NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.

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An American National Standard

Designation: D 6557 – 00

Standard Test Method for

Evaluation of Rust Preventive Characteristics of Automotive
Engine Oils1
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

1.1 This test method covers a Ball Rust Test (BRT) proce- and its properties. (D 5844)
dure for evaluating the antirust ability of fluid lubricants. The 3.1.3 non-reference oil, n—any oil other than a reference
procedure is particularly suitable for the evaluation of automo- oil, such as a research formulation, commercial oil, or candi-
tive engine oils under low-temperature, acidic service condi- date oil. (D 5844)
tions. 3.1.4 reference oil, n—an oil of known performance char-
1.2 Information Letters are published occasionally by the acteristics, used as a basis for comparison. (D 5844)
ASTM Test Monitoring Center (TMC)2 to update this test 3.1.4.1 Discussion—Reference oils are used to calibrate
method. Copies of these letters can be obtained by writing the testing facilities, to compare the performance of other oils, or
center. to evaluate other materials (such as seals) that interact with
1.3 The values stated in either SI units or in other units shall oils.
be regarded separately as standard. The values stated in each 3.1.5 rust, n—of ferrous alloys, a corrosion product consist-
system may not be exact equivalents; therefore, use each ing primarily of hydrated iron oxides. (D 5844)
system independently of the other, without combining values in 3.1.6 test oil, n—any oil subjected to evaluation in an
any way. established procedure.
1.4 This standard does not purport to address all of the 3.2 Definitions of Terms Specific to This Standard:
safety concerns, if any, associated with its use. It is the 3.2.1 average gray value (AGV), n—measurement of
responsibility of the user of this standard to establish appro- brightness units on test specimens, indicating the degree of rust
priate safety and health practices and determine the applica- protection.
bility of regulatory limitations prior to use. See 7.1.1, 7.1.2, 3.2.2 specimen, n—a carbon steel ball, 7⁄32 in. (AISI 1040).
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
2.1 ASTM Standards: specimen, are placed in a test tube rack, which is attached to a
D 5844 Test Method for Evaluation of Automotive Engine mechanical shaker. The shaker speed and temperature are
Oils for Inhibition of Rusting (Sequence IID)3 controlled.
E 344 Terminology Relating to Thermometry and Hydrom- 4.2 Air and an acidic solution are continuously fed into each
etry4 test tube over an 18 h period to create a corrosive environment.
4.3 The specimens are then removed, rinsed, and analyzed
3. Terminology by an optical imaging system designed to quantify the antirust
3.1 Definitions: capability of each test oil.
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.
(E 344) 5.1 This bench test method was designed as a replacement
3.1.2 corrosion, n—the chemical or electrochemical reac- for Test Method D 5844. Test Method D 5844 was designed to
tion between a material, usually a metal surface, and its measure the ability of an engine oil to protect valve train
components against rusting or corrosion under low tempera-
ture, short-trip service, and was correlated with vehicles in that
1
This test method is under the jurisdiction of ASTM Committee D02 on type of service prior to 1978.5
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
3
Annual Book of ASTM Standards, Vol 05.03. Automotive Engine Oils, Part, Sequence IIID ASTM STP 315H, Available from
4
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.

1
 D 6557 – 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
6.1.1 Specimen preparation equipment includes various
common laboratory apparatus and an ultrasonic cleaning bath. FIG. 3 Photograph of Acid Delivery System
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
apparatus. 6.5 Temperature and Shaking Speed Control System—A
mechanical shaker, Bench-Top Environ Shaker Model 4628,7

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
is Central Parts Distributor, Test Engineering Inc., 12718 Cimmaron Path, San is Labine, Inc., 15th 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.

