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1. Scope 1.6 ASTM No. 5 Oil was accepted into Specification D5900
1.1 This test method covers the required procedures to as an industry reference material in 2010 and designated as
evaluate the comparative ability of rubber and rubber-like IRM 905. The composition, and properties of this immersion
compositions to withstand the effect of liquids. It is designed oil were not changed and the data in Table 1 remains current.
for testing: (1) specimens of vulcanized rubber cut from Refer to Appendix X4 for other details.
standard sheets (see Practice D3182), (2) specimens cut from 1.7 The specifications and properties listed in Table 1 for
fabric coated with vulcanized rubber (see Test Methods D751), IRM 901, IRM 902, IRM 903, and IRM 905 are also
or (3) finished articles of commerce (see Practice D3183). This maintained in Specification D5900.
test method is not applicable to the testing of cellular rubbers, 1.7.1 The subcommittee responsible for maintaining Test
in 2005 was replaced with IRM 901; refer to Table 1 and 1.10 The values stated in SI units are to be regarded as the
Appendix X3 for details. standard. The values in parentheses are for information only.
1.11 This standard does not purport to address all of the
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This test method is under the jurisdiction of ASTM Committee D11 on Rubber safety concerns, if any, associated with its use. It is the
and is the direct responsibility of Subcommittee D11.15 on Degradation Tests.
responsibility of the user of this standard to establish appro-
Current edition approved July 1, 2016. Published July 2016. Originally approved
in 1937. Last previous edition approved in 2016 as D471 – 16. DOI: 10.1520/ priate safety and health practices and determine the applica-
D0471-16A. bility of regulatory limitations prior to use.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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TABLE 1 Specifications and Typical Properties of IRM Reference Oils
Property IRM 901A IRM 902 IRM 903 IRM 905 ASTM Method
Specified Properties:
Aniline Point, °C (°F) 124 ± 1 (255 ± 2) 93 ± 3 (199 ± 5) 70 ± 1 (158 ± 2) 115 ± 1 (239± 2) D611
Kinematic Viscosity
(mm2/s [cSt])
38°C (100°F) ... 31.9–34.1 ... D445
99°C (210°F) 18.12–20.34 19.2–21.5 ... 10.8–11.9 D445
Gravity, API, 16°C 28.8 ± 1 19.0–21.0 21.0–23.0 ... D287
(60°F)
Viscosity-Gravity Con- 0.790–0.805 0.860–0.870 0.875–0.885 ... D2501
stant
Typical Properties:
Pour Point, °C (°F) −12 (10) −15 (5) −42.8 (−45) −15 (5) D97
ASTM Color L 3.5 L 2.0 L 0.5 L 1.0 D1500
Refractive Index 1.4848 1.5083 1.5004 1.4808 D1747
UV Absorbance, 260 nm 0.8 1.43 1.43 ... D2008
Aromatics, CA (%) 3 10 12 4 D2140
A
Refer to Appendix X3. Table X3.1 reflects the differences in the properties between ASTM No. 1 Oil and IRM 901 for reference purposes.
Naphthenics, 26 26 27 28
Paraffinics, 71 71 69 70
D2140 70 72 71
Cp% 71 71 71 70
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D1500 Test Method for ASTM Color of Petroleum Products 3.3 The precision statement in Appendix X2 is based on an
(ASTM Color Scale) interlaboratory test program conducted in 1993 to establish
D1747 Test Method for Refractive Index of Viscous Mate- replacements for ASTM Oils No. 2 and No. 3. Because of the
rials limited number of participating laboratories, only repeatability
D2008 Test Method for Ultraviolet Absorbance and Absorp- could be evaluated, and it was necessary to use pooled values
tivity of Petroleum Products of four No. 2 type oils (No. 2 plus three candidate replacement
D2140 Practice for Calculating Carbon-Type Composition oils) and four No. 3 type oils (No. 3 plus three candidate
of Insulating Oils of Petroleum Origin replacement oils). Twelve rubbers were tested in this program.
D2240 Test Method for Rubber Property—Durometer Hard- 3.4 ASTM Oils No. 1, No. 2, and No. 3 have been replaced
ness
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TABLE 3 B: Immersion Periods (continued) TABLE 4 ASTM Reference Fuels
Immersion Period, h Fuel Type Composition, Volume %
22 Reference Fuel A IsooctaneA , 100
46 Reference Fuel B IsooctaneA , 70; TolueneA , 30
70 Reference Fuel C IsooctaneA , 50; TolueneA , 50
166 Reference Fuel D IsooctaneA , 60; TolueneA , 40
670 Reference Fuel E TolueneA , 100
1006 Reference Fuel F Diesel Fuel, Grade No. 2B , 100
2998 Reference Fuel G Fuel D, 85; anhydrous denatured ethanolC , 15
4990 Reference Fuel H Fuel C, 85; anhydrous denatured ethanolC , 15
Reference Fuel I Fuel C, 85; anhydrous methanol, 15
Reference Fuel K Fuel C, 15; anhydrous methanol, 85
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tightly fitted to the immersion tube by means of a stopper (see
8.2.1). The bottom of the condenser tube shall project about 12
mm (0.47 in.) below the stopper. A suitable (water-cooled)
reflux condenser shall be used for water or other low-boiling
liquids. Glass beads shall be used as in 8.1.
