Designation: D 3677 – 00 (Reapproved 2004)

Standard Test Methods for

Rubber—Identification by Infrared Spectrophotometry1
This standard is issued under the fixed designation D 3677; 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.

1. Scope 4. Reagents
1.1 These test methods cover rubber identification and are 4.1 Purity of Reagents—Reagent grade chemicals shall be
based on infrared examination of pyrolysis products (pyrolyz- used in all tests. Unless otherwise indicated, it is intended that
ates) and films. all reagents shall conform to the specifications of the Commit-
1.2 These test methods are applicable to rubbers in the raw tee on Analytical Reagents of the American Chemical Society,
state and, when compounded, both in the cured and uncured where such specifications are available.3 Other grades may be
state. used, provided it is first ascertained that the reagent is of
1.3 The values stated in SI units are to be regarded as sufficiently high purity to permit its use without lessening the
standard. accuracy of the determination.
1.4 This standard does not purport to address all of the 4.2 Acetone.
safety concerns, if any, associated with its use. It is the 4.3 Alcohol, specially denatured (Formula 2-B or 30 is
responsibility of the user of this standard to establish appro- satisfactory).
priate safety and health practices and determine the applica- 4.4 2-Butanone.
bility of regulatory limitations prior to use. Specific precau- 4.5 Chloroform.
tionary statements are given in Section 17. 4.6 Congo Red Paper.
4.7 Diatomaceous Filter Aid4,5—Some grades are quite
2. Referenced Documents unsatisfactory in that they will not sufficiently absorb carbon
2.1 ASTM Standards: 2 black.
D 297 Test Methods for Rubber Products—Chemical 4.8 1,2-Dichlorobenzene6, 5—A check on suitability may be
Analysis made by evaporating 50 cm3 to dryness and making an infrared
D 1418 Practice for Rubber and Rubber Latices— spectrum of the residue. Any substantial absorbance at posi-
Nomenclature tions near those wavenumbers that will be used for rubber
D 3452 Practice for Rubber—Identification by Pyrolysis- analysis, indicates that the 1,2-dichlorobenzene is unsuitable
Gas Chromatography for use.
E 168 Practices for General Techniques of Infrared Quanti- 4.9 Dry Compressed Air and Nitrogen, in cylinders, or
tative Analysis provided as a laboratory service.
4.10 Sodium Sulfate, anhydrous.
3. Significance and Use 4.11 Toluene.
3.1 For research, development, and quality control pur-
poses, it is advantageous to determine the composition of
rubbers in cured, compounded products.
3.2 This test method provides such composition analysis 3
Reagent Chemicals, American Chemical Society Specifications, American
utilizing an infrared technique. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
1
These test methods are under the jurisdiction of ASTM Committee D11 on and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Rubber and are the direct responsibility of Subcommittee D11.11 on Chemical MD.
4
Analysis. The sole source of supply of the diatomaceous filter aid known to the
Current edition approved Dec. 1, 2004. Published December 2004. Originally committee at this time is Fisher Scientific, Catalog No. C211 (Celite).
5
approved in 1978. Last previous edition approved in 2000 as D 3677 – 00. If you are aware of alternative suppliers, please provide this information to
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or ASTM International Headquarters. Your comments will receive careful consider-
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM ation at a meeting of the responsible technical committee,1 which you may attend.
6
Standards volume information, refer to the standard’s Document Summary page on The sole source of supply of 1,2-dichlorobenzene known to the committee at
the ASTM website. this time is J. T. Baker Chemical Co., Phillipsburg, NJ 08865, Catalog No. 9217.

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

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 D 3677 – 00 (2004)

