ASTM D7528-09

Standard Test Method for Bench Oxidation of Engine Oils by ROBO Apparatus

SIGNIFICANCE AND USE
This bench test method is intended to produce comparable oil aging characteristics to those obtained with ASTM TMC Sequence IIIGA matrix reference oils 434, 435 and 438 after aging in the Sequence IIIG engine test.
To the extent that the method generates aged oils comparable to those from the Sequence IIIG engine test, the measured increases in kinematic and MRV viscosity indicate the tendency of an oil to thicken because of volatilization and oxidation, as in the Sequence IIIG and IIIGA (see Appendix X1 in Test Method D 7320) engine tests, respectively.
This bench test procedure has potential use in specifications and classifications of engine lubricating oils, such as Specification D 4485.
SCOPE
1.1 This test method describes a bench procedure to simulate the oil aging encountered in Test Method D 7320, the Sequence IIIG engine test method. These aged oils are then tested for kinematic viscosity and for low-temperature pumpability properties as described in the Sequence IIIGA engine test, Appendix X1 of Test Method D 7320.
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.2.1 Exceptions—There are no SI equivalents for some apparatus in Section 6, and there are some figures where inch units are to be regarded as 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. Specific warning statements are given in Sections 7 and 8.
1.4 This test method is arranged as follows: Section Scope1 Reference Documents2 Terminology3 Summary of Test Method4 Significance and Use5 Apparatus6 Reagents and Materials7 Hazards8 Reference Oil Testing and Test Stand Calibration9 Procedure10 Cleaning11 Calculations and Determination of Test Results12 Report13 Precision and Bias14 Keywords15 Annexes Reaction VesselAnnex A1 Reaction Vessel HeadAnnex A2 Reaction Vessel-to-Head SealAnnex A3 Agitator Turbine BladeAnnex A4 Agitator Packing GlandAnnex A5 Nitrogen Dioxide Graduated TubeAnnex A6 Vacuum System PlumbingAnnex A7 Vacuum Trap CondensersAnnex A8 Setting the Vacuum Control ValveAnnex A9 Appendixes Sample Preparation and AdditionAppendix X1 Charging the Liquid Nitrogen DioxideAppendix X2 Nitrogen Dioxide Precision Needle ValveAppendix X3 Example of an Assembled ROBO ApparatusAppendix X4 Information Package to Aid Setting Up a New Robo ApparatusAppendix X5

General Information

• Status: Historical
• Publication Date: 14-Apr-2009
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.B0.07 - Development and Surveillance of Bench Tests Methods

Relations

• Replaced By: ASTM D7528-13 - Standard Test Method for Bench Oxidation of Engine Oils by ROBO Apparatus
• Effective Date: 01-May-2013
• Referred By: ASTM D4485-22e1 - Standard Specification for Performance of Active API Service Category Engine Oils
• Effective Date: 15-Apr-2009

