RFP 693JJ926R000004 Attachment J.3 - TP-116-04.pdf

TP-116-04

April 22, 2005

U.S. DEPARTMENT OF TRANSPORTATION

NATIONAL HIGHWAY TRAFFIC SAFETY ADMINISTRATION

LABORATORY TEST PROCEDURE

FOR

FMVSS 116

Motor Vehicle Brake Fluids

ENFORCEMENT

Office of Vehicle Safety Compliance Room 6115, NVS-222 400 Seventh Street, SW Washington, DC 20590

OVSC LABORATORY TEST PROCEDURE NO. 116

TABLE OF CONTENTS

PAGE

1. PURPOSE AND APPLICATION

2. GENERAL REQUIREMENTS

3. SECURITY

4. GOOD HOUSEKEEPING

5. TEST SCHEDULING AND MONITORING

6. TEST DATA DISPOSITION

7. GOVERNMENT FURNISHED PROPERTY (GFP)

8. CALIBRATION OF TEST INSTRUMENTS

9. PHOTOGRAPHIC DOCUMENTATION

10. DEFINITIONS

11. PRETEST REQUIREMENTS

12. COMPLIANCE TEST EXECUTION

13. POST TEST REQUIREMENTS

14. REPORTS

14.1. MONTHLY STATUS REPORTS

14.2. APPARENT TEST FAILURE

14.3. FINAL TEST REPORTS

14.3.1. COPIES

14.3.2. REQUIREMENTS

14.3.3. FIRST THREE PAGES

14.3.4. TABLE OF CONTENTS

15. DATA SHEETS

16. FORMS

REVISION CONTROL LOG

FOR OVSC LABORATORY

TEST PROCEDURES

TP-116

Motor Vehicle Brake Fluids

TEST PROCEDURE FMVSS 116

REV.

No.

DATE AMENDMENT EFFECTIVE

DATE

DESCRIPTION

00 Original Issue

04 April 22, 69 FR 67654 Jan. 18, 2005

Nov. 21, 2005

Deletion of evaporation test.

Modification of corrosion test.

1. PURPOSE AND APPLICATION

The Office of Vehicle Safety Compliance (OVSC) provides contracted laboratories with Laboratory Test Procedures (TPs) which serve as guidelines for obtaining compliance test data. The data are used to determine if a specific vehicle or item of motor vehicle equipment meets the minimum performance requirements of the subject Federal Motor Vehicle Safety Standard (FMVSS). The purpose of the OVSC Laboratory Test Procedures is to present a uniform testing and data recording format, and provide suggestions for the use of specific equipment and procedures. Any contractor interpreting any part of an OVSC Laboratory Test Procedure to be in conflict with a Federal Motor Vehicle Safety Standard or observing any deficiencies in a Laboratory Test Procedure is required to advise the Contracting Officer's Technical Representative (COTR) and resolve the discrepancy prior to the start of compliance testing.

Contractors are required to submit a detailed test procedure to the COTR before initiating the compliance test program. The procedure must include a step-by-step description of the methodology to be used.

The OVSC Laboratory Test Procedures are not intended to limit or restrain a contractor from developing or utilizing any testing techniques or equipment which will assist in procuring the required compliance test data.

NOTE:

The OVSC Laboratory Test Procedures, prepared for use by independent laboratories under contract to conduct compliance tests for the OVSC, are not intended to limit the requirements of the applicable FMVSS(s). In some cases, the OVSC Laboratory Test Procedures do not include all of the various FMVSS minimum performance requirements. Sometimes, recognizing applicable test tolerances, the Test Procedures specify test conditions which are less severe than the minimum requirements of the standards themselves. Therefore, compliance of a vehicle or item of motor vehicle equipment is not necessarily guaranteed if the manufacturer limits certification tests to those described in the OVSC Laboratory Test Procedures.

2. GENERAL REQUIREMENTS

FMVSS 116 specifies requirements for fluids for use in hydraulic brake systems of motor vehicles, containers for these fluids, and labeling of the containers.

The purpose of FMVSS 116 is to reduce failures in the hydraulic braking systems of motor vehicles which may occur because of the manufacture or use of improper or contaminated fluid.

The standard applies to all fluid for use in hydraulic brake systems of passenger cars, multipurpose passenger vehicles, trucks, buses, trailers, and motorcycles which are equipped with a hydraulic brake system. The fluid for use in the

2. GENERAL REQUIREMENTS....Continued referenced vehicle shall have been manufactured and packaged in conformity with the requirements of FMVSS 116. The tests which are contained within this test procedure are used to determine compliance with the specified requirements. These tests are as follows:

A. Equilibrium Reflux Boiling Point (ERBP) B. Wet ERBP C. Kinematic Viscosity D. Ph Value E. Fluid Stability F. Corrosion G. Fluidity and Appearance (Low Temperature) H. Water Tolerance I. Compatibility J. Resistance to Oxidation K. Effect on SBR Cups L. Stroking Properties (This test is only conducted when specifically specified in the contract) M. Container Information

3. SECURITY

The contractor shall provide appropriate security measures to protect the OVSC test equipment from unauthorized personnel during the entire compliance testing program.

The contractor is financially responsible for any acts of theft and/or vandalism which occur during the storage of test equipment. Any security problems which arise shall be reported by telephone to the Industrial Property Manager (IPM), Office of Contracts and Procurement, within two working days after the incident. A letter containing specific details of the security problem will be sent to the IPM (with copy to the COTR) within 48 hours.

The contractor shall protect and segregate the data that evolves from compliance testing before and after each test. No information concerning the safety compliance testing program shall be released to anyone except the COTR, unless specifically authorized by the COTR, the COTR's Branch or Division Chief, or by the Contracting Officer.

NO INDIVIDUALS, OTHER THAN CONTRACTOR PERSONNEL, SHALL BE

ALLOWED TO WITNESS ANY COMPLIANCE TEST UNLESS SPECIFICALLY

AUTHORIZED BY THE COTR.

