This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D3194 − 17

Standard Test Method for

Rubber From Natural Sources—Plasticity Retention Index
(PRI)1
This standard is issued under the fixed designation D3194; 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 (´) indicates an editorial change since the last revision or reapproval.

1. Scope pellets of specified dimensions are cut, three to be tested in

1.1 This test method gives an indication of the oxidation original condition and three to be aged under specified condi-
resistance of raw natural rubber at a specified temperature. This tions.
resistance is indicated by the Plasticity Retention Index (PRI), 3.2 Plasticity on both the original and aged samples is
a ratio expressed as a percentage of the aged plasticity to the measured as the median final thickness of each set of samples
original plasticity determined by means of a parallel plate after a compressive force of 100 N 6 1 N is applied for a
plastometer. A low PRI value indicates a poor resistance to specified time. The PRI is the ratio expressed as a percentage
oxidation. of the aged to the original plasticity.
1.2 The values stated in SI units are to be regarded as the
4. Significance and Use
standard.
1.3 This standard does not purport to address all of the 4.1 This test method may be used to evaluate the heat and/or
safety concerns, if any, associated with its use. It is the oxidation stability (aging) of raw rubber under controlled
responsibility of the user of this standard to establish appro- conditions. High original and aged plasticity values usually
priate safety and health practices and determine the applica- correspond to good aging properties. The ratio of the aged to
bility of regulatory limitations prior to use. original plasticity values expressed as a percentage, the PRI, is
used as an indication of aging.
2. Referenced Documents
5. Apparatus
2.1 ASTM Standards:2
D1485 Practice for Rubber from Natural Sources— 5.1 Parallel Plate Plastometer4, with a 10 mm diameter
Sampling and Sample Preparation platen. The platen temperature shall be 100 6 1°C and the
D3040 Practice for Preparing Precision Statements for Stan- plastometer shall have a timer unit capable of giving a 15 6 1
dards Related to Rubber and Rubber Testing (Withdrawn s initial conditioning period during which the sample shall be
1987)3 compressed to 1 6 0.01 mm and a test period of 15 6 1 s under
D3182 Practice for Rubber—Materials, Equipment, and Pro- a compression force of 100 N 61 N. The plastometer shall also
cedures for Mixing Standard Compounds and Preparing have a measuring device gauge reading to 0.01 mm. Calibra-
Standard Vulcanized Sheets tion procedures recommended by the manufacturer of the
E145 Specification for Gravity-Convection and Forced- plastometer should be followed.
Ventilation Ovens 5.2 Punch, that will die out cylindrical specimens approxi-
3. Summary of Test Method mately 13 mm in diameter from a prepared sheet of rubber.
3.1 A homogenized sample of raw rubber is prepared by a 5.3 Circulating Air Oven, specified in Specification E145,
specified procedure to create a sheet from which six cylindrical Type IIA. The oven must be capable of maintaining 140 6
0.5°C.
1
This test method is under the jurisdiction of ASTM Committee D11 on Rubber 5.4 Dishes or Tray, aluminum, for test specimens, light-
and Rubber-like Materials and is the direct responsibility of Subcommittee D11.22
on Natural Rubber.
weight aluminum dishes approximately 38 mm (1.5 in.) in
Current edition approved Jan. 1, 2017. Published January 2017. Originally diameter or an aluminum tray approximately 150 by 150 mm
approved in 1973. Last previous edition approved in 2009 as D3194 – 04 (2009). (7 by 7 in.) for aging specimens in the oven.
DOI: 10.1520/D3194-17.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM The sole source of supply of the Wallace Rapid Plastimeter known to the
Standards volume information, refer to the standard’s Document Summary page on committee at this time is Leverett A. Anderson Co., P.O. Box 5400, Akron, OH
the ASTM website. 44313. If you are aware of alternative suppliers, please provide this information to
3
The last approved version of this historical standard is referenced on ASTM International Headquarters. Your comments will receive careful consider-
www.astm.org. ation at a meeting of the responsible technical committee,1 which you may attend.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 D3194 − 17
5.5 Tissue paper or cigarette paper, approximately 40 by 40 8.2.4 Die out six or more test specimens from the doubled
mm (1.5 by 1.5 in.). This paper shall be bleached, unglazed sheet with the punch and measure their thickness until six test
acid-free tissue paper, of approximately 1.7 g/m2. pellets are obtained with a thickness of 3.4 6 0.2 mm (0.134 6
0.008 in.) having a volume of 0.40 6 0.04 cm3 (0.2441 6
6. Precautions 0.002441 in.3). Randomly divide these into two sets of three,