2
 D 6557 – 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 rack8 (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
system9 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,
8
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
Headquarters. Your comments will receive careful consideration at a meeting of the (a) Hardware—Pentium 133 MHz CPU, 16 MB RAM, 540
responsible technical committee, which you may attend. MB hard drive, 1.44 MB 3.5-in. floppy, 1.44 MB 5.25-in.
9
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.
If you are aware of alternative suppliers, please provide this information to ASTM
101 or Windows 95 keyboard, SVGA local bus video card with
Headquarters. Your comments will receive careful consideration at a meeting of the 2 MB RAM (4 MB recommended), 2 button serial mouse with
responsible technical committee, which you may attend. pad, 2 parallel ports, and 2 serial ports.

3
 D 6557 – 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
Ethyl acetate,A 99.5+ % (37.5 % vol) are free of contamination. Dry the specimens with nitrogen for
Denatured ethyl alcoholB (27.5 % vol) 3 min.
Butanol,C 99 % (5.0 % vol)
Tetrahydrofuran (THF),C 99+ % (30.0 % vol) NOTE 2—The specimens can be prepared up to one week in advance
A
Warning—See the appropriate Materials Safety Data Sheet. and stored in heptane until needed for testing.
B
Warning—Flammable. Cannot be made nontoxic. Health hazard.
C
Warning—Flammable. Health hazard. 8.2 Test Tube Assembly, Tube Rack, and Shaker for Each
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
RGB color video monitor, all necessary cables, connectors, and capillary tubing. Clean the tubing with heptane (Warning—
adapters (including a surge and spike suppressing power strip). see 7.1.3), followed by acetone (Warning—see 7.1.2), and dry
6.8.3 BRT Image Analysis Software: with compressed air.
6.8.3.1 BRT macro program, and 8.2.2 Check the flangeless fitting for 1⁄16-in. O.D. TFE-
6.8.3.2 Optimate image analysis engine. fluorocarbon tubing for deterioration, and replace as necessary.
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
7.1 Reagents: syringe barrel to the short capillary tubing, using couplings,
1⁄4-28 thread, and female Luer CTFE fittings, 1⁄4-28 thread, and
7.1.1 Acid Solution (Warning—Corrosive. Combustible.
Health Hazard.)—Obtain the acid solution from the CPD. with a 1.5-mm bore.
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 C7 isomers. (Warning—Flammable. Health Hazard.) 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.
7.2.1 TFE-fluorocarbon FEP Tubing, 1⁄32-in. I.D. by 1⁄16-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 controller10 is used.) 8.2.7 Secure the test tubes to the tube holder with three
7.2.2 Vinyl Tubing, 1⁄8 in.-inside diameter (I.D.) by 1⁄4 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 1⁄4-28 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
Brooks Model 8744 NRS Flow Controller has been determined to be 8.3.4 There are three multiple syringe pumps, and eight of
acceptable for this application. The sole source of supply of the apparatus known to the 5-mL syringes are attached to each of the pumps.
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 information to ASTM Headquarters. Your comments will receive careful
consideration at a meeting of the responsible technical committee, which you may to 220.82 mL/min, maximum. Required accuracy is 6 1 %,
attend. and reproducibility is 6 0.1 %.

