0359510 Ob15892 803

ASTM D 471

ADOPTION NOTICE

ASTM D 471,“Standard Test Method for Rubber Property-Effect of Liquids”, was adopted on
11 September 1998 for use by the Department of Defense @OD). Proposed changes by DoD
activities must be submittedto the DoD Adoption Activity:U.S. Army Tank-automotive and
Armaments Command, ATTN: AMSTA-TR-D/210, Warren, MI 48397-5000.DoD activities
may obtain copiesof this standard from the Defense Automated Printing Service,Bldg. 4D
(Customer Service), 700 Robbins Ave., Philadelphia, PA 191 11-5094. The private sector and
other Government agencies may purchase copies from the American Society
for Testing and
Materials (ASTM),100 Barr Harbor Drive, West Conshohocken, PA 19428-2959.

ASTM D 471 should be used insteadof TT-S-735A, which was cancelled on11 September 1998.

Custodians: Adoption Activity:

Army - AT Army - AT
Navy - SH
Air Force - 11
(Project 6810-1632)

Review Activities:
Army - AV, EA, MI
Navy - OS
Air Force - 68
DLA - GS, PS

FCS 6810
is unlimited.
DISTRIBUTION STATEMENT A. Approved for public release; distribution

COPYRIGHT American Society for Testing and Materials

Licensed by Information Handling Services
 Standard Test Method for
Rubber Property-Effect of Liquids'
This standard is issued under the Fued designation D 471; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.

e' Nm-Table 3 was editoriallv uodated in Seotember 1999.

1. Scope D 92 Test Method for Flash and Fire Points by Cleveland

1.1 This testmethodcovers the requiredproceduresto Open Cup2
evaluate the comparativeability of rubberandrubber-like D 97 Test Method for Pour Point of Petroleum Products2
compositions to withstand the effect of liquids. It is designed D 287 Test Method for API Gravity of Crude Petroleum and
fortesting: ( I ) specimens of vulcanizedrubbercutfrom Petroleum Products (Hydrometer Method)'
standard sheets (see Practice D 3182), (2) specimens cut from D 412 Test Methods for Vulcanized Rubber and Thermo-
fabric coated with vulcanized rubber(see Test Method D 751), plastic Rubbers and Thermoplastic Elastomers- Tension3
or (3)finished articles of commerce (see Practice D 3183). This D 445 Test Method for Kinematic Viscosity of Transparent
test method is not applicable to the testing of cellular rubbers, andOpaqueLiquids(and the Calculation of Dynamic
porous compositions, and compressed sheet packing, except as Viscosity)2
described in 11.2.2. D 611 Test Methods for Aniline Point and Mixed Aniline
1.2 ASTM Oils No. 2 and No. 3, formerly used in this test Point of Petroleum Products and Hydrocarbon Solvents2
method as standard test liquids, are no longer commercially D 751 Test Methods for Coated Fabrics4
available and in 1993 were replaced with IRM 902 and IRM D 975 Specification for Diesel Fuel Oils'
903, respectively (see Appendix X1 for details). D 1217 TestMethod forDensityandRelativeDensity
1.3 This test method includes the following: (Specific Gravity) of Liquids by Bingham Pycnometes
(after
Change
Mass in immersion)
Section 10
D 1415 TestMethod forRubberProperty-International
mmersion)
Section
(after
VolumeinChange 11 Hardness3
Dimensional-Change Methodfor Water-Insoluble Lq- D 1500 Test Method for ASTM Color of Petroleum Prod-
and uids 12
ChangeMass
in with Lquid on
One
Surface
Only
Section 13
ucts (ASTM Color Scale)2
DeterminingMass of Soluble Malter Extracted bythe D 1747 Test Method for Refractive Index of Viscous Mate-
Liquid 14 rials2
Change in Tensile Strength, Elongation and Hardness
) (after 15 D 2008 Test Method for Ultraviolet Absorbance and Ab-
Change in Breaking Resistance, Burst Strength, Tear sorptivity of Petroleum Products'
Strength and Adhesion for Coated Fabrics
Section 16 D 2140 Test Method for Carbon-Type Composition of In-
Section results) (of test
Calculation 17
sulating Oils of Petroleum Origin5
1.4 The values stated in SI units are to be regarded as the D 2240 TestMethod for RubberProperty-Durometer
standard. The values in parentheses are for information only. Hardness3
1.5 This standard does not purport to address all ofthe D 2699 TestMethod for Research Octane Number of
safetyconcerns, if any, associatedwith its use. It is the Spark-Ignition Engine Fuel6
responsibility of the user of this standard to establish appro- D 3182 PracticeforRubber-Materials,Equipment,and
priate safety and health practices and determine the applica- Procedures for Mixing Standard Compounds and Prepar-
bility of regulatory limitations prior to use. ing Standard Vulcanized Sheets3
D 3 183 Practice forRubber-Preparation of Pieces for Test
2. Referenced Documents Purposes from Products3
2.1 ASTM Standards: D 4483 Practice for Determining Precision for Test Method
Standards in the Rubber and Carbon Black Industries3

''Ihis test methodis under the jurisdictionof ASTM Committee D-I I on Rubber 'Annual Book of ASTM Slandanis, Vol 05.01.
and is the direct responsibility of Subcommittee DI I. 15 on Degradation Tests. Annual Book of ASTM Standards, Vol 09.01.
Current edition approvedNovember 10, 1998. PublishedDecember 1998. 'Annual Book of ASTM Standards. Vol 09.02.
Originally published as D 471 - 37 T. Last previous edition D 47 1 - 97. 'Annual Book of ASTM Standards, Vol 10.03.
'Annual Book of ASTM Staruiards, Vol 05.05.

W r i g h t BASTM. 100 BarrHarbor Drive. West Conshohocken. PA 19428-2959. United States.

