ASTM D6557-00

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An American National Standard
Designation: D 6557 – 00
Standard Test Method for
Evaluation of Rust Preventive Characteristics of Automotive
Engine Oils
This standard is issued under the fixed designation D 6557; 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.
1. Scope environment that can produce a deterioration of the material
and its properties. (D 5844)
1.1 This test method covers a Ball Rust Test (BRT) proce-
3.1.3 non-reference oil, n—any oil other than a reference
dure for evaluating the antirust ability of fluid lubricants. The
oil, such as a research formulation, commercial oil, or candi-
procedure is particularly suitable for the evaluation of automo-
date oil. (D 5844)
tive engine oils under low-temperature, acidic service condi-
3.1.4 reference oil, n—an oil of known performance char-
tions.
acteristics, used as a basis for comparison. (D 5844)
1.2 Information Letters are published occasionally by the
2 3.1.4.1 Discussion—Reference oils are used to calibrate
ASTM Test Monitoring Center (TMC) to update this test
testing facilities, to compare the performance of other oils, or
method. Copies of these letters can be obtained by writing the
to evaluate other materials (such as seals) that interact with
center.
oils.
1.3 The values stated in either SI units or in other units shall
3.1.5 rust, n—of ferrous alloys, a corrosion product consist-
be regarded separately as standard. The values stated in each
ing primarily of hydrated iron oxides. (D 5844)
system may not be exact equivalents; therefore, use each
3.1.6 test oil, n—any oil subjected to evaluation in an
system independently of the other, without combining values in
established procedure.
any way.
3.2 Definitions of Terms Specific to This Standard:
1.4 This standard does not purport to address all of the
3.2.1 average gray value (AGV), n—measurement of
safety concerns, if any, associated with its use. It is the
brightness units on test specimens, indicating the degree of rust
responsibility of the user of this standard to establish appro-
protection.
priate safety and health practices and determine the applica-
3.2.2 specimen, n—a carbon steel ball, ⁄32 in. (AISI 1040).
bility of regulatory limitations prior to use. See 7.1.1, 7.1.2,
7.1.3, 8.2.1.1, and Table 1.
4. Summary of Test Method
2. Referenced Documents 4.1 Multiple test tubes, each containing test oil and a
specimen, are placed in a test tube rack, which is attached to a
2.1 ASTM Standards:
mechanical shaker. The shaker speed and temperature are
D 5844 Test Method for Evaluation of Automotive Engine
3 controlled.
Oils for Inhibition of Rusting (Sequence IID)
4.2 Air and an acidic solution are continuously fed into each
E 344 Terminology Relating to Thermometry and Hydrom-
4 test tube over an 18 h period to create a corrosive environment.
etry
4.3 The specimens are then removed, rinsed, and analyzed
3. Terminology by an optical imaging system designed to quantify the antirust
capability of each test oil.
3.1 Definitions:
3.1.1 calibrate, v—to determine the indication or output of
5. Significance and Use
a measuring device with respect to that of a standard.
5.1 This bench test method was designed as a replacement
(E 344)
for Test Method D 5844. Test Method D 5844 was designed to
3.1.2 corrosion, n—the chemical or electrochemical reac-
measure the ability of an engine oil to protect valve train
tion between a material, usually a metal surface, and its
components against rusting or corrosion under low tempera-
ture, short-trip service, and was correlated with vehicles in that
This test method is under the jurisdiction of ASTM Committee D02 on type of service prior to 1978.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.B0.01 on Passenger Car Engine Oils.
Current edition approved June 10, 2000. Published August 2000.
2 5
ASTM Test Monitoring Center, 6555 Penn Avenue, Pittsburgh, PA 15206-4489. Special Technical Publication, “Multicylinder Test Sequences for Evaluating
Annual Book of ASTM Standards, Vol 05.03. Automotive Engine Oils, Part, Sequence IIID ASTM STP 315H, Available from
Annual Book of ASTM Standards, Vol 14.03. ASTM Headquarters.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6557–00
FIG. 2 Schematic of Air Delivery System
FIG. 1 Photograph of Air Delivery System
5.1.1 Correlation between these two test methods has been
demonstrated for most, but not all, of the test oils evaluated.
6. Apparatus
6.1 Specimen Preparation System—Obtain the specimens
from the Central Parts Distributor (CPD).
6.1.1 Specimen preparation equipment includes various
FIG. 3 Photograph of Acid Delivery System
common laboratory apparatus and an ultrasonic cleaning bath.
6.2 Air Supply System—A compressed air supply is re-
quired, with two air filters, two pressure regulators, a gas
purifier, a gassing manifold (25 port outlet), TFE-fluorocarbon
tubing (25 600-ft lengths) or equivalent multiport flow control
system, and a gas mass flowmeter (see Annex A1 and Figs. 1
and 2).
6.3 Acid Solution Delivery System—An acid solution deliv-
ery system that includes a multiple syringe pump with a ten
position rack is required. The flow rate range minimum is
0.0001 μL/h (using a 0.5-μL syringe) to a maximum 220.82
mL/min (using a 140-mL syringe) (see Figs. 3 and 4).