4
 D 6557 – 00
8.3.5 Ensure that the syringe barrel flange and the plunger 9. Procedure
flange are firmly held by the retaining clamps (six 2-in. 9.1 Turn the three-way valve to two-way open, activate the
C-clamps that secure the ends of the hold-down bars of the syringe pumps, and eject 1 mL of acid solution into a waste
multiple syringes pump). beaker at 0.1-mL/min speed.
8.3.5.1 Good alignment of all 24 acid delivery syringes 9.1.1 Make sure that the retaining brackets properly align all
against the retaining brackets is crucial to ensure repeatability. 24 syringe plungers.
(See Fig. 3 for a photograph of the acid delivery system, and 9.2 Adjust the acid solution flow rate to 0.193 mL/h (test
Fig. 4 for a schematic.) flow rate), and run for 1 h to ensure that all syringe plungers are
8.3.6 Cut 24 pieces of TFE-fluorocarbon tubing; each piece properly aligned at the retaining brackets of the pusher block.
to be 51 6 1 in. in length. 9.3 Set the actual air flow rate to 40 mL/min.
8.3.6.1 Attach each of these tubes to the mixed air/acid 9.3.1 Monitor the airflow rate with the digital mass flow
outlet ports of the three-way switching valves. meter connected to the reference air capillary tubing. Refer to
8.4 Air Delivery System: the calibration chart developed in Annex A1 to determine the
8.4.1 Clean, dry air, compressed to at least 50 psig, is actual air flow rate setting.
required. 9.4 Turn the three-way valves to the three-way open posi-
8.4.2 A single stage, high-purity stainless steel pressure tion, and dry the nominal 51-in. lengths of capillary tubing with
regulator is the first in the line; this is equipped with a 0 to air for 30 min.
160-psi maximum pressure gage. 9.5 Measure and record the airflow rates of all lines, and
8.4.3 Two compressed air filters capable of removing par- then shut off the main airflow valve.
ticles and mists are required, and are next in the line. 9.6 Connect the long capillary tubing (that is, the nominal
51-in. lengths) to the short capillary tubing from the test tubes.
8.4.3.1 The first filter in the line is an A912-DX type,
followed by an A912-BX type. These have polycarbonate 9.7 Connect all 24 stopper vent lines to the top of the test
bowls and should be equipped with aluminum shields. They tubes.
have 1⁄4-in. NPT (F) ports and will withstand 150-psig pressure 9.7.1 TFE-fluorocarbon thermometer adapters are used as
maximum. stoppers, 19⁄22 joint.
9.7.2 Attach the vent lines to barbed tee connectors (clear
NOTE 3—Alternatively, zero grade air cylinders can be used and will polypropylene, for 1⁄8-in. I.D. tubing).
not require the extensive filtering outlined above. 9.7.3 Then, connect the vent outlets to a gassing manifold (8
8.4.4 A Drierite gas purifier, with a maximum working port inlet with 1⁄4-in. hose barb; use vinyl tubing, 1⁄8-in. I.D. by
1⁄4-in. O.D. (see Fig. 7).
pressure of 100 psig, is next in the line.
8.4.4.1 The first portion of the purifier (about 75 %) con- 9.7.4 Finally, connect the gassing manifold’s outlet to a
tains a molecular sieve, activated, Type 4A, 8 to 12 mesh. condensate trap flask, with side arm (1000 mL), placed such
8.4.4.2 The remaining portion of the purifier (about 25 %) that gravity drains the condensate from the test tubes. Make
contains Drierite absorbent, color indicating type, 8 mesh. sure that all of the capillary tubes are free to move with the
shaker platform.
8.4.5 Next in the line is the downstream regulator, single
9.8 Set the shaker temperature to maintain 48 6 0.1°C, as
stage high-purity stainless steel, which is equipped with a 0 to
measured in an actual oil sample, and warm up the entire
60-psi pressure gage.
system to the control temperature in the oil sample. Refer to the
8.4.6 The next installation is a relief valve, in-line adjust- calibration chart developed in Annex A2 to determine the
able CA series, 50 to 150-psi cracking pressure range, set at 80 shaker temperature setting.
psi (optional to control over pressure). 9.9 Following the warm-up period, turn on the shaker, set
8.4.7 Lastly, a gassing manifold with 25 port outlets and the shaker speed to 300 r/min, and ensure that each ball freely
1⁄4-in. tube fittings is installed. (See Figs. 5 and 6 for a
rotates against each syringe wall.
schematic and photograph of the air system.) 9.10 Start introducing the acid solution at an actual flow rate
8.4.8 Cut 25 pieces of the TFE-fluorocarbon tubing, each of 0.193 mL/h. Refer to the calibration chart developed in
piece to be approximately 600 ft in length. Annex A3 to determine the actual flow rate setting.
8.4.8.1 These long tubes provide the necessary backpressure 9.11 Check and adjust, if necessary, the upstream pressure
to allow good control of the very low airflow rate. The (that is, upstream from the three-way valves) to ensure that the
individual lengths may need to be adjusted slightly to ensure actual air flow rate is 40 mL/min.
the same flow rates at a given delivery pressure. An equivalent 9.12 Maintain the above test conditions for 18 h.
multiport flow control system can be used.10 9.13 At the end of the test, stop the syringe pumps, shut off
8.4.8.2 Connect these tubes to the gassing manifold. the airflow, and turn off the shaker.
(a) One of these tubes is then connected to a gas mass 9.14 Disconnect the acid/air delivery tubes from the test
flowmeter, capable of measuring up to 200 mL/min, and with tube assembly, and remove the stoppers from the test tubes.
0.1-mL/min resolution (see Annex A1). NOTE 4—The preceding procedure described the use of three multiple
(b) The other 24 tubes are then connected to the air inlet syringe pumps and 24 test tubes. However, as a minimum, one multiple
ports on the 24 three-way valves. syringe pump with a maximum of 10 test tubes can also be utilized.