COPYRIGHT American Society for Testing and Materials

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 D 4485 Specification for Performance Engine Oils7 5. l. 1 When the temperatureof the testing roomis other than
D 4678 Practice for Rubber- Preparation, Testing, Accep- the standard 23 ? 2°C (73 2 4°F) the temperature of test shall
tance, Documentation, and Use of Reference Materials3 be reported.
D 5900 Specifications for Physical and Chemical Properties
of Industry Reference Materials TABLE 1 Test Temperatures and Immersion Periods
E 145SpecificationforGravity-ConvectionandForced- Immersion
Temperature in "C ("F)
Ventilation Ovens' Period. h
2.2 SAE standard^:^ -75 2 2 (-103t- 4) 85 2 2 (185-C 4) 22
J 300 Engine Oil Viscosity Classification -55 ? 2 (-67 2 4) 100 2 2 (212 2 4) 46
-4O-C2(-4024) 125 2 2 (2575 4)
70
3. Summary of Test Method -25 2 2 (-132 4) 150 2 2 (302 2 4)
166
-10 t- 2 (14-C 4) 175? 2 (347? 4) 670
3.1 This test method provides procedures for exposing test O 2 2 (32t- 4) 200 2 2 (392? 4)1006
specimens to the influenceof liquids under definite conditions 23 t- 2 (73 -C 4) 225 2 2 (4372 4)2998
50 2 2 (122 ? 4) 250 2 2 (482 5 4)4990
of temperature and time. The resulting deterioration is deter- 70 -C 2 ( 1 5 8 2 4)
mined by measuring the changesin physical properties, such as
stressktrain properties, hardness, and changes in mass, volume,
and dimension, before and after immersion in the test liquid. 5.1.2 The choice of the immersion period will dependupon
3.2 The precision statement in Section 19 is basedonan the nature of the vulcanizate,thetesttemperature,andthe
interlaboratory test program run in 1981, using six different liquid to be used. To obtaininformation on therate of
rubbers with ASTM Reference Fuels B, C, D'' and ASTM Oils deterioration it is necessarytomakedeterminationsafter
No. 1 and No.3. several immersion periods. The tolerance for any immersion
3.3 The precision statement in Appendix X 2 is based on an period shall be 21.5 min or ? 1 % of the immersion period,
interlaboratorytestprogramconducted in 1993toestablish whichever is greater.
replacements for ASTM Oils No. 2 and No. 3. Because of the 5.2 Illumination-Immersiontestsshall be madeinthe
limited number of participating laboratories, only repeatability absence of direct light.
could be evaluated, and it was necessary to use pooled values
of four No. 2 type oils (No.2 plus three candidate replacement 6. Standard Test Liquids
oils)andfourNo. 3 type oils (No. 3 plus three candidate 6.1 For test purposes, it is usually desirableto use the liquid
replacement oils). Twelve rubbers were tested in this program. that will come into contact with the vulcanizate in service. For
4. Significance and Use comparative tests with liquids of unknown or doubtful com-
4.1 Certainrubberarticles,forexample, seals, gaskets, position, samples of liquid from the same container or ship-
hoses,diaphragms,andsleeves, maybe exposedto oils, ment shall be used. Many commercial products, particularly
greases, fuels, and other fluids during service. The exposure those of petroleum origin, are subject to sufficient variation that
maybe continuous or intermittent and may occur over wide it is not practical touse themfortest liquids. Itisthen
temperature ranges. advisable to use a standard test liquid, such as described in
4.2 Properties of rubber articles deteriorate during exposure 6.1.1 and 6.1.2, covering the range of properties that may be
to these liquids, affecting the performance of the rubber part, encountered in the particular service.
which can result in partial failure. 6. l.1 ASTM and IRM Oils-The test shall be conducted in
4.3 This test method attempts to simulateservice conditions one of the petroleum-base ASTMor IRM oils(Note 1)
through controlled accelerated testing, but may not give any specified in Table 2 that has its aniline point nearest thatof the
direct correlation with actual part performance, since service oil with which the vulcanizate is expected to come in contact
conditions vary too widely. It yields comparative data on which in service except as indicated in 6.1.3.
to base judgment as to expected service quality. NOTE1-The aniline point of a petroleum oil appears to characterize
4.4 This test method is suitable for specification compliance the swelling action of that oil on rubber vulcanizates. Ingeneral, the lower
testing,quality control, refereepurposes,andresearchand the aniline point, the more severe the swelling action by the oil. The oils
development work. specified in Table 2 cover a range of aniline points commonly found in
lubricating oils.
5. Test Conditions
6.1.2 ASTMReferenceFuels-When gasolinesordiesel
5.1 Temperature and Immersion Periodr"Unless otherwise fuels are to be encounteredinservice,thetestshall be
specified the test temperature and immersion period shall be as conducted in one of the ASTM referencefuels(Note2)
indicated in Table 1, depending upon the anticipated service specified in Table 3, except as indicated in 6.1.3.
conditions:
NOTE 2-The ASTM reference fuels in Table 3 have been selected to
provide the maximumandminimum swelling effects producedby
'Annual Book of ASTM Standards, Vol 05.02. commercial gasolines. ReferenceFuel A hasamildactiononrubber
R Annual Book ofASTM Standards, Vol 14.02.
Available from Society of Automotive Engineers (SAE), 400 Commonwealth
vulcanizates andproduces results ofthe same order as low swelling
Drive, Warrendale. PA 15096. gasolines of the highly paraffinic,straight run type. Reference Fuels B, C,
'O Reference Fuels A, B, C. D. and E are available from Phillips Petroleum Co.,
and D simulate the swelling behavior of themajority of commercial
CustomerServiceCenter, P.O. Box 968. Borger, TX 79007:Phone: 1 (800) gasolines, with Reference Fuel C producing the highest swellingwhich is
858-4327; FAX: 1 (806) 275-3771. typical of highly aromatic premium grades of automotive gasoline.

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 ~ ~~ ~ ~~ ~ ~~ ~

STD.ASTfl Dq'IL-ENGL 3998

0759530
Ob547b3 Tb4 m
D 471
TABLE 2 Specifications and Typical Propetties of ASTM and
IRM Reference Oils
Propertv ASTM Oil
No. 1 ASTM Oil No. 5 IRM 902 IRM 903
Method
ASTM
~ ~~ ____ ~~~ ~ ~~~ ~ ~ _ _ _ _ ~~ ____ ~~~

Specilied Properties:
Aniline
Point,
"C ("F) 124 Z(255
1 5 2) 115 Z 1 (2392 2) 93 (199
23 t 5) 702
l(158 t 2) D 611
Kinematic Viscosity
(mm% [cst])
38°C 00F ') ... ... ... 319-34.1 D 445
99°C 0°F) 18.7-21 .O 10.9-11.9 19.2-21.5 ... D445
Gravity, API, 16°C (60°F) ... ... 19.0-21.0 21.O-23.0 D 287
Constant ViSCoSity-GraVity ... ... 0.875-0.885 0.860-0.870 D 2140
"C
COC.Flash 92 D min
Point (325)
163
("F)
min
(464)
240min243min
(469) (469)
Naphthenics, C,.,(%) ... ... 35 min 40 min D 2140
Paraffinics, Cd%) ... ... 50 max 45 rnax D 2140

Tjpical Properties:
I
Point,
l
Pour 'C ("F) ... (5) 5 (-24)-1 -31 (10) -12 97 D
ASTM Color ... L 1.0 L 2.5 L 0.5 D 15-00
dex Refractive ... 1. W 8 1.5105 1.m26 D 1747
UV Absotbance, 260 nrn ,.. ... 2.2 4.0 D 2008
Aromatics, C"(%) ... 4 12 14 D 2140

