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ASTM D7040-04(2010)

(Test Method)

Standard Test Method for Determination of Low Levels of Phosphorus in ILSAC GF 4 and Similar Grade Engine Oils by Inductively Coupled Plasma Atomic Emission Spectrometry

Standard Test Method for Determination of Low Levels of Phosphorus in ILSAC GF 4 and Similar Grade Engine Oils by Inductively Coupled Plasma Atomic Emission Spectrometry

SIGNIFICANCE AND USE
This test method usually requires several minutes per sample. Other test methods which can be used for the determination of phosphorus in lubricating oils include WDXRF Test Method D4927 and ICPAES Test Methods D4951 and D5185. However, this test method provides more precise results than Test Methods D4951 or D5185.
Lubricating oils are typically blends of additive packages, and their specifications are also determined, in part, by elemental composition. This test method can be used to determine if unused lubricating oils meet specifications with respect to elemental composition.
It is expected that GF 4 grade engine oils marketed in the years 2004-2005 will have a maximum phosphorus concentration level of 500 to 800 mg/kg. These limits are required to minimize poisoning of automotive emission control catalysts by volatile phosphorus species. It is anticipated that the later grades of oils may have even lower phosphorus levels.
SCOPE
1.1 This test method covers the quantitative determination of phosphorus in unused lubricating oils, such as International Lubricant Standardization and Approval Committee (ILSAC) GF 4 and similar grade engine oils, by inductively coupled plasma atomic emission spectrometry.
1.2 The precision statements are valid for dilutions in which the mass % sample in solvent is held constant in the range of 1 to 5 mass % oil.
1.3 The precision tables define the concentration ranges covered in the interlaboratory study (500 to 800 mg/kg). However, both lower and higher concentrations can be determined by this test method. The low concentration limits are dependent on the sensitivity of the ICP instrument and the dilution factor. The high concentration limits are determined by the product of the maximum concentration defined by the linear calibration curve and the sample dilution factor.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.5 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.

General Information

Status
Historical
Publication Date
30-Apr-2010
ICS
75.100 - Lubricants, industrial oils and related products
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.03 - Elemental Analysis
Current Stage
Ref Project

Relations

Replaces
ASTM D7040-04 - Standard Test Method for Determination of Low Levels of Phosphorus in ILSAC GF 4 and Similar Grade Engine Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
Effective Date
01-May-2010
Replaced By
ASTM D7040-04(2015) - Standard Test Method for Determination of Low Levels of Phosphorus in ILSAC GF 4 and Similar Grade Engine Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
Effective Date
01-Apr-2015
Referred By
ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
Effective Date
01-May-2010
Referred By
ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
01-May-2010
Referred By
ASTM D7260-20 - Standard Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
01-May-2010

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ASTM D7040-04(2010) - Standard Test Method for Determination of Low Levels of Phosphorus in ILSAC GF 4 and Similar Grade Engine Oils by Inductively Coupled Plasma Atomic Emission SpectrometryASTM D7040-04(2010) - Standard Test Method for Determination of Low Levels of Phosphorus in ILSAC GF 4 and Similar Grade Engine Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
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ASTM D7040-04(2010) - Standard Test Method for Determination of Low Levels of Phosphorus in ILSAC GF 4 and Similar Grade Engine Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
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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: D7040 − 04(Reapproved 2010)
Standard Test Method for
Determination of Low Levels of Phosphorus in ILSAC GF 4
and Similar Grade Engine Oils by Inductively Coupled
1
Plasma Atomic Emission Spectrometry
This standard is issued under the fixed designation D7040; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D4307Practice for Preparation of Liquid Blends for Use as
Analytical Standards
1.1 This test method covers the quantitative determination
D4927Test Methods for Elemental Analysis of Lubricant
of phosphorus in unused lubricating oils, such as International
and Additive Components—Barium, Calcium,
Lubricant Standardization and Approval Committee (ILSAC)
Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive
GF 4 and similar grade engine oils, by inductively coupled
X-Ray Fluorescence Spectroscopy
plasma atomic emission spectrometry.
D4951TestMethodforDeterminationofAdditiveElements
1.2 Theprecisionstatementsarevalidfordilutionsinwhich
in Lubricating Oils by Inductively Coupled Plasma
the mass% sample in solvent is held constant in the range of
Atomic Emission Spectrometry
1 to 5 mass% oil.
D5185Test Method for Multielement Determination of
1.3 The precision tables define the concentration ranges Used and Unused Lubricating Oils and Base Oils by
Inductively Coupled Plasma Atomic Emission Spectrom-
covered in the interlaboratory study (500 to 800 mg/kg).
However, both lower and higher concentrations can be deter- etry (ICP-AES)
D6299Practice for Applying Statistical Quality Assurance
mined by this test method. The low concentration limits are
dependent on the sensitivity of the ICP instrument and the and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
dilutionfactor.Thehighconcentrationlimitsaredeterminedby
the product of the maximum concentration defined by the D6792Practice for Quality System in Petroleum Products
and Lubricants Testing Laboratories
linear calibration curve and the sample dilution factor.
1.4 The values stated in SI units are to be regarded as the
3. Summary of Test Method
standard. The values given in parentheses are for information
3.1 A sample portion is weighed and diluted by mass with
only.
mixed xylenes or other solvent.An internal standard, which is
1.5 This standard does not purport to address all of the
required,iseitherweighedseparatelyintothetestsolutionoris
safety concerns, if any, associated with its use. It is the
previously combined with the dilution solvent. Calibration
responsibility of the user of this standard to establish appro-
standards are prepared similarly. The solutions are introduced
priate safety and health practices and determine the applica-
to the ICP instrument by a peristaltic pump (required). By
bility of regulatory limitations prior to use.
comparing emission intensity of phosphorus in the test speci-
men with emission intensities measured with the calibration
2. Referenced Documents
standardsandbyapplyingtheappropriateinternalstandardand
2
2.1 ASTM Standards:
background corrections, the concentrations of phosphorus in
D4057Practice for Manual Sampling of Petroleum and
the sample is calculated.
Petroleum Products
4. Significance and Use
4.1 This test method usually requires several minutes per
1
This test method is under the jurisdiction of ASTM Committee D02 on
sample. Other test methods which can be used for the deter-
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
mination of phosphorus in lubricating oils include WDXRF
Current edition approved May 1, 2010. Published May 2010. Originally
Test Method D4927 and ICPAES Test Methods D4951 and
approved in 2004. Last previous edition approved in 2004 as D7040–04. DOI:
D5185. However, this test method provides more precise
10.1520/D7040-04R10.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or results than Test Methods D4951 or D5185.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
4.2 Lubricating oils are typically blends of additive
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. packages, and their specifications are also determined, in part,
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7040 − 04 (2010)
by elemental composition. This test method can be used to 7. Reagents and Materials
determine if unused lubricating oils meet specifications with
7.1 Purity of Re
...