5
 D 6557 – 00
10. Reference Oil Testing 10.6.1 If the test is determined to be operationally valid, the
10.1 Procure a supply of reference oils directly from the test results will then be evaluated, using statistical acceptance
TMC. criteria established by the governing surveillance panel.
10.1.1 These oils have been formulated or selected to 10.6.1.1 The acceptance criteria are subject to change at the
represent specific chemistry types or performance levels, or discretion of the surveillance panel.
both. Each reference oil is identified with a unique identifica- 10.6.2 If the initial transmitted data is determined to be both
tion code on the container label. operationally valid and statistically acceptable, the TMC will
10.2 Request a reference oil assignment from the TMC. so notify the testing laboratory.
Assignments will be made by the unique identifying codes on 10.6.2.1 The TMC will also disclose the uncoded reference
the reference oil samples. oil identification to the testing laboratory.
10.2.1 Provide the TMC with the bath identification for the 10.6.2.2 The TMC’s first determinations are considered
test. preliminary until the formally signed final report is received
10.3 Test the assigned reference oil along with each batch of and reviewed by the TMC. Discrepancies between the initial
non-reference oil tests, simultaneously with and in the same transmitted data and the mailed final report may result in
bath as the non-reference oils. reversal of the preliminary determinations.
10.3.1 Run the reference oil test in accordance with the 10.7 In the event that a reference test is determined unac-
same procedure used for the non-reference oil tests. ceptable by the TMC, the TMC will provide an explanation to
10.3.2 Inclusion of this coded (that is, blind) reference oil the testing laboratory.
helps protect against the possibility of bias in the testing. 10.7.1 If there is an obvious operational problem for the
unacceptable test results, the problem has to be corrected
NOTE 5—Annex A4 discusses the involvement of the TMC with respect before requesting another reference oil assignment from the
to the reference oil-monitoring program. TMC.
10.4 The testing laboratory tacitly agrees to use the refer- 10.7.2 If the reason for the unacceptable results is not
ence oils in accordance with Policies for Use and Analysis of obvious, all test-related equipment shall be rechecked for
ASTM Reference Oils,11 and to run and report the reference oil compliance with the procedure and good laboratory practice.
test results in accordance with TMC guidelines. 10.7.3 Following this rechecking process, the TMC will
10.5 Report the reference oil test results to the TMC in assign another coded reference oil for testing.
accordance with the following guidelines: 10.8 The batch of non-reference oil tests, which accompany
10.5.1 Use the data reporting formats detailed in Annex A5 the coded reference oil test, is considered valid only if the
(see Figs. A5.1 through A5.4) for reporting all reference oil test results of the reference oil test meet the predetermined accep-
results to the TMC. tance criteria for the particular reference oil tested.
10.5.2 Do not include any non-reference oil test results. 11. Test Results
10.5.3 Complete all of the required blank fields on the
forms. 11.1 Prepare Specimens for Image Analysis:
10.5.4 Transmit reference oil test data by electronic means 11.1.1 Remove the specimens from the test tubes, using
or by telephone facsimile to the TMC immediately upon extra-long forceps (7 in. with serrated tips).
completion of the test analysis. 11.1.2 Swirl each specimen in a 400-mL beaker containing
10.5.4.1 Include all of the reporting forms in the transmis- heptane (Warning—see 7.1.3) to remove most of the adsorbed
sion. oil layer.
11.1.3 Place each specimen into a separate 20-mL scintilla-
NOTE 6—Specific protocols for the electronic transmission of test data tion wash vial (make one perforation in the bottom to facilitate
are available from the TMC. cleaning) in a vial holder.
10.5.5 In addition to the previously transmitted data, send 11.1.4 Put the vial holder into a utility tray (stainless steel,
by mail or other courier one copy of the final reference oil test 121⁄4 by 73⁄4 by 21⁄4 in.), pour enough heptane into the tray to
report to the TMC. cover the specimens, and shake the tray gently for 2 min before
10.5.5.1 The signatory line on the mailed Final Report decanting the heptane.
Cover Sheet (see Fig. A5.1) requires an original signature by an 11.1.5 Put enough organic solvent (see 7.1.4) (Warning—
authorized representative of the testing laboratory. The signa- See Table 1, Footnotes A through C.) into the tray to cover the
ture affirms the statements made in the affidavit on the Final specimens, and soak the specimens for 10 min, to remove any
Report Cover Sheet. remaining organic deposits, before decanting the solvent.
10.5.5.2 Mail the final test report so that it is received by the 11.1.6 Put enough heptane into the tray to cover the speci-
TMC within 30 days from the test completion date. mens, and shake the tray gently for 2 min before decanting the
10.6 Upon receipt of the initial reference oil test results, the heptane.
TMC will review the data for operational adherence to the 11.1.7 Transfer the specimens into clean, dry 20-mL scin-
published procedure. tillation vials that have been previously labeled the same as the
test tubes in 8.2.3.1.
11.1.8 Dry the specimens with nitrogen gas, and then
securely fasten the vial caps.
11
Available from the TMC. 11.2 Prepare Image Analysis System for Rust Evaluation:

