ASTM D3590-11
(Test Method)Standard Test Methods for Total Kjeldahl Nitrogen in Water
Standard Test Methods for Total Kjeldahl Nitrogen in Water
SIGNIFICANCE AND USE
These test methods are useful for measuring organic nitrogen and ammoniacal nitrogen, which are essential growth nutrients.
Nitrogen compounds are widely distributed in the environment. Sources of nitrogen include surface-applied fertilizers, cleaning products, and drinking water treatment aids. Because nitrogen is a nutrient for photosynthetic organisms, it may be important to monitor and control discharge into the environment.
SCOPE
1.1 These test methods cover the determination of total Kjeldahl nitrogen. The following test methods are included:
Sections Test Method AManual Digestion/Distillation 8 to 14 Test Method BSemiautomated Colorimetric Bertholt15 to 23
1.2 The analyst should be aware that precision and bias statements included may not necessarily apply to the water being tested.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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.
8.1 This test method covers the determination of total Kjeldahl nitrogen in water. It measures free ammonia or ammonia formed from the conversion of nitrogen components of biological origin such as amino acids and proteins. However, the procedure may not convert the nitrogenous compounds of some wastes to ammonia. Examples of such compounds that may not be measured are nitro compounds, hydrozones, oximes, nitrates, semicarbazones, pyridines, and some refractory tertiary amines.
8.2 Three alternatives are described for the final determination of the ammonia: a titrimetric method, which is applicable to concentrations above 1 mg N/L; a Nesslerization method, which is applicable to concentrations below 1 mg N/L; and a potentiometric method which is applicable to the range from 0.04 to 1000 mg N/L.
8.3 This test method is described for micro and macro systems. Micro determination can be made on sample aliquots containing up to 10 mg of nitrogen.
15.1 This test method covers the automated determination of total Kjeldahl nitrogen in water and wastewater and is based on the same principle and subject to the same limitations as the manual method (see 8.1).
15.2 This test method is a semiautomated procedure applicable to drinking water, surface water, and domestic and industrial wastes containing from 0.3 to 5 mg/L of nitrogen.
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Designation: D3590 − 11
Standard Test Methods for
1
Total Kjeldahl Nitrogen in Water
This standard is issued under the fixed designation D3590; 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.
1. Scope* 3.2 Definitions of Terms Specific to This Standard:
3.2.1 total Kjeldahl nitrogen, n—the sum of the nitrogen
1.1 These test methods cover the determination of total
contained in the free ammonia and other nitrogen compounds,
Kjeldahl nitrogen. The following test methods are included:
which are converted to ammonium sulfate [(NH ) SO ] under
4 2 4
Sections
the specified digestion conditions.
Test Method A—Manual Digestion/Distillation 8–13
Test Method B—Semiautomated Colorimetric Bertholt 15–22
4. Significance and Use
1.2 The analyst should be aware that precision and bias
4.1 These test methods are useful for measuring organic
statements included may not necessarily apply to the water
nitrogen and ammoniacal nitrogen, which are essential growth
being tested.
nutrients.
1.3 The values stated in SI units are to be regarded as
4.2 Nitrogen compounds are widely distributed in the envi-
standard. No other units of measurement are included in this
ronment. Sources of nitrogen include surface-applied
standard.
fertilizers, cleaning products, and drinking water treatment
1.4 This standard does not purport to address all of the
aids. Because nitrogen is a nutrient for photosynthetic
safety concerns, if any, associated with its use. It is the
organisms, it may be important to monitor and control dis-
responsibility of the user of this standard to establish appro-
charge into the environment.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Interferences
5.1 Nitrateisknowntocauseaseriousnegativeinterference
2. Referenced Documents
in the test. Reportedly, a concentration of 250 mg/L NO
3
2
2.1 ASTM Standards:
results in zero recovery of some level of N added as some N
D1129 Terminology Relating to Water
compound.
D1193 Specification for Reagent Water
5.2 The analyst is cautioned that ammonia in the laboratory
D1426 Test Methods for Ammonia Nitrogen In Water
may easily become an interference in these test methods from
D2777 Practice for Determination of Precision and Bias of
contamination of reagents, caps, or from the laboratory atmo-
Applicable Test Methods of Committee D19 on Water
sphere. Care should be taken that ammonium hydroxide, either
D3370 Practices for Sampling Water from Closed Conduits
as a reagent or as a cleaning substance, is not used in the same
D5810 Guide for Spiking into Aqueous Samples
room.