4. GOOD HOUSEKEEPING

Contractors shall maintain the entire equipment compliance testing area, test fixtures and instrumentation in a neat and clean condition with test instruments arranged in an orderly manner consistent with good test laboratory housekeeping

4. GOOD HOUSEKEEPING....Continued practices.

5. TEST SCHEDULING AND MONITORING

The contractor shall submit a test schedule to the COTR prior to testing. Tests shall be completed as required in the contract. All testing shall be coordinated to allow monitoring by the COTR.

6. TEST DATA DISPOSITION

The contractor shall make all equipment preliminary compliance test data available to the COTR on location within four hours after the test. Final test data, including digital printouts and computer generated plots (if applicable), shall be furnished to the COTR in accordance with the contract schedule.

All backup data sheets, strip charts, recordings, plots, technicians notes, etc., shall be retained by the contractor for a minimum of five years after conclusion of each delivery order, purchase order, etc. The COTR shall direct final disposition at that time.

7. GOVERNMENT FURNISHED PROPERTY (GFP) AND TEST SAMPLES

TEST SAMPLE IDENTIFICATION AND STORAGE

Upon receipt at the laboratory, the items to be tested shall be assigned laboratory serial numbers.

EXAMPLE:

Brand X Heavy Duty Brake Fluid; Lab Group #00X

An inventory shall be made of the number, name and condition of samples received.

The test samples shall be stored in a dry and clean area specifically designated by the Laboratory Project Manager.

8. CALIBRATION OF TEST INSTRUMENTS

Before the contractor initiates the safety compliance test program, a test instrumentation calibration system will be implemented and maintained in accordance with established calibration practices. Guidelines for setting up and maintaining such calibration systems are described in MIL-C-45662A, "Calibration System Requirements". The calibration system shall be set up and maintained as follows:

8. CALIBRATION....Continued

A. Standards for calibrating the measuring and test equipment will be stored and used under appropriate environmental conditions to assure their accuracy and stability.

B. All measuring instruments and standards shall be calibrated by the contractor, or a commercial facility, against a higher order standard at periodic intervals NOT TO EXCEED TWELVE (12) MONTHS except for static types of measuring devices such as rulers, weights, etc., which shall be calibrated at periodic intervals not to exceed two years. Records, showing the calibration traceability to the National Institute of Standards and Technology (NIST), shall be maintained for all measuring and test equipment.

C. All measuring and test equipment and measuring standards will be labeled with the following information:

(1) Date of calibration

(2) Date of next scheduled calibration

D. A written calibration procedure shall be provided by the contractor which includes as a minimum the following information for all measurement and test equipment unless the calibration is performed by a licensed commercial facility.

(1) Type of equipment, manufacturer, model number, etc.

(2) Measurement range

(3) Accuracy

(4) Calibration interval

(5) Type of standard used to calibrate the equipment (calibration traceability of the standard must be evident)

E. Records of calibration for all test instrumentation shall be kept by the contractor in a manner which assures the maintenance of established calibration schedules.

All such records shall be readily available for inspection when requested by the COTR. The calibration system will need the acceptance of the COTR before the test program commences.

9. PHOTOGRAPHIC DOCUMENTATION

Each final test report shall include glossy photographs (minimum size 4 x 6 inches) of the test setup used for each phase of testing. One set of original photographs shall be included in the final test report which will be used for optical scanning by the OVSC.

Other copies of the final test report may contain multilith or other suitable photographic copies of the original photographs.

10. DEFINITIONS

BLISTER

Cavity or sac on the surface of a brake cup.

BRAKE FLUID

Liquid designed for use in a motor vehicle hydraulic brake system in which it will contact elastomeric components made of styrene and butadiene rubber (SBR), ethylene and propylene rubber (EPR), polychloroprene (CR) brake hose inner tube stock or natural rubber (NR).

CHIPPING

Condition in which small pieces are missing from the outer surface of a brake cup.

DUPLICATE SAMPLES

Two samples of brake fluid taken from a single packaged lot and tested simultaneously.

HYDRAULIC SYSTEM MINERAL OIL

Mineral-oil-based fluid designed for use in motor vehicle hydraulic brake systems in which the fluid is not in contact with components made of SBR, EPR or NR.

PACKAGED LOT

That quantity of brake fluid shipped by the manufacturer to the packager in a single container, or that quantity of brake fluid manufactured by a single plant run of 24 hours or less, through the same processing equipment and with no change in ingredients.

PACKAGER

Person who fills containers with brake fluid that are distributed for retail sale.

SCUFFING

Visible erosion of a portion of the outer surface of a brake cup.

SILICONE BASE BRAKE FLUID (SBBF)

A brake fluid which consists of not less than 70 percent by weight of a diorgano polysiloxane.

10. DEFINITIONS....Continued

SLOUGHING

Degradation of a brake cup as evidenced by the presence of carbon black loosely held on the brake cup surface, such that a visible black streak is produced when the cup, with a 500 ∀ 10 gram dead weight on it, is drawn base down over a sheet of white bond paper placed on a firm flat surface.

STICKINESS

Condition on the surface of a brake cup such that fibers will be pulled from a wad of U.S.P. absorbent cotton when it is drawn across the surface.

11. PRETEST REQUIREMENTS

IN-HOUSE TEST PROCEDURE

Prior to conducting any compliance test, contractors are required to submit a detailed in-house compliance test procedure to the COTR which includes a step-by-step description of the methodology to be used. Written approval must be obtained from the COTR before initiating the compliance test program so that all parties are in agreement.

TEST DATA LOSS

A compliance test is not to be conducted unless all of the various test conditions specified in the applicable OVSC Laboratory Test Procedure have been met. Failure of a contractor to obtain the required test data and to maintain acceptable limits on test parameters in the manner outlined in the applicable OVSC Laboratory Test Procedure may require a retest at the expense of the contractor. The retest costs will include the cost of the replacement brake fluid and all costs associated with conducting the retest.

The Contracting Officer of NHTSA is the only NHTSA official authorized to notify the contractor that a retest is required. The retest shall be completed within two (2) weeks after receipt of notification by the Contracting Officer that a retest is required. If a retest is conducted, no test report is required for the original test.

