ASTM D4628-16

Standard Test Method for Analysis of Barium, Calcium, Magnesium, and Zinc in Unused Lubricating Oils by Atomic Absorption Spectrometry

SIGNIFICANCE AND USE
4.1 Some oils are formulated with metal-containing additives that act as detergents, antioxidants, antiwear agents, etc. Some of these additives contain one or more of these metals: barium, calcium, zinc, and magnesium. This test method provides a means of determining the concentration of these metals that gives an indication of the additive content in these oils.  
4.2 Several additive metals and their compounds are added to the lubricating oils to give beneficial performance. (See Table 1.)
SCOPE
1.1 This test method is applicable for the determination of mass percent barium from 0.005 % to 1.0 %, calcium and magnesium from 0.002 % to 0.3 %, and zinc from 0.002 % to 0.2 % in lubricating oils.  
1.2 Higher concentrations can be determined by appropriate dilution. Lower concentrations of metals such as barium, calcium, magnesium, and zinc at about 10 ppm level can also be determined by this test method. Use of this test method for the determination at these lower concentrations should be by agreement between the buyer and the seller.  
1.3 Lubricating oils that contain viscosity index improvers may give low results when calibrations are performed using standards that do not contain viscosity index improvers.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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. Specific warning statements are given in 3.1, 6.3, and 8.1.

General Information

• Status: Historical
• Publication Date: 30-Nov-2016
• ICS: 71.040.50 - Physicochemical methods of analysis
• 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4628 − 16
Standard Test Method for
Analysis of Barium, Calcium, Magnesium, and Zinc in
Unused Lubricating Oils by Atomic Absorption
1
Spectrometry
This standard is issued under the fixed designation D4628; 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
1.1 This test method is applicable for the determination of 3.1 A sample is weighed and base oil is added to 0.25 g 6
mass percent barium from 0.005 % to 1.0 %, calcium and 0.01 g total mass. Fifty millilitres of a kerosene solution,
magnesium from 0.002 % to 0.3 %, and zinc from 0.002 % to containing potassium as an ionization suppressant, are added,
0.2 % in lubricating oils. and the sample and oil are dissolved. (Warning—Hazardous.
Potentially toxic and explosive.) Standards are similarly
1.2 Higher concentrations can be determined by appropriate
prepared, always adding oil if necessary to yield a total mass of
dilution. Lower concentrations of metals such as barium,
0.25 g. These solutions are burned in the flame of an atomic
calcium, magnesium, and zinc at about 10 ppm level can also
absorption spectrophotometer. An acetylene/nitrous oxide
be determined by this test method. Use of this test method for
flame is used. (Warning—Combustible. Vapor harmful.)
the determination at these lower concentrations should be by
agreement between the buyer and the seller.
4. Significance and Use
1.3 Lubricating oils that contain viscosity index improvers
4.1 Some oils are formulated with metal-containing addi-
may give low results when calibrations are performed using
tives that act as detergents, antioxidants, antiwear agents, etc.
standards that do not contain viscosity index improvers.
Some of these additives contain one or more of these metals:
1.4 The values stated in SI units are to be regarded as
barium, calcium, zinc, and magnesium. This test method
standard. No other units of measurement are included in this
provides a means of determining the concentration of these
standard.
metals that gives an indication of the additive content in these
1.5 This standard does not purport to address all of the
oils.
safety concerns, if any, associated with its use. It is the
4.2 Several additive metals and their compounds are added
responsibility of the user of this standard to establish appro-
to the lubricating oils to give beneficial performance. (See
priate safety and health practices and determine the applica-
Table 1.)
bility of regulatory limitations prior to use. Specific warning
statements are given in 3.1, 6.3, and 8.1.
5. Apparatus
5.1 Atomic Absorption Spectrophotometer.
2. Referenced Documents
2
2.1 ASTM Standards: 5.2 Analytical Balance.
D6299 Practice for Applying Statistical Quality Assurance
5.3 Automatic Measuring Pipet or Volumetric Class A Pipet,
and Control Charting Techniques to Evaluate Analytical
50 mL capacity.
Measurement System Performance
5.4 Bottles with Screw Caps, 60 mL.
NOTE 1—Suitable volumetric flasks or plastic bottles may be substi-
1
This test method is under the jurisdiction of ASTM Committee D02 on
tuted.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
5.5 Shaker, Mechanical Stirrer, or Ultrasonic Bath, capable
Current edition approved Dec. 1, 2016. Published January 2017. Originally
of handling 60 mL bottles.
approved in 1986. Last previous edition approved in 2014 as D4628 – 14. DOI:
10.1520/D4628-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Reagents
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
6.1 Base Oil, metal-free, with a viscosity of about 4 cSt at
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 100 °C. A 100 neutral oil which provides good solvency for
*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 ----------------------
D4628 − 16
TABLE 1 Lubricants and Additive Materials
Element Compounds Purpose/Application
Barium Sulfonates, phenates Detergent inhibitors, corrosion inhibitors, detergents, rust
inhibitors, automatic transmission fluids
Calcium Sulfonates, phenates Detergent inhibitors, dispersants
Magnesium Sulfonates, phenates Detergent inhibitors
Zinc Dialkyldithiophosphates, dithiocarbamates, Anti-oxidant, corrosion i
...