TABLE 3 ASTM Reference Fuels TABLE 4 ASTM Service Liquids

Composition,
Fuel Type Composition Volume % Liquid
Reference
Fuel A kooctane", 100 Service Liquid 101" di-2 ethyl hexyl sebacate, 99.5 mass %; phenothiazine,
Reference
Fuel B I s o o c t a n e " . 70;
TolueneA,
30 0.5 mass %
Reference Fuel C Isooctane", 50;
Toluene", 50 Service Liquid 102' ASTM Oil No. l.95 mass %; hydrocabon compound
Fuel D
Reference Isooctane", 60;
Toluen$\.
40 additivec. 5 mass % (29.5-33.5 mass % sulfur,
Reference
Fuel E Toluene", 100 1.=.O mass% phosphorus. 0.7 mass % nitrogen)
Reference Fuel F Diesel Fuel, Grade No. 2,' 100 Service Liquid 103" tri-n-butyl phosphate, 100 mass %
Reference Fuel G Fuel D, 85; anhydrousdenaturedethanolc,
15 Service Liquid 104€ ethylene glycolF, 50 volume %; distilled water, 50
Fuel H
Reference Fuel C, 85; anhydrousdenaturedethanolc,15 volume %
Reference Fuel I Fuel C, 8 5 ; anhydrous methanol,15 Service Liquid 105G ASTM Reference Oil TMC 1006
Reference
Fuel K Fuel C, 15;anhydrous methanol,85 Service Liquid lmH ARM 200 (Aerospace Reference Material 200)
Wotor Fuels, Section 1, Test Method D 2699 "Serviceliquid101 is intendedtosimulatetheswellingactionofsynthetic
%pecification D 975. diester-type lubricating oils.
~ CAnhydrous ethanol
denatured
with
unleaded
gasoline
(CDAformula
No. 20). 'Service liquid 102 approximates the swelling behavior of hydraulic oils.
available from Archer-Daniels-Midland,P.O. Box 1470, Decatur, IL 62525. %is hydrocarbon oil additive is available as Anglamol99from Lubrizol Corp..
29400 Lakeland Blvd., Wickliffe, OH 44092. Properties are as follows: Kinematic
viscosity (mm% [cStj) at 99°C (210°F) - 9.70 ? 0.52eslt( Method D 445); Flash
Reference Fuel F(diesel fuel)swells rubber vulcanizates to lesser
a extent pointCOC"C("F) - 45(113)min(TestMethod D 92); Densityat 16°C
than ReferenceFuel B. ReferenceFuels G, H, and I are fuel-alcohol (61°F) - 1.065 2 0.015 (Test Method D 1217).
blends (gasohol), which have a stronger swelling action than the corre- %ervice liquid 103 simulates phosphate ester-type aircraft hydraulic oils.
sponding fuel alone, where blends with methanol are more severe than 'Service liquid 104 approximates the swelling behavior of automotive engine
blendswithethanol.Reference Fuel K, amethanol-richblend,hasa coolant.
substantially weaker swelling action than that of the fuel used to prepare FEthylene glycol, reagent grade, shallbe used.
" v i c e Liquid 105is an API SJllLSAC GF-2 SAE 5W-30 reference engine oil
the blend. Reference Fuels 1 and K are also referred to as M15 and M85, meeting the requirements of ASTM D 4485 and SAE J 300. It is available from
respectively. ASTM Test Monitoring Center, 6555 Penn Avenue. Pittsburgh, PA 15206-4489.
Phone (412) 365-1O00, Fax (412) 3651047.
6.1.3 Service Liquids- Somecommercial oils, fuels and ?Service Liquid 106 is intended to eventually replace Service Liquid 101 which
other service liquids (see Table 4) are either non-petroleum or is no longer readily available for purchase aas mixture. ARM 200 is available from
are compounded from special petroleum hydrocarbon fractions SAE, 400 Commonwealth Drive, Warrendale, PA 15096.
ormixtures of petroleumhydrocarbonfractionsandother
ingredients resulting in materials having properties beyond the outside diameter of 38 mm (1.5 in.) and an overall length of
range of thereferencefluidslisted in Table2andTable 3. 300 mm (12 in.) fitted loosely with a stopper (see 8.2.1) shall
Immersiontests of rubbervulcanizatesthatareto come into be used." Glass beads shall be used in the liquid as a bumper
contact with such fluids should be made in the actual service and to separate the specimens.
liquid. 8.2 For volatile liquids, the test tube described in 8.1 shall
6.1.4 Water-Since thepurity of watervariesthroughout be tightlyfittedwithastopper (see 8.2.1) and areflux
theworld, all waterimmersiontestsareto be conductedin condenser.Anair-cooledrefluxcondensershallbeusedfor
distilled or deionized water. ASTM Oils No. 1" . I 3 and No. 5 and for IRh4 90212 *13 and
7. Preparation of Specimen
7.1 Except as otherwise specified in the applicable specifi- I' Test tubes available under Part No. LGB24 and LGB24C (case of 30) from

cations, specimens shall be preparedin accordance with the Edwin H. Benz Co. Inc., 73T Maplehurst Ave., Providence. R1 02908 or under Pan
requirements of Practices D 3182 and D 3183. No. LG226 from Precision Scientific, 2777 Washington Blvd.. Bellwood, IL 6 0 1 0 4 .
have been found suitable for this purpose.
8. Apparatus 121nformationaboutASTMOil No. 1 is included inResearchReportRR:
Dll-1004 and information about IRM 902 and IRM 903 in Research Report RR:
8.1Fornon-volatileliquids, a glass testtube,havingan Dll-1069. Both repons are available from ASTM Headquarters.

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 STD*ASTM D47L-ENGL 3998 I
I 0759530 Ob54762 9TO m
D 471
IRM 9O3l2,l3at test temperatures of 125°C (257°F) or more. 8.3.2.9Bafflesshall be used as required to prevent local
This condenser shall be a glass tube, approximately 500 mm overheating and dead spots.
(20 in.) or longer, in length and 15 mm (0.6 in.) in outside 8.3.2.10 The thermostatic control device shall beso located
diameter, tightly fitted to the immersion tube by means of a as to give accurate temperature control of the heating medium.
stopper (see 8.2.1). The bottom of the condenser tube shall The preferred location is adjacent to the recording thermom-
project about 12 mm (0.47 in.) below the stopper. A suitable eter.
(watercooled) reflux condenser shall be used for water or other 8.3.2.11Anactualcheckshallbemade by meansof
low-boiling liquids. Glass beads shall be used as in 8.1. maximum reading thermometers placed in various partsof the
8.2.1 The stoppershallnotcontaminatethetestliquid. oven to verify the uniformity of the heating.
When in doubt, cover the stopper with aluminum foil.
8.3 Maintaining TestTemperatures-The apparatusand 9. Test Specimens-Change in Mass or Volume
method chosen to maintain the specified temperature during 9.1 The standardspecimenshallberectangular,having
immersiontestingvarieswithtestconditions,requirements, dimensions of 25 by 50 by 2.0 2 0.1 mm (1 by 2 by 0.08 2
and circumstances. Water baths, appropriate temperature trans- 0.004 in.). Specimens from commercial articles shall be the
fer oil baths, hot air ovens Note 3, or aging blocks14 may be thickness of the material as received when they are less than 2
used. mm (0.08 in.); otherwise they should be reduced to a thickness
of2.0 5 0.1 mm (0.08 2 0.004 in.). Data obtained on test
NOTE3-When hot air ovens are used, it should be notedthat
contaminationwith volatile components of the immersion liquid may specimens having different original thicknesses are not com-
occur. This can affect test results, when the same ovens are subsequently parable.
used for hot air agng.
10. Procedure for Change in Mass
8.3.1 The preferred method for above room temperatures is
the use of aging blocks, since they have the widest temperature 10.1 Test three specimens of a single composition. Calculate
capability. the test results of the three specimens (see 17.1, Eq 1) and
8.3.2Ovens-Type LIB ovensspecifiedinTestMethod average the results. Weigh each specimen in air to the nearest
E 145aresatisfactoryforusethrough70°C.Forhigher 1 mg, record the mass as M,, and immerse in the test tube (see
temperatures, Type IL4ovens are necessary. 8.1) containing 100 cm3 of the test liquid (see 10.1.1). Separate
8.3.2.1Theinteriorsizeshallbe as follows or of an each test specimen from any adjacent test specimen and the
equivalent volume: walls of the test tube by approximately 6 mm (0.25 in.), for
Interior size of air oven:
example, by perforated glass beads15 as shown in Fig. 1. The
min 300 by 300 by 300 mm (12 by 12 by 12 in.)
max WO by WO by 1200 mm (36 by 36 by 48 in.)
Hollowperforatedglassbeads,availableunder Catalog No. Il-311C from
8.3.2.2 Provision shall be made for placing immersion test Fisher Scientific Co., 711T Forbes Ave., Pittsburgh, PA 15219. have been found
tubes in the oven without touching each other or the sides of suitable for this purpose.
the aging chamber and allowing proper air circulation around
them. I
8.3.2.3 The heating medium for the aging chamber shall be
air circulated within it at atmospheric pressure.
8.3.2.4 The source of heat is optional but shall be located in
the air supply outside of the aging chamber proper.
8.3.2.5 A recording thermometer located in the upper cen-
tralportionofthechambernearthecenteroftheaging
specimens shall be provided to record the actual aging tem-
perature.
8.3.2.6 Automatic temperature control by means of thermo-
static regulation shall be used.
8.3.2.7 The following special precautions shall be taken in
order that accurate, uniform heating is obtained in all parts of
the aging chamber:
8.3.2.8 The heated air shall be thoroughly circulated in the
oven by means of mechanical agitation. When a motor-driven
fan is used, the air must not come in contact with the fan motor
brush discharge because of danger of ozone formation.

l 3 ASTM Oil No. 1, IRM 902 and IRM 903 may be ordered from Penreco, 4426
East Washington Blvd.. Los Angeles, CA 900234476. ASTM Oils No. 1. No. 5,
IRM 902,and IRM 903aredistributed by R. E. Carroll,Inc.. P.O. Box 5806,
Trenton, N1 08638-0806.
Aging blocks. available under Model No. LGB9 (9 cavities) and LGB28 (28
cavities) from Edwin H. Benz Co., Inc.,73T MaplehurstAve.,Providence, RI
02908, have been found suitable for this purpose. FIG. 1 Method of Separation