TEST CONDITIONS

Unless otherwise specified, all tests and measurements shall be conducted under the following environmental conditions:

A. Temperature 75ΕF ∀ 15ΕF B. Relative Humidity 50% ∀ 10% C. Atmospheric Pressure 28 to 32 inches of mercury

11. PRETEST....Continued

Continuous recording of environmental temperature and relative humidity of the testing area shall be available during all tests. Test samples, unless otherwise specified, shall be stabilized at test room conditions for a period of at least 24 hours immediately prior to testing.

TEST PERSONNEL PERFORMANCE

Personnel supervising and/or performing the compliance test program shall be thoroughly familiar with the requirements, test conditions, equipment for the test to be conducted, and safety requirements.

RECORDING OF TEST DATA

Environmental data and test data shall be recorded on permanent strip charts, circular recording charts, or other acceptable print-out media. Where permanent trace recording is not required, data will be recorded on standard report forms. Changes or corrections shall be made by drawing a line through the original entry, which must still remain legible, and adding the change alongside.

Test data will be submitted on the standard form Test Data Sheets specified for use in the final test report and shown in Section 15. Data will be typed before the sheets are submitted. If stroking test is conducted, Data Sheet No. 3 shall be used.

12. COMPLIANCE TEST EXECUTION

TEST QUANTITIES

The amount of brake fluid required for one complete test group is shown below:

TEST QUANT.

6.1 Equilibrium Reflux Boiling Point (ERBP) 125 ml

6.2 Wet ERBP 205 ml

6.3 Kinematic Viscosity 120 ml

6.4 pH Value 55 ml

6.5 Fluid Stability 125 ml

6.6 Corrosion 1520 ml

6.7 Fluidity & Appearance (Low Temp.) 205 ml

6.8 Water Tolerance 105 ml

6.9 Compatibility 55 ml

6.10 Resistance to Oxidation 65 ml

6.11 Effect on SBR Cups 150 ml

6.12 Stroking Properties 3785 ml

6.13 Container Information 348 ml

Reserve 2850 ml TOTAL 9713 ml (328 oz)

12. COMPLIANCE....Continued

TEST REQUIREMENTS

The fluid samples shall meet specific requirements when tested in accordance with the procedures in FMVSS 116.

6.1 Equilibrium reflux boiling point. Determine the ERBP of a brake fluid by running duplicate samples according to the following procedure and averaging the results.

6.1.1 Summary of procedure. Sixty milliliters (ml.) of brake fluid are boiled under specified equilibrium conditions (reflux) at atmospheric pressure in a 100-ml. flask. The average temperature of the boiling fluid at the end of the reflux period, corrected for variations in barometric pressure if necessary, is the ERBP.

6.1.2 Apparatus. (See Figure 1) The test apparatus shall consist of— (a) Flask. (See Figure 2) A 100-ml. round-bottom, short-neck heat-resistant glass flask having a neck with a 19.38 standard taper, female groundglass joint and a side-entering tube, with an outside diameter of 10 millimeters (mm.), which centers the thermometer bulb in the flask 6.5 mm. from the bottom; (b) Condenser. A water-cooled, reflux, glass-tube type, condenser having a jacket 200 mm. in length, the bottom end of which has a 19.38 standard-taper, drip-tip, male ground-glass joint; (c) Boiling stones. Three clean, unused silicon carbide grains (approximately 2 mm. (0.08 inch) in diameter, grit No. 8); (d) Thermometer. Standardized calibrated partial immersion (76 mm.), solid stem, thermometers conforming to the requirements for an ASTM 2C or 2F, and an ASTM 3C or 3F thermometer; and (e) Heat source. Variable autotransformer-controlled heating mantle designed to fit the flask, or an electric heater with rheostat heat control.

6.1.3 Preparation of apparatus. (a) Thoroughly clean and dry all glassware. (b) Insert thermometer through the side tube until the tip of the bulb is 6.5 mm. (1.4 inch) from the bottom center of the flask. Seal with a short piece of natural rubber, EPDM, SBR, or butyl tubing. (c) Place 60±1 ml. of brake fluid and the silicon carbide grains into the flask. (d) Attach the flask to the condenser. When using a heating mantle, place the mantle under the flask and support it with a ring-clamp and laboratory-type stand, holding the entire assembly in place by a clamp. When using a rheostat- controlled heater, center a standard porcelain or hard asbestos refractory, having a diameter opening 32 to 38 mm., over the heating element and mount the flask so that direct heat is applied only through the opening in the refractory. Place the assembly in an area free from drafts or other types of sudden temperature changes. Connect the cooling water inlet and outlet tubes to the condenser. Turn on the cooling water. The water supply temperature shall not exceed 28 °C. (82.4 °F.) and the temperature rise through the condenser shall not exceed 2 °C. (3.6 °F.).

FIG. 1. BOILING POINT TEST APPARATUS

FIG. 2. DETAIL OF 100 ML SHORT-NECK FLASK

6.1.4 Procedure. Apply heat to the flask so that within 10±2 minutes the fluid is refluxing in excess of 1 drop per second. The reflux rate shall not exceed 5 drops per second at any time. Immediately adjust the heating rate to obtain an equilibrium reflux rate of 1 to 2 drops per second over the next 5±2 minutes. Maintain this rate for an additional 2 minutes, taking four temperature readings at 30–second intervals. Record the average of these as the observed ERBP. If no reflux is evident when the fluid temperature reaches 260 °C (500 °F), discontinue heating and report ERBP as in excess of 260 °C (500 °F).

6.1.5 Calculation. (a) Thermometer inaccuracy. Correct the observed ERBP by applying any correction factor obtained in standardizing the thermometer. (b) Variation from standard barometric pressure. Apply the factor shown in Table I to calculate the barometric pressure correction to the ERBP.

(c) If the two corrected observed ERBP’s agree within 2 °C. (4 °C. for brake fluids having an ERBP over 230 °C./446 °F.) average the duplicate runs as the ERBP;

otherwise, repeat the entire test, averaging the four corrected observed values to determine the original ERBP.

Table I – Correction for Barometric Pressure Correction per 1mm difference in pressureaObserved ERBP corrected for thermometer inaccuracy °C. °F.