FIG. 4 Schematic of Acid Delivery System
6.4 Test Tube Assembly—The test tube assembly consists of
24 disposable plastic syringes and other common laboratory
6.5 Temperature and Shaking Speed Control System—A
apparatus.
mechanical shaker, Bench-Top Environ Shaker Model 4628,
6 7
The sole source of supply of the apparatus known to the committee at this time The sole source of supply of the apparatus known to the committee at this time
th
is Central Parts Distributor, Test Engineering Inc., 12718 Cimmaron Path, San is Labine, Inc., 15 and Bloomingdale, Melrose Park, IL 60160. If you are aware of
Antonio, TX 78249. If you are aware of alternative suppliers, please provide this alternative suppliers, please provide this information to ASTM Headquarters. Your
information to ASTM Headquarters. Your comments will receive careful consider- comments will receive careful consideration at a meeting of the responsible
ation at a meeting of the responsible technical committee, which you may attend. technical committee, which you may attend.
D6557–00
FIG. 6 Photograph of Test Tube Assembly Rack
FIG. 5 Test Tube Assembly Rack
provides an orbital shaking motion in a controlled speed and
temperature environment.
6.5.1 A special test tube assembly rack (see Figs. 5 and 6)
has 24 tube positions and is attached to the shaker platform (18
in. by 18 in.).
6.6 Gassing Manifold, required.
6.7 Venting System—Common laboratory apparatus is em-
ployed for the required venting system (see Fig. 7).
6.8 Image Analysis System—A specific imaging analysis
system is required. This system is composed of:
6.8.1 Optics and Illumination:
6.8.1.1 Nikon Epiphot 200 inverted metallurgical micro-
FIG. 7 Gassing Manifold for Venting
scope,
6.8.1.2 BZ binocular head,
6.8.1.13 Lamphouse adapter,
6.8.1.3 RV 3 plate mechanical stage,
6.8.1.14 12 V/100 W halogen bulbs,
6.8.1.4 CFWN 103 wide field eyepiece, high point eye-
6.8.1.15 300/200 100 W power supply.
piece,
6.8.1.16 Remote control cable,
6.8.1.5 Manual BD 5 place nosepiece,
6.8.1.17 C-mount coupler for video camera,
6.8.1.6 Epiphot 300 EB block,
6.8.1.18 NCB 11 filter,
6.8.1.7 DF module,
6.8.1.19 Power cords, and
6.8.1.8 CF BD plan 53/0.13 plan achromat objective,
6.8.1.20 Ultracentrifuge tube spacer with a 5-mm hole
6.8.1.9 CF BD plan 103/0.13 plan achromat objective,
drilled in the center (used as a sample holder and sample
6.8.1.10 EPI polarizer,
randomizer for sample orientation).
6.8.1.11 Analyzer,
6.8.2 Image Capture Hardware and Software:
6.8.1.12 Lamphouse for 12 V/100 W quartz halogen light
6.8.2.1 Research grade, high resolution, NTSC RGB/RS-
source,
170 camera system,
6.8.2.2 Research grade, high resolution, NTSC RGB/RS-
170 frame grabber,
The sole source of supply of the apparatus known to the committee at this time
6.8.2.3 The host computer system (shall meet or exceed the
is West End Machine and Weld, Inc., P.O. Box 9444, Richmond, VA 23228. If you
following specifications):
are aware of alternative suppliers, please provide this information to ASTM
(a) Hardware—Pentium 133 MHz CPU, 16 MB RAM, 540
Headquarters. Your comments will receive careful consideration at a meeting of the
MB hard drive, 1.44 MB 3.5-in. floppy, 1.44 MB 5.25-in.
responsible technical committee, which you may attend.
The sole source of supply of the apparatus known to the committee at this time
floppy (optional), CD-ROM (highly recommended option),
is Meyer Instruments, Inc., 1304 Langham Creek, Suite 235, Houston, TX 77084.
101 or Windows 95 keyboard, SVGA local bus video card with
If you are aware of alternative suppliers, please provide this information to ASTM
2 MB RAM (4 MB recommended), 2 button serial mouse with
Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. pad, 2 parallel ports, and 2 serial ports.
D6557–00
TABLE 1 Organic Solvent
8.1.3 Rinse two more times with heptane and follow with an
Composition acetone (Warning—see 7.1.2) rinse to ensure the specimens
A
are free of contamination. Dry the specimens with nitrogen for
Ethyl acetate, 99.5+ % (37.5 % vol)
B
Denatured ethyl alcohol (27.5 % vol)
3 min.
C
Butanol, 99 % (5.0 % vol)
C
Tetrahydrofuran (THF), 99+ % (30.0 % vol) NOTE 2—The specimens can be prepared up to one week in advance
A and stored in heptane until needed for testing.
Warning—See the appropriate Materials Safety Data Sheet.
B
Warning—Flammable. Cannot be made nontoxic. Health hazard.
C
8.2 Test Tube Assembly, Tube Rack, and Shaker for Each
Warning—Flammable. Health hazard.
