ASTM D3228-01

Standard Test Method for Total Nitrogen In Lubricating Oils and Fuel Oils By Modified Kjeldahl Method

SCOPE
1.1 This test method is applicable for 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 given in acceptable SI units are to be regarded as the 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 precautionary statements, see 6.6, 6.9, and 8.8.

General Information

• Status: Historical
• Publication Date: 09-Nov-2001
• 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

Relations

• Replaces: ASTM D3228-96 - Standard Test Method for Total Nitrogen In Lubricating Oils and Fuel Oils By Modified Kjeldahl Method
• Effective Date: 10-Nov-2001
• Replaced By: ASTM D3228-03 - Standard Test Method for Total Nitrogen in Lubricating Oils and Fuel Oils by Modified Kjeldahl Method
• Effective Date: 01-Nov-2003
• Referred By: ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 10-Nov-2001
• Referred By: ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
• Effective Date: 10-Nov-2001
• Referred By: ASTM D8056-18 - Standard Guide for Elemental Analysis of Crude Oil
• Effective Date: 10-Nov-2001
• Referred By: ASTM D6823-08(2021) - Standard Specification for Commercial Boiler Fuels With Used Lubricating Oils
• Effective Date: 10-Nov-2001
• Referred By: ASTM D7666-12(2019) - Standard Specification for Triglyceride Burner Fuel
• Effective Date: 10-Nov-2001

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
An American National Standard
Designation: D 3228 – 01
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 (e) 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 * E 200 Practice for Preparation, Standardization, and Stor-
age of Standard and Reagent Solutions for Chemical
1.1 This test method is applicable for the determination of
5
Analysis
nitrogen in lubricating oils when present in the concentration
from 0.03 to 0.10 mass %, and for the determination of
3. Summary of Test Method
nitrogen in fuel oils when present in the concentration from
3.1 The sample is digested in a mixture of concentrated
0.015 to 2.0 mass %. This test method is also applicable to the
sulfuric acid, potassium sulfate, mercuric oxide, and copper
analysis of additive concentrates and additive packages.
sulfate. After digestion, sodium sulfide is added to precipitate
NOTE 1—This test method may not be applicable to certain materials
the mercury, and the mixture is made alkaline with caustic.
containing N–O or N–N linkage. However, the samples used in the
Nitrogen, now in the form of ammonia, is distilled into a boric
cooperative program to establish the precision of the test method were
acid solution. The ammonia is titrated with standard sulfuric
compounded with currently available ashless additives containing nitro-
acid using methyl purple as an indicator.
gen. Complete recovery of the nitrogen present in these additives was
obtained.
4. Significance and Use
1.2 The values given in acceptable SI units are to be
4.1 The concentration of nitrogen is a measure of the
regarded as the standard.
presence of nitrogen-containing additives. Knowledge of its
1.3 This standard does not purport to address all of the
concentration can be used to predict performance.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety and health practices and determine the applica-
5.1 Buret, 50-mL, graduated in 0.1-mL subdivisions, one for
bility of regulatory limitations prior to use. For specific
each titrant. Other size burettes may also be used.
precautionary statements, see 6.6, 6.9, and 8.8.
5.2 Flask, Erlenmeyer, 300-mL. Other sizes are also accept-
able.
2. Referenced Documents
5.3 Heater, electrical or gas.
2.1 ASTM Standards:
5.4 Kjeldahl Distillation Apparatus.
2
D 1193 Specification for Reagent Water
D 4057 Practice for Manual Sampling of Petroleum and NOTE 2—Commercially available semi-automatic Kjeldahl apparatus
3
are acceptable. In such cases manufacturer prescribed sizes of burettes and
Petroleum Products
flasks may be used.
D 6299 Practice for Applying Statistical Quality Assurance
Techniques to Evaluate Analytical Measurement System 5.5 Kjeldahl Flask, at least 500-mL volume.
4
Performance
6. Reagents
6.1 Purity of Reagents—Reagent grade chemicals shall be
1
This test method is under the jurisdiction of ASTM Committee D02 on
used in all tests. Unless otherwise indicated, it is intended that
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
all reagents shall conform to the specifications of the Commit-
D02.03 on Elemental Analysis.
Current edition approved Nov. 10, 2001. Published December 2001. Originally tee on Analytical Reagents of the American Chemical Society,
published as D 3228 – 73. Last previous edition D 3228 – 96.
2
Annual Book of ASTM Standards, Vol 11.01.
3
Annual Book of ASTM Standards, Vol 05.02.
4 5
Annual Book of ASTM Standards, Vol 05.04. Annual Book of ASTM Standards, Vol 15.05.
*A Summary of Changes section appears at the end of this standard.
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D 3228
6
where such specifications are available. Other grades may be 7. Sampling
used, provided it is first ascertained that the reagent is of
7.1 Take the sample in accordance with the instructions in
sufficiently high purity to permit its use without lessening the
Practice D 4057.
accuracy of the determination.
7.2 Ensure that the sample is thoroughly representative of
6.2 Purity of Water—Unless otherwise indicated, references
the material to be tested and that the portion of the sample used
to water shall be understood to mean reagent water as defined
for test is thoroughly represent
...