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: D7528 − 09
StandardTest Method for
Bench Oxidation of Engine Oils by ROBO Apparatus
This standard is issued under the fixed designation D7528; 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.
INTRODUCTION
Any properly equipped laboratory, without outside assistance, can use the procedure described in
this test method. However, theASTM Test Monitoring Center (TMC) provides reference oils and an
assessment of the test results obtained on those oils by the laboratory. By these means, the laboratory
will know whether its use of the test method gives results statistically similar to those obtained by
other laboratories. Furthermore, various agencies require that a laboratory utilize the TMC services in
seeking qualification of oils against specifications. For example, the U.S. Army imposes such a
requirement in connection with several Army engine lubricating oil specifications.
Accordingly, this test method is written for use by laboratories that utilize the portions of the test
method that refer to the TMC services. Laboratories that choose not to use the TMC services may
simply ignore these portions.
This test method may be modified by means of information letters issued by the TMC. In addition,
the TMC may issue supplementary memoranda related to the method.
1. Scope bility of regulatory limitations prior to use. Specific warning
statements are given in Sections 7 and 8.
1.1 This test method describes a bench procedure to simu-
1.4 This test method is arranged as follows:
late the oil aging encountered in Test Method D7320, the
Section
Sequence IIIG engine test method. These aged oils are then
Scope 1
tested for kinematic viscosity and for low-temperature pump-
Reference Documents 2
ability properties as described in the Sequence IIIGA engine Terminology 3
Summary of Test Method 4
test, Appendix X1 of Test Method D7320.
Significance and Use 5
Apparatus 6
1.2 Units—The values stated in SI units are to be regarded
Reagents and Materials 7
as standard. No other units of measurement are included in this
Hazards 8
standard.
Reference Oil Testing and Test Stand Calibration 9
Procedure 10
1.2.1 Exceptions—There are no SI equivalents for some
Cleaning 11
apparatus in Section 6, and there are some figures where inch
Calculations and Determination of Test Results 12
units are to be regarded as standard.
Report 13
Precision and Bias 14
1.3 This standard does not purport to address all of the
Keywords 15
safety concerns, if any, associated with its use. It is the
Annexes
Reaction Vessel Annex A1
responsibility of the user of this standard to establish appro-
Reaction Vessel Head Annex A2
priate safety and health practices and determine the applica-
Reaction Vessel-to-Head Seal Annex A3
Agitator Turbine Blade Annex A4
Agitator Packing Gland Annex A5
Nitrogen Dioxide Graduated Tube Annex A6
This test method is under the jurisdiction of ASTM Committee D02 on
Vacuum System Plumbing Annex A7
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
Vacuum Trap Condensers Annex A8
D02.B0.07 on Development and Surveillance of Bench Tests Methods.
Setting the Vacuum Control Valve Annex A9
Current edition approved April 15, 2009. Published June 2009. DOI: 10.1520/
Appendixes
D7528-09.
2 Sample Preparation and Addition Appendix X1
ASTMTestMonitoringCenter,6555PennAvenue,Pittsburgh,PA15206-4489.
Charging the Liquid Nitrogen Dioxide Appendix X2
www.astmtmc.cmu.edu.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7528 − 09
mixtureisstirredandheatedfor40hat170ºCwithairflowing
Section
Nitrogen Dioxide Precision Needle Valve Appendix X3
across the liquid surface under negative pressure. In addition,
Example of an Assembled ROBO Apparatus Appendix X4
nitrogen dioxide and air are introduced below the reaction
Information Package to Aid Setting Up a New Robo Apparatus Appendix X5
surface. After cooling, the oxidized, concentrated test oil is
2. Referenced Documents
subjected to pertinent viscometric tests. Evaporated oil is
condensed in order to weigh it and calculate evaporative loss.
2.1 ASTM Standards:
D445 Test Method for Kinematic Viscosity of Transparent
5. Significance and Use
and Opaque Liquids (and Calculation of Dynamic Viscos-
ity) 5.1 This bench test method is intended to produce compa-
D4175 Terminology Relating to Petroleum, Petroleum rable oil aging characteristics to those obtained with ASTM
TMC Sequence IIIGA matrix reference oils 434, 435 and 438
Products, and Lubricants
D4485 Specification for Performance of Active API Service after aging in the Sequence IIIG engine test.
Category Engine Oils
5.2 To the extent that the method generates aged oils
D4684 Test Method for Determination of Yield Stress and
comparable to those from the Sequence IIIG engine test, the