TEST METHOD A QUALITATIVE ANALYSIS

5. Scope 6.2 Exceptions to the rubbers listed in 6.1 are:

5.1 This test method, based on infrared examination of 6.2.1 A blend of natural or synthetic isoprene (20 %) and
pyrolysis products (pyrolyzates) and films, will identify the chloroprene (80 %), or both, may present difficulties, and
rubbers in 6.1 occurring alone or in binary blends in the range identification of the minor component may be achieved only
from 80 % major component to 20 % minor component. when its content is equal to or more than 30 % in the blend.
Exceptions to this will be found in 6.2. 6.2.2 A blend of butadiene-styrene rubber (80 %) and high
5.2 This test method is applicable to rubbers in the raw state cis polybutadiene rubber (20 %) may present difficulties, and
and, when compounded, both in the cured and uncured state. identification of the minor component may only be achieved
5.3 This test method implies that sample preparation and when it is equal to or more than 30 % in the blend.
infrared spectrum are prepared and analyzed by experienced 6.2.3 Ethylene-propylene rubber in blends with other rub-
personnel and that the equipment used for the production of the bers present difficulties when its content is in the range from 20
spectra is operated according to the manufacturer’s directions to 40 %.
for optimum performance. No details for operation of infrared 6.3 In difficult cases, examination of the gaseous products of
spectrophotometers are included in these test methods. pyrolysis by gas chromatography (Practice D 3452) may give
further information.
6. Field of Application
7. Summary of Test Method
6.1 Infrared examinations of pyrolyzates and films will
identify mixtures of two of the following types of rubbers in 7.1 Identification from Pyrolyzates:
the range from 80 % major component to 20 % minor compo- 7.1.1 A small quantity of extracted and dried rubber is
nent. (See the exceptions in 6.2.) pyrolyzed in a stream of nitrogen in a test tube held in a small
6.1.1 Isoprene Rubbers (see 6.2.1): electric, thermo-regulated furnace at 450 to 500°C, or alterna-
6.1.1.1 Natural rubber, synthetic polyisoprene, gutta percha, tively, rapidly pyrolyzed in a small test tube held in the hot
and balata are included. zone of a gas flame.
6.1.1.2 Examination of the pyrolyzate will not distinguish 7.1.2 A test for chlorine is conducted during pyrolysis.
between the different forms of polyisoprene. 7.1.3 A few drops of the pyrolyzate are transferred to a salt
6.1.1.3 Examination of a film will distinguish natural and plate and an infrared spectrum recorded over the 2.5 to 15-µm
synthetic polyisoprene from balata and gutta percha. wavelength region.
6.1.2 Styrene-Butadiene Rubbers with Styrene Content of 7.1.4 The rubber is identified by comparison to standard
Approximately 23.5 % Styrene (see 6.2.2): reference spectra and by reference to a table of diagnostic
6.1.2.1 For the purpose of this standard, all copolymers of absorptions (significant absorption frequencies).
styrene and butadiene and their oil-extended forms are in- 7.1.5 Each laboratory employing this standard must prepare
cluded. spectra of all rubbers they might be expected to identify. These
6.1.2.2 Examination of the pyrolyzate will not distinguish spectra must be prepared in the same manner and using the
between emulsion and solution polymerized rubbers. same equipment as will be used for unknown samples.
6.1.2.3 Examination of films may give some information 7.2 Identification from Films:
about the monomer ratio and the polymerization system. 7.2.1 A small quantity of extracted and dried rubber is
6.1.3 Acrylonitrile-Butadiene Rubber with Acrylonitrile dissolved in 1,2-dichlorobenzene, filtered, and a film cast on a
Content of Approximately 33 %: salt plate. This film is used as in 7.1.4.
6.1.3.1 Examination of the pyrolyzate will not measure the 7.2.2 A small quantity of extracted and dried rubber is
ratio of acrylonitrile to butadiene. subjected to mild thermal degradation at 200 6 5°C for a short
6.1.3.2 Examination of a film may give some information time. The degraded sample is dissolved in trichloroethylene
about the acrylonitrile content. then chloroform, and a film cast on a salt plate. This film is
6.1.4 Chloroprene Rubber—This test method will not dis- used as in 7.1.4.
tinguish between the different types of chloroprene rubbers.
6.1.5 Butyl Rubber— This test method will not distinguish 8. Apparatus
between butyl rubber and its halogenated forms. 8.1 Extraction Apparatus:
6.1.6 Polybutadiene Rubber (High cis): 8.1.1 The extraction apparatus used shall be of the general
6.1.6.1 Examination of the pyrolyzate will not distinguish type and dimensions shown in Fig. 1.
between polybutadiene rubbers having different isomer ratios. 8.2 Test Tubes, small, and other necessary glassware suffi-
6.1.6.2 Examination of a film may give some information cient to carry out the test as written.
about the monomer ratio. 8.3 Pyrolysis Apparatus (Fig. 2)—The pyrolysis apparatus
6.1.7 Ethylene-Propylene Rubbers (see 6.2.3)—This test consists of a glass tube (P) having inward projections to
method will not distinguish between rubbers having different prevent the sample from falling to the bottom of the tube and
ratios of ethylene to propylene nor between copolymers and a lateral condenser tube. The tube (P) has a ground-glass
terpolymers. standard taper (S) which carries a small glass adductor tube. A