8.2.1 The stopper shall not contaminate the test liquid.
When in doubt, cover the stopper with aluminum foil.
8.3 Maintaining Test Temperatures—The apparatus and
method chosen to maintain the specified temperature during
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9. Alternative Test Specimens and Dual Level Specimen 11.1.1 Test liquids shall not be reused.
Hangars 11.1.1.1 For non-volatile liquids, condition the test tube
9.1 Alternative specimens to those enumerated in Sections assembly at the specified temperature within the limits given in
10, 11, 12, and 14 shall be 25 by 25 by 2.0 6 0.1 mm or 1.0 5.1 for the specified length of time. A check of the actual
by 1.0 by 0.079 6 0.004 in. and prepared as described in the temperature of the test liquid contained in the test tube should
test specimen sections of each. be made to ensure that the liquid is within the test temperature
9.1.1 The employment of alternative specimens shall be specified.
noted in the report, refer to 19.1.12, or when the specimen 11.1.1.2 For volatile liquids, fit the test tube assembly with
differs in size or configuration from that described in the a reflux condenser (see 8.2) and condition at the specified
9.3 The specimens may be used in performing different 11.2 After the immersion test has proceeded for the required
post-immersion tests. length of time, remove the test specimens. If the immersion has
been at elevated temperature, cool the test specimens to room
9.4 When employing a dual level specimen hangar (Fig. 1), temperature by transferring them to a cool clean portion of the
immersion specimens shall be from a single source (sample) test liquid for 30 to 60 min. Then dip the specimens quickly in
and identical composition. Immersion and specimen suspen- acetone (see Note 4) at room temperature, blot lightly with
sion shall follow the procedure described in Section 8. filter paper free of lint and foreign material, place them
9.5 When combining specimens of differing configurations, immediately in a tared, stoppered weighing bottle, and deter-
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test tube. Cool the specimens to room temperature by transfer- NOTE 5—A Jolly balance, adequately shielded from air currents, may be
ring them to a cool, clean portion of the test liquid for 30 to 60 used for making these determinations. When utilizing liquids that tend to
volatilize at room temperature, no more than 30 s should elapse between
min, then dip quickly in acetone (see Note 4) at room removal from the test liquid and completion of the weighing operation.
temperature, blot lightly with filter paper free of lint or foreign
material, place in a tared, stoppered weighing bottle, weigh, 12.3 Displacement Method for Water-Soluble Liquids and
and record the mass as M3. Remove each specimen from the Mixed Liquids (Other Than Water)—For immersion liquids
bottle, weigh in distilled water, and record the mass as M4 in that are readily miscible with water or react with it, the water
immediate consecutive order to determine the water displace- displacement method as described in 12.1 may not be suitable.
ment after immersion (see 12.2.2 and Note 5). When data on For such liquids that are not too viscous or volatile at room
progressive changes with increasing time of immersion are temperature, weighings for M2 and M4 may be made in the
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6 in 18.5. Report the results as the average if more than one
specimen of the same composition is tested.
15.3 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 in the test tube three
times with 25 cm3 of fresh liquid and transfer the liquid to the
same vessel. Evaporate the liquid and dry the residue to a
constant mass under an absolute pressure of 20 kPa (150 mm
Hg) and a temperature of approximately 40°C (104°F). Record
FIG. 2 Typical Surface Immersion Apparatus
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liquid, immerse the specimens in the test liquid in accordance strength, and adhesion of specimens after evaporation of a
with 16.2. At the end of the required immersion time, remove volatile immersion liquid, such as ASTM reference fuels (see
the specimens and, if necessary, cool them to room temperature 6.1.2), immerse the specimens in the test liquid in accordance
in a fresh sample of the same liquid for 30 to 60 min. with 16.2. At the end of the required immersion time, remove
16.4.1 For room temperature drying, suspend the specimens the specimens, suspend them for 2 h 6 5 min at ambient
for 4 6 0.25 h in air at ambient conditions shielded from drafts. conditions shielded from draft and then place them in a
After the drying period apply bench marks and determine circulating-air oven at a temperature of 70 6 2°C (158 6 4°F)
tensile strength and ultimate elongation in accordance with for a period of 2 h 6 5 min. At the end of the drying period,
Test Methods D412 using the original thickness or cross- remove the specimens from the oven, allow them to cool to
sectional area of the untreated specimens (see 18.6, Eq 8) and room temperature and measure the required physical properties
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where: ∆P = change in property (tensile strength and ultimate
∆MA = change in mass per unit surface area, kg/m2, elongation) after immersion, %,
M1 = initial mass of specimen in air, g, Po = original property before immersion,
M 2 = mass of specimen in air after exposure to the test Pi = property after immersion,
liquid, g, and ∆H = hardness change after immersion, units,
A = area of the specimen in actual contact with the test Ho = original hardness before immersion, units, and
liquid, mm2. Hi = hardness after immersion, units.