100 °C. (212 °F.) to 190 °C. (374 °F.) 0.039 (0.07) Over 190 °C. (374 °F.) 0.04 (0.08) a To be added in case barometric pressure is below 760 mm.; to be subtracted in case barometric pressure is above 670 mm.

6.1.6 Pass/Fail Criteria. The ERBP shall not be less than the following value for the grade indicated: (a) DOT 3: 205 °C. (401 °F.). (b) DOT 4: 230 °C. (446 °F.). (c) DOT 5:

260 °C. (500 °F.).

6.2 Wet ERBP. Determine the wet ERBP of a brake fluid by running duplicate samples according to the following procedure.

6.2.1. Summary of procedure. A 350 ml. sample of the brake fluid is humidified under controlled conditions; 350 ml. of SAE triethylene glycol monomethyl ether, brake fluid grade, referee material (TEGME) as described in appendix E of SAE Standard J1703 Nov. 83, ‘‘Motor Vehicle Brake Fluid,’’ November 1983, is used to establish the end point for humidification. After humidification, the water content and ERBP of the brake fluid are determined.

6.2.2 Apparatus for humidification. (See Figure 3). Test apparatus shall consist of— (a) Glass jars. Four SAE RM–49 corrosion test jars or equivalent screwtop, straight-sided, round glass jars each having a capacity of about 475 ml. and approximate inner dimensions of 100 mm. in height by 75 mm. in diameter, with matching lids having new, clean inserts providing water-vapor-proof seals; (b) Desiccator and cover. Two bowlform glass desiccators, 250-mm. inside diameter, having matching tubulated covers fitted with No. 8 rubber stoppers; and (c) Desiccator plate. Two 230-mm.

diameter, perforated porcelain desiccator plates, without feet, glazed on one side.

6.2.3 Reagents and materials. (a) Distilled water, see S7.1. (b) SAE TEGME referee material.

6.2.4 Preparation of apparatus. Lubricate the ground-glass joint of the desiccator. Pour 450±10 ml. of distilled water into each desiccator and insert perforated porcelain desiccator plates. Place the desiccators in an oven with temperature controlled at 50±1 °C. (122±1.8 °F.) throughout the humidification procedure.

6.2.5 Procedure. Pour 350±5 ml. of brake fluid into an open corrosion test jar. Prepare in the same manner a duplicate test fluid sample and two duplicate specimens of the SAE TEGME referee material (350±5 ml. of TEGME in each jar). The water content of the SAE TEGME fluid is adjusted to 0.50±0.05 percent by weight at the start of the test in accordance with S7.2. Place one sample each of the test brake fluid and the prepared TEGME sample into the same desiccator. Repeat for the second sample of test brake fluid and TEGME in a second desiccator. Place the desiccators in the 50 °C.

(122 °F.) controlled oven and replace desiccator covers. At intervals, during oven humidification, remove the rubber stoppers in the tops of desiccators. Using a long needled hypodermic syringe, take a sample of not more than 2 ml. from each TEGME sample and determine its water content. Remove no more than 10 ml. of fluid from each SAE TEGME sample during the humidification procedure. When the water content of the SAE fluid reaches 3.70±0.05 percent by weight (average of the duplicates). remove the two test fluid specimens from their desiccators and promptly cap each jar tightly.

Allow the sealed jars to cool for 60 to 90 minutes at 23°±5 °C. (73.4°±9 °F.). Measure the water contents of the test fluid specimens in accordance with S7.2 and determine their ERBP’s in accordance with S6.1. If the two ERBPs agree within 4 °C. (8 °F.), average them to determine the wet ERBP; otherwise repeat and average the four individual ERBPs as the wet ERBP of the brake fluid.

6.2.6 Pass/Fail Criteria. The wet ERBP shall not be less than the following value for the grade indicated: (a) DOT 3: 140 °C. (284 °F.). (b) DOT 4: 155 °C. (311 °F.). (c) DOT 5:

1 180 °C. (356 °F.).

6.3 Kinematic viscosities. Determine the kinematic viscosity of a brake fluid in mm2/s by the following procedure. Run duplicate samples at each of the specified temperatures, making two timed runs on each sample.

6.3.1 Summary of the procedure. The time is measured for a fixed volume of the brake fluid to flow through a calibrated glass capillary viscometer under an accurately reproducible head and at a closely controlled temperature. The kinematic viscosity is then calculated from the measured flow time and the calibration constant of the viscometer.

6.3.2 Apparatus. (a) Viscometers. Calibrated glass capillary- type viscometers, ASTM D2515– 66, ‘‘Standard Specification for Kinematic Glass Viscometers,’’ measuring viscosity within the precision limits of S6.4.7. Use suspended level viscometers for viscosity measurements at low temperatures. Use Cannon-Fenske Routine or other modified Ostwald viscometers at ambient temperatures and above. (b) Viscometer holders and frames. Mount a viscometer in the constanttemperature bath so that the mounting tube is held within 1° of the vertical. (c) Viscometer bath. A transparent liquid bath of sufficient depth such that at no time during the measurement will any portion of the sample in the viscometer be less than 2 cm. below the surface or less than 2 cm.

above the bottom. The bath shall be cylindrical in shape, with turbulent agitation sufficient to meet the temperature control requirements. For measurements within 15° to 100 °C. (60°to 212 °F.) the temperature of the bath medium shall not vary by more than

0.01 °C. (0.02 °F.) over the length of the viscometers, or between the positions of the viscometers, or at the locations of the thermometers. Outside this range, the variation shall not exceed 0.03 °C. (0.05 °F.). (d) Thermometers. Liquid-in-Glass Kinematic Viscosity Test Thermometers, covering the range of test temperatures indicated in Table II and conforming to ASTM E1–68, ‘‘Specifications for ASTM Thermometers,’’ and in the IP requirements for IP Standard Thermometers. Standardize before use (see S6.3.3(b)). Use two standardized thermometers in the bath.

Table II – Kinematic Viscocity Thermometers For tests at Subdivisions Thermometer Number

°C. °F. °C. °F. °C. °F. ASTM IP

Minus 55.3 to minus 52.5

Minus 67.5 to minus

62.5 Minus 55 Minus 67 0.05 0.1 74 F 69 F. or C.

Minus 41.4 to minus 38.6

Minus 42.5 to minus

37.5 Minus 40 Minus 40 0.05 0.1 73 F 68 F. or C.

98.6 to 101.4 207.5 to 212.5 100 212 0.05 0.1 30 F 32 F. or C.

