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

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 the 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 precautionary statements are given in 3.1, 6.3, and 8.1.

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09-Nov-2002
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ASTM D4628-02 - Standard Test Method for Analysis of Barium, Calcium, Magnesium, and Zinc In Unused Lubricating Oils By Atomic Absorption Spectrometry
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation:D4628–02
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 D 4628; 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.
1. Scope* containing potassium as an ionization suppressant, are added,
and the sample and oil are dissolved. (Warning—Hazardous.
1.1 This test method is applicable for the determination of
Potentially toxic and explosive.) Standards are similarly pre-
mass percent barium from 0.005 to 1.0 %, calcium and
pared, always adding oil if necessary to yield a total mass of
magnesium from 0.002 to 0.3 %, and zinc from 0.002 to 0.2 %
0.25 g. These solutions are burned in the flame of an atomic
in lubricating oils.
absorption spectrophotometer. An acetylene/nitrous oxide
1.2 Higher concentrations can be determined by appropriate
flame is used. (Warning—Combustible. Vapor harmful.)
dilution. Lower concentrations of metals such as barium,
calcium, magnesium, and zinc at about 10 ppm level can also
4. Significance and Use
be determined by this test method. Use of this test method for
4.1 Some oils are formulated with metal-containing addi-
the determination at these lower concentrations should be by
tives that act as detergents, antioxidants, antiwear agents, etc.
agreement between the buyer and the seller.
Some of these additives contain one or more of these metals:
1.3 Lubricating oils that contain viscosity index improvers
barium, calcium, zinc, and magnesium. This test method
may give low results when calibrations are performed using
provides a means of determining the concentration of these
standards that do not contain viscosity index improvers.
metals that gives an indication of the additive content in these
1.4 The values stated in SI units are to be regarded as the
oils.
standard.
1.5 This standard does not purport to address all of the
5. Apparatus
safety concerns, if any, associated with its use. It is the
5.1 Atomic Absorption Spectrophotometer.
responsibility of the user of this standard to establish appro-
5.2 Analytical Balance.
priate safety and health practices and determine the applica-
5.3 AutomaticMeasuringPipetorVolumetricClassAPipet,
bility of regulatory limitations prior to use. Specific precau-
50-mL capacity.
tionary statements are given in 3.1, 6.3, and 8.1.
5.4 Bottles with Screw Caps, 60 mL (2 oz).
2. Referenced Documents
NOTE 1—Suitable volumetric flasks or plastic bottles may be substi-
2.1 ASTM Standards: tuted.
D 6299 Practice for Applying Statistical Quality Assurance
5.5 Shaker, Mechanical Stirrer, or Ultrasonic Bath, capable
Techniques to Evaluate Analytical Measurement System
of handling 60-mL bottles.
2
Performance
6. Reagents
3. Summary of Test Method
6.1 Base Oil, metal-free, with a viscosity of about 4 cSt at
3.1 A sample is weighed and base oil is added to 0.25 6
100°C. A100 neutral oil which provides good solvency for
0.01-g total mass. Fifty millilitres of a kerosine solution,
standards and additive concentrate is satisfactory. Highly
paraffinic oils should be avoided.
6.2 2-EthylHexanoicAcid,whichhasbeendeterminedtobe
1
This test method is under the jurisdiction of ASTM Committee D02 on
free of interfering metals.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved Nov. 10, 2002. Published February 2003. Originally
approved in 1986. Last previous edition approved in 1997 as D 4628–97.
2
Annual Book of ASTM Standards, Vol 05.03.
*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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D4628–02
FIG. 1 Plot Graphs for Barium and Calcium
NOTE 5—In addition to the calibration standards identified in 6.4,
6.3 Kerosine, Metal-Free—See Notes 2-4. (Warning—
single-elementormultielementcalibrationstandardsmayalsobeprepared
Combustible.Vapor harmful.) Distillation range from 170°C to
from materials similar to the samples being analyzed, provided the
280°C at 100 kPa (1 atm). When the kerosine solvent is
calibration standards to be used have previously been characterized by
contaminated,itmaybepurifiedmetal-freebyrunningthrough
independent, primary (for example, gravimetric or volumetric), and
attapulgus clay.
analytical techniques to establish the
...

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