18.5 Calculate percent extracted soluble matter as follows 18.7 Calculate breaking resistance, burst strength, tear
(Section 15): strength, and adhesion both on the immediate deteriorated
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result (as used for these calculations) is the average of three These large values are essentially meaningless for precision
individual test specimen values. Each laboratory conducted comparisons when average values are near zero.
tests (that is, obtained one test result) on each of two days. Both
20.6 The precision of the test method may be expressed in
repeatability and reproducibility are therefore short term; a
the following statements that use an appropriate value of r and
period of a few days separates test results.
R. The appropriate value is that value of r or R, associated with
20.4 The results of the precision evaluation are given in a mean level in the tables closest to the mean level under
Table 6 and Table 7 for each of the six rubbers or materials for consideration for any immersion liquid or rubber, for any test
immersion tests in (1) Reference Fuels B, C and D, for 70 h at result for a similar material in routine testing operations.
23 6 2°C (73 6 4°F), and (2) ASTM Oil No. 2 and ASTM Oil
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TABLE 7 Precision DataA
Change in Volume, %
Rubber Within-Laboratory Between-Laboratories
Mean Sr r SR R
ASTM Reference Fuel B:
CR 66.2 0.94 2.7 5.40 15.3
FKM 1.5 0.36 1.0 0.34 1.0
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 1.0 1.27 3.6
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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 subject to cancer ASTM Subcommittee D11.15 and the SAE Committee on
hazard warning label requirements under the OSHA Hazard Automotive Rubber Specifications (SAE-CARS). Calumet No.
Communication Standard, published November 25, 1983. This 2, the replacement for No. 2 oil, provided a closer match than
contributed to the discontinuation of commercial production in Calumet No. 3, the replacement for No. 3 oil. The two oils
X2.1 This precision statement was prepared using data from TABLE X2.1 Precision Data for Within-Laboratory Variation
the comprehensive ITP evaluation program conducted in 1993 N OTE 1—Sr = repeatability standard deviation; r = repeatabil-
to establish replacement oils for ASTM Oils No. 2 and No. 3. ity = 2.83 × Sr; (r) = repeatability on relative basis (percent of percent);
Because of the limited number of laboratories (three), only and CV = coefficient of variation, % = (Sr/Mean) × 100.
within-laboratory variation or repeatability could be evaluated. Change in Volume, % (Pooled Values)
Rubber
Some terminology used in this appendix is contained in Mean Sr r (r) CV
Practice D4483. Refer to Practice D4483 for background ASTM Oil No. 2 Types:A
details. ACM 1.3 0.57 1.60 119.0 42.2
AEM 27.8 0.82 2.33 8.4 3.0
CR 36.0 1.63 4.61 12.8 4.5
X2.2 In the evaluation program twelve compounds were
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that (1) there is a direct (positive slope) log-log relationship for X2.5.1 Two test results of the commercial rubber that differ
Sr versus mean volume swell, and (2) an inverse (negative by more than the tabulated r or (r) values as selected by the
slope) relationship between the relative repeatability (r) and above process, must be considered to have come from different
mean volume swell. These relationships apply to both sets of sample populations (that is, be significantly different).
data and to the combined data sets. X2.5.2 Alternatively normal testing operations should pro-
duce values for duplicate test results that are within the r and
X2.5 The results of Table X2.1 may be applied to within- (r) intervals as selected by the above process.
laboratory data comparisons using either IRM 902 or IRM 903
for any commercial or proprietary compound by selecting the X2.6 Bias reference values do not exist for this type of
Table X2.1 rubber closest to the commercial compound and testing, since the value of the test property is defined exclu-
X3.1 A precision statement has not been prepared due to the IRM 901 and a supply of ASTM No. 1 remained in existence.
sudden unavailability of ASTM Oil No. 1. The Precision and It is provided for reference only. The data was obtained in 2005
Bias statement will be prepared in accordance with Practice in a study conducted by Smithers Scientific Services, Akron,
D4483 at the conclusion of the forthcoming interlaboratory test Ohio.
program.
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TABLE X3.1 ASTM Oil No. 1 Replacement Program
#1 #2 #3 #4 #5 #6 #7 #9 #10 #11
Test
CR EVM EPDM NBR HNBR ECO ACM AEM VMQ TPV
ORIGINAL PROPERTIES
Hardness, Shore A 73 79 74 61 69 72 72 74 64 75
Tensile strength, psi 2877 2863 2153 3208 3818 1977 1990 2267 1295 745
Stress @ 300 % strain ... ... ... 1200 ... ... ... ... 1110 ...
Elongation at break, % 259 % 155 % 268 % 625 % 262 % 284 % 171 % 284 % 339 % 120 %
IMMERSION – ASTM #1
Hardness, Shore A 66 72 47 59 67 71 68 72 59 63
#2-EVM 70 h 125°C
#3-EPDM 70 h 125°C
#4-NBR 70 h 100°C
#5-HNBR 70 h 150°C
#6-ECO 70 h 100°C
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