ASTM D4047-00(2005)

Standard Test Method for Phosphorus in Lubricating Oils and Additives by Quinoline Phosphomolybdate Method

SIGNIFICANCE AND USE
Knowledge of the phosphorus content, and thus the phosphorus-containing additives, in a lubricating oil or additive can be used to predict performance characteristics.
SCOPE
1.1 This test method covers the determination of 0.005 to 10.0 mass % phosphorus in unused lubricating oil and additive concentrates. There is no reason to doubt its applicability to filtered, used lubricating oils, but no systematic study of this application has been made.
1.2 The test method is applicable to samples containing any of the phosphorus compounds in normal use.
Note 1—This test method extends the scope of the previous version of IP 149 and replaces IP 148 and the previous version of IP 149 as a referee method.
1.3 The values stated in SI units are to be regarded as the standard.
1.4 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 hazard statements, see 6.9.

General Information

• Status: Historical
• Publication Date: 30-Apr-2005
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Replaces: ASTM D4047-00 - Standard Test Method for Phosphorus in Lubricating Oils and Additives by Quinoline Phoshomolybdate Method
• Effective Date: 01-May-2005
• Replaced By: ASTM D4047-00(2011) - Standard Test Method for Phosphorus in Lubricating Oils and Additives by Quinoline Phosphomolybdate Method
• Effective Date: 01-May-2011
• Referred By: ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-May-2005
• Referred By: ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
• Effective Date: 01-May-2005

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D4047–00 (Reapproved 2005)
Designation: 149/93
Standard Test Method for
Phosphorus in Lubricating Oils and Additives by Quinoline
1
Phosphomolybdate Method
This standard is issued under the fixed designation D4047; 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 0.005 to
Measurement System Performance
10.0 mass % phosphorus in unused lubricating oil and additive
2.2 IP Standard:
concentrates. There is no reason to doubt its applicability to
IP 148 Test Method for Phosphorous in Lubricating Oils
filtered, used lubricating oils, but no systematic study of this
3
and Additives
application has been made.
1.2 The test method is applicable to samples containing any
3. Summary of Test Method
of the phosphorus compounds in normal use.
3.1 Additive concentrates are diluted with phosphorus-free
NOTE 1—This test method extends the scope of the previous version of
white oil to produce a working blend.
IP149 and replaces IP148 and the previous version of IP149 as a referee
3.2 Thesampleisignitedwithexcessofzincoxidewhereby
method.
phosphorus is converted to phosphate.The residue is dissolved
1.3 The values stated in SI units are to be regarded as the
in hydrochloric acid and any sulfide formed is oxidized with
standard.
potassium bromate. Phosphorus is then precipitated as quino-
1.4 This standard does not purport to address all of the
line phosphomolybdate and determined volumetrically by
safety concerns, if any, associated with its use. It is the
addition of excess standard alkali and back titration with
responsibility of the user of this standard to establish appro-
standard acid.
priate safety and health practices and determine the applica-
4. Significance and Use
bility of regulatory limitations prior to use. For specific hazard
statements, see 6.9.
4.1 Knowledge of the phosphorus content, and thus the
phosphorus-containing additives, in a lubricating oil or addi-
2. Referenced Documents
tive can be used to predict performance characteristics.
2
2.1 ASTM Standards:
5. Apparatus
D1193 Specification for Reagent Water
5.1 Silica Crucibles, 40-mm internal diameter at the top and
40 mm in height. The internal surface should be smooth and
free from pitting.
1
This test method is under the jurisdiction of ASTM Committee D02 on
5.2 Muffle Furnace,capableofmaintainingatemperatureof
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
approximately 700°C, and fitted with ports to allow air
Current edition approved May 1, 2005. Published May 2005. Originally
circulation.
approved in 1981. Last previous edition approved in 2000 as D4047 – 00. DOI:
5.3 Beakers, 25-mL capacity.
10.1520/D4047-00R05.
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
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Standards volume information, refer to the standard’s Document Summary page on Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
the ASTM website. U.K.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D4047–00 (2005)
6. Reagents and Materials
P = approximate percent phosphorus in the sample, and
A = grams of sample required for a 10-g blend.
6.1 Purity of Reagents—Reagent grade chemicals shall be
7.3 Calculate the mass of white oil for a 10-g blend as
used in all tests. Unless otherwise indicated, it is intended that
follows:
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
B 5 10 2 A (2)
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where such specifications are available. Other grades may be
where:
used, provided it is first ascertained that the reagent is of
B = mass of white oil, g.
sufficiently high purity to permit its use without lessening the
7.4 Weigh a quantity of sample A 6 0.01 g into a 25-mL
accuracy of the determination.
beaker.
6.2 Purity of Water—Unless otherwise indicated, references
7.5 Weigh into the same beaker B g of white oil.
to water shall be understood to mean reagent water as defined
7.6 Mix the sample and white oil thoroughly by stirring and
by Type II or Type III of Specification D1193.
warming to approximately 50°C.
6.3 Hydrochloric Acid, approximately 1 N reagent
...