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 D 3677 – 00 (2004)
8.7 Salt Plates, polished (sodium chloride or potassium
bromide), 4 by 25 mm, to serve as windows for the spectro-
photometer.7,5
8.8 High-Resolution Infrared Spectrophotometer, double
beam, capable of recording a spectrum over the 2.5 to 15-µm
(4000 to 667 cm−1 or 400 000 to 66 700 m−1) region. (High
resolution8 requires that the spectral slit width should not
exceed 2 cm−1 over 80 % of the wavenumber range and at no
place should it exceed 5 cm−1.) Any spectrophotometer com-
plying with these requirements may be used. The equipment
shall be operated by an experienced analyst according to the
manufacturer’s directions for optimum performance.9,5

9. Preparation of Test Portion

9.1 Temperature Controlled Pyrolysis in a Stream of Nitro-
gen (Fig. 2; Preferred Method):
9.1.1 Prepare the test portion by milling into a thin sheet on
a laboratory mill or cutting into cubes about 2 mm wide and
wrap approximately 0.5 g in filter paper or nylon cloth. Extract
the wrapped test portion in an extraction cup in accordance
with Section 18 of Test Methods D 297, for a minimum of 4 h
with methanol, ethanol, or 2-propanol. A vulcanizate may be
extracted with acetone or 2-butanone, in addition to the above
alcohols. Alternatively, the rapid reflux procedure may be used
FIG. 1 Extraction Apparatus with Glass Condenser for 1 h in accordance with Section 25 of Test Methods D 297.
and Ground Glass Joint
9.1.2 Remove the extracted rubber from the apparatus and
dry at 100°C until free of solvent. One to two hours is usually
required.
9.1.3 Introduce a small amount of anhydrous sodium sulfate
into the collecting tube (T) to absorb water produced during
pyrolysis.
9.1.4 Place a strip of moistened Congo red paper across the
mouth of the tube, as a test for chlorine (a change from red to
blue).
9.1.5 If alternative chlorine determining methods are em-
ployed, this procedure must be suitably modified.
9.1.6 Bring the electrical furnace (F) to 450 to 500°C and
hold at this temperature. This range is recommended to obtain
fast pyrolysis, without excessive degradation and carboniza-
tion. Temperatures below this range should be avoided.
9.1.7 Pass a slow stream of nitrogen through the pyrolysis
tube and introduce the tube into a hole of the aluminum block
(H). The nitrogen serves to displace air, prevent oxidation, and
facilitate transfer of the pyrolysis products to the collecting
F electric, thermoregulated furnace
H aluminum block, bored to hold tubes
tube (T).
P glass tube for sample container 9.1.8 Carry on heating to complete distillation, which re-
S ground-glass taper quires approximately 15 min.
T collecting tube
9.1.9 Transfer a few drops of the pyrolyzate from the tube to
FIG. 2 Temperature Controlled Pyrolysis Apparatus a sodium chloride or potassium bromide plate, using a capillary
pipet.

collecting tube (T) is placed under the condenser tube. An

electric, thermoregulated furnace (F) accommodates an alumi-
7
num block (H) with holes for one or more tubes (P). The sole source of supply of the salt plates known to the committee at this time
is Barnes Engineering Co., Stamford, CT 06902, Catalog No. 7000-316.
8.4 Capillary Pipets. 8
High resolution is defined in “Specification for Evaluation of Research Quality
8.5 Oven, capable of maintaining a temperature of 200 6 Analysis of Infrared Spectra,” Analytical Chemistry, ANCHA, Vol 47, No. 11, p.
94A.
5°C for use in 10.2. 9
The sole source of supply of the spectrophotometer known to the committee at
8.6 Water Bath, for use in 10.2. this time is Perkin-Elmer, Model 283, Perkin-Elmer Corp., Norwalk, CT 96856.