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 STDmASTM D117L-ENGL 1798 M O759530Ob547b3 837 R
D 471
materials used to suspend and separatethe specimens shall not quickly in acetone at room temperature, blot lightly with filter
affect the test liquid or the rubber. paper freeof lint or foreign material, place ina tared,stoppered
10.1.1 Test liquids shall not be reused. weighing bottle, weigh, and record the mass as M3.Remove
10.1.1.1 For non-volatileliquids,conditionthetesttube each specimen from the bottle, weigh in distilled water, and
assembly at the specified temperature within the limits given in recordthemass as M4 in immediate consecutive order to
5.1 for the specified length of time. A check oftheactual determine the water displacement after immersion (see 11.2.2
temperature of the test liquid contained in the test tube should and Note4).When data on progressive changes with increasing
be made to ensure that the liquid is within the test temperature time of immersionaredesired, dip eachspecimen after
specified. weighing in alcohol (methanolor ethanol) to remove water(see
10.1.1.2 For volatile liquids, fit the test tube assembly with 11.2.3),blot dry withfilterpaper free oflintand foreign
a reflux condenser (see 8.2) andconditionatthespecified material,andagainimmersein the sametest liquid (see
temperaturewithinthe limits givenin5.1forthespecified 11.2.1).It is importantthat each manipulation following
length of time. A check of the actual temperature of the test removal of the test specimen from the test medium take place
liquid contained in the test tube should be madeto ensure that promptly with the least possible lapse in time. When utilizing
the test liquid is within the test temperature specified. liquids that tend to volatilize at room temperature, no more
10.2 After the immersion testhas proceeded for the required than 30 S should elapse between removal from the test liquid
length of time, removethe test specimens.If the immersion has and stopperingtheweighing bottle, and nomorethanan
been at elevated temperature, cool the test specimens to room additional 30 S between removal from the weighing bottle and
temperature by transferring them to a cool clean portionof the immersion in water.
test liquid for 30 to 60 min. Then dip the specimens quicklyin 11.2 Relatively viscous oilsmay be difficult to remove from
acetone at room temperature, blotlightly with filter paper free the specimens with a quick acetone dip and blotting or even
of lint and foreignmaterial, place them immediately in a tared, more vigorous wiping when specimens are cooled in the test
stoppered weighing bottle, and determine the mass after test, liquid after immersion; this can yield erroneous test results.
M*, of each specimen to the nearest 1 mg. Afterweighing, Refer to 10.3 for an alternate method of specimen cooling.
again immerse the test specimen in the same test liquid (see 11.2.1Reportiffreshtest liquid is used, whichcanbe a
11.2.1) ifdata are desired on the progressive changes that occurrequirement for certain test methods or specifications.
with increasing time of immersion. It is important that each 11.2.2 It is important that all air bubbles clinging tothe test
manipulation take place promptly with theleast possible lapse specimen be removed before weighing in distilled water. I€, in
of time. When utilizing liquids that tend to volatilize at room the course of weighing, air bubbles appear on the surface of the
temperature, no more than 30S should elapse between removal specimen, or the computed volumechanges 0.5 % in 5 min, the
fiom the test liquid and stoppering the weighing bottle. specimen is too porous to permit volume determination in this
10.3 Relatively viscous oilsmay be difficult to remove from manner. In that case, the initial volume of the specimen, if the
the specimens with a quick acetone dip and blotting or even latter is a simple geometricalsolid, can be determined from the
more vigorous wiping when the specimens are cooled in the overall dimensions by employing an appropriate mensuration
test liquid after immersion; this can yield erroneous test results.formula, and the same procedure followed in determining the
Since these oils do not readily volatilize, specimens maybe volume after the immersion test; or, if volume increase occurs
cooled by suspending them for about 30 min in air at room principally in thethickness dimension, a simple change in
temperature shielded fiom draft, after removal from the im- thickness may be substituted for change in volume. If, in the
mersion liquid at the testtemperature. This willallowthe courseofweighingthetestspecimenfloats,AIS1 No. 316
majority of the oil to drip off the surfaceof the specimen. Then stainlesssteelcan beused as ballast to immersethetest
proceed with the acetone dip and blotting as described in 10.2. specimen in the testliquid. In those cases where ballast is
Report whenthis alternate method of specimen coolingis used. neededtosubmergethespecimen,thefollowingprocedure
may be used.
11. Procedure for Change in Volume
11.2.2.1 Weigh the test specimen with ballast in water,
11.1 Water Displacement Method for Water-Insoluble Liq- 11.2.2.2 Weigh the ballast alone in water, and
uids and Mixed Liquids-Test three specimens, calculate the 11.2.2.3Determinethe difference between the weighings,
test results foreach specimen (see 17.2, Eq 2), and average the and proceed with the calculations.
results. Obtain the mass M , of each specimen (see 11.2.2) in 11.2.3 The acetone dip before and after immersion shall be
air,to the nearest 1 mg, and then obtain the mass M of each
omitted when water is employed as the test medium.
specimenimmersedin distilled wateratroomtemperature.
Quickly dip each specimen in alcohol (methanolor ethanol) to NOTE4-A jolly balance, adequatelyshielded from air currents, may be
remove water (see 11.2.3), blotdry with filter paper freeof lint used for making these determinations. When utilizing liquids that tend to
and foreign material, and place in theimmersionapparatus volatilize at room temperature, no more than 30 S should elapse between
removal from the test liquid and completion of the weighing operation.
described in 8.1 or 8.2. Add 100 cm3 of liquid (see 10.1.1) to
the test tube and complete the immersion test as described in 11.3 Displacement Method for Water-Soluble Liquids and
10.1.1.1or10.1.1.2. At the end ofthe requiredimmersion Mixed Liquids (Other Than WaterpFor immersionliquids
period,remove each specimen fromthetesttube.Coolthe that are readily miscible with water or react with it, the water
specimens to room temperature by transferring them to a cool, displacement method as described in 11.1 may not be suitable.
cleanportionofthetest liquidfor30 to 60 min,thendip For such liquids that are not too viscous or volatile at room