6
 D 6557 – 00
11.2.1 Set the microscope adjustments as follows:
11.2.1.1 Illumination change-over knob B/D—D (dark
field).
11.2.1.2 ND16 filter slider—IN (push to first click).
11.2.1.3 A filter slider—IN (push to second click).
11.2.1.4 F (field diaphragm control lever)—OPEN.
11.2.1.5 A (aperture diaphragm control lever)—OPEN.
11.2.1.6 Neutral density filter—ND16.
11.2.1.7 Objective lens—53.
11.3 Optronics Controller:
11.3.1 Shutter speed—1⁄60 + (manual).
11.3.2 White balance—ON.
11.4 Turn on the Image Analysis Computer and initiate the
Optimate software program.
11.5 Select the macro titled BRT51.MAC (BRT Macro
Version 5.1, or later).
11.6 Rust Rating Procedure: FIG. 8 Microscope, Stage, and Computer
11.6.1 Wipe each specimen, using a lint-free laboratory
wipe; remove all solvent film and loose surface deposits from
the rating surfaces prior to the digital image rating. 12.1.1 Intermediate Precision (formerly called
11.6.2 Place the Calibration Reference Specimen onto the repeatability)—The difference between two results obtained
microscope stage, and follow the dialog box instructions that with the same oil, using the same test method, in the same
appear on the screen (operator interface) (see Fig. 8). laboratory, using the same apparatus (different test tubes),
would, in the normal and the correct operation of the test
NOTE 7—Refer to the software manual for the detailed procedure of
imaging analysis. method, exceed the following value in only one case in twenty:
15.15 AGV
11.6.2.1 Answer the operator interface questions to allow
12.1.2 Reproducibility—The difference between two single
automatic recording of the data into the spreadsheet program.
and independent test results obtained with the same oil in
11.6.3 Rotate (without skin contact) the Calibration Refer-
different laboratories would, in the normal and the correct
ence Specimen, and take 20 different readings.
operation of the test method, exceed the following value in
11.6.4 Repeat the previous step for each specimen. (The
only one case in twenty:
Calibration Reference Specimen is the first and last specimen
18.89 AGV
analyzed to ensure no drift has occurred during analysis.)
12.2 Bias—No bias is believed to exist. However, this
11.6.5 Print the spreadsheet program results.
aspect of the test will be reevaluated after the test method has
12. Precision and Bias been in use by several laboratories over an appropriate period
of time.
12.1 Precision:12
13. Keywords
12
See RR:D02-1483 for details. Available from ASTM Headquarters. 13.1 Ball Rust Test; corrosion; engine oil; rust