(e) Timing device. Stop watch or other timing device graduated in divisions representing not more than 0.2 second, with an accuracy of at least ±0.05 percent when tested over intervals of 15 minutes. Electrical timing devices may be used when the current frequency is controlled to an accuracy of 0.01 percent or better.

6.3.3 Standardization. (a) Viscometers. Use viscometers calibrated in accordance with appendix 1 of ASTM D445–65, ‘‘Viscosity of Transparent and Opaque Liquids (Kinematic and Dynamic Viscosities).’’ The calibration constant, C, is dependent upon the gravitational acceleration at the place of calibration. This must, therefore, be supplied by the standardization laboratory together with the instrument constant. Where the acceleration of gravity, g, in the two locations differs by more than 0.1 percent, correct the calibration constant as follows:

C2=(g2/g1)*C1 where the subscripts 1 and 2 indicate respectively the standardization laboratory and the testing laboratory. (b) Thermometers. Check liquid-inglass thermometers to the nearest 0.01 °C. (0.02 °F.) by direct comparison with a standardized thermometer.

Kinematic Viscosity Test Thermometers shall be standardized at ‘‘total immersion.’’ The ice point of standardized thermometers shall be determined before use and the official corrections shall be adjusted to conform to the changes in ice points. (See ASTM E77– 66, ‘‘Verification and Calibration of Liquid-in-Glass Thermometers.’’) (c) Timers. Time signals are broadcast by the National Bureau of Standards, Station WWV, Washington, DC at 2.5, 5, 10, 15, 20, 25, 30, and 35 Mc/sec (MHz). Time signals are also broadcast by Station CHU from Ottawa, Canada, at 3.330, 7.335, and 14.670 Mc/sec, and Station MSF at Rugby, United Kingdom, at 2.5, 5, and 10 Mc/sec.

6.3.4 Procedure. (a) Set and maintain the bath at the appropriate test temperature (see S5.1.3) within the limits specified in S6.3.2(c). Apply the necessary corrections, if any, to all thermometer readings. (b) Select a clean, dry, calibrated viscometer giving a flow time not less than its specified minimum, or 200 seconds, whichever is the greater. (c) Charge the viscometer in the manner used when the instrument was calibrated. Do not filter or dry the brake fluid, but protect it from contamination by dirt and moisture during filling and measurements. (1) Charge the suspended level viscometers by tilting about 30° from the vertical and pouring sufficient brake fluid through the fill tube into the lower reservoir so that when the viscometer is returned to vertical position the meniscus is between the fill marks. For measurements below 0 °C. (32 °F.), before placing the filled viscometer into the constant temperature bath, draw the sample into the working capillary and timing bulb and insert small rubber stoppers to suspend the fluid in this position, to prevent accumulation of water condensate on the walls of the critical portions of the viscometer. Alternatively, fit loosely packed drying tubes into the open ends of the viscometer to prevent water condensation, but do not restrict the flow of the sample under test by the pressures created in the instrument. (2) If a Cannon-Fenske Routine viscometer is used, charge by inverting and immersing the smaller arm into the brake fluid and applying vacuum to the larger arm. Fill the tube to the upper timing mark, and return the viscometer to an upright position. (d) Mount the viscometer in the bath in a true vertical position (see S6.3.2(b)). (e) The viscometer shall remain in the bath until it reaches the test temperature. (f) At temperatures below 0 °C. (32 °F.)

conduct an untimed preliminary run by allowing the brake fluid to drain through the capillary into the lower reservoir after the test temperature has been established. (g) Adjust the head level of the brake fluid to a position in the capillary arm about 5 mm.

above the first timing mark. (h) With brake fluid flowing freely measure to within 0.2 second the time required for the meniscus to pass from the first timing mark to the second. If this flow time is less than the minimum specified for the viscometer, or 200 seconds, whichever is greater, repeat using a viscometer with a capillary of smaller diameter. (i) Repeat S6.3.4 (g) and (h). If the two timed runs do not agree within 0.2 percent, reject and repeat using a fresh sample of brake fluid.

6.3.5 Cleaning the viscometers. (a) Periodically clean the instrument with chromic acid to remove organic deposits. Rinse thoroughly with distilled water and acetone, and dry with clean dry air. (b) Between successive samples rinse the viscometer with ethanol (isopropanol when testing DOT 5 fluids) followed by an acetone or ether rinse. Pass a slow stream of filtered dry air through the viscometer until the last trace of solvent is removed.

6.3.6 Calculation. (a) The following viscometers have a fixed volume charged at ambient temperature, and as a consequence C varies with test temperature: Cannon- Fenske Routine, Pinkevitch, Cannon-Manning Semi- Micro, and Cannon Fenske Opaque. To calculate C at test temperatures other than the calibration temperature for these viscometers, see ASTM D2515–66, ‘‘Kinematic Glass Viscometers’’ or follow instructions given on the manufacturer’s certificate of calibration. (b) Average the four timed runs on the duplicate samples to determine the kinematic viscosities.

6.3.7 Precision (at 95 percent confidence level). (a) Repeatability. If results on duplicate samples by the same operator differ by more than 1 percent of their mean, repeat the tests.

6.3.8. Pass/Fail Criteria. The kinematic viscosities in square millimeters per second at stated temperatures shall be neither less than 1.5 mm2/s at 100 °C. (212 °F.) nor more than the following maximum value for the grade indicated: (a) DOT 3: 1,500 mm2/s at minus 40 °C. (minus 40 °F.). (b) DOT 4: 1,800 mm2/s at minus 40 °C. (minus 40 °F.).

(c) DOT 5: 900 mm2/s at minus 40 °C. (minus 40 °F.).

6.4 pH value. Determine the pH value of a brake fluid by running one sample according to the following procedure.

6.4.1 Summary of the procedure. Brake fluid is diluted with an equal volume of an ethanol-water solution. The pH of the resultant mixture is measured with a prescribed pH meter assembly at 23 °C. (73.4 °F.).

