ASTM D5185-05

Standard Test Method for Determination of Additive Elements, Wear Metals, and Contaminants in Used Lubricating Oils and Determination of Selected Elements in Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)

SIGNIFICANCE AND USE
This test method covers the rapid determination of 22 elements in used lubricating oils and in base oils, and it provides rapid screening of used oils for indications of wear. Test times approximate a few minutes per test specimen, and detectability for most elements is in the low mg/kg range. In addition, this test method covers a wide variety of metals in virgin and re-refined base oils. Twenty-two elements can be determined rapidly, with test times approximating several minutes per test specimen.
When the predominant source of additive elements in used lubricating oils is the additive package, significant differences between the concentrations of the additive elements and their respective specifications can indicate that the incorrect oil is being used. The concentrations of wear metals can be indicative of abnormal wear if there are baseline concentration data for comparison. A marked increase in boron, sodium, or potassium levels can be indicative of contamination as a result of coolant leakage in the equipment. This test method can be used to monitor equipment condition and define when corrective actions are needed.
The concentrations of metals in re-refined base oils can be indicative of the efficiency of the re-refining process. This test method can be used to determine if the base oil meets specifications with respect to metal content.
SCOPE
1.1 This test method covers the determination of additive elements, wear metals, and contaminants in used lubricating oils by inductively coupled plasma atomic emission spectrometry (ICP-AES). The specific elements are listed in .
1.2 This test method covers the determination of selected elements, listed in , in re-refined and virgin base oils.
1.3 For analysis of any element using wavelengths below 190 nm, a vacuum or inert-gas optical path is required. The determination of sodium and potassium is not possible on some instruments having a limited spectral range.
1.4 This test method uses oil-soluble metals for calibration and does not purport to quantitatively determine insoluble particulates. Analytical results are particle size dependent, and low results are obtained for particles larger than a few micrometers.
1.5 Elements present at concentrations above the upper limit of the calibration curves can be determined with additional, appropriate dilutions and with no degradation of precision.
1.6 For elements other than calcium, sulfur, and zinc, the low limits listed in and were estimated to be ten times the repeatability standard deviation. For calcium, sulfur, and zinc, the low limits represent the lowest concentrations tested in the interlaboratory study.
1.7 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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. Specific warning statements are given in , , and .