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 D 3677 – 00 (2004)
9.1.10 Place a spacer of suitable thickness in position, close 10.1.8 Concentrate the centrifuged or filtered solution to a
the cell with a second plate of the same material, and mount the small volume under vacuum in a stream of nitrogen.
cell in the infrared spectrophotometer. 10.1.9 Evaporate a few drops of the concentrated solution
9.1.11 Record the spectrum over the wavelength range from on a salt plate to give a film thickness with 10 to 20 %
2.5 to 15 µm. transmittance at 6.9 µm.
9.1.12 Spectra should be obtained immediately after pyroly- 10.1.10 Record the spectrum over the 2.5 to 15-µm wave-
sis to minimize further change in the pyrolysis products. length region.
9.2 Gas Flame Pyrolysis (Alternative Test Method): 10.2 Mild Thermal Degradation for Vulcanizates:
9.2.1 Prepare the extract, dry 2 g of test portion (9.1.1 and 10.2.1 Prepare, extract, and dry about 2 g of rubber in
9.1.2), and place 0.1 to 0.2 g of the test portion in the bottom accordance with 9.1.1 and 9.1.2.
of a small glass test tube. Place a strip of moistened Congo red 10.2.2 Place the dried rubber in a test tube capped with glass
paper across the mouth of the tube. Hold the tube horizontally, wool and heat to 200 6 5°C in the oven (8.5) for approxi-
and quickly bring the lower end containing the test portion into mately 10 min.
the hot zone of a gas burner, so that the rubber is rapidly 10.2.3 Transfer the rubber to a beaker and add 50 cm3 of
pyrolyzed and charring is kept to a minimum. Note any color trichloroethylene.
change in the Congo red paper, from red to blue, indicating the 10.2.4 Allow the beaker and contents to stand on a water
presence of chlorine. bath for approximately 30 min with occasional stirring to effect
9.2.2 Maintain the heating until the pyrolyzate condenses in dissolution of the degraded rubber.
the cool end of the tube, withdraw the test tube from the flame, 10.2.5 Filter the mixture (10.2.4) through filter paper to
and cool while holding horizontally. remove any undissolved vulcanizate or fillers.
9.2.3 Alternatively, the sample may be placed in a small 10.2.6 If free carbon is released by the vulcanizate (some-
glass tube and the end of the tube drawn out to a “retort” shape times found with polyisoprene and butyl rubbers), add a small
with a blast lamp. Pyrolysis is carried out as described in 9.2.1. amount of filter aid (4.7) to the solution before filtering.
Care should be taken to keep the delivery end of the pyrolysis 10.2.7 Remove the trichloroethylene by evaporation, distil-
tube warm enough so that pyrolysis products do not condense lation, or by the use of a rotary evaporator with vacuum. In no
and block the opening, causing the tube to explode. The case should the solution be heated to over 80°C.
condensate can be collected in a small test tube containing 10.2.8 Dissolve the residue in a small amount of chloro-
anhydrous sodium sulfate to remove moisture. Proceed in form.
accordance with 9.1.9-9.1.12. 10.2.9 If the analyst suspects that the filtrate from 10.2.6
9.2.4 If alternative chlorine detecting methods are em- contains material other than rubber, which might interfere in
ployed, this procedure must be suitably modified. interpretation of the final infrared spectrum, the polymer
should be precipitated from the solution of 10.2.5 or 10.2.6 by
10. Sample Preparation for Films methanol. Filter the recovered polymer and dissolve in chlo-
10.1 Dissolution for Vulcanizates: roform.
10.1.1 Prepare a test portion in accordance with 9.1.1 and 10.2.10 Cast a film having 10 to 20 % transmittance at 6.9
9.1.2. µm, on a salt plate (see 8.7). Record the infrared spectrum over
10.1.2 Pyrolyze and test for chlorine in accordance with the 2.5 to 15-µm wavelength region, using the infrared equip-
9.1.4 and 9.1.5 or 9.2.1-9.2.4. ment (8.8).
10.1.3 Place 1 g of the prepared rubber (9.1.1 and 9.1.2) and 10.3 Dissolution for Raw Rubbers:
50 cm3 of 1,2-dichlorobenzene in a 100-cm3 flask fitted with a 10.3.1 Prepare a test portion in accordance with 9.1.1 and
reflux condenser. Boil until the rubber is dispersed or dis- 9.1.2, pyrolyze, and test for chlorine in accordance with 9.1.4
solved. and 9.1.5 or 9.2.1-9.2.4.
10.1.3.1 The time required for dissolution varies with the 10.3.2 Place 1 g of the prepared rubber (9.1.1 and 9.1.2) and
rubber. Natural rubber requires 3 to 4 h, while chloroprene 50 cm3 of chloroform in a 100-cm3 flask fitted with a reflux
requires more than 24 h. Some rubbers never completely condenser. Boil until the rubber dissolves.
dissolve. 10.3.3 Cool and transfer to a beaker.
10.1.3.2 Discontinue refluxing at the end of 48 h to mini- 10.3.4 Concentrate the solution to a small volume under
mize the risk of altering the molecular structure of the rubber. vacuum in a stream of nitrogen.
10.1.3.3 Even though complete dissolution is not affected in 10.3.5 Cast a film on a salt plate and record the infrared
48 h, enough rubber has usually dissolved to provide a good spectrum over the 2.5 to 15-µm wavelength region, taking care
spectrum. that the film has a thickness sufficient to give approximately 10
10.1.4 Cool the mixture and transfer to a beaker with 50 cm3 to 20 % transmittance at 6.9 µm.
of toluene.
10.1.5 If the compound does not contain carbon black, 11. Interpretation of Spectra
centrifuge to eliminate mineral fillers. 11.1 Reference Spectra:
10.1.6 If the compound contains carbon black, add 10 to 20 11.1.1 Because of the different modes of presentation of
g of filter aid (4.7) to facilitate filtration through filter paper. spectra, it is strongly recommended that a set of reference
10.1.7 If the filtrate from 10.1.6 still contains carbon black, spectra on the same instrument should be prepared before
repeat the filtration with additional filter aid. proceeding to unknown samples.

