nessler tube. Add 2 drops of D2777–06, these precision and bias data do meet existing
sodium potassium tartrate solution (or disodium dihydrogen requirements for interlaboratory studies of Committee D19 test
ethylenediamine tetraacetate) to prevent cloudy tubes, and mix. methods.
Add 1 mL of Nessler solution and measure photometrically at
a wavelength of 425 nm. TEST METHOD B—ION SELECTIVE ELECTRODE
13.2 If a visual comparison method is used, select a volume 16. Scope
containing not more than 0.04 mg of ammonia nitrogen and
dilute to 50 mL. Mix, add 1 mL of Nessler reagent, and remix. 16.1 This test method is applicable to the measurement of
Compare the color developed after 10 min with the previously ammonia in reagent and effluent water.
prepared standards. If the ammonia nitrogen concentration is
17. Summary of Test Method
below 0.008 mg (in the 50-mL tube) compare after 30 min.
17.1 The sample is made alkaline with sodium hydroxide to
14. Calculation convert ammonium ion to ammonia. The ammonia thus formed
diffuses through a gas-permeable membrane of an ion selective
14.1 Calculate the ammonia concentration in mg/L of nitro- electrode (ISE) and alters the pH of its internal solution which,
gen in the original sample, using Eq 1: in turn, is sensed by a pH electrode. The potential is measured
Ammonia nitrogen, mg/L 5 @ ~ A 3 1000! /S # (1) by means of a pH meter or an ISE meter. If the pH meter is
used, the ammonia content is determined from a calibration
where: curve; if the ISE meter is used, the ammonia content is read
directly from the meter.
A = ammonia nitrogen observed, mg, and
S = sample, mL.
14.2 Calculate the ammonia concentration in mg/L of am- 7
Supporting data have been filed at ASTM International Headquarters and may
monia in the original sample, using Eq 2: be obtained by requesting Research Report RR:D19-1015.