ASTM D3867-04

Standard Test Methods for Nitrite-Nitrate in Water

SIGNIFICANCE AND USE
Both test methods use identical reagents and sample processing. The only difference between the two methods is that one test method is automated and the other is manual. The ranges and interferences are identical.  
The automated test method is preferred when large numbers of samples are to be analyzed. The manual test method is used for fewer samples or when automated instrumentation is not available.
These test methods replace Test Methods D 1254 (Nitrite) and D 992 (Nitrate). The nitrite test method (Test Method D 1254) used a reagent that is considered to be a potential carcinogen. The nitrate test method (Test Method D 992) has been shown to have relatively large errors when used in wastewaters and also has greater manipulative difficulties than the test method described herein.
SCOPE
1.1 These test methods cover the determination of nitrite nitrogen, nitrate nitrogen, and combined nitrite-nitrate nitrogen in water and wastewater in the range from 0.05 to 1.0 mg/L nitrogen. Two test methods are given as follows:SectionsTest Method A-Automated Cadmium Reduction9 to 16Test Method B-Manual Cadmium Reduction17 to 24
1.2 These test methods are applicable to surface, saline, waste, and ground waters. It is the user's responsibility to ensure the validity of these test methods for waters of untested matrices.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.  For specific hazard statements, see Note 1 and Note 2.

General Information

• Status: Historical
• Publication Date: 30-Jun-2004
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.05 - Inorganic Constituents in Water

Relations

• Replaces: ASTM D3867-99 - Standard Test Methods for Nitrite-Nitrate in Water
• Effective Date: 01-Jul-2004
• Replaced By: ASTM D3867-09 - Standard Test Methods for Nitrite-Nitrate in Water
• Effective Date: 15-May-2009
• Referred By: ASTM D7781-23 - Standard Test Method for Nitrite-Nitrate in Water by Nitrate Reductase
• Effective Date: 01-Jul-2004
• Referred By: ASTM D6146-97(2018) - Standard Guide for Monitoring Aqueous Nutrients in Watersheds
• Effective Date: 01-Jul-2004
• Referred By: ASTM E1197-12(2021) - Standard Guide for Conducting a Terrestrial Soil-Core Microcosm Test
• Effective Date: 01-Jul-2004
• Referred By: ASTM D6469-20 - Standard Guide for Microbial Contamination in Fuels and Fuel Systems
• Effective Date: 01-Jul-2004
• Referred By: ASTM D4195-23 - Standard Guide for Water Analysis for Reverse Osmosis and Nanofiltration Application
• Effective Date: 01-Jul-2004
• Referred By: ASTM D6666-20 - Standard Guide for Evaluation of Aqueous Polymer Quenchants
• Effective Date: 01-Jul-2004
• Referred By: ASTM D8083-16(2023) - Standard Test Method for Total Nitrogen, and Total Kjeldahl Nitrogen (TKN) by Calculation, in Water by High Temperature Catalytic Combustion and Chemiluminescence Detection
• Effective Date: 01-Jul-2004

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D 3867–04
Standard Test Methods for
1
Nitrite-Nitrate in Water
This standard is issued under the fixed designation D 3867; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope* D 3370 Practices for SamplingWater from Closed Conduits
D 5810 Guide for Spiking Into Aqueous Samples
1.1 These test methods cover the determination of nitrite
D 5847 Practice for Writing Quality Control Specifications
nitrogen, nitrate nitrogen, and combined nitrite-nitrate nitrogen
for Standard Test Methods for Water Analysis
in water and wastewater in the range from 0.05 to 1.0 mg/L
2
E60 Practices for Analysis of Metals, Ores, and Related
nitrogen. Two test methods are given as follows:
Materials by Molecular Absorption Spectrometry
Sections
E 275 Practice for Describing and Measuring Performance
Test Method A—Automated Cadmium Reduction 9 to 16
Test Method B—Manual Cadmium Reduction 17 to 24
of Ultraviolet, Visible, and Near Infrared Spectrophotom-
eters
1.2 These test methods are applicable to surface, saline,
waste, and ground waters. It is the user’s responsibility to
3. Terminology
ensure the validity of these test methods for waters of untested
3.1 Definitions: For definitions of terms used in these test
matrices.
methods, refer to Terminology D 1129.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Methods
responsibility of the user of this standard to establish appro-
4.1 Total Oxidized Nitrogen—a filtered sample is passed
priate safety and health practices and determine the applica-
through a column containing copper-coated cadmium granules
bility of regulatory limitations prior to use. For specific hazard
to reduce nitrate ion to nitrite ion. The combined nitrite-nitrate
statements, see Note 1 and Note 2.
nitrogen is determined by diazotizing the total nitrite ion with
2. Referenced Documents sulfanilamide and coupling with N-(1-
3
naphthyl)ethylenediamine dihydrochloride to form a highly
2.1 ASTM Standards:
4
colored azo dye that is measured spectrophotometrically.
D 992 Test Method for Nitrate Ion in Water
4.2 Nitrite—the nitrite ion originally present in the sample
D 1129 Terminology Relating to Water
canbedeterminedseparatelybycarryingouttheprocedureand
D 1141 Practice for the Preparation of Substitute Ocean
omitting the cadmium reduction step.
Water
4.3 Nitrate—the nitrate ion can be calculated as the differ-
D 1192 Specification for Equipment for Sampling Water
4 ence between the combined nitrite-nitrate nitrogen and the
and Steam in Closed Conduits
nitrite nitrogen.
D 1193 Specification for Reagent Water
4
D 1254 Test Method for Nitrite Ion in Water
5. Significance and Use
D 2777 Practice for Determination of Precision and Bias of
5.1 Both test methods use identical reagents and sample
Applicable Methods of Committee D19 on Water
processing. The only difference between the two methods is
that one test method is automated and the other is manual. The
1
These test methods are under the jurisdiction of ASTM Committee D19 on
ranges and interferences are identical.
Water and are the responsibility of Subcommittee D19.05 on Inorganic Constituents
5.2 The automated test method is preferred when large
in Water.
numbers of samples are to be analyzed. The manual test
Current edition approved July 1, 2004. Published July 2004. Originally approved
in 1979. Last previous edition approved in 1999 as D 3867 – 99.
method is used for fewer samples or when automated instru-
2
Methods similar to these appear in Methods of Chemical Analysis of Water and
mentation is not available.
Wastes, 2nd edition, U.S. Environmental Protection Agency.
3 5.3 These test methods replace Test Methods D 1254 (Ni-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
trite) and D 992 (Nitrate).The nitrite test method (Test Method
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
D 1254) used a reagent that is considered to be a potential
the ASTM website.
carcinogen. The nitrate test method (Test Method D 992) has
4
Withdrawn.
*A Summary of Changes section appears at the end of this standard.
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D 3867–04
been shown to have relatively large errors when used in 8. Sampling and Sample Preservation
wastewaters and also has greater manipulative difficulties than
...