6.4.2 Apparatus. The pH assembly consists of the pH meter, glass electrode, and calomel electrode, as specified in Appendices A1.1, A1.2, and A1.3 of ASTM D 1121– 67, ‘‘Standard Method of Test for Reserve Alkalinity of Engine Antifreezes and Antirusts.’’ The glass electrode is a full range type (pH 0–14), with low sodium error.

6.4.3 Reagents. Reagent grade chemicals conforming to the specifications of the

Committee on Analytical Reagents of the American Chemical Society. (a) Distilled water. Distilled water (S7.1) shall be boiled for about 15 minutes to remove carbon dioxide, and protected with a soda-lime tube or its equivalent while cooling and in storage. (Take precautions to prevent contamination by the materials used for protection against carbon dioxide.) The pH of the boiled distilled water shall be between

6.2 and 7.2 at 25 °C. (77 °F.). (b) Standard buffer solutions. Prepare buffer solutions for calibrating the pH meter and electrode pair from salts sold specifically for use, either singly or in combination, as pH standards. Dry salts for 1 hour at 110 °C. (230 °F.)

before use except for borax which shall be used as the decahydrate. Store solutions with pH less than 9.5 in bottles of chemically resistant glass or polyethylene. Store the alkaline phosphate solution in a glass bottle coated inside with paraffin. Do not use a standard with an age exceeding three months. (1) Potassium hydrogen phthalate buffer solution (0.05 M, pH=4.01 at 25 °C. (77 °F.)). Dissolve 10.21 g. of potassium hydrogen phthalate (KHC8 H4 O4) in distilled water. Dilute to 1 liter. (2) Neutral phosphate buffer solution (0.025 M with respect to each phosphate salt, pH=6.86 at 25 °C. (77 °F.)).

Dissolve 3.40 g. of potassium dihydrogen phosphate (KH2 PO4) and 3.55 g. of anhydrous disodium hydrogen phosphate (Na2 HPO4) in distilled water. (3) Borax buffer solution (0.01 M, pH=9.18 at 25 °C. (77 °F.)). Dissolve 3.81 g. of disodium tetraborate decahydrate (Na2 B4 O7°10H2 O) in distilled water, and dilute to 1 liter.

Stopper the bottle except when actually in use. (4) Alkaline phosphate buffer solution (0.01 M trisodium phosphate, pH=11.72 at 25 °C. (77 °F.)). Dissolve 1.42 g. of anhydrous disodium hydrogen phosphate (Na2 HPO4) in 100 ml. of a 0.1 M carbonate-free solution of sodium hydroxide. Dilute to 1 liter with distilled water. (5) Potassium chloride electrolyte. Prepare a saturated solution of potassium chloride (KCl) in distilled water. (c) Ethanol-water mixture. To 80 parts by volume of ethanol (S7.3) add 20 parts by volume of distilled water. Adjust the pH of the mixture to 7±0.1 using 0.1 N sodium hydroxide (NaOH) solution. If more than 4 ml. of NaOH solution per liter of mixture is required for neutralization, discard the mixture.

6.4.4 Preparation of electrode system. (a) Maintenance of electrodes. Clean the glass electrode before using by immersing in cold chromic-acid cleaning solution. Drain the calomel electrode and fill with KCl electrolyte, keeping level above that of the mixture at all times. When not in use, immerse the lower halves of the electrodes in distilled water, and do not immerse in the mixture for any appreciable period of time between determinations. (b) Preparation of electrodes. Condition new glass electrodes and those that have been stored dry as recommended by the manufacturer. Before and after using, wipe the glass electrode thoroughly with a clean cloth, or a soft absorbent tissue, and rinse with distilled water. Before each pH determination, soak the prepared electrode in distilled water for at least 2 minutes. Immediately before use, remove any excess water from the tips of the electrode.

6.4.5 Standardization of the pH assembly and testing of the electrodes. (a) Immediately before use, standardize the pH assembly with a standard buffer solution. Then use a second standard buffer solution to check the linearity of the response of the electrodes at different pH values, and to detect a faulty glass electrode or incorrect temperature compensation. The two buffer solutions bracket the anticipated pH value of the test brake fluid. (b) Allow instrument to warm up, and adjust according to the manufacturer’s instructions. Immerse the tips of the electrodes in a standard buffer solution and allow the temperature of the buffer solution and the electrodes to equalize. Set the temperature knob at the temperature of the buffer solution. Adjust the standardization or asymmetry potential control until the meter registers a scale reading, in pH units, equal to the known pH of the standardizing buffer solution. (c) Rinse the electrodes with distilled water and remove excess water from the tips. Immerse the electrodes in a second standard buffer solution. The reading of the meter shall agree with the known pH of the second standard buffer solution within ±0.05 unit without changing the setting of the standardization of asymmetry potential control. (d) A faulty electrode is indicated by failure to obtain a correct value for the pH of the second standard buffer solution after the meter has been standardized with the first.

6.4.6 Procedure. To 50±1 ml. of the test brake fluid add 50±1 ml. of the ethanol- water (6.4.3(c)) and mix thoroughly. Immerse the electrodes in the mixture. Allow the system to come to equilibrium, readjust the temperature compensation if necessary, and take the pH reading.

6.4.6 Pass/Fail Criteria. The pH value shall not be less than 7.0 nor more than 11.5 (except DOT 5 SBBF).

6.5 Fluid stability. Evaluate the heat and chemical stability of a brake fluid by the following procedure, running duplicate samples for each test and averaging the results.

6.5.1 Summary of the procedure. The degradation of the brake fluid at elevated temperature, alone or in a mixture with a reference fluid, is evaluated by determining the change in boiling point after a period of heating under reflux conditions.

