ASTM D3228-19

Standard Test Method for Total Nitrogen in Lubricating Oils and Fuel Oils by Modified Kjeldahl Method

SIGNIFICANCE AND USE
4.1 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 6.6, 6.9, and 8.8.  
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

• Status: Historical
• Publication Date: 31-Oct-2019
• ICS: 75.100 - Lubricants, industrial oils and related products
• ICS: 75.160.20 - Liquid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D3228 −19
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
D6299 Practice for Applying Statistical Quality Assurance
lubricating oils when present in the concentration from 0.03 %
and Control Charting Techniques to Evaluate Analytical
to0.10 %bymass,andforthedeterminationofnitrogeninfuel
Measurement System Performance
oils when present in the concentration from 0.015 % to 2.0 %
E200 Practice for Preparation, Standardization, and Storage
by mass. This test method is also applicable to the analysis of
of Standard and Reagent Solutions for ChemicalAnalysis
additive concentrates and additive packages.
NOTE 1—This test method may not be applicable to certain materials
3. Summary of Test Method
containing N–O or N–N linkage. However, the samples used in the
3.1 The sample is digested in a mixture of concentrated
cooperative program to establish the precision of the test method were
compounded with currently available ashless additives containing nitro- sulfuric acid, potassium sulfate, mercuric oxide, and copper
gen. Complete recovery of the nitrogen present in these additives was
sulfate. After digestion, sodium sulfide is added to precipitate
obtained.
the mercury, and the mixture is made alkaline with caustic.
1.2 The values stated in SI units are to be regarded as
Nitrogen, now in the form of ammonia, is distilled into a boric
standard. No other units of measurement are included in this
acid solution. The ammonia is titrated with standard sulfuric
standard.
acid using methyl purple as an indicator.
1.3 This standard does not purport to address all of the
4. Significance and Use
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4.1 The concentration of nitrogen is a measure of the
priate safety, health, and environmental practices and deter-
presence of nitrogen-containing additives. Knowledge of its
mine the applicability of regulatory limitations prior to use.
concentration can be used to predict performance.
For specific warning statements, see 6.6, 6.9, and 8.8.
1.4 This international standard was developed in accor-
5. Apparatus
dance with internationally recognized principles on standard-
5.1 Buret, 50 mL, graduated in 0.1 mLsubdivisions, one for
ization established in the Decision on Principles for the
each titrant. Other size burettes may also be used.
Development of International Standards, Guides and Recom-
5.2 Flask, Erlenmeyer, 300 mL. Other sizes are also accept-
mendations issued by the World Trade Organization Technical
able.
Barriers to Trade (TBT) Committee.
5.3 Heater, electrical or gas.
2. Referenced Documents
5.4 Kjeldahl Distillation Apparatus.
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water NOTE2—CommerciallyavailablesemiautomaticKjeldahlapparatusare
acceptable. In such cases manufacturer prescribed sizes of burettes and
flasks may be used.
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 5.5 Kjeldahl Flask, at least 500 mL volume.
Subcommittee D02.03 on Elemental Analysis.
Current edition approved Nov. 1, 2019. Published November 2019. Originally
6. Reagents
approved in 1973. Last previous edition approved in 2019 as D3228 – 08 (2019).
DOI: 10.1520/D3228-19.
6.1 Purity of Reagents—Reagent grade chemicals shall be
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
used in all tests. Unless otherwise indicated, it is intended that
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
all reagents shall conform to the specifications of the Commit-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. tee onAnalytical Reagents of theAmerican Chemical Society,
*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 ----------------------
D3228 − 19
3
where such specifications are available. Other grades may be 6.12 Quality Control (QC) Sample, preferably are por
...

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 − 08 (Reapproved 2019) D3228 − 19
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 Scope*
1.1 This test method covers the determination of nitrogen in lubricating oils when present in the concentration from
0.03 mass % to 0.10 mass %, 0.03 % to 0.10 % by mass, and for the determination of nitrogen in fuel oils when present in the
concentration from 0.015 mass % to 2.0 mass %. 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 6.6, 6.9, and 8.8.
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
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. Summary of Test Method
3.1 The sample is digested in a mixture of concentrated sulfuric acid, potassium sulfate, mercuric oxide, and copper sulfate.
After digestion, sodium sulfide is added to precipitate the mercury, and the mixture is made alkaline with caustic. Nitrogen, now
in the form of ammonia, is distilled into a boric acid solution. The ammonia is titrated with standard sulfuric acid using methyl
purple as an indicator.
4. Significance and Use
4.1 The concentration of nitrogen is a measure of the presence of nitrogen-containing additives. Knowledge of its concentration
can be used to predict performance.
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 May 1, 2019Nov. 1, 2019. Published June 2019November 2019. Originally approved in 1973. Last previous edition approved in 20142019 as
D3228 – 08 (2014).(2019). DOI: 10.1520/D3228-08R19.10.1520/D3228-19.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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 ----------------------
D3228 − 19
5. Apparatus
5.1 Buret, 50 mL, graduated in 0.1 mL subdivisions, one for each titrant. Other size burettes may also be used.
5.2 Flask, Erlenmeyer, 300 mL. Other sizes are also acceptable.
5.3 Heater, electrical or gas.
5.4 Kjeldahl Distillation Apparatus.
NOTE 2—Commercially available semiautomatic Kjeldahl apparatus are acceptable. In such cases manufacturer prescribed sizes of burettes and flasks
...