ASTM D3228-08
(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
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 mass %, and for the determination of nitrogen in fuel oils when present in the concentration from 0.015 to 2.0 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 and health practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see 6.6, 6.9, and 8.8.
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Designation: D3228 −08
StandardTest 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 Department of Defense.
1. Scope* D6299 Practice for Applying Statistical Quality Assurance
and Control Charting Techniques to Evaluate Analytical
1.1 This test method covers the determination of nitrogen in
Measurement System Performance
lubricating oils when present in the concentration from 0.03 to
E200 Practice for Preparation, Standardization, and Storage
0.10 mass %, and for the determination of nitrogen in fuel oils
of Standard and Reagent Solutions for ChemicalAnalysis
when present in the concentration from 0.015 to 2.0 mass %.
This test method is also applicable to the analysis of additive
3. Summary of Test Method
concentrates and additive packages.
3.1 The sample is digested in a mixture of concentrated
NOTE 1—This test method may not be applicable to certain materials
sulfuric acid, potassium sulfate, mercuric oxide, and copper
containing N–O or N–N linkage. However, the samples used in the
sulfate. After digestion, sodium sulfide is added to precipitate
cooperative program to establish the precision of the test method were
the mercury, and the mixture is made alkaline with caustic.
compounded with currently available ashless additives containing nitro-
Nitrogen, now in the form of ammonia, is distilled into a boric
gen. Complete recovery of the nitrogen present in these additives was
obtained. acid solution. The ammonia is titrated with standard sulfuric
acid using methyl purple as an indicator.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Significance and Use
standard.
4.1 The concentration of nitrogen is a measure of the
1.3 This standard does not purport to address all of the
presence of nitrogen-containing additives. Knowledge of its
safety concerns, if any, associated with its use. It is the
concentration can be used to predict performance.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Apparatus
bility of regulatory limitations prior to use. For specific
5.1 Buret,50-mL,graduatedin0.1-mLsubdivisions,onefor
warning statements, see 6.6, 6.9, and 8.8.
each titrant. Other size burettes may also be used.
2. Referenced Documents 5.2 Flask, Erlenmeyer, 300-mL. Other sizes are also accept-
2 able.
2.1 ASTM Standards:
D1193 Specification for Reagent Water 5.3 Heater, electrical or gas.
D4057 Practice for Manual Sampling of Petroleum and
5.4 Kjeldahl Distillation Apparatus .
Petroleum Products
NOTE2—CommerciallyavailablesemiautomaticKjeldahlapparatusare
acceptable. In such cases manufacturer prescribed sizes of burettes and
1
flasks may be used.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
5.5 Kjeldahl Flask, at least 500-mL volume.
D02.03 on Elemental Analysis.
Current edition approved Dec. 1, 2008. Published December 2008. Originally
6. Reagents
approved in 1973. Last previous edition approved in 2005 as D3228–05. DOI:
10.1520/D3228-08.
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 service@astm.org. 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 − 08
3
where such specifications are available. Other grades may be 6.12 Quality Control (QC) Samples ,preferablyareportions
used, provided it is first ascertained that the reagent is of of one or more liquid petroleum materials that are stable and
sufficiently high purity to permit its use without lessening the representative of the samples of interest. These QC samples
accuracy of the determination. can be used to check the validity of the testing process as
described in Section 10.
6.2 Purity
...
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.
An American National Standard
Designation:D3228–05 Designation: D 3228 – 08
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 D 3228; 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*
1.1 Thistestmethodcoversthedeterminationofnitrogeninlubricatingoilswhenpresentintheconcentrationfrom0.03to0.10
mass %, and for the determination of nitrogen in fuel oils when present in the concentration from 0.015 to 2.0 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.
1.2The values stated in SI units are to be regarded as the standard.
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 and health practices and determine the applicability of regulatory
limitations prior to use. For specific warning statements, see 6.6, 6.9, and 8.8.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
D 4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D 6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
E 200 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.
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 .
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.03.03
on Elemental Analysis.XRF Methods.
Current edition approved Nov.Dec. 1, 2005.2008. Published November 2005.December 2008. Originally approved in 1973. Last previous edition approved in 20032005
as D 3228–035.
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 ----------------------
D3228–08
NOTE 2—Commercially available semiautomatic Kjeldahl apparatus are acceptable. In such cases manufacturer prescribed sizes of burettes and flasks
may be used.
5.5 Kjeldahl Flask, at least 500-mL volume.
6. Reagents
6.1 Purity of Reagents—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
3
such specifications are available. Other grades may be used, provided it is
...
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.
An American National Standard
Designation:D3228–05 Designation: D 3228 – 08
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 D 3228; 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*
1.1 Thistestmethodcoversthedeterminationofnitrogeninlubricatingoilswhenpresentintheconcentrationfrom0.03to0.10
mass %, and for the determination of nitrogen in fuel oils when present in the concentration from 0.015 to 2.0 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.
1.2The values stated in SI units are to be regarded as the standard.
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 and health practices and determine the applicability of regulatory
limitations prior to use. For specific warning statements, see 6.6, 6.9, and 8.8.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
D 4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D 6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
E 200 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.
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 .
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.03.03
on Elemental Analysis.XRF Methods.
Current edition approved Nov.Dec. 1, 2005.2008. Published November 2005.December 2008. Originally approved in 1973. Last previous edition approved in 20032005
as D 3228–035.
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 ----------------------
D3228–08
NOTE 2—Commercially available semiautomatic Kjeldahl apparatus are acceptable. In such cases manufacturer prescribed sizes of burettes and flasks
may be used.
5.5 Kjeldahl Flask, at least 500-mL volume.
6. Reagents
6.1 Purity of Reagents—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
3
such specifications are available. Other grades may be used, provided it is
...
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