4
 D 3677 – 00 (2004)
11.1.2 Reference spectra must be produced from test pieces 6.9 1450
of known composition following either Section 9 or 10. NOTE 1—The SI unit for wavenumber is the reciprocal metre. Until
11.1.3 Spectra of mixtures are not given because it is such units are used on instruments and graphs, the reciprocal centimetre
preferable for each laboratory to prepare its own set from test will be retained in this standard.
pieces of known composition.
11.1.4 Small, but unavoidable, variations in experimental 12.2 The principal absorptions in order of diagnostic value
conditions and instrument characteristics may give rise to are as follows:
slight differences in spectra. Spectra produced at different times 12.2.1 Isoprene Rubber (see Figs. 3 and 4):
may not be identical in terms of peak height (intensity of Wavelength, µm Wavenumber, cm−1 Intensity

absorption) or absorption wavelength. The experienced spec- 11.3 885 very strong
troscopist will recognize this. 7.3 1370 strong
11.1.5 Vulcanizates may give slightly different liquid pyro- 12.5 800 medium
6.1 1640 medium
lyzate and film spectra than those prepared from corresponding 11.0 909 shoulder
raw rubber, and the interpretation of such spectra requires
particular care, when strong characteristic features are lacking. In vulcanizates the absorption at 12.5 µm (800 cm−1) may
11.1.6 The precautions of 11.1.4 and 11.1.5 are cited to alert sometimes decrease in intensity with the appearance of a
the spectroscopist to difficulties that may arise from the use of broader, less intense absorption at 12.3 µm (813 cm−1).
this method and to encourage the practice of maintaining a 12.2.2 Styrene-Butadiene Rubber (see Figs. 5 and 6):
reference file of films and pyrolyzates of all the rubbers that Wavelength, µm Wavenumber, cm−1 Intensity

