ASTM D3228-22
(Test Method)Standard Test Method for Total Nitrogen in Lubricating Oils and Fuel Oils by Modified Kjeldahl Method
Standard Test Method for Total Nitrogen in Lubricating Oils and Fuel Oils by Modified Kjeldahl Method
SIGNIFICANCE AND USE
5.1 The concentration of nitrogen is a measure of the presence of nitrogen-containing additives. Knowledge of its concentration can be used to predict performance.
SCOPE
1.1 This test method covers the determination of nitrogen in lubricating oils when present in the concentration from 0.03 % to 0.10 % by mass, and for the determination of nitrogen in fuel oils when present in the concentration from 0.015 % to 2.0 % by mass. This test method is also applicable to the analysis of additive concentrates and additive packages.
Note 1: This test method may not be applicable to certain materials containing N–O or N–N linkage. However, the samples used in the cooperative program to establish the precision of the test method were compounded with currently available ashless additives containing nitrogen. Complete recovery of the nitrogen present in these additives was obtained.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see 7.6, 7.9, and 9.8.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
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Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D3228 −22
Standard Test Method for
Total Nitrogen in Lubricating Oils and Fuel Oils by Modified
1
Kjeldahl Method
This standard is issued under the fixed designation D3228; 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 U.S. Department of Defense.
1. Scope* D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
1.1 This test method covers the determination of nitrogen in
D4175 Terminology Relating to Petroleum Products, Liquid
lubricating oils when present in the concentration from 0.03 %
Fuels, and Lubricants
to0.10 %bymass,andforthedeterminationofnitrogeninfuel
D6299 Practice for Applying Statistical Quality Assurance
oils when present in the concentration from 0.015 % to 2.0 %
and Control Charting Techniques to Evaluate Analytical
by mass. This test method is also applicable to the analysis of
Measurement System Performance
additive concentrates and additive packages.
E200 Practice for Preparation, Standardization, and Storage
NOTE 1—This test method may not be applicable to certain materials
of Standard and Reagent Solutions for ChemicalAnalysis
containing N–O or N–N linkage. However, the samples used in the
cooperative program to establish the precision of the test method were
3. Terminology
compounded with currently available ashless additives containing nitro-
3.1 Definitions:
gen. Complete recovery of the nitrogen present in these additives was
obtained. 3.1.1 For definitions of terms used in this test method, refer
to Terminology D4175.
1.2 The values stated in SI units are to be regarded as
3.2 Definitions of Terms Specific to This Standard:
standard. No other units of measurement are included in this
3.2.1 digestion, n—treating a sample with the use of heat or
standard.
elevated pressures, or both, usually in the presence of chemical
1.3 This standard does not purport to address all of the
additives, to bring analytes of interest into solution or to
safety concerns, if any, associated with its use. It is the
remove interfering matrix components, or both.
responsibility of the user of this standard to establish appro-
3.2.1.1 Discussion—In this test method acid, a catalyst and
priate safety, health, and environmental practices and deter-
heat are used to break the carbon nitrogen bonds to form
mine the applicability of regulatory limitations prior to use.
ammonium sulfate.
For specific warning statements, see 7.6, 7.9, and 9.8.
3.2.2 lubricating oil, n—a liquid lubricant, usually compris-
1.4 This international standard was developed in accor-
ing several ingredients, including a major portion of base oil
dance with internationally recognized principles on standard-
and minor portions of various additives.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 3.2.3 titration, n—quantitative chemical analysis method
mendations issued by the World Trade Organization Technical
used to determine the unknown concentration of a specified
Barriers to Trade (TBT) Committee. element by reacting a solution prepared from the sample to be
analyzed with a known concentration and volume of specific
2. Referenced Documents
reagent.
2
2.1 ASTM Standards: 3.2.3.1 Discussion—Sensing electrodes or color indicators
D1193 Specification for Reagent Water
can be used to follow titrations if they respond to either the
species being determined or the titrant ion.
1
This test method is under the jurisdiction of ASTM Committee D02 on
3.2.4 Total Kjeldahl Nitrogen (TKN), n—the sum of the
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
nitrogen contained in the free ammonia and other nitrogen
Subcommittee D02.03 on Elemental Analysis.
compounds which are converted to ammonium sulfate
Current edition approved Oct. 1, 2022. Published November 2022. Originally
approved in 1973. Last previous edition approved in 2020 as D3228 – 20. DOI: [(NH ) SO ] under the specified digestion conditions.
4 2 4
10.1520/D3228-22.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 4. Summary of Test Method
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
4.1 The sample is digested in a mixture of concentrated
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. sulfuric acid, potassium sulfate, and a catalyst of mercur
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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: D3228 − 20 D3228 − 22
Standard Test Method for
Total Nitrogen in Lubricating Oils and Fuel Oils by Modified
1
Kjeldahl Method
This standard is issued under the fixed designation D3228; 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 U.S. Department of Defense.
1. Scope*
1.1 This test method covers the determination of nitrogen in lubricating oils when present in the concentration from 0.03 % to
0.10 % by mass, and for the determination of nitrogen in fuel oils when present in the concentration from 0.015 % to 2.0 % by
mass. This test method is also applicable to the analysis of additive concentrates and additive packages.
NOTE 1—This test method may not be applicable to certain materials containing N–O or N–N linkage. However, the samples used in the cooperative
program to establish the precision of the test method were compounded with currently available ashless additives containing nitrogen. Complete recovery
of the nitrogen present in these additives was obtained.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. For specific warning statements, see 6.67.6, 6.97.9, and 8.89.8.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis
3. Terminology
3.1 Definitions:
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved July 1, 2020Oct. 1, 2022. Published July 2020November 2022. Originally approved in 1973. Last previous edition approved in 20192020 as
D3228 – 19.D3228 – 20. DOI: 10.1520/D3228-20.10.1520/D3228-22.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM 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
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D3228 − 22
3.1.1 For definitions of terms used in this test method, refer to Terminology D4175.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 digestion, n—treating a sample with the use of heat or elevated pressures, or both, usually in the presence of chemical
additives, to bring analytes of interest into solution or to remove interfering matrix components, or both.
3.2.1.1 Discussion—
In this test method acid, a catalyst and heat are used to break the carbon nitrogen bonds to form ammonium sulfate.
3.2.2 lubricating oil, n—a liquid lubricant, usually comprising several ingredients, including a major portion of base oil and minor
portions of various additives.
3.2.3 titration, n—quantitative chemical analysis method used to determine the unknown concentration of a specified element by
reacting a solution prepared from the sample to be analyzed with a known concentration and volume of specific reagent.
3.2.3.1 Discussion—
Sensing electrodes or color indicators can be used to fol
...
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