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 STD-ASTM D471-ENGL 3778 W 0759530 Ob547b4 773 S
471
temperature, weighings for M 2 andM4may be made in the chamber, B, which is held tightly against the test specimen, C,
immersion liquid instead of water with weighmg for M4 made by wingnuts, D, mounted on bolts, E. During the test, the
in a fresh portion of the immersion liquid. These values are opening in the top of the chamber is tightly closed by a suitable
then used in calculating volume change using Eq 2 in 17.2. If plug, F.
this is not practicable, the water displacement method shallbe 13.4 Procedure-Weigh thetestspecimen in air tothe
used,exceptthatthefinalweighingfor M4 isomittedand nearest1mg,record as M,, andplaceintheapparatus as
change in volumeis calculated according toEq 3 in 17.2. This indicated in Fig. 2. Fill the chamber of the apparatus with the
formula may be only approximate if the immersion liquid is a test liquid to a depth of 15 mm (0.6 in.), replace plug F and
mixture, because the density of the absorbed liquid may differ complete the testat the specified conditionsas described in 5.1
from that of the bulk. Also the densityof any matter extracted and 5.2. At theend of the required immersion period, bring the
from the rubber may differ from that of the immersion liquid. apparatus to standard room temperature, remove the test liquid,
and release the test specimen. Remove any excess liquid from
12. Dimensional-Change Method for Water-Insoluble the surface by wiping or blotting with filter paper free of lint
Liquids and Mixed Liquids and foreign material and place the specimen immediatelyin a
12.1DimensionalChangeMethod-Measuretheoriginal tared, stoppered weighmg bottle. Determine the mass of the
length and width of three test specimens used in 11.1 to the specimen to the nearest 1 mg and record as M z. When the
nearest 0.5 mm (0.02 in.) using an average of three measure- immersion liquid tends to volatilize at room temperature, no
ments in each direction recording the dimensions as L o and W,, morethan 30 S should elapsebetweenremovalofthetest
respectively. Measure the hckness of each test piece using a specimen from the liquid and stoppering the weighing bottle.
dial micrometeras described in 6.3 of TestMethods D 412, and Use Eq 5 in 17.4 to calculate test results. If more than one
record as T,. Placespecimensintheimmersionapparatus specimen of the same composition is tested, report the result as
described in 8.1 and 8.2.Add 100 cm3 of liquid (see 10.1.1) to the average.
the test tube and complete the immersion test as described in
10.1.1.1 or 10.1.1.2.Attheendoftherequiredimmersion 14. Procedure for Determining Mass of Soluble Matter
period, remove each specimen from the test tube and bring to Extracted by the Liquid
room temperature by transferring them to a cool clean portion 14.1 Th~stestmethodisapplicableforimmersions in
of the test liquid for 30 to 60 min. Dip the specimens quickly volatile-type immersion liquids, suchas ASTM reference fuels
in acetone at room temperature, blot lightly with filter paper (see6.1.2).Conducttheimmersions as describedin10.1,
free of lint and foreign material, and promptly remeasure as 10.1.1.1,and10.1.1.2.Testthreespecimens of asingle
described above, recording the immersed length, width, and composition, and report the result as the average.The extracted
thickness as L, W, and T, respectively. If the immersion liquid matter can be determined either by the difference in mass of the
tendstovolatilizeat roomtemperature,themeasurements specimen before and after immersion by or evaporating the test
should be completedwithin 30 S afterremovingthetest liquidandweighingthenon-volatileresidue(Note5).The
specimens from the liquid at room temperature. Calculate test mass is determined in air to the nearest 1 mg.
results according toEq 4 in 17.3 and report the average of three
NOTE5-Both methods are subject to error. Results obtained by the
specimens. mass difference of specimens before and after immersioncan be affected
by possible oxidation of the material during immersion. Results obtained
13. Procedure for Change in Mass with Liquid on One by evaporating the test liquid may be affected by partial loss of volatile
Surface Only extracted material during drying. The methodof choice will depend on the
13.1 Scope-Thistestmethodprovidesaprocedurefor material under test and the test conditions. For example, the evaporation
exposingthinsheetmaterials(rubber-coatedfabrics,dia- method would bepreferred if further testingis to be done on the extracted
matter.
phragms, etc.) that are in contact with the immersion liquid on
only one surface under definite conditions of time and tem- 14.2 Mass-Difference Method-At the end of the required
perature. immersion period, remove the test specimens from the tube test
13.2 Test Specimen- A disk 60 mm (2.4 in.) in diameter and dry to a constant mass at a temperature of approximately
and thickness oft h n sheet or rubber-coated fabric being tested. 40°C (104°F) and an absolute pressure20ofkPa (150mm Hg).
13.3Apparatus-Theessentialfeaturesareillustratedin Record the original mass of the test specimen before immer-
Fig. 2 and consist of a base plate,A, an open-ended cylindrical sion as M , , the mass after immersion as M 2 , and express the
change in mass as a percentage of the original mass, usingEq
6 in 17.5. Report the results as the average if more than one
specimen of the same composition is tested.
14.3 Evaporation Method-Transfer the liquid from the test
tube in which the three test specimens have been immersed to
a suitable vessel, wash the specimens inthetesttubethree
times with 25 cm3 of fresh liquid and transfer the liquid to the
same vessel.Evaporatetheliquid anddrytheresidue to a
constant mass under an absolute pressureof 20 kPa (150 mm
C Hg) and a temperature of approximately 40°C (104°F). Record
FIG. 2 Surface Immersion Apparatus the sum oftheoriginalmass of threespecimensbefore

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 STD.ASTM Dq73-ENGL 3498 m 0759530 Ob547b5 bOT 0
D 471
immersion as EM,,the mass of the dried residue as M,,and
express M, as a percentage of EM,,using Eq 7 in 17.5.
15. Changes in Tensile Strength,Elongation, and
Hardness
15.1 Original Properties-Theoriginaltensile strength,
ultimate elongation (Test Methods D 412, Die C)and hardness
(Test Methods D 1415 or D 2240) shall be determined, using
three specimens cut from the sheet or article adjacent to those
that are tobeimmersedintheliquid.Reportresultsin
accordance with the appropriate test method.
15.2 Immediate Deteriorated Properties-For determining
the tensile strength, ultimate elongation, and hardness, prepare
t h r e e test specimens from flat vulcanized sheets 2.02 0.1 mm
(0.08t 0.004in.) in thickness (see 9.1) using Die C of Test
Methods D 412. Measure the thickness of each test specimen,
place the specimens in the test tube described in 8.1, and add
150 cm3 of liquid (see 10.1.1) to the test tube. Complete the
immersion period in accordance with 10.1.1.1 or 10.1.1.2. At
the end of the required immersion period, remove the speci-
mens from thetesttubesandcoolimmediatelytoroom
temperature in a fresh sample of the same liquid for 30 to 60
min. Then quicklydip each sample in acetoneand blot lightly
with filter paper that is free of lint and foreign material and
immediately apply bench marks.
15.2.1 Determine the tensile strength and ultimate elonga-
tion in accordance with Test Methods D 412, using the original
unimmersed thickness or cross-sectional area (see17.6, Eq 8).
Determine the hardness of each immersed specimen in accor-
dance with Test MethodsD 1415 or D 2240. The time interval
between removal from the cool liquid and testing shall be not
less than 2 nor more than 3 min.
15.2.2 It may be desirable to calculate the tensile strength
based on the swollen cross-sectional area. In that case Eq 9 in
17.6 shall be used. Report when this method of calculation is
employed.
15.3 Relatively viscous oilsmay be difficult to remove from
the specimens with a quick acetone dip and blotting or even
more vigorous wiping when specimens are cooled in the test
liquid after immersion; this can yield erroneous test results.
Refer to 10.3 for an alternate method of specimen cooling.
15.4 Properties After Evaporation of Test Liquid-This test
method is applicable for immersions in volatile-type immer-
sion liquids, such as AST" reference fuels (see 6.1.2). For
determiningthetensilestrength,ultimateelongation,and
hardness of specimensafterevaporation ofthe immersion
liquid, immerse the specimens in the test liquid in accordance
with 15.2. At the end of the required immersion time, remove
the specimens and,if necessary, cool them to roomtemperature
in a fresh sample of the same liquid for 30 to 60 min.
15.4.1 For room temperature drying, suspend the specimens
for 4 2 0.25 h in air at ambient conditions shielded from drafts.
Afterthedryingperiodapplybenchmarksanddetermine
tensilestrength andultimateelongation in accordancewith
TestMethods D 412 usingthe originalthicknessorcross-
sectionalarea of theuntreatedspecimens(see 17.6, 8) and
hardness according to Test Methods D 1415 or D 2240.
15.4.2 For determining properties after complete evapora-
tion of thetestliquid,suspendspecimensafterthe 4-h
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airdryiig cycle at room temperaturefor 20 h 2 15 min at 70 t
2°C (158 2 4°F) in a circulating-airoven. Afterthe heat drying
cycle, removethe specimens from theoven, allow them to cool
to room temperature and measure the required physical prop-
erties as described in 15.4.1. Reportwhentheheatdrying
procedure is used.
15.5 The tensile strength and ultimate elongationafter
immersion and evaporation also can be expressed as percent
changefromtheoriginalvalues,usingEq 10 in 17.6, and
hardness in unit change from the original value, according to
Eq 11 in 17.6.
16. Changes in Breaking Resistance, Burst Strength, Tear
Strength, and Adhesion for Coated Fabrics
16.1 Original Properties-The original properties for
breaking resistance, burst strength, tear strength, and adhesion
shall be determined in accordance with Test Method D 751,
using the specified number of specimens cut from the coated
fabric adjacentto those that are tobe immersed in the liquid, or,
ifnecessary, from other pieces of coated fabric thatwere
producedfrom the same lot(s) of materials underthesame
conditions.
16.2 Immediate Deteriorated Properties-For determining
breaking resistance, burst strength, tear strength, and adhesion,
prepare the number of specimens specifiedfor each parameter
inTestMethod D 751. Place the specimens in the test tube
described in 8.1 and add 150 cm3 of liquid (see 10.1.l)to the
testtube.Completetheimmersion test inaccordance with
10.1.1.1 or 10.1.1.2. At theend of therequiredimmersion
period,remove the specimens from the test tubes, and cool
immediately to room temperaturein a fresh sample of the same
liquid for 30 to 60 min. Then quickly dip each specimen in
acetone and blot lightly with filter paper that is free of lint or
foreign material. Measure the required physical properties in
accordancewithTestMethod D 751 (see 17.7). Thetime
interval between removal from the cool liquid and testing shall
be not less than 2 min nor more than 3 min.
16.3 Relatively viscousoils may be difficult to remove from
the specimens with a quick acetone dip and blotting or even
more vigorous wiping when specimens are cooled in the test
liquid after immersion; this can yield erroneous test results.
Refer to 10.3 for an alternate method of specimen cooling.
16.4 Properties After Evaporation of Volatile Test Liquid-
Fordeterminingbreakingresistance,burst strength, tear
strength,and adhesion of specimens after evaporation of a
volatile immersion liquid, such as ASTM reference fuels (see
6.1.2), immerse the specimens in the test liquid in accordance
with 15.2. At the end of the required immersion time, remove
thespecimens, suspend them for 2 h 2 5 minatambient
conditionsshieldedfrom draft andthen place them in a
circulating-air ovenat a temperature of 70 t 2°C (158 t 4°F)
for a period of 2 h t 5 min. At the end of the drying period,
removethe specimens fromtheoven, allow themto cool to
room temperature and measure the required physical properties
inaccordancewithTestMethod D 751 (see 17.7). The time
interval between removal from the oven and testing shall be not
less than 1 h nor more than 2 h.
 16.5 If desired, report results after immersion and evapora- where:
tion in percent change from the original property values, as ME = extractedsolublematter, %,
described in 15.5. M, = initialmass of specimeninair, g,
M2 = mass of specimen in air after immersion and drying,
17. Calculation g9