Test Tube:
8.2.1 Cut 24 separate pieces of TFE-fluorocarbon FEP
(b) Software—Windows 3.x/DOS 6.22 or Windows 95 tubing, each piece to be 9.5-in. (24-cm) long.
Operating System, Microsoft Excel 7.0 (Microsoft Office 97 8.2.1.1 Use compressed air (Warning—For technical use
recommended). only.), 50 psig minimum, to remove most of the water/oil
(c) Monitor—Medical grade high-resolution 19-in. NTSC emulsion that may be trapped inside the short lengths of
capillary tubing. Clean the tubing with heptane (Warning—
RGB color video monitor, all necessary cables, connectors, and
adapters (including a surge and spike suppressing power strip). see 7.1.3), followed by acetone (Warning—see 7.1.2), and dry
with compressed air.
6.8.3 BRT Image Analysis Software:
6.8.3.1 BRT macro program, and 8.2.2 Check the flangeless fitting for ⁄16-in. O.D. TFE-
fluorocarbon tubing for deterioration, and replace as necessary.
6.8.3.2 Optimate image analysis engine.
8.2.3 Remove and discard the plunger from a new 20-mL
7. Reagents and Materials disposable plastic syringe (Luer-Lok), and securely fasten the
syringe barrel to the short capillary tubing, using couplings,
7.1 Reagents:
1 1
⁄4-28 thread, and female Luer CTFE fittings, ⁄4-28 thread, and
7.1.1 Acid Solution (Warning—Corrosive. Combustible.
with a 1.5-mm bore.
Health Hazard.)—Obtain the acid solution from the CPD.
8.2.3.1 Label the syringes (test tubes) from 1 to 24.
NOTE 1—For information only. Appendix X1 contains details of the
8.2.4 Place the assembled test tube in the tube rack with the
acid solution.
capillary tubing facing upward in the adjacent small hole.
7.1.2 Acetone, 99.5 %. (Warning—Flammable. Health
8.2.4.1 The test tube assembly rack is a specially designed
Hazard.)
aluminum fabrication. It holds 24 test tubes with easy snap-on
7.1.3 n-Heptane, 38 to 42 % (purity), commercial grade,
lock, wing nuts, and hold-down bars (see Fig. 5).
with C isomers. (Warning—Flammable. Health Hazard.)
7 8.2.5 Place one precleaned specimen into each test tube,
7.1.4 Organic Solvent—blend as shown in Table 1:
using extra-long forceps (7 in. with serrated tips) to avoid
7.2 Materials:
contamination.
1 1
7.2.1 TFE-fluorocarbon FEP Tubing, ⁄32-in. I.D. by ⁄16-in.
8.2.6 Insert 10 mL of test oil into each test tube, using a
outside diameter (O.D.); 17 rolls of 1000 ft/roll. (Not required
10-mL disposable syringe.
if the optional NRS flow controller is used.)
8.2.7 Secure the test tubes to the tube holder with three
1 1
7.2.2 Vinyl Tubing, ⁄8 in.-inside diameter (I.D.) by ⁄4
hold-down bars and three wing nuts.
in.-O.D.; about 15 ft.
8.2.8 Fasten the test tube assembly rack to the shaker
7.2.3 Miscellaneous Common Laboratory Equipment, in-
platform with four custom-made wing bolts.
cluding glassware, tubing fittings, trays, vials, and plastic
8.3 Acid Delivery System:
syringes.
8.3.1 Withdraw 6 mL of acid solution by hand from a
wide-mouth beaker into an individual 5-mL disposable plastic
8. Preparation of Apparatus
syringe (Luer-Lok).
8.1 Specimens: 8.3.1.1 Attach the syringe to an acid inlet port of one of the
8.1.1 Remove the appropriate number of specimens from 24 three-way switching valves, with ⁄4-28 thread. (The other
vacuum-sealed packages, into a 4-oz bottle (clear, medium- two ports are used for air inlet and mixed air/acid outlet.)
round with cap). Add sufficient heptane (Warning—see 7.1.3), 8.3.2 Turn the three-way valve to two-way open and eject,
approximately 2 oz, to cover the specimens. by hand, about 0.5 mL of acid solution into a waste beaker,
8.1.2 Cap the bottle loosely and place it in an ultrasonic
while ensuring that no air bubbles remain in the syringe.
cleaning bath. Sonicate for 30 min, and then decant the 8.3.2.1 Place the syringe that now contains about 5.5 mL of
heptane.
acid solution on the holder of the multiple syringes pump.
8.3.3 Repeat the above procedure for the other 23 acid
delivery syringes.
10 8.3.4 There are three multiple syringe pumps, and eight of
Brooks Model 8744 NRS Flow Controller has been determined to be
the 5-mL syringes are attached to each of the pumps.
acceptable for this application. The sole source of supply of the apparatus known to
the committee at this time is McPac Process Automation and Control, 8040 Bavaria
8.3.4.1 The pumps each have a ten-position rack and are
Rd., Twinsburg, OH 44087. If you are aware of alternative suppliers, please provide
required to satisfy a flow rate range of 0.0001 μL/h, minimum,
this
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