6.1 The initial thickness of the prepared sheet can affect the one for test before aging and the other for test after aging.
final thickness after testing. Ascertain the required mill opening
9. Procedure
by preliminary trial; it will vary with the rubber and the mill.
9.1 Aging:
6.2 The temperature and speed of the testing operations can
9.1.1 Before aging is started, the oven must be stabilized at
affect the results. An increase in temperature or the time to
140 6 0.5°C for at least 1⁄2 h.
preheat or time to read the dial micrometer can result in low,
9.1.2 The dishes or tray containing the three pellets (8.3) to
final plasticity readings.
be aged must be arranged within the calibrated region of the
oven. Insert the tray and close the oven door quickly to prevent
7. Sampling
excessive oven heat loss. Start timing as soon as the oven door
7.1 The natural rubber sample shall be obtained in accor- is closed.
dance with Practice D1485. 9.1.3 After 30 6 0.25 min remove the tray from the oven
and remove the dishes from the tray. Allow them to cool to
8. Test Specimen Preparation room temperature for a minimum of 30 min and a maximum of
8.1 Test Specimen Preparation Method A (original proto- 2 h before testing.
col): 9.2 Measurement of Plasticity:
8.1.1 Homogenize the piece to be tested (mass approxi- 9.2.1 The platen of the plastometer shall have come to
mately 360 g) 10 times through a mill as described in Practice equilibrium at 100 6 1°C for 15 min before making measure-
D3182. The mill rolls should be at 70 6 5°C (158 6 9°F) with ments.
an opening of approximately 1.65 mm (0.065 in.). After each of 9.2.2 Place two pieces of tissue paper (5.5) between the
the first six passes, roll the rubber into a cylinder and pass heated platens and set the thickness measuring device to zero
endwise through the mill rolls. After the sixth pass, the sample when the platens are closed.
shall not be rolled, but is folded. 9.2.3 Insert a pellet at room temperature between two pieces
8.1.2 Take a test portion of about 30 g from the homog- of tissue paper and place the whole assembly centrally between
enized sample and pass it three times (doubling the sheet the heated platens. Put the machine lever into operation. After
between passes) between mill rolls at room temperature with a 15-s conditioning period, the timing device automatically
the opening adjusted so that the final sheet thickness is releases the force of 100 N 61 N to compress the specimen.
approximately 1.7 mm (0.07 in.). After the third pass, double This load period is automatically adjusted, exactly 15-s dura-
the sheet, which should be uniform in texture and free of holes, tion. The final thickness expressed in units equivalent to 0.01
and press the two halves lightly together. mm remains locked after the 15–s load period on the dial
8.1.3 Die out six or more test specimens from the doubled micrometer until the operating handle is moved to open the
sheet with the punch and measure their thickness until six test instrument. Record the measured thickness from the dial
pellets are obtained with a thickness of 3.4 6 0.2 mm (0.134 6 micrometer. Repeat the above for each of the pellets, both aged
0.008 in.) having a volume of 0.40 6 0.04 cm3 (0.2441 6 and in original condition.
0.002441 in.3). Randomly divide these into two sets of three, 9.2.4 The measured thickness for each pellet within either of
one for test before aging and the other for test after aging. the groups should not vary by more than 6 0.01 mm from the
8.2 Test Specimen Preparation Method B (alternative pro- median value of that group. Run additional pellets, if needed,
tocol): to get three of each group within this tolerance.
8.2.1 Homogenize the piece to be tested (mass approxi-
mately 360 g) 10 times through a mill as described in Practice 10. Calculation
D3182. 10.1 The plasticity is 100 times the final thickness as
8.2.2 The mill rolls should be at room temperature with an expressed in units equivalent to 0.01 mm.
opening of approximately 1.65 mm (0.065 in.). After each of 10.2 Using the median values of these plasticity results of
the first six passes, roll the rubber into a cylinder and pass both original (Po) and aged test specimens, calculate the PRI as
endwise through the mill rolls. After the sixth pass, the sample follows:
shall not be rolled, but is folded.
8.2.3 Take a test portion of about 30 g from the homog- PRI 5 ~ plasticity aged/plasticity original! 3 100 (1)
enized sample and pass it three times (doubling the sheet
between passes) between mill rolls at room temperature with 11. Report
the opening adjusted so that the final sheet thickness is 11.1 The report shall include the following:
approximately 1.7 mm (0.07 in.). After the third pass, double 11.1.1 Three values of the plasticity for the original and the
the sheet, which should be uniform in texture and free of holes, aged test pieces,
and press the two halves lightly together. 11.1.2 Type of oven used, and