EMl = sum of the initial mass of three specimens in air, g,

17.1Calculatethepercentchangeinmass as follows and
(Sec tion O):
1 M3 = mass of theresidueinairafterevaporatingand
(M2 - Ml) drying the immersion liquid of three specimens, g.
U,%= (1)
Ml
17.6Calculatetensilestrength of thespecimensbothon
where: immediate deteriorated properties and properties after evapo-
AM = changeinmass, %,
ration of the test liquid as described in the Calculation section
M, = initialmass of specimenin air, g, and
M, = mass of specimeninairafterimmersion, g. of Test Methods D 412.
17.6.1Basedontheoriginalunstretchedcross-sectional
17.2Calculatethepercentchange in volume as follows area:
(Section Il):
F
-
TS, = A (8)

17.6.2Basedontheswollenunstretchedcross-sectional
area:
F
TS, = (9)
where:
AV = change in volume, %,
M, = initial mass of specimen in air, g,
(
A 1+- K)"
17.6.3 To express tensile strength and ultimate elongation
M , = initial mass of specimen in water, g, afterimmersion as apercentagechangefromtheoriginal
M3 = mass of specimen in air after immersion, g ,
properties, use the following formula:
M4 = mass of specimen in water after immersion, g, and
d = density of immersion liquid at standard laboratory Pi- P,
D,%=- .lo0 ( 10)
room temperature, Mg/m '. Po

17.3 Calculate the percent changein dimensions as follows 17.6.4 Calculate hardness change after immersion in hard-
(Section12): ness units:
AH=Hi-H, (11)

where:
where: TS, = tensilestressbasedonoriginalunstretchedcross-
AL = change in length, %, sectional area,
= initial length of specimen, mm, and TS, = tensilestressbasedonswollenunstretchedcross-
L = lengthofspecimenafterimmersion,mm. sectional area,
Calculate the percent change in width, AW, and thickness, F = observed force,
AT, accordingly. A = original unstretched cross-sectional area of the test
specimen before immersion,
17.4 Calculate the change in mass for single surface expo- AV = volume swell after immersion, %,
sure as follows (Section 13): A P = change in property(tensilestrengthandultimate
elongation) after immersion, %,
P, = original property before immersion,
Pi = property after immersion,
where: A H = hardness change after immersion, units,
AM, = change in mass per unit surface area, kg/m2, H, = original hardness before immersion, units, and
M, = initial mass of specimen in air, g, H , = hardness after immersion, units.
M, = mass of specimen in air after exposure to the test 17.7Calculatebreakingresistance,burststrength,tear
liquid, g, and strength,andadhesionbothontheimmediatedeteriorated
A = area of the specimen in actual contact with the test propertiesandpropertiesafterevaporationofvolatiletest
liquid, m m 2 . liquid as described in Test Method D 751. If desired, results
17.5 Calculate percent extracted soluble matter as follows may also be expressed in percentage change after immersion as
(Section 14): detailed in 17.6.3.

18. Report
18.1 State that the test was conducted in accordance with
Test Method D 471 and report the following:

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 S T D - A S T M D47L-ENGL L998
471
18.1.1 Description of the sample and its origin,
18.1.2 Date and temperature of testing room (see 5.1),
18.1.3 Duration, temperature, and date of vulcanization of
test specimens,
18.1.4 Dates of the various periods of exposure,
18.1.5 Immersion liquid used,
18.1.6 Temperature of exposure,
18.1.7 Exposure period,
18.1.8 All observedand recorded data,to include the typeof
properties being reported,
18.1.9 Results calculated in accordance with Section 17,
18.l . 10 Statement of condition of exposed specimens from
visual and manual examination,
18.1.11 Report which test method was used for determina-
tion of hardness, and
18.1.12 Any deviations from standard test methods.
19. Precision and Bias
19.1 This precision andbiassectiondeals withproperty
changes in tensile strength, ultimate elongation, hardness, and
volume after immersion in test liquids and has been prepared
accordance with Practice D 4483. Refer to this practice for
terminology and other statistical calculation details.
19.2 The precision results in this precision and bias section
give an estimate of the precision of this test method with the
materials used inthe particular interlaboratory test programas
described in the following paragraphs. The precision param-
eters should not be used for acceptance or rejection testing of
any group of materials without documentation thatthe param-
eters are applicable to the particulargroup of materials and the method has been establishedas the appropriate value tabulated
specific testing protocols of the test method.
19.3 A Type 1 interlaboratory test programwas evaluated in
1981 using six different vulcanized rubber compounds (mate-
rials). These compounds were prepared in one laboratory and
test specimens were distributed to nine participating laborato-
ries. Each laboratory prepared and purchased from approved
sources, the liquids and fuels, or both, used for testing. A test
result (asused for these calculations) is the average of three
individualtestspecimenvalues.Eachlaboratoryconducted
tests (that is, obtained one test result) on each of two days. Both method. Bias, therefore, cannot be determined.
repeatabilityandreproducibilityarethereforeshortterm;
period of a few days separates test results.
Details and suppotting data of the precision evaluation program are available
in a research report from ASTM Headquarters. Request RR: Dll-1069.
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0754510 Ob547b7 Y82 9
19.4 Theresults oftheprecision evaluation are givenin
Table 5 and Table6 for eachof the six rubbers or materials for
immersion tests in(I) Reference FuelsB, C and D, for 70 h at
23 2 2°C (73 2 4"F),and (2) ASTM Oil No. 2 and ASTM Oil
No. 3 for 70 h at 150 2 2°C (302 2 4°F).
19.5 The precision is given in terms of Sc r, SR, and R for
four measured physical properties: (I)percent change intensile
strength, (2) percentchange in ultimate elongation (that is,
percent change in percent elongation), (3) hardness change in
hardness units, and (4) percent change in volume of the test
specimen. No values are given for ( r) and (R), the normal
precision parameters used to express relative precision because
numerous average values for properties ( I ) , (2), and ( 4) are
near zero, thus resulting in extremely large ( r) and (R) values.
These large values are essentially meaningless for precision
comparisons when average values are near zero.
19.6 The precision of the test method may be expressed in
the following statements thatuse an appropriate valueof r and
R. The appropriate valueis that value of r or R, associated with
a mean level inthetablesclosesttothemean level under
in consideration for any immersion liquid or rubber, for any test
result for a similar material in routine testing operations.
19.7 Repeutubility- The repeatability, r, of this test method
has been established as the appropriate value tabulated in Table
5 and Table 6. Two single test results, obtained under normal
test method procedures, that differby more than this tabulated
r (for any given level) must be considered as derived from
different or nonidentical sample populations.
19.8 Reproducibility- The reproducibility, R, of this test
in Table 4 through Table 6. Two single test results obtained in
twodifferentlaboratories,undernormaltestmethodproce-
dures, that differ by more than the tabulated R (for any given
value) must be consideredto havecomefrom dfferent or
nonidentical sample populations.
19.9 Bias"1n testterminology,bias is the difference be-
tween an average test value and the reference (or true) value.
Reference values do not exist for th~stest method since the
value (of the test property) is exclusively defined by the test
a
20. Keywords
20.1 elevated temperature; fluid immersion; liquid immer-
sion; reference fuel; rubber articles; rubber products; service
liquid
 STD-ASTM D471-ENGL 1998 m 0759520 06547b8 319 m
e# D 471
TABLE 5 Tvw 1 Precision DataA
Change
StrenMh,
Tensile
in % Elongation.%
Hardness.
Units
Chanae
in
Chanae
in
_____

