ASTM D1091-11
(Test Method)Standard Test Methods for Phosphorus in Lubricating Oils and Additives
Standard Test Methods for Phosphorus in Lubricating Oils and Additives
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. This test method is suitable for most applications requiring the determination of phosphorus.
SCOPE
1.1 These test methods cover the determination of phosphorus in unused lubricating oils and lubricating oil additives and their concentrates. The test methods are not restricted with respect to the type of phosphorus compounds that may be presentfor example, trivalent or pentavalent phosphorus compounds, phosphines, phosphates, phosphonates, phosphorus sulfides, and so forthsince all are quantitatively converted to an aqueous solution of orthophosphate ion by oxidation of the sample during the course of analysis.
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.
7.1 This test method covers a procedure for removal of organic material and subsequent conversion of phosphorus to phosphate ion in samples of unused lubricating oils, lubricating oil additives, and their concentrates.
12.1 This test method covers determination of total phosphorus in concentrations of less than two mass % (see Note 6), calculated on the basis of the original test specimen, in samples treated by the acid-oxidation procedure described in Sections 7-11.
Note 6—For phosphorus concentrations greater than or equal to two mass %, see Sections 19-25.
19.1 This test method covers the determination of total phosphorus in concentrations of 2 mass % or more, (see Note 10), calculated on the basis of the original sample, in samples treated by the acid-oxidation procedure described in Sections 7-11.
Note 10—For phosphorus concentrations less than 2 mass %, see Sections 12-18.
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Designation: D1091 − 11
StandardTest Methods for
1
Phosphorus in Lubricating Oils and Additives
This standard is issued under the fixed designation D1091; 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* 3. Summary of Test Method
3.1 Organic material in the sample is removed and the
1.1 These test methods cover the determination of phospho-
phosphorus is converted to phosphate ion by oxidation with
rus in unused lubricating oils and lubricating oil additives and
sulfuric acid, nitric acid, and hydrogen peroxide. One of these
their concentrates. The test methods are not restricted with
procedures is then followed:
respect to the type of phosphorus compounds that may be
present—for example, trivalent or pentavalent phosphorus Sections
Oxidation of the Sample 7–11
compounds, phosphines, phosphates, phosphonates, phospho-
Photometric (Molydivanado) Method 12–18
rus sulfides, and so forth—since all are quantitatively con-
Gravimetric Method 19–25
verted to an aqueous solution of orthophosphate ion by
3.2 The photometric method is used where the phosphorus
oxidation of the sample during the course of analysis.
content is estimated to be under 2 %, and the gravimetric
method is used for phosphorus contents of 2 % or over.
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 Knowledge of the phosphorus content, and thus the
1.3 This standard does not purport to address all of the
phosphorus-containing additives, in a lubricating oil or addi-
safety concerns, if any, associated with its use. It is the
tive can be used to predict performance characteristics. This
responsibility of the user of this standard to establish appro-
test method is suitable for most applications requiring the
priate safety and health practices and determine the applica-
determination of phosphorus.
bility of regulatory limitations prior to use.
5. Purity of Reagents
2. Referenced Documents
5.1 Purity of Reagents—Reagent grade chemicals shall be
2
2.1 ASTM Standards:
used in all tests. Unless otherwise indicated, it is intended that
D1193 Specification for Reagent Water
all reagents conform to the specifications of the Committee on
D4057 Practice for Manual Sampling of Petroleum and
Analytical Reagents of the American Chemical Society where
3
Petroleum Products
such specifications are available. Other grades may be used,
D4177 Practice for Automatic Sampling of Petroleum and
provided it is first ascertained that the reagent is of sufficiently
Petroleum Products
high purity to permit its use without lessening the accuracy of
D6299 Practice for Applying Statistical Quality Assurance
the determination.
and Control Charting Techniques to Evaluate Analytical
5.2 Purity of Water—Unless otherwise indicated, references
Measurement System Performance
to water shall be understood to mean reagent water as defined
by Type II or Type III of Specification D1193.
1 6. Sampling
These test methods are under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and are the responsibility of
6.1 Obtain samples in accordance with the instructions in
Subcommittee D02.03 on Elemental Analysis.
Practices D4057 or D4177.
CurrenteditionapprovedJune1,2011.PublishedJuly2011.Originallyapproved
in 1950. Last previous edition approved in 2005 as D1091–00(2005). DOI:
10.1520/D1091-11.
3
This test method has been adopted for use by government agencies to replace Reagent Chemicals, American Chemical Society Specifications , American
Method 5661 of Federal Test Method Standard No. 791b. Chemical Society, Washington, D.C. 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
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D1091 − 11
TABLE 1 Sample Size
6.2 Take care that the test specimen
...
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.
Designation:D1091–00 (Reapproved 2005) Designation:D1091–11
Standard Test Methods for
1
Phosphorus in Lubricating Oils and Additives
This standard is issued under the fixed designation D1091; 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 These test methods cover the determination of phosphorus in unused lubricating oils and lubricating oil additives and their
concentrates. The test methods are not restricted with respect to the type of phosphorus compounds that may be present—for
example, trivalent or pentavalent phosphorus compounds, phosphines, phosphates, phosphonates, phosphorus sulfides, and so
forth—since all are quantitatively converted to an aqueous solution of orthophosphate ion by oxidation of the sample during the
course of analysis.
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.
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
Measurement System Performance
3. Summary of Test Method
3.1 Organicmaterialinthesampleisremovedandthephosphorusisconvertedtophosphateionbyoxidationwithsulfuricacid,
nitric acid, and hydrogen peroxide. One of twothese procedures is then followed:
Sections
Photometric (Molydivanado) Method 7-18
Gravimetric Method Oxidation of the
Sample
and Photometric (Molydivanado) Method 12-18
Photometric (Molydivanado) Method 12-18
19-25
Gravimetric Method 19-25
3.2 The photometric method is used where the phosphorus content is estimated to be under 2 %, and the gravimetric method
is used for phosphorus contents of 2 % or over.
4. 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. This test method is suitable for most applications requiring the determination of
phosphorus.
1
These test methods are under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and are the responsibility of Subcommittee D02.03 on
Elemental Analysis.
Current edition approved MayJune 1, 2005.2011. Published May 2005.July 2011. Originally approved in 1950. Last previous edition approved in 20002005 as D1091–00.
D1091–00(2005). DOI: 10.1520/D1091-11.
This test method has been adopted for use by government agencies to replace Method 5661 of FederalTest Method Standard No. 791b DOI: 10.1520/D1091-00R05.791b.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book ofASTM 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
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D1091–11
5. Purity of Reagents
5.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
3
specifications are available. Other grades may be 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.
5.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by
Type II or Type III of Specification D1193.
6. Sampling
6.1 Obtain samples in accord
...
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