ASTM D3228-05

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An American National Standard
Designation: D 3228 – 05
Standard Test Method for
Total Nitrogen in Lubricating Oils and Fuel Oils by Modified
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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* 3. Summary of Test Method
1.1 This test method covers the determination of nitrogen in 3.1 The sample is digested in a mixture of concentrated
lubricating oils when present in the concentration from 0.03 to sulfuric acid, potassium sulfate, mercuric oxide, and copper
0.10 mass %, and for the determination of nitrogen in fuel oils sulfate. After digestion, sodium sulfide is added to precipitate
when present in the concentration from 0.015 to 2.0 mass %. the mercury, and the mixture is made alkaline with caustic.
This test method is also applicable to the analysis of additive Nitrogen, now in the form of ammonia, is distilled into a boric
concentrates and additive packages. acid solution. The ammonia is titrated with standard sulfuric
acid using methyl purple as an indicator.
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
4. Significance and Use
cooperative program to establish the precision of the test method were
4.1 The concentration of nitrogen is a measure of the
compounded with currently available ashless additives containing nitro-
gen. Complete recovery of the nitrogen present in these additives was
presence of nitrogen-containing additives. Knowledge of its
obtained.
concentration can be used to predict performance.
1.2 The values stated in SI units are to be regarded as the
5. Apparatus
standard.
5.1 Buret,50-mL,graduatedin0.1-mLsubdivisions,onefor
1.3 This standard does not purport to address all of the
each titrant. Other size burettes may also be used.
safety concerns, if any, associated with its use. It is the
5.2 Flask, Erlenmeyer, 300-mL. Other sizes are also accept-
responsibility of the user of this standard to establish appro-
able.
priate safety and health practices and determine the applica-
5.3 Heater, electrical or gas.
bility of regulatory limitations prior to use. For specific
5.4 Kjeldahl Distillation Apparatus.
warning statements, see 6.6, 6.9, and 8.8.
NOTE 2—Commercially available semiautomatic Kjeldahl apparatus
2. Referenced Documents
areacceptable.Insuchcasesmanufacturerprescribedsizesofburettesand
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2.1 ASTM Standards:
flasks may be used.
D 1193 Specification for Reagent Water
5.5 Kjeldahl Flask, at least 500-mL volume.
D 4057 Practice for Manual Sampling of Petroleum and
Petroleum Products 6. Reagents
D 6299 Practice for Applying Statistical Quality Assurance
6.1 Purity of Reagents—Reagent grade chemicals shall be
Techniques to Evaluate Analytical Measurement System
used in all tests. Unless otherwise indicated, it is intended that
Performance
all reagents shall conform to the specifications of the Commit-
E 200 Practice for Preparation, Standardization, and Stor-
tee onAnalytical Reagents of theAmerican Chemical Society,
age of Standard and Reagent Solutions for Chemical 3
where such specifications are available. Other grades may be
Analysis
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
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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 on Elemental Analysis.
3
Current edition approved Nov. 1, 2005. Published November 2005. Originally Reagent Chemicals, American Chemical Society Specifications, American
approved in 1973. Last previous edition approved in 2003 as D 3228–03. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
*A Summary of Changes section appears at the end of this standard.
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