General Information

• Status: Historical
• Publication Date: 31-Oct-2005
• ICS: 75.080 - Petroleum products in general
• 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 D5185-02e2 - Standard Test Method for Determination of Additive Elements, Wear Metals, and Contaminants in Used Lubricating Oils and Determination of Selected Elements in Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 01-Nov-2005
• Replaced By: ASTM D5185-09 - Standard Test Method for Determination of Additive Elements, Wear Metals, and Contaminants in Used Lubricating Oils and Determination of Selected Elements in Base Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 15-Apr-2009
• Referred By: ASTM D8315-20 - Standard Test Method for Determination of Wear Metals and Contamination Elements in Used Industrial Oils by Sweeping Flat Electrode Atomic Emission Spectrometry
• Effective Date: 01-Nov-2005
• Referred By: ASTM D4485-22e1 - Standard Specification for Performance of Active API Service Category Engine Oils
• Effective Date: 01-Nov-2005
• Referred By: ASTM D7151-15 - Standard Test Method for Determination of Elements in Insulating Oils by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 01-Nov-2005
• Referred By: ASTM D8184-18e1 - Standard Test Method for Ferrous Wear Debris Monitoring in In-Service Fluids Using a Particle Quantifier Instrument
• Effective Date: 01-Nov-2005
• Referred By: ASTM D6823-08(2021) - Standard Specification for Commercial Boiler Fuels With Used Lubricating Oils
• Effective Date: 01-Nov-2005
• Referred By: ASTM D7549-23 - Standard Test Method for Evaluation of Heavy-Duty Engine Oils under High Output Conditions—Caterpillar C13 Test Procedure
• Effective Date: 01-Nov-2005
• Referred By: ASTM D8047-23 - Standard Test Method for Evaluation of Engine Oil Aeration Resistance in a Caterpillar C13 Direct-Injected Turbocharged Automotive Diesel Engine
• Effective Date: 01-Nov-2005
• Referred By: ASTM D7414-22 - Standard Test Method for Condition Monitoring of Oxidation in In-Service Petroleum and Hydrocarbon Based Lubricants by Trend Analysis Using Fourier Transform Infrared (FT-IR) Spectrometry
• Effective Date: 01-Nov-2005
• Referred By: ASTM D7468-22 - Standard Test Method for Cummins ISM Test
• Effective Date: 01-Nov-2005
• Referred By: ASTM D7919-14(2021) - Standard Guide for Filter Debris Analysis (FDA) Using Manual or Automated Processes
• Effective Date: 01-Nov-2005
• Referred By: ASTM D7111-16(2021) - Standard Test Method for Determination of Trace Elements in Middle Distillate Fuels by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
• Effective Date: 01-Nov-2005
• Referred By: ASTM D7589-16e1 - Standard Test Method for Measurement of Effects of Automotive Engine Oils on Fuel Economy of Passenger Cars and Light-Duty Trucks in Sequence VID Spark Ignition Engine<rangeref></rangeref >
• Effective Date: 01-Nov-2005
• Referred By: ASTM D6891-23 - Standard Test Method for Evaluation of Automotive Engine Oils in the Sequence IVA Spark-Ignition Engine
• Effective Date: 01-Nov-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
An American National Standard
Designation: D 5185 – 05
Standard Test Method for
Determination of Additive Elements, Wear Metals, and
Contaminants in Used Lubricating Oils and Determination of
Selected Elements in Base Oils by Inductively Coupled
1
Plasma Atomic Emission Spectrometry (ICP-AES)
This standard is issued under the fixed designation D 5185; 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 (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
INTRODUCTION
Costs associated with maintenance due to engine and machine wear can be significant. Therefore,
diagnostic methods for determining the condition of engines and other machinery can be important.
This test method is intended to quantify, for the purpose of equipment monitoring, the concentration
of metals in used lubricating oils. Although the precision statement was determined by analyzing a
varietyofusedoilsthistestmethodcan,inprinciple,beusedfortheanalysisofunusedoilstoprovide
more complete elemental composition data than Test Methods D 4628, D 4927,or D 4951.
1. Scope* and zinc, the low limits represent the lowest concentrations
tested in the interlaboratory study.
1.1 This test method covers the determination of additive
1.7 The values stated in SI units are to be regarded as the
elements, wear metals, and contaminants in used lubricating
standard. The values given in parentheses are for information
oils by inductively coupled plasma atomic emission spectrom-
only.
etry (ICP-AES). The specific elements are listed in Table 1.
1.8 This standard does not purport to address all of the
1.2 This test method covers the determination of selected
safety concerns, if any, associated with its use. It is the
elements, listed in Table 1, in re-refined and virgin base oils.
responsibility of the user of this standard to establish appro-
1.3 For analysis of any element using wavelengths below
priate safety and health practices and determine the applica-
190 nm, a vacuum or inert-gas optical path is required. The
bility of regulatory limitations prior to use. Specific warning
determinationofsodiumandpotassiumisnotpossibleonsome
statements are given in 6.1, 8.2, and 8.4.
instruments having a limited spectral range.
1.4 This test method uses oil-soluble metals for calibration
2. Referenced Documents
and does not purport to quantitatively determine insoluble
3
2.1 ASTM Standards:
particulates.Analytical results are particle size dependent, and
C 1109 Test Method for Analysis of Aqueous Leachates
low results are obtained for particles larger than a few
2 from Nuclear Waste Materials Using Inductively Coupled
micrometers.
Plasma-Atomic Emission Spectrometry
1.5 Elementspresentatconcentrationsabovetheupperlimit
D 1552 Test Method for Sulfur in Petroleum Products
of the calibration curves can be determined with additional,
(High-Temperature Method)
appropriate dilutions and with no degradation of precision.
D 4057 Practice for Manual Sampling of Petroleum and
1.6 For elements other than calcium, sulfur, and zinc, the
Petroleum Products
lowlimitslistedinTable2andTable3wereestimatedtobeten
D 4307 PracticeforPreparationofLiquidBlendsforUseas
times the repeatability standard deviation. For calcium, sulfur,
Analytical Standards
D 4628 Test Method for Analysis of Barium, Calcium,
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
3
Current edition approved Nov. 1, 2005. Published November 2005. Originally For referenced ASTM standards, visit the ASTM website, www.astm.org, or
e2
approved in 1991. Last previous edition approved in 2002 as D 5185–02 . contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
2
Eisentraut, K. J., Newman, R. W., Saba, C. S., Kauffman, R. E., and Rhine, W. Standards volume information, refer to the standard’s Document Summary page on
E., Analytical Chemistry, Vol 56, 1984. the ASTM website.
*A Summary of Changes section appears at the end of this standard.
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D5185–05
A
TABLE 1 Elements Determined and Suggested Wavelengths TABLE 3 Reproducibility
A
Element Wavelength, nm Element Range, mg/kg Reproducibility, µg/g
0.26
Aluminum 308.22, 396.15, 309.27 Aluminum 6–40 3.8 X
0.92
Barium 233.53, 455.40, 493.41 Barium 0.5–4 0.59 X
0.01
Boron 249.77 Boron 4–30 13 X
1.3
Calcium 315.89, 317.93, 364.44, 422
...