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 D3194 − 17
11.1.3 Plasticity Retention Index (PRI) using Method A or TABLE 1 ASTM Test Method D3194 Type 1 Precision—Wallace
Method B. Plasticity (PRI)AB
Mean Within Laboratories Between Laboratories
Sample
12. Precision and Bias5 Value sr r (r) SR R (R)
6 58.95 2.58 7.30 12.4 9.33 26.41 44.8
12.1 This precision and bias section has been prepared in 4 63.22 1.70 4.82 7.6 4.91 13.88 22.0
accordance with Practice D4483. Refer to this practice for 3 63.44 2.22 6.28 9.9 9.40 26.57 41.9
terminology and other statistical details. 5 79.56 2.10 5.94 7.5 7.31 20.68 26.0
2 87.23 3.34 9.45 10.8 10.79 30.55 35.0
12.2 The precision results in this precision and bias section 1C 95.15 1.95 5.52 5.8 2.52 7.13 7.5
give an estimate of the precision of the test method with the Mean 70.48
Pooled 2.45 6.94 9.8 8.6 24.32 34.5
materials used in the particular interlaboratory program as A
This is short-term precision with p = 13, q = 6, and n = 3.
described below. The precision parameters should not be used sr = Within laboratory standard deviation,
for acceptance/rejection testing of any group of materials r = Repeatability in measured units (sr x 2.83),
without documentation that they are applicable to those par- (r) = Repeatability in percent ((r/mean) x 100),
SR = Between laboratory standard deviation,
ticular materials and the specific testing protocols that include R = Reproducibility in measured units (SR x 2.83), and
this test method. (R) = Reproducibility in percent ((R/mean) x 100).
Outliers have been rejected from the tabled data.
12.3 A Type 1, Class II interlaboratory precision program B
Units: PRI is the ratio expressed as a percentage of the aged to the original
was conducted (except for sample No. 6, which was Type 1, plasticity. The basic plasticity units represent the thickness of the samples in 0.01
mm times 100.
Class I). Both repeatability and reproducibility are short term. C
Sample No. 1 excluded from mean and pooled values.
A period of a few days separate test results, which were
repeated on three separate days. Participation included 13
laboratories, and six materials were used. Therefore, p = 13, q nations) that differ by more than the tabulated (r) (expressed as
= 6, and n = 3. A test result is the median value obtained from percentage of their mean value) must be considered suspect,
three determinations as specified in Section 10. that is, having arisen from different sample populations. Such
12.4 Other than sample No. 1, which was IIR, the materials a decision dictates that appropriate action be taken.
used were natural rubber. They were prepared through step 8.2 12.6.2 Reproducibility—The reproducibility (R) of this test
of this test method. Participants were required to die out and has been established as 34.5 %. Two single measurements
test the cut pellets. Sample identification: No. 1 = Butyl rubber, (determinations) that differ by more than the tabulated (R)
No. 2 = PA80 coagulated latex, No. 3 = SIR20, No. 4 = No. (expressed as percentage of their mean value) must be consid-
1RSS, No. 5 = CV50, and No. 6 = SIR20 cut pellets. ered suspect, that is, having arisen from different sample
populations. Such a decision dictates that appropriate action be
12.5 The results of the precision calculations are given in taken.
Table 1, with the materials arranged in increasing mean PRI
value. 12.7 Bias—In test method terminology, bias is the difference
between an average test value and the reference (true) test
12.6 The precision for these tests on a relative basis may be property value. Reference values do not exist for this test
expressed as follows (sample No. 1 IIR excluded): method since the value or level of the test property is
12.6.1 Repeatability—The repeatability (r) of this test has exclusively defined by the test method. Bias, therefore, cannot
been established as 9.8 %. Two single measurements (determi- be determined.

5
13. Keywords
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D11-1066. 13.1 natural rubber; plasticity; P.R.I.; retention index

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