may require identification. 14.3 699 very strong

11.1.7 In all cases, spectra must be interpreted in the light of 12.9 775 strong
the test for chlorine. If the test for chlorine is negative, then the 6.7 1490 medium
11.0 909 strong
rubber is characterized as a hydrocarbon or nitrile type. 10.1 990 fairly strong
11.2 Diagnostic Absorptions: 10.4 962 medium
11.2.1 The tables of diagnostic absorptions (Sections 12 and The relative intensities of absorptions at 11.0 µm (909 cm−1),
13) should be used only in conjunction with the reference 10.1 µm (990 cm−1), and 10.4 µm (962 cm−1) depend on the
spectra. Their purpose is to indicate the principal absorptions ratio of isomers in the polybutadiene component and, therefore,
by which the spectra may be related to films and pyrolyzates, may vary.
such as the specific nature of certain peaks, their relationship 12.2.3 Acrylonitrile-Butadiene Rubber (see Figs. 7 and 8):
with neighboring peaks or other regions of the spectrum, etc.
Wavelength, µm Wavenumber, cm−1 Intensity
11.2.2 The table also serves to augment the reference
spectra by drawing attention to absorptions that are absent, 4.5 2220 medium strong
10.4 962 medium
thereby eliminating certain rubbers when ambiguity might
6.2 1610 medium
arise. 6.3 1590 medium
11.2.3 In Sections 12 and 13, diagnostic absorptions are 11.0 909 medium
arranged in order from strong to weak. By “diagnostic value” 12.2.4 Chloroprene Rubber (see Figs. 9 and 10):
is meant those features of the absorption, subjectively assessed, Wavelength, µm Wavenumber, cm−1 Intensity
which a practiced spectroscopist recognizes as of significance
in rubber identification. Such absorptions are not necessarily 12.2 820 medium
13.4 747 weak, sometimes absent
specific nor necessarily very intense. They are, however, 13.0 769 weak, sometimes absent
identifiable with certain compositional or structural features of 11.3 885 medium
the liquid pyrolyzates and films, and reproducible in the sense 14.3 699 medium
that they are not seriously influenced by moderate variations in The pyrolyzate of chloroprene rubber can give a variable
pyrolysis and dissolution conditions. spectrum that also tends to be lacking in characteristic features.
11.2.4 In general, it can be assumed with confidence that, The most useful absorption is that at 12.2 µm (820 cm−1), but
apart from exceptions stated, all the absorptions listed in this is rather broad and often not very intense. A weak
Sections 12 and 13 will appear in the spectrum of the absorption at 13.4 µm (747 cm−1) sometimes fails to appear,
corresponding pyrolyzate or film, and if absent, it is inferred while the stronger absorptions at 11.3 µm (885 cm−1) and 14.3
that the rubber sought is absent. µm (699 cm−1) are common in some degree to all the other
polymers.
12. Diagnostic Absorptions for Pyrolyzates 12.2.5 Butyl Rubber (see Figs. 11 and 12):
12.1 The following absorptions, when they occur, are of no Wavelength, µm Wavenumber, cm−1 Intensity
diagnostic value and should not be used for rubber identifica-
7.3 1370 strong
tion: 7.2 1390 strong
Wavelength, µm Wavenumber, cm−1 11.3 885 strong
8.0 to 8.2 1250 to 1220 medium doublet, some-
3.0 3330 times absent
3.5 2860 13.8 727 very weak, sometimes
5.9 1700 absent

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 D 3677 – 00 (2004)
12.2.6 Polybutadiene Rubber (see Figs. 13 and 14): Wavelength, µm Wavenumber, cm−1
−1
Wavelength, µm Wavenumber, cm Intensity
3.0 3330
11.0 909 strong 3.5 2860
10.4 962 strong 5.9 1700
10.1 990 medium 6.9 1450
12.3 813 weak
14.4 695 weak 13.2 The principal absorptions in the order of diagnostic
value are as follows:
12.2.6.1 Some of the principal absorptions in the spectrum 13.2.1 Isoprene Rubber (see Figs. 19 and 20):
obtained from the pyrolyzate of polybutadiene rubber are Wavelength, µm Wavenumber, cm−1 Intensity
closely similar both in frequency and intensity to those found
in the spectrum of chlorosulfonated polyethylene pyrolyzate 12.0 833 strong
7.3 1370 strong
and the result of the test for chlorine should be taken into 6.0 1665 medium
account when deciding between these two rubbers (see also 11.3 885 weak
12.2.8). Particular care should be exercised in the interpretation
of spectra from vulcanizates, and the 12 to 15-µm (833 to Reported diagnostic absorptions and related spectra for
667-cm−1) region should be well scrutinized for small, but natural rubber and synthetic polyisoprene are tabulated above.
diagnostically significant absorptions. Gutta percha and balata have different diagnostic absorptions
and spectra.
12.2.6.2 Polybutadiene rubbers having different isomer ra-
tios may, on pyrolysis, show absorptions of differing relative 13.2.2 Styrene-Butadiene Rubber (see Figs. 21 and 22):
Wavelength, µm Wavenumber, cm−1 Intensity
intensities, notably those at 10.4 and 11.0 µm (962 and 909
cm−1). 14.3 699 very strong
12.2.6.3 The spectrum of the polybutadiene pyrolyzate dif- 13.2 758 strong
6.7 1490 medium
fers from that of the styrene–butadiene pyrolyzate in that the 11.0 909 strong
absorptions due to aromatic constituents are absent or much 10.4 962 very strong
reduced.
Reported diagnostic absorptions and related spectra refer to
12.2.7 Ethylene Propylene Rubber (see Figs. 15 and 16): styrene-butadiene rubber with a styrene content of about
Wavelength, µm Wavenumber, cm−1 Intensity 23.5 %, produced by emulsion polymerization. Other copoly-
7.3 1370 strong mers having different monomer ratios or copolymers produced
11.0 909 strong by solution polymerization may have slightly different diag-
11.3 885 strong nostic absorption and spectra.
10.4 962 medium
13.8 725 medium 13.2.3 Acrylonitrile-Butadiene Rubber (see Figs. 23 and