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: D4628 − 14 D4628 − 16
Standard Test Method for
Analysis of Barium, Calcium, Magnesium, and Zinc in
Unused Lubricating Oils by Atomic Absorption
1
Spectrometry
This standard is issued under the fixed designation D4628; 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 is applicable for the determination of mass percent barium from 0.0050.005 % to 1.0 %, calcium and
magnesium from 0.0020.002 % to 0.3 %, and zinc from 0.0020.002 % to 0.2 % in lubricating oils.
1.2 Higher concentrations can be determined by appropriate dilution. Lower concentrations of metals such as barium, calcium,
magnesium, and zinc at about 10 ppm 10 ppm level can also be determined by this test method. Use of this test method for the
determination at these lower concentrations should be by agreement between the buyer and the seller.
1.3 Lubricating oils that contain viscosity index improvers may give low results when calibrations are performed using
standards that do not contain viscosity index improvers.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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. Specific warning statements are given in 3.1, 6.3, and 8.1.
2. Referenced Documents
2
2.1 ASTM Standards:
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
3. Summary of Test Method
3.1 A sample is weighed and base oil is added to 0.250.25 g 6 0.01-g0.01 g total mass. Fifty millilitres of a kerosinekerosene
solution, containing potassium as an ionization suppressant, are added, and the sample and oil are dissolved. (Warning—
Hazardous. Potentially toxic and explosive.) Standards are similarly prepared, always adding oil if necessary to yield a total mass
of 0.25 g. 0.25 g. These solutions are burned in the flame of an atomic absorption spectrophotometer. An acetylene/nitrous oxide
flame is used. (Warning—Combustible. Vapor harmful.)
4. Significance and Use
4.1 Some oils are formulated with metal-containing additives that act as detergents, antioxidants, antiwear agents, etc. Some of
these additives contain one or more of these metals: barium, calcium, zinc, and magnesium. This test method provides a means
of determining the concentration of these metals that gives an indication of the additive content in these oils.
4.2 Several additive metals and their compounds are added to the lubricating oils to give beneficial performance. (See Table 1.)
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved Dec. 1, 2014Dec. 1, 2016. Published January 2015January 2017. Originally approved in 1986. Last previous edition approved in 20112014 as
ε1
D4628 – 05 (2011)D4628 – 14. . DOI: 10.1520/D4628-14.10.1520/D4628-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM 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

---------------------- Page: 1 ----------------------
D4628 − 16
TABLE 1 Lubricants and Additive Materials
Element Compounds Purpose/Application
Barium Sulfonates, phenates Detergent inhibitors, corrosion inhibitors, detergents, rust
inhibitors, automatic transmission fluids
Calcium Sulfonates, phenates Detergent inhibitors, dispersants
Magnesium Sulfonates, phenates Detergent inhibitors
Zinc Dialkyldithiophosphates, dithiocarbamates, Anti-oxidant, corrosion inhibitors, antiwear additives,
phenolates carboxylates detergents, crankcase oils, hypoi
...