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ANNEXES

(Mandatory Information)

A1. DIGITAL AIR FLOWMETER CALIBRATION

A1.1 Connect the reference air line to the digital gas water, and secure the cylinder in an inverted position to a stand.
flowmeter inlet port, and attach capillary tubing from the Make sure the cylinder is perpendicular to the water level.
flowmeter outlet to a calibrated bubble meter. A1.6.1 Attach capillary tubing from the top of the cylinder,
A1.2 Calculate the actual air flow rate for the digital and place the tubing outlet into the partially filled beaker.
flowmeter by using the following formula: A1.7 Adjust the pressure gage valve to set the digital
100 mL indicator at 30.0 mL/min. Allow 5 min to ensure that the
air flow rate ~mL/min! 5 time ~min! (A1.1)
airflow has stabilized.
A1.3 Repeat A1.2 for digital indicator readings of 35.0, A1.8 Remove the capillary air line from the beaker, and
40.0, 45.0, and 50.0 mL/min. attach it to the bottom valve of the inverted volumetric
cylinder.
A1.4 Plot the calibration curve of digital airflow set point
versus actual airflow rate to provide an airflow correction chart. A1.9 Measure the minutes required to displace 100 mL of
water from the cylinder.
A1.5 Alternatively, connect the reference air line to the
digital gas flowmeter inlet port, and attach capillary tubing A1.10 Record the set pressure, digital air flowmeter read-
from the flowmeter outlet to a large (1 L or larger) open beaker, ing, and displacement time.
partially filled with water.
A1.11 Repeat directions provided in A1.2-A1.4 to calculate
A1.6 Fill a 100-mL volumetric cylinder with deionized the actual airflow rate for the digital flowmeter.

A2. SHAKER TEMPERATURE CALIBRATION

A2.1 Insert 10 mL of a representative oil sample into a A2.4 Adjust the shaker temperature control to 40°C.
20-mL plastic syringe, as part of a test tube assembly, and place Record the actual temperature from the calibrated digital
the assembly in the test tube rack at rack location No. 10 thermometer every 30 min for 4 h.
(second row from the vent line manifold and fourth slot from
the left). A2.5 Repeat A2.2-A2.4 for shaker temperature set points of
50°C and 60°C.
A2.2 Immerse a calibrated digital thermometer into the oil
sample without blocking the air inlet port that is left open. A2.6 Plot the calibration curve of shaker set point tempera-
ture versus actual temperature to provide a temperature control
A2.3 Introduce 40 cm3/min of air to circulate the oil. correction chart.