6.5.2 Apparatus. Use the apparatus and preparation specified in S6.1.2 and S6.1.3.

6.5.3 High temperature stability.

6.5.3.1 Procedure. (a) Heat a new 60±1 ml. sample of the brake fluid to 185°±2 °C.

(365°±3.6 °F.). Hold at this temperature for 120±5 minutes. Bring to a reflux rate in excess of 1 drop per second within 5 minutes. The reflux rate should not exceed 5 drops per second at any time. Over the next 5±2 minutes adjust the heating rate to obtain an equilibrium reflux rate of 1 to 2 drops per second. Maintain this rate for an additional 2 minutes, taking four temperature readings at 30–second intervals. Average these as the observed ERBP. If no reflux is evident when the fluid temperature reaches 260 °C. (500 °F), discontinue heating and report ERBP as in excess of 260 °C. (500 °F.).

6.5.3.2 Calculation. Correct the observed ERBP for thermometer and barometric pressure factors according to S6.1.5 (a) and (b). Average the corrected ERBP’s of the duplicate samples. The difference between this average and the original ERBP obtained in S6.1 is the change in ERBP of the fluid.

6.5.4 Chemical stability.

6.5.4.1 Materials. SAE RM–66–04 Compatibility Fluid as described in appendix B of

SAE Standard J1703 JAN 1995, ‘‘Motor Vehicle Brake Fluid.’’ (SAE RM–66–03 Compatibility Fluid as described in appendix A of SAE Standard J1703 Nov83, ‘‘Motor Vehicle Brake Fluid,’’ November 1983, may be used in place of SAE RM–66–04 until January 1, 1995.)

6.5.4.2 Procedure. (a) Mix 30 ± 1 ml. of the brake fluid with 30 ± 1 ml. of SAE RM–66–04 Compatibility Fluid in a boiling point flask (S6.1.2(a)). Determine the initial ERBP of the mixture by applying heat to the flask so that the fluid is refluxing in 10 ±2 minutes at a rate in excess of 1 drop per second, but not more than 5 drops per second. Note the maximum fluid temperature observed during the first minute after the fluid begins refluxing at a rate in excess of 1 drop per second. Over the next 15 ±1 minutes, adjust and maintain the reflux rate at 1 to 2 drops per second. Maintain this rate for an additional 2 minutes, recording the average value of four temperature readings taken at 30 second intervals as the final ERBP. (b) Thermometer and barometric corrections are not required.

6.5.4.3 Calculation. The difference between the initial ERBP and the final average temperature is the change in temperature of the refluxing mixture. Average the results of the duplicates to the nearest 0.5 °C (1.0 °F).

6.5.5 Pass/Fail Criteria.

6.5.5.1 High-temperature stability. When brake fluid is tested according to S6.5.3 the ERBP shall not change by more than 3 °C. (5.4 °F.) plus 0.05°for each degree that the ERBP of the fluid exceeds 225 °C. (437 °F.).

6.5.5.2 Chemical stability. When brake fluid, except DOT 5 SBBF, is tested according to S6.5.4, the change in temperature of the refluxing fluid mixture shall not exceed 3.0 °C (5.4 °F.) plus 0.05°for each degree that the ERBP of the fluid exceeds 225 °C (437 °F.).

6.6 Corrosion. Evaluate the corrosiveness of a brake fluid by running duplicate samples according to the following procedure.

6.6.1 Summary of the procedure. Six specified metal corrosion test strips are polished, cleaned, and weighed, then assembled as described. Assembly is placed on a standard wheel cylinder cup in a corrosion test jar, immersed in the water-wet brake fluid, capped and placed in an oven at 100 °C. (212 °F.) for 120 hours. Upon removal and cooling, the strips, fluid, and cups are examined and tested.

6.6.2 Equipment. (a) Balance. An analytical balance having a minimum capacity of 50 grams and capable of weighing to the nearest 0.1 mg. (b) Desiccators. Desiccators containing silica gel or other suitable desiccant. (c) Oven. Gravity convection oven capable of maintaining the desired set point within 2 °C. (3.6 °F.). (d) Micrometer. A machinist’s micrometer 25 to 50 mm. (1 to 2 inches) capacity, or an optical comparator, capable of measuring the diameter of the SBR wheel cylinder (WC) cups to the nearest

0.02 mm. (0.001 inch).

6.6.3 Materials. (a) Corrosion test strips. Two sets of strips from each of the metals listed in appendix C of SAE Standard J1703b. Each strip shall be approximately 8 cm.

long, 1.3 cm. wide, not more than 0.6 cm. thick, and have a surface area of 25±5 sq.

cm. and a hole 4 to 5 mm. (0.16 to 0.20 inch) in diameter on the centerline about 6 mm.

from one end. The hole shall be clean and free from burrs. Tinned iron strips shall be unused. Other strips, if used, shall not be employed if they cannot be polished to a high finish. (b) SBR cups. Two unused standard SAE SBR wheel cylinder (WC) cups, as specified in S7.6. (c) Corrosion test jars and lids. Two screw-top straight-sided round glass jars, each having a capacity of approximately 475 ml. and inner dimensions of approximately 100 mm. in height and 75 mm. in diameter, and a tinned steel lid (no insert or organic coating) vented with a hole 0.8±0.1 mm. (0.031±0.004 inch) in diameter (No. 68 drill). (d) Machine screws and nuts. Clean, rust and oil-free, uncoated mild steel round or fillister head machine screws, size 6 or 8–32 UNC–Class 2A, fiveeighths or three-fourths inch long (or equivalent metric sizes), and matching uncoated nuts. (e) Supplies for polishing strips. Waterproof silicon carbide paper, grit No. 320 A and grit 1200; lint-free polishing cloth. (f) Distilled water as specified in S7.1.

(g) Ethanol as specified in S7.3. (h) Isopropanol as specified in S7.7.

6.6.4 Preparation. (a) Corrosion test strips. Except for the tinned iron strips, abrade corrosion test strips on all surface areas with 320A silicon carbide paper wet with ethanol (isopropanol when testing DOT 5 SBBF fluids) until all surface scratches, cuts and pits visible to an observer having corrected visual acuity of 20/40 (Snellen ratio) at a distance of 300 mm (11.8 inches) are removed. Use a new piece of paper for each different type of metal. Except for the tinned iron strips, further abrade the test strips on all surface areas with 1200 silicon carbide paper wet with ethanol (isopropanol when testing DOT 5 SBBF fluids), again using a new piece of paper for each different type of metal. Wash all strips, including the tinned iron and the assembly hardware, with ethanol (isopropanol when testing DOT 5 SBBF fluids); dry the strips and assembly hardware with a clean lint free cloth or use filtered compressed air and place the strips and hardware in a desiccator containing silica gel or other suitable desiccant and maintained at 23°±5 °C. (73.4°±9 °F.), for at least 1 hour. Handle the strips with forceps after polishing. Weigh and record the weight of each strip to the nearest 0.1 mg.

