ASTM D1091-11(2016)

Standard Test Methods for Phosphorus in Lubricating Oils and Additives (Withdrawn 2021)

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.
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.  
1.2 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.
WITHDRAWN RATIONALE
These test methods covered the determination of phosphorus in unused lubricating oils and lubricating oil additives and their concentrates. The test methods were 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.
Formerly under the jurisdiction of Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants, these test methods were withdrawn in November 2021. This standard is being withdrawn without replacement. Test Methods D1091 was originally developed in 1950 when there were few approaches for the determination of phosphorus in petroleum products. Since that time, instrumental methods have been developed for the determination of phosphorus in petroleum products, for example, Test Methods D4951, D5185, and D6481. It is the judgement of the D02.03 officers that this method is no longer needed and could not be revised to comply with the negative voter’s request without a new interlaboratory study, which would be difficult to get the required participation.

General Information

• Status: Withdrawn
• Publication Date: 31-Mar-2016
• Withdrawal Date: 11-Nov-2021
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

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: D1091 − 11 (Reapproved 2016)
Standard Test Methods for
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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
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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
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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.
Current edition approved April 1, 2016. Published May 2016. Originally
approved in 1950. Last previous edition approved in 2011 as D1091 – 11. DOI:
10.1520/D1091-11R16.
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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 [e-mail]. 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.
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D1091 − 11 (2016)
TABLE 1 Sample Size
6.2 Take care that the test specimen is thoroughly represen-
tative o
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