bWithin-Lab Rubber
Mean Sr r Sß ß Mean Sr r SR ß Mean Sr r Sß R
ASTM Reference fuel B:
CR 2.1 0.76 -16.0 15.2-48.05.36 12.9
3.124.55 -43.7
8.8 9.2 3.26 1.87 5.3
FKM -2.3 1.94
10.1 -7.9
3.58 9.2 3.25 -0.15.510.0 3.55 4.80.901.68 2.6
0 2.47 -27.1FVMQ
17.2 6.08 11.8 4.17 -30.6
3.44 -50.3 12.1
NBR-1 4.27 8.2 2.90 -63.6
2.59 -11.8NBR-2
4.19 -26.0 14.8
CO 5.23 9.5 3.35 -8.6
Pooled Values
12.6 4.47 ___8.7 3.07 ... 3.52 10.0 5.38 15.2 1.76 ...2.8 0.98 5.0
ASTM Reference fuel C:
2 9.9 3.49
CR 7.6 2.70 -57.4
.32 -11.1 FKM
2.74 -30.9FVMQ 5.08.1 2.87
NBR-1 -68.9 2.77 7.8 4.17 11.8 -58.1 5.27 14.9 5.53 15.7 -10.7 1.33 3.8 1.22 3.5
NBR-2 -14.8 3.78 10.7 5.15 14.6 -21.0 2.87 8.1 6.30 17.8 -18.3 1.12 3.2 2.95 8.3
CO -18.0 3.24 9.2 3.38 9.6 -33.9 4.52 12.8 2.64 7.5 -17.3 1.18 3.3 1.85 5.2
Pwled Values ... 3.10 8.814.6 5.16 16.2 5.73... 11.0 3.89 6.9 2.43... 3.8 1.35
ASTM Reference fuel D:
1.83 -50.9 CR
6.6 2.36 7.6 2.69 -54.8 7.3
0.602.57 1.7
3 -0.2 17.0 FKM6.00 6.4 2.26 -9.2
3.44 -28.5 16.7
FVMQ 5.90 9.8 3.45 -33.2
.7 2.35-55.8NBR-1
11.3 4.00 5.7 2.01-67.4 2.8 0.98 3.0 5.05
1.06 -10.9 14.3
3.05 -12.4NBR-2 9.6 3.39
-15.12.2 0.79
CO 3.02 -14.6 9.7 3.41
8.59.5
3.3 3.36
1.17 -15.3 9.4 3.31
-30.0 8.7 3.08
Pooled Values
12.1 4.29 ...7.9 2.81 15.9 5.63 ... 7.4 2.63 7.6 2.67 ... 2.9 1.02
ASTM oil No. 1:
CR 7.9 2.78-15.4 51.94 5.5 14.7 5.20
.01 -31.3 14.2 7.9 2.80 3.9 1.39 -8.6
FKM6.11 14.8 5.25 -6.1
4.38 -9.3 17.3
.8 4.89-11.9FVMQ
26.8 9.48 16.8 5.93 -4.3 9.0 3.20
-2.4 4.4 1.54
NBR-1 3.55-18.9 29.710.4914.3 5.07-12.518.1 6.38
10.0 7.8 -4.0
2.74 3.1 1.09
3.38 -7.7 NBR-2
CO20.5 7.25 13.6 4.81 20.2 9.2 3.24 1.9 0.67 8.6 11.8-48.5 4.17 10.5 3.72
~~~ ~~ ~

... 12.5 4.43

Pwled Values21.3 7.52 18.5 6.55...11.5 4.06 8.8 3.11 ... 3.8 1.36
ASTM Oil No. 3:
11.9 4.19 9.7 3.43-42.5
CR 12.6 4.46 3.6 1.27-19.112.5 4.41
-42.07.5 2.64
95 12.9 4.58 FKM
-2.4 48.717.2012.1 4.27-11.3 10.4 3.67 3.3
22.51.15 -2.9
14.9 5.28-17.9 30.110.65 8.0 2.84-18.2
FVMQ
NBR-I 5.32-37.2 12.19
17.36.12
-19.536.6
15.1 12.82 34.5 -12.7 13.2 4.67 4.1
1.44
3 5.67
2.22 -27.0
3.9
NBR-2 1.39 10.6 16.2 5.72 17.3 3.80 -69.7
16.041.4 14.64
CO 29.110.2918.4 6.50 21.7
10.7 5.42-39.7 2.73 2.8 0.97 3.3 12.4 4.40 7.7

_ _ _ _ ~
... 13.7 4.85
Pooled Values 34.9 12.33
____ _____~~
... 13.5 4.76
21.4 7.55
~~~ _____ ~~
10.2 3.61... 3.5 1.25
%r = repeatabilitystandarddeviation,inmeasurementunits, r = repeatability = 2.83 x Sr, SR = reproducibilitystandarddeviation,inmeasurementunits,and
R = reproducibility = 2.83 x SR.

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 STD-ASTM D473-ENGL L998 m 0759530 Ob547b9 255 R
D 471
TABLE 6 Precision Data"
Change in Volume, %
Rubber Within-Laboratory
Mean Sr r SR R
ASTM Reference Fuel 13:
CR 66.2 0.94 2.7 5.40 15.3
FW 1.5 0.36 1.o 0.34 1.o
FVMQ 5.1 0.48 1.4 0.92 2.8
NBR-1 46.9 0.38 1.1 3.96 11.2
NBR-2 12.0 0.73 2.1 0.63 1.8
CO 15.6 0.39 1.o 1.27 3.6
ues Pooled ... 0.60 1.7 2.95 8.4
~

ASTM Refemnce Fuel C:

CR1 108.9 4.99 .o4 2.9 14.1
0.46FKM 2.6 0.32 0.9
FVMQ 17.8 1.61 0.53 1.5 4.5
0.59NBR-1 76.8
NBR-2 2 22.6 O .69 .o o.n 2.2
0.51 CO 25.3
Pooled 7.4 ... 2.60 0.64 1.8
ASTM Reference Fuel D:
1.52 CR 90.6
FKM 2.3 0.33 0.9 0.56 1.6
FVMQ 8.6 15.9 3.05 0.92 2.6
NBR-1 5.9
1.23 62.2 2.10 3.5
NBR-2 4.4 1.55 .38 3.9
0.89 CO 3.5 20.4 1.25 2.5
Pooled Values
6.4 ... 2.26 1.11 3.1
ASTM Oil No. I :
CR 15.8 0.50 1.4 0.61 1.7
F W 1.2 0.29 0.8 1.12 3.2
FVMP 0.6 0.57 1.6 1.O5 3.0
NBR-1 3.4 0.69 1.9 1.a8 5.3
NBR-2 -11.2 0.45 1.3 0.47 1.3
CO -5.2 0.42 1.2 0.64 1.8
Pooled Values ... 0.50 1.4 1.67 4.7
ASTM Oil No. 3:
CR1 2.9 75.6 .O3 1.84 5.2
1.47FKM 3.1
0.61FVMQ 2.8
0.18
NBR-1 31.4
1.9
NBR-2 -2.1 0.67 0.14 2.5
0.24
CO 4.2 0.7 0.77 2.2
Pooled 7.6 ... 2.70 0.88 2.5
= repeatabilitystandarddeviation,inmeasurementunits, r = repeatability = 2.83 X Sr, S ß = reproducibilitystandarddeviation,inmeasurementunits,and
R = reproducibility = 2.83 x SR.