Assemble the strips on a clean dry machine screw, with matching plain nut, in the order of tinned iron, steel, aluminum, cast iron, brass, and copper. Bend the strips, other than the cast iron, so that there is a separation of 3±1.2 mm. (1.8±1.64 inch) between adjacent strips for a distance of about 5 cm. (2 inches) from the free end of the strips.

(See Figure 4.) Tighten the screw on each test strip assembly so that the strips are in electrolytic contact, and can be lifted by either of the outer strips (tinned iron or copper) without any of the strips moving relative to the others when held horizontally. Immerse the strip assemblies in 90 percent ethyl alcohol. Dry with dried filtered compressed air, then desiccate at least 1 hour before use.

(b) SBR WC cups. Measure the base diameters of the two standard SBR cups, using an optical comparator or micrometer, to the nearest 0.02 mm. (0.001 inch) along the centerline of the SAE and rubber-type identifications and at right angles to this centerline. Take the measurements at least 0.4 mm. (0.015 inch) above the bottom edge and parallel to the base of the cup. Discard any cup if the two measured diameters differ by more than 0.08 mm. (0.003 inch). Average the two readings on each cup.

Determine the hardness of the cups according to S7.4.

FIG. 4 CORROSION STRIP ASSEMBLY

6.6.5 Procedure. Rinse the cups in ethanol (isopropanol when testing DOT 5 SBBF fluids) for not more than 30 seconds and wipe dry with a clean lintfree cloth. Place one cup with lip edge facing up, in each jar. Insert a metal strip assembly inside each cup with the fastened end down and the free end extending upward. (See Figure 5.) When testing brake fluids, except DOT 5 SBBF, mix 760 ml. of brake fluid with 40 ml. of distilled water. When testing DOT 5 SBBF’s, humidify 800 ml. of brake fluid in accordance with S6.2, eliminating determination of the ERBP. Using this water-wet mixture, cover each strip assembly to a minimum depth of 10 mm. above the tops of the strips. Tighten the lids and place the jars for 120±2 hours in an oven maintained at 100°±2 °C. (212°±3.6 °F.). Allow the jars to cool at 23°±5 °C. (73.4°±9 °F.) for 60 to 90 minutes. Immediately remove the strips from the jars using forceps, agitating the strip assembly in the fluid to remove loose adhering sediment. Examine the test strips and jars for adhering crystalline deposits. Disassemble the metal strips, and remove adhering fluid by flushing with water; clean each strip by wiping with a clean cloth wetted with ethanol (isopropanol when testing DOT 5 fluids). Examine the strips for evidence of corrosion and pitting. Disregard staining or discoloration. Place the strips in a desiccator containing silica gel or other suitable desiccant, maintained at 23°±5 °C. (73.4°±9 °F.), for at least 1 hour. Weigh each strip to the nearest 0.1 mg. Determine the change in weight of each metal strip. Average the results for the two strips of each type of metal.

Immediately following the cooling period, remove the cups from the jars with forceps.

Remove loose adhering sediment by agitation of the cups in the mixture. Rinse the cups in ethanol (isopropanol when testing DOT 5 fluids) and air-dry. Examine the cups for evidence of sloughing, blisters, and other forms of disintegration. Measure the base diameter and hardness of each cup within 15 minutes after removal from the mixture.

Examine the mixture for gelling. Agitate the mixture to suspend and uniformly disperse sediment. From each jar, transfer a 100 ml. portion of the mixture to an ASTM cone-shaped centrifuge tube. Determine the percent sediment after centrifuging as described in S7.5. Measure the pH value of the corrosion text fluid according to S6.4.6. Measure the pH value of the test mixture according to S6.4.6.

6.6.6 Calculation. (a) Measure the area of each type of test strip to the nearest square centimeter. Divide the average change in mass for each type by the area of that type.

(b) Note other data and evaluations indicating compliance with S5.1.6. In the event of a marginal pass on inspection by attributes, or of a failure in one of the duplicates, run another set of duplicate samples. Both repeat samples shall meet all requirements of S5.1.6.

6.6.7 Pass/Fail Criteria. (a) The metal test strips shall not show weight changes exceeding the limits stated in Table III below;

Table III - Weight Change Limits Test Strip Material Maximum permissible weight change, mg./sq.cm. of surface Steel, tinned iron, cast iron 0.2 Aluminum 0.1 Brass, copper 0.4

(b) Excluding the area of contact (13±1 mm. (1.2±1.32 inch) measured from the bolt hole end of the test strip), the metal test strips shall not show pitting or etching to an extent discernible without magnification; (c) The water-wet brake fluid at the end of the test shall show no jelling at 23±5 °C (73.4±9 °F.); (d) No crystalline deposit shall form and adhere to either the glass jar walls or the surface of the metal strips; (e) At the end of the test, sedimentation of the water-wet brake fluid shall not exceed 0.10 percent by volume; (f) The pH value of water-wet brake fluid, except DOT 5 SBBF, at the end of the test shall not be less than 7.0 nor more than 11.5; (g) The cups at the end of the test shall show no disintegration, as evidenced by blisters or sloughing; (h) The hardness of the cup shall not decrease by more than 15 International Rubber Hardness Degrees (IRHD); and (i) The base diameter of the cups shall not increase by more than 1.4 mm.

(0.055 inch).

FIG. 5 CORROSION TEST APPARATUS

6.7 Fluidity and appearance at low temperatures. Determine the fluidity and appearance of a sample of brake fluid at each of two selected temperatures by the following procedure.

6.7.1 Summary of procedure. Brake fluid is chilled to expected minimum exposure temperatures and observed for clarity, gellation, sediment, separation of components, excessive viscosity or thixotropy.

6.7.2 Apparatus. (a) Oil sample…