Apparent Viscosity of Engine Oils at Low Temperature
measured increases in kinematic and MRV viscosity indicate
D5293 Test Method for Apparent Viscosity of Engine Oils
the tendency of an oil to thicken because of volatilization and
and Base Stocks Between –5 and –35°C Using Cold-
oxidation,asintheSequenceIIIGandIIIGA(seeAppendixX1
Cranking Simulator
in Test Method D7320) engine tests, respectively.
D7320 Test Method for Evaluation of Automotive Engine
5.3 This bench test procedure has potential use in specifi-
Oils in the Sequence IIIG, Spark-Ignition Engine
cations and classifications of engine lubricating oils, such as
2.2 SAE Standard:
Specification D4485.
SAE J300 Engine Oil Viscosity Classification
6. Apparatus
3. Terminology
6.1 Balances:
3.1 Definitions:
6.1.1 Analytical Balance—Capable of weighing 200 g with
3.1.1 candidate oil, n—an oil that is intended to have the
a minimum indication resolution of 0.1 g.
performance characteristics necessary to satisfy a specification
6.1.2 Analytical Balance—Capableofweighing0.1gwitha
and is to be tested against that specification. D4175
minimum indication resolution of 0.001 g.
3.1.2 reference oil, n—an oil of known performance
6.2 Fume Hood, that vents to the outside atmosphere (see
characteristics, used as a basis for comparison.
Section 8).
3.1.2.1 Discussion—Reference oils are used to calibrate
testing facilities, to compare the performance of other oils, or
6.3 Reaction Vessel (ACE Glass, Inc. part number
6,7
to evaluate other materials (such as seals) that interact with
D120676), a 1-L, thick-walled glass vessel having a nominal
oils. D4175
100-mm inner diameter and with a bottom, sample/drain valve.
7,8
3.1.3 non-reference oil, n—anyoilotherthanareferenceoil, The lower half has an Instatherm coating, rated at approxi-
mately 400W, for heating the test mixture.Adiagram is shown
suchasaresearchformulation,commercialoilorcandidateoil.
D4175 in Fig. A1.1.
3.1.4 test oil, n—any oil subjected to evaluation in an
6.4 Vessel Head—Thevesselheadisastainlesssteelplateof
established procedure. D4175
sufficient diameter to completely cover the lower glass vessel
and provide ample material for a sturdy mounting system.
3.2 Definitions of Terms Specific to This Standard:
7,9
Reimel Machine, Inc. part number RMI-1002-DH has been
3.2.1 aged oil, n—a test oil after it has been subjected to the
shown to be suitable for this application. The vessel head may
40-h aging process in a ROBO apparatus.
also be constructed as described in AnnexA2. Users may also
3.3 Acronyms:
source some parts from Reimel Machine, Inc. and some
3.3.1 ROBO, n—Romaszewski Oil Bench Oxidation
in-house.Ensuretheplatehasacenterholeforanagitatorshaft
and threaded ports to allow filling and for the attachment of
4. Summary of Test Method
air/nitrogen dioxide lines, vacuum control and relief valves,
4.1 The test oil is combined with a small amount of iron
and a temperature probe. Fig. A2.1 defines the locations of
ferrocene catalyst and placed in a 1-L reaction vessel. That
these ports. Mill the bottom surface of this stainless steel plate
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM The sole source of supply of the apparatus known to the committee at this time
Standards volume information, refer to the standard’s Document Summary page on is Ace Glass, Inc., P.O. Box 688, 1430 NW Blvd., Vineland, NJ 08362-0688.
the ASTM website. If you are aware of alternative suppliers, please provide this information to
Available from SAE International, 400 Commonwealth Drive, Warrendale, PA ASTM. Your comments will receive careful consideration at a meeting of the
15096-0001, http://www.sae.org. responsible technical committee which you may attend.
5 8
Kinker, B. G., Romaszewski, R. A., and Palmer, P. A., “ROBO–A Bench InstathermisaregisteredtrademarkofAceGlass,Inc.,P.O.Box688,1430NW
Procedure to Replace Sequence IIIGAEngineTest,” Journal of ASTM International Blvd., Vineland, NJ 08362-0688.
(JAI), Vol 4, No. 10, 2007, Paper ID JAI 100916. Available online from The sole source of supply of the apparatus known to the committee at this time
www.astm.org. is Reimel Machine, Inc., 2575 Wyandotte Rd., Willow Grove, PA 19090.
D7528 − 09
to accept a polytetrafluoroethylene (PTFE) ring seal for cen- 6.10.1 Acrylic Block Airflow Meter (King Instrument Co.,
7,10
tered attachment of the glass vessel as described in AnnexA3. 7520 Series, Order number 2C-17), having a scale of 0.4 to
7,9
Reimel Machine, Inc. part number RMI-1007-DH has been 4 Standard Cubic Feet per Minute (SCFM), with ⁄4-in. NPT
found suitable for this purpose. threaded female pipe end. It is used for measuring air flow in
10.3.2. The machined fitting for the top of the flow meter shall
6.5 Stirrer Motor—An electric motor with drill chuck collet
