ASTM D4047-18
(Test Method)Standard Test Method for Phosphorus in Lubricating Oils and Additives by Quinoline Phosphomolybdate Method
Standard Test Method for Phosphorus in Lubricating Oils and Additives by Quinoline Phosphomolybdate Method
SIGNIFICANCE AND USE
4.1 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 % by 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 This test method is free from most interferences because the high insolubility of the quinoline phosphomolybdate precipitate leads to constant composition and freedom from most adsorbed or occluded impurities, especially from cations which would otherwise interfere in the subsequent titration of the precipitate.
1.4 Barium, calcium, magnesium, zinc, iron, aluminum, alkali salts, citric acid and citrates, chromium up to 18 times the phosphorus content, and titanium up to 3.5 times do not interfere with the test method.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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 hazard statements, see 6.9.
1.7 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.
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Standards Content (Sample)
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.
Designation: D4047 − 18
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 U.S. Department of Defense.
1. Scope* 1.7 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This test method covers the determination of 0.005 % to
ization established in the Decision on Principles for the
10.0 % by mass phosphorus in unused lubricating oil and
Development of International Standards, Guides and Recom-
additive concentrates. There is no reason to doubt its applica-
mendations issued by the World Trade Organization Technical
bility to filtered, used lubricating oils, but no systematic study
Barriers to Trade (TBT) Committee.
of this application has been made.
1.2 The test method is applicable to samples containing any
2. Referenced Documents
of the phosphorus compounds in normal use.
2
2.1 ASTM Standards:
NOTE 1—This test method extends the scope of the previous version of
D1193 Specification for Reagent Water
IP149 and replaces IP148 and the previous version of IP149 as a referee
D4057 Practice for Manual Sampling of Petroleum and
method.
Petroleum Products
1.3 Thistestmethodisfreefrommostinterferencesbecause D4177 Practice for Automatic Sampling of Petroleum and
the high insolubility of the quinoline phosphomolybdate pre-
Petroleum Products
cipitate leads to constant composition and freedom from most D6299 Practice for Applying Statistical Quality Assurance
adsorbedoroccludedimpurities,especiallyfromcationswhich
and Control Charting Techniques to Evaluate Analytical
would otherwise interfere in the subsequent titration of the Measurement System Performance
precipitate.
2.2 IP Standard:
IP 148 Test Method for Phosphorous in Lubricating Oils
1.4 Barium, calcium, magnesium, zinc, iron, aluminum,
3
alkali salts, citric acid and citrates, chromium up to 18 times and Additives
the phosphorus content, and titanium up to 3.5 times do not
interfere with the test method. 3. Summary of Test Method
3.1 Additive concentrates are diluted with phosphorus-free
1.5 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this white oil to produce a working blend.
standard.
3.2 Thesampleisignitedwithexcessofzincoxidewhereby
1.6 This standard does not purport to address all of the phosphorus is converted to phosphate.The residue is dissolved
safety concerns, if any, associated with its use. It is the in hydrochloric acid and any sulfide formed is oxidized with
responsibility of the user of this standard to establish appro- potassium bromate. Phosphorus is then precipitated as quino-
priate safety, health, and environmental practices and deter- line phosphomolybdate and determined volumetrically by
mine the applicability of regulatory limitations prior to use. addition of excess standard alkali and back titration with
For specific hazard statements, see 6.9. standard acid.
1 2
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Subcommittee D02.03 on Elemental Analysis. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved April 1, 2018. Published April 2018. Originally the ASTM website.
3
approved in 1981. Last previous edition approved in 2013 as D4047– 13. DOI: Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR,
10.1520/D4047-18. U.K., http://www.energyinst.org.
*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 ----------------------
D4047 − 18
4. Significance and Use product. Collect the colorless distillate in the boiling range
from 232 °C to 238 °C. Store the quinoline in an amber bottle
4.1 Knowledge of the phosphorus content, and thus the
in the dark.
phosphorus-containing additives, in a lubricating oil or addi-
tive can be used to pred
...
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: D4047 − 13 D4047 − 18
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 U.S. Department of Defense.
1. Scope*
1.1 This test method covers the determination of 0.0050.005 % to 10.0 10.0 % by 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 This test method is free from most interferences because the high insolubility of the quinoline phosphomolybdate precipitate
leads to constant composition and freedom from most adsorbed or occluded impurities, especially from cations which would
otherwise interfere in the subsequent titration of the precipitate.
1.4 Barium, calcium, magnesium, zinc, iron, aluminum, alkali salts, citric acid and citrates, chromium up to 18 times the
phosphorus content, and titanium up to 3.5 times do not interfere with the test method.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific hazard statements, see 6.9.
1.7 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
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
2.2 IP Standard:
3
IP 148 Test Method for Phosphorous in Lubricating Oils and Additives
3. Summary of Test Method
3.1 Additive concentrates are diluted with phosphorus-free white oil to produce a working blend.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
Current edition approved June 15, 2013April 1, 2018. Published August 2013April 2018. Originally approved in 1981. Last previous edition approved in 20112013 as
D4047– 00 (2011). – 13. DOI: 10.1520/D4047-13.10.1520/D4047-18.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM 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.
3
Available from Energy Institute, 61 New Cavendish St., London, WIGW1G 7AR, U.K., http://www.energyinst.org.uk.http://www.energyinst.org.
*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 ----------------------
D4047 − 18
3.2 The sample is ignited with excess of zinc oxide whereby phosphorus is converted to phosphate. The residue is dissolved
in hydrochloric acid and any sulfide formed is oxidized with potassium bromate. Phosphorus is then precipitated as quinoline
phosphomolybdate and determined volumetrically by addition of excess standard alkali and back titration with standard acid.
4. Significance and Use
4.1 Know
...
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