A3. MULTIPLE SYRINGE PUMP LIQUID FLOW CALIBRATION

A3.1 Determine the density of the acid solution, in g/mL. It hand, and attach the syringes to the acid inlet ports of the
is convenient to weigh the 1 L of solution after it has been three-way valves.
prepared (see 7.1.8.2). Use a calibrated balance to obtain the
A3.3.1 Turn the three-way valves to the two-way open
weight of the 1 L of solution, and subtract the weight of the
position, and withdraw by hand about 0.5 mL of solution from
empty flask to obtain the actual weight of the solution. (Or, use
each syringe into a waste beaker while ensuring that no air
a calibrated density meter.)
bubbles remain in the syringes.
A3.2 Weigh 24 of the 20-mL scintillation vials (labeled 1 to
24) individually on a calibrated balance. A3.4 Place the individual syringes, which now contain 5.5
mL of solution, on the holder of the multiple syringe pumps
A3.3 Withdraw 6 mL of acid solution from a wide-mouth (consists of three separate pumps with eight syringes operated
beaker into each of the twenty-four 5-mL plastic syringes by by each pump).

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A3.4.1 Press the retaining brackets firmly against the sy- A3.8 Start the pump, and also start a calibrated clock for 18
ringe barrel flange and the plunger flange and tighten the h.
retaining screws. A good alignment of all 24 syringes against A3.8.1 At the end of 18 h, stop the pump and remove the
the retaining brackets is crucial for good calibration. parafilm and capillary lines.
A3.5 Activate the multiple syringe pumps and withdraw 1 A3.9 Reweigh the vials, and calculate the weight gain for
mL of solution from each of the 24 plastic syringes into a waste each vial. Total the weight gains for each bank of the
beaker for 2 min at 0.5 mL/min. During this 2 min of pump appropriate eight vials to obtain the weight gain for an
operation, make sure that all 24 syringe plungers are well individual pump.
seated in the retaining brackets.
A3.10 Calculate the actual pump flow rate for the indi-
A3.6 Reduce the pump speed to 0.150 mL/h, and operate
vidual three pumps by using the following formula:
for 1 h. Ensure that all syringe plungers are properly aligned at
the retaining brackets of the pusher block. weight gain ~g!
flow rate ~mL/h! 5 density ~g/mL! 3 time ~h! (A3.1)
A3.6.1 Stop the pump, and ensure that no air bubbles
remain in the capillary lines. A3.11 Repeat A3.3-A3.10 for pump flow rate set points of
0.20 and 0.25 mL/h.
A3.7 Place filled capillary lines into corresponding 20-mL
vials. A3.12 For each pump, plot the calibration curve of set flow
A3.7.1 Seal the vial opening with parafilm to avoid any rate versus actual flow rate to provide a pump flow correction
evaporation of the acid solution during the calibration. chart.

A4. THE ROLE OF THE ASTM TEST MONITORING CENTER (TMC)

A4.1 The TMC is a nonprofit organization located in A4.7.2 It is the laboratories’ responsibility to maintain the
Pittsburgh, PA. calibration of the test method, and to keep on-site reference oil
inventory at or above the minimum level specified by the
A4.2 Operation—The TMC operates in accordance with the TMC.
Rules and Regulations Governing the ASTM Test Monitoring
System, which was developed and approved by Subcommittee A4.8 New Laboratories—New laboratories desiring to par-
D02.B0, and subsequently, approved by Committee D02. ticipate in the ASTM Test Monitoring System should contact
the TMC Administrator. Information concerning fees, labora-
A4.3 Management—The management of the ASTM Test
tory inspections, testing practices, appropriate surveillance
Monitoring System is vested in the Test Monitoring Board
panel membership, and rater training will be provided.
(TMB) elected by Subcommittee D02.B0. The TMB, in turn,
selects the TMC Administrator who is responsible for directing A4.8.1 Initially, a new laboratory will be requested to
the activities at the TMC. conduct reference oil tests to ensure that the laboratory is using
the proper testing techniques.
A4.4 Duties—The TMC is staffed to administer technical
studies, conduct laboratory visits, perform statistical analyses A4.9 New Reference Oils—When new reference oils are
of reference oil test data, provide reference oils to test introduced, participating laboratories will be requested to run
laboratories, and maintain the calibration programs for various and donate the tests necessary to develop performance targets
test methods as directed by the TMB. and precision, and performance acceptance limits.
A4.9.1 The appropriate surveillance panel with TMC input
A4.5 Coordination—The TMC coordinates its activities
will design the test program for prospective new reference oils.
among the test sponsors, test developers, surveillance panels,
and testing laboratories.
A4.10 Information Letters—Occasionally, it may become
A4.6 Income—The TMC’s operating income is obtained necessary to change a test method, and notify participating
from fees levied on the reference oils supplied to the test laboratories of the change, prior to approval of the change by
laboratories and on the calibration tests conducted. Subcommittee D02.B0. In such a case, the TMC will issue an
Information Letter.
A4.7 Laboratory Participation—For those laboratories A4.10.1 Normally, prior to each Subcommittee D02.B0
choosing to utilize the services of the TMC in maintaining the meeting held in conjunction with the semiannual Committee
calibration of a monitored ASTM test method, calibration D02 meeting, the accumulated information letters are balloted
testing is required at regular intervals as determined by the by Subcommittee D02.B0.
responsible surveillance panel. A4.10.2 Subsequently, test methods that are affected by
A4.7.1 These calibration tests are conducted using coded changes in Information Letters are revised accordingly, bal-
reference oils as outlined in Section 10 of this test method. loted in Committee D02, and finally approved by ASTM.