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5.1 The bromine number is useful as a measure of aliphatic unsaturation in petroleum samples. When used in conjunction with the calculation procedure described in Annex A2, it can be used to estimate the percentage of olefins in petroleum distillates boiling up to approximately 315 °C (600 °F).  
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5.1 The low-temperature, low-shear-rate viscosity of automatic transmission fluids, gear oils, torque and tractor fluids, and industrial and automotive hydraulic oils (see Appendix X4) are of considerable importance to the proper operation of many mechanical devices. Measurement of the viscometric properties of these oils and fluids at low temperatures is often used to specify their acceptance for service. This test method is used in a number of specifications.  
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1.3 Spectra and distribution profiles presented herein are for illustrative purposes only and are not to be construed as representing or establishing lubricant or machinery guidelines.  
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1.1 This test method covers quantitative procedures for the evaluation of the compatibility of automotive engine oils with several reference elastomers typical of those used in the sealing materials in contact with these oils. Compatibility is evaluated by determining the changes in volume, Durometer A hardness, and tensile properties when the elastomer specimens are immersed in the oil for a specified time and temperature.  
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1.3 This test method provides a preliminary or first order evaluation of oil/elastomer compatibility only. Because seals might be subjected to static or dynamic loads, or both, and they can operate over a range of conditions, a complete evaluation of the potential sealing performance of any elastomer-oil combination in any service condition usually requires tests additional to those described in this test method.  
1.4 The several reference elastomer formulations specified in this test method were chosen to be representative of those used in both heavy-duty diesel engines (detailed in Annex A1) and passenger-car spark-ignition engines (the latter are covered in Annex A2). The procedures described in this test method can, however, also be used to evaluate the compatibility of automotive engine oils with different elastomer types/formulations or different test durations and temperatures to those employed in this test method.
Note 2: In such cases, the precision and bias statement in Section 12 does not apply. In addition to agreeing acceptable limits of precision, where relevant, the user and supplier should also agree:  (1) test temperatures and immersion times to be used; (2) the formulations and typical properties of the elastomers; and (3) the sourcing and quality control of the elastomer sheets.
Note 3: The TMC may also issue In...

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ASTM
ASTM D7918-23(Test Method)
Standard Test Method for Measurement of Flow Properties and Evaluation of Wear, Contaminants, and Oxidative Properties of Lubricating Grease by Die Extrusion Method and Preparation

SIGNIFICANCE AND USE
5.1 Trending the wear, contamination, consistency, and oxidative properties of a lubricating grease is a crucial part of condition-monitoring programs. Changes in these properties or deviations from the new grease can be indicative of problems within the lubricated component, such as the mixing of incompatible thickener types, excessive wear or contaminant levels, or significant depletion of antioxidant levels. These test methods also makes it possible to develop trends that can be used to predict failures before they occur and allow for corrective action to be taken.
SCOPE
1.1 This test method covers the determination and evaluation of flow properties, wear levels, contaminants, and oxidative condition of new and in-service lubricating grease.  
1.2 This test method provides guidance on evaluating in-service grease samples, NLGI grades 00 to 3, for wear, consistency, contamination, and oxidation.  
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3.1 Exception—The exception to this will be where units of references were developed by the developers of the test equipment and necessary to report the results of the test.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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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ASTM
ASTM D7922-23(Test Method)
Standard Test Method for Determination of Glycol for In-Service Engine Oils by Gas Chromatography

SIGNIFICANCE AND USE
5.1 Some glycol/antifreeze dilution of in-service engine oil is normal under typical operating conditions. However, excessive glycol dilution can lead to decreased performance, premature wear, or sudden engine failure. This test method provides a means of quantifying the level of glycol based antifreeze dilution, allowing the user to take necessary action.
SCOPE
1.1 This test method covers the determination of glycol based antifreeze for in-service engine oil by derivative headspace/gas chromatography.  
1.2 Sample is derivatized in-situ directly in a headspace sampling vial prior to vapor phase extraction and injection into a gas chromatograph.  
1.3 The chemistry of the derivatization is unique to the detection of the molecules of ethylene glycol and 1,2-propylene glycol. 1,3-propylene glycol could also be detected but is not used in any known anti-freeze at this time. Other coolant analyses are beyond the scope of this test method.  
1.4 The derivatization process does not affect glycol breakdown products such as glycolate and formate and hence the presence of these compounds in the oil will not be quantified.  
1.5 The test method concentration range is from 50 µg/g to 1000 µg/g. Lower levels are possible by method modifications. Higher levels are possible through sample dilution.  
1.6 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 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.  
1.8 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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