APPENDIXES

(Nonmandatory Information)

X1. REPLACEMENT OF ASTM OILS NO. 2 AND NO. 3 WITH IRM 902 AND IRM 903

X1.1 ASTM Oils No. 2 and No. 3 became subjectto cancer different suppliers, using twelve different types of vulcanized
hazard warning label requirements under the OSHA Hazard rubbers.Asaresult of this ITF', two oilsfromCalumet
Communication Standard, published November 25, 1983.This Lubricants Company were selected as best (but not equivalent)
contributed to the discontinuation of commercial production in matches for the ASTM oils, and confirmed independently by
1990. ASTMSubcommittee D11.15 andthe SAE Committeeon
X1.2 ASTM Subcommittee Dl 1.15 on Degradation Testing Automotive Rubber Specifications (SAE-CARS). Calumet No.
began a program in 1985-1986 to establish replacements for 2, the replacement for No. 2 oil, provided a closer match than
these oils, with the objective to match the action on vulcanized Calumet No. 3, the replacement for No. 3 oil. The two oils
rubbers as closely as possible, while eliminating the need for wereestablishedasindustryreferencematerials, IRM 902
cancerhazardlabeling(negativemodifiedAmesTest). An (Calumet No. 2, replacement for ASTM Oil No. 2) and IRM
interlaboratory test program (ITP) was organized in 1993 with 903 (Calumet No. 3, replacement for ASTM Oil No. 3).
six candidate oils as No. 2 and No. 3 replacements from three X1.2.1 Details of the 1°F' are described in Research Report

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 STDmASTM D471-ENGL 1998 m 0759510 Ob54770 T77 E
0)D 471
RR: Dll-1069, which can be obtained from ASTM headquar- was depleted by the end of 1993, Committee D-11 published
ters. A precision statement on volume swells generated in this Emergency StandardES 27 in 1994 to address the replacement
test program is given in AppendixX2. with IRM 902 and IRM 903.
X1.3 Since the inventory of ASTM Oils No. 2 and No. 3

X2. PRECISION AND BIAETEST PROGRAM FOR THE REPLACEMENT OF ASTM OILS NO. 2 AND NO. 3

X2.1 This precisionstatementwaspreparedusing data TABLE X2.1 Precision Data for Within-Laboratory Variation
from the comprehensiveITP evaluation program conducted in NOTE1-Sr = repeatability standard deviation,
1993 to establish replacement oils for ASTM Oils No. 2 and r = repeatability = 2.83 X Sr, ( r ) = repeatability on relative basis (per-
No. 3. Because of the limited number of laboratories (three), cent of percent), and CV = coefficient of variation, % = (Sr/
onlywithin-laboratoryvariation or repeatabilitycould be Mean) X 100.
evaluated.Someterminologyused in thisappendixiscon- Change in Volume, % (Pooled Values)
Rubber
tainedinPracticeD4483.Refer to PracticeD4483for Mean Sr r (0 cv
background details. ASTM Oil No. 2 TypesA
42.2 119.0 ACM1.60 0.57 1.3
X2.2Intheevaluationprogramtwelvecompoundswere 3.0 8.4 AEM
2.33 0.82 27.8
tested in groups of four; each group of fourwas tested
4.5 by three
12.8 CR4.61 1.63 36.0
laboratories. There are only three duplicates (one duplicate set ECO 42.7 1.65
EPDM 6.14
0.58
2.17
3.9
120.2 5.1
15.1
1.8
of tests in each laboratory) for an estimate of within-laboratory EVM
1.8 4.9 1.68
34.1 0.60
variationforanycombinationofrubberandoil. 27.0is an 76.5 FKM0.57
This 0.20 0.7
FVMQ
inadequate number of degrees of freedom (DF) for such an 70.0 198.0HNBR 0.87 0.31
0.30
0.4
9.4 0.85 9.1 0.3
estimate. However, a reasonable assumption may4.be6 made 13 that
.1 NBR
0.99 0.35 7.6
for any given rubber, the true test variation with each of the TPV 1.98 48.4 54..612 11.6
13.1 37.0 VMQ 3.84 1.36 10.4
four oilsis equivalent. On this basis for any candidate of setthe
ASTM Oil No. 3 Typesf
four oils, the three DF estimates of test standard 1deviation
5.8
for
44.6 ACM
3.71 1.31 8.3
each of the four oils may be pooled to obtain1.a4 twelve DF 4.0 AEM
2.01 0.71 50.3
estimate of teststandarddeviation.Thewithin-laboratory CR 1.768.1 41.15
.8 3.26
ECO
3.48 1.22 7.1 48.5 17.1
precision of this appendix is based on such pooled values. 3.2 9.1 EPDM 14.70 5.19 161.5
1.8 5.0 EVM
2.94 1.04 58.7
X2.3Theprecisionresults are given inTableX2.1for FKM 20.9
1.6 59.1
0.34 0.95
percentvolumeswell. ThIs is theonlypropertythatwas21.0 59.5 FVMQ1.21 0.43 2.0
it shows the highest 2.9
evaluated for precision, since 8.1to HNBR
sensitivity 1.29 0.46 15.9
4.9 13.8 NBR 2.05 0.72 14.8
variation. 2.4 6.8 TPV
5.43 1.92 79.5
VMQ
6.52 2.30 43.4 15.0 5.3
X2.4TableX2.1 lists the repeatability standard deviation, APooled results for No. 2 oil plus three candidate replacements.
Sr; the repeatability, r , in units of% volume swell, the relative BPooled results for No. 3 oil plus three candidate replacements.
repeatability, ( r), which is a percent of a percent for volume
swell measurements, and for completeness, the coefficient of selecting the level of volume swell value in Table X2.1 closest
variation, CV, in %. The mean volume swell values range from to the measured volume swell of the commercial rubber.
nearzerotoabout 160 %. The precisionparameters also X2.5.1 Two test results of the commercial rubber that differ
display a wide range. Regression and graphical analysis revealsby more than the tabulated r or (r) values as selected by the
that (1) there is a direct (positive slope) log-log relationship for above process, mustbe considered to have come from different
Sr versus mean volume swell, and (2 ) an inverse (negative sample populations (that is, be significantly different).
slope) relationship between the relative repeatability ( r ) and X2.5.2 Alternatively normal testing operations should pro-
mean volume swell. These relationships apply to both sets of duce values for duplicate test results that are within the r and
data and to the combined data sets. (r) intervals as selected by the above process.
X2.5 The results of Table X2.1 may be applied to within- X2.6Biasreferencevaluesdonotexistforthistypeof
laboratory data comparisons using either IRM 902 or IRM 903 testing, since the value of the test property is defined exclu-
for any commercial or proprietary compound by selecting the sively by thetestmethod.Bias,therefore,cannotbedeter-
Table X2.1 rubber closest to the commercial compound and mined.

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 STD-ASTM D47L-ENGL L998 0759510
Ob54771 903 m

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