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 D 6557 – 00
A4.10.3 By these actions, ASTM due process procedures A4.10.5 Information letters issued subsequent to the issue
are applied to the TMC Information Letters. date of this test method update the test method and should be
A4.10.4 The ASTM Committee on Technical Committee obtained from the TMC.
Operations (COTCO) in 1984 gave authority for the issuance
of information letters, as follows: “COTCO recognizes that A4.11 Memoranda—The TMC may also issue memoranda
D02 has a unique and complex situation. The use of Informa- to convey information, such as clarification of the test proce-
tion Letters is approved providing each letter contains a dure and approval for alternative test parts or materials or for
disclaimer to the effect that such has not obtained ASTM any other matters having no affect on test performance, results,
consensus. These Information Letters should be moved to such precision, and bias.
consensus as rapidly as possible.”

A5. REPORT FORMAT AND DATA DICTIONARY

A5.1 Use the standardized report form package detailed in transmission as defined by the Data Communications Commit-
A5.2 to report all test results for both reference and non- tee (see Figs. A5.1-A5.4).
reference oils.
A5.2.1 The test report variable data dictionary (see Fig.
A5.2 Test Report Forms with Data Dictionary Variable A5.4) contains all of the field names used in the A5.2 report
Mnemonics—The following report forms contain field names form package.
for all reported variables. Use these variables in electronic data

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 D 6557 – 00

FIG. A5.1 Final Report Cover Sheet

11
12
D 6557 – 00

FIG. A5.2 Summary of Results

 D 6557 – 00

FIG. A5.3 Comments

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FIG. A5.4 Data Dictionary

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 D 6557 – 00

FIG. A5.4 Data Dictionary (continued)

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 D 6557 – 00

FIG. A5.4 Data Dictionary (continued)

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 D 6557 – 00

APPENDIX

(Nonmandatory Information)

X1. PREPARATION OF ACID SOLUTION

TABLE X1.1 Acid Solution X1.1.2 Put a magnetic stir bar into the 1-L flask, put a
Component Amount stopper in the flask, and place the flask on a stirring plate.
(ensure accuracy within 0.2 %) Adjust to a moderate stirring speed, and allow stirring for 30
Acetic acid 6.646 g min at room temperature. Remove the stir bar from the flask.
HBr 4.892 g
HCl 103.232 g
Deionized water Fill to 1-L mark

X1.1 Acid Solution Preparation (Example: 1-L of solution):

X1.1.1 Accurately weigh each of the chemicals listed in
Table X1.1 into separate clean, dry 50-mL beakers (100-mL
beaker for the HCl 1.0 N), using a three-place balance. Flush
and rinse a 1-L flask with a small amount of deionized water,
and empty the individual beakers into the flask. Fill the 1-L
flask with deionized water up to the 1-L mark.

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