accommodate the vacuum line from the condenser to the
capable of sustained operation at 200 6 5 r/min.
reactor with a ⁄8-in. inside diameter or larger. The machined
fitting for the bottom of the flow meter shall accommodate the
6.6 Stirrer—An 8-mm diameter stainless steel rod, 30-mm
⁄4-in. vacuum control valve.
long with a means of attaching a blade assembly at the bottom.
The turbine blade assembly diameter is 2.58 in. with 1.4-mm
NOTE 2—SCFM is the volumetric flow rate of a gas corrected to
thickbladesattachedata45°pitchwithanoverallbladeheight
standardized conditions of temperature, pressure, and relative humidity,
of 0.985 in. Construct the stirrer as described in Annex A4. thus representing a precise mass flow rate. However, the definitions of
7,9
standard conditions vary. In this method, the flow meter is calibrated with
Reimel Machine, Inc. part number RMI-1001-DH has been
air at standard conditions defined as a temperature of 70°F, a pressure of
found suitable for this purpose.Attach the stirrer to the reactor
14.6 psia and 0 % relative humidity.
head by means of a packing gland constructed as described in
6.10.2 Airflow Meter, with a scale calibrated in mL/min for
Annex A5. Reimel Machine, Inc. part number RMI-1004-
7,9
measuring subsurface airflow of 185 mL/min in 10.3.1 and
DH has been found suitable for this application. Attach the
10.3.2.
stirrer to the stirrer motor by inserting the 8-mm steel rod
through the opening in the reactor head and the packing gland,
6.11 Vacuum System—A pump with a free air capability of
and insert PTFE rope packing to create a seal. Position the
at least 160 L/min is required to ensure a constant air flow
blade 6 mm from the bottom of the vessel.
across the reaction surface in the vessel of 2.0 6 0.1 SCFM
with 61 kPa vacuum for 40 h. Instructions for constructing the
6.7 Air Supply System—Capable of delivering an uninter-
vacuum plumbing for the vessel are given in Annex A7.As
rupted flow of dry air into the test oil via a subsurface feed
explainedinAnnexA7,itiscriticaltofollowtheseinstructions
throughout the reaction time period. An in-line, desiccant-
precisely.
charged, drying system has been found suitable. Ensure the
6.12 Vacuum Control Valve—A stainless steel needle valve
subsurface feed tube opening remains below the surface of the
with ⁄4-in. outside diameter tube connections and a flow
test fluid for the duration of the test.
coefficient (Cv) of 0.37. A McMaster-Carr Supply Company
NOTE1—Astheamountoftestoilremainingattheendofthetestisnot
7, 11
always known at the beginning of the test, it is advisable to configure the needle valve part number 45585K86 has been found
dry-air tube location such that the opening of the tube is as close to the
suitable for this application.
agitator and as close to the bottom of the reactor as practical (without
6.13 Vacuum Trap System—Supplies coolant at an inlet
contacting the agitator or blocking the tube opening).
temperature < 20 °C to the vacuum trap condensers in order to
6.8 Graduated Tube (Ace Glass, Inc., part number
remove vapors from the effluent prior to entering (and possibly
6,7
D120677), 12-mL capacity, with 0.1 mL graduations and
damaging) the vacuum system and has a means of recovering
having appropriate provisions for connection to the reaction
the distillate for weighing. Redundant (serial) condensers are
vessel’s subsurface gas delivery system—see Annex A6 for
beneficial as long as the required airflow across the reaction
more details. By receiving liquid phase nitrogen dioxide from
surface is maintained. Annex A8 provides information on two
a gas bottle, this tube allows measurement of nitrogen dioxide
systems that have been found to be satisfactory.
depletion from the tube over the course of the reaction.
6.14 Time Controller—Atiming device accurate to 1 min is
6.9 Temperature Control System—A controller and probe
used to deactivate the heat source.
capable of being programmed to control reaction temperature
6.15 Precision Needle Valve—Having a low Cv for precise
via low output wattage at or below 40 VAC and with an
controloftheflowofnitrogendioxide.Examplesofvalvesthat
operational hysteresis of 0.1 °C using an on/off algorithm.
have been found satisfactory are given in Appendix X3.
Alternatively, a proportional-integral-derivative (PID) algo-
rithm may also be used. Position the temperature probe tip so 6.16 Beaker—300-mL capacity.
that it is level with the bottom of the turbine blade with a
6.17 Glass Jar—250-mL capacity which can be sealed.
distance of 8 mm between the probe center and the blade edge.
6.18 Shaker—Use either a reciprocal or an elliptical shaker.
6.9.1 Asthetemperaturemaynotbeuniformthroughoutthe
6.19 Assembled ROBO Apparatus—Fig. X4.1 shows an
...