D5847 Practice for Writing Quality Control Specifications
for Standard Test Methods for Water Analysis
6. Purity of Reagents
6.1 Reagent-grade chemicals shall be used in all tests.
3. Terminology
Unless otherwise indicated, it is intended that all reagents shall
3.1 Definitions—For definitions of terms used in these test
conform to the specifications of the Committee on Analytical
methods, refer to Terminology D1129.
Reagents of the American Chemical Society, where such
3
specifications are available. Other grades may be used, pro-
vided it is first ascertained that the reagent is of sufficient high
1
These test methods are under the jurisdiction of ASTM Committee D19 on
purity to permit its use without lessening the accuracy of the
Water and are the direct responsibility of Subcommittee D19.05 on Inorganic
Constituents in Water. determination.
Current edition approved April 1, 2011. Published April 2011. Originally
approved in 1977. Last previous edition approved in 2006 as D3590 – 02 (2006).
3
DOI: 10.1520/D3590-11. Reagent Chemicals, American Chemical Society Specifications, American
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Chemical Society, Washington, DC. For suggestions on the testing of reagents not
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM listed by theAmerican Chemical Society, and the United States Pharmacopeia and
Standards volume information, refer to the standard’s Document Summary page on National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
*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
---------------------- Page: 1 ----------------------
D3590 − 11
6.2 Purity of Water—Unless otherwise indicated, reference 10.3 Spectrophotometer or Colorimeter, for use at 425 nm
to water shall be understood
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D3590–02 (Reapproved 2006) Designation:D3590–11
Standard Test Methods for
1
Total Kjeldahl Nitrogen in Water
This standard is issued under the fixed designation D3590; 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.
1. Scope*
1.1 These test methods cover the determination of total Kjeldahl nitrogen. The following test methods are included:
Sections
Test Method A—Manual Digestion/Distillation 8 to 14
Test Method B—Semiautomated Colorimetric Bertholt 15 to 23
1.2 The analyst should be aware that precision and bias statements included may not necessarily apply to the water being tested.
1.3
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D1426 Test Methods for Ammonia Nitrogen In Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
D5810 Guide for Spiking into Aqueous Samples
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
3. Terminology
3.1 Definitions—For definitions of terms used in these test methods, refer to Terminology D1129.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 total Kjeldahl nitrogen, n—the sum of the nitrogen contained in the free ammonia and other nitrogen compounds, which
are converted to ammonium sulfate [(NH ) SO ] under the specified digestion conditions.
4 2 4
4. Significance and Use
4.1 These test methods are useful for measuring organic nitrogen and ammoniacal nitrogen, which are essential growth
nutrients.
4.2 Nitrogen compounds are widely distributed in the environment. Sources of nitrogen include surface-applied fertilizers,
cleaning products, and drinking water treatment aids. Because nitrogen is a nutrient for photosynthetic organisms, it may be
important to monitor and control discharge into the environment.
5. Interferences
5.1 Nitrate is known to cause a serious negative interference in the test. Reportedly, a concentration of 250 mg/L NO results
3
in zero recovery of some level of N added as some N compound.
1
These test methods are under the jurisdiction of ASTM Committee D19 on Water and are the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
in Water.
Current edition approved Dec. 15, 2006. Published February 2007. Originally approved in 1977. Last previous edition approved in 2002 as D3590–02. DOI:
10.1520/D3590-02R06.
Current edition approved April 1, 2011. Published April 2011. Originally approved in 1977. Last previous edition approved in 2006 as D3590 – 02(2006). DOI:
10.1520/D3590-11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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
---------------------- Page: 1 ----------------------
D3590–11
5.2 The analyst is cautioned that ammonia in the laboratory may easily become an interference in these test methods from
contamination of reagents, caps, or from the laboratory atmosphere. Care should be taken that ammonium hydroxide, either as a
reagent or as a cleaning substance, is not used in the same room.
6. Purity of Reagents
6.1 Reagent-grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform
to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are
3
available. Other grades may be used, provided it is first ascertained that the reagent is of sufficient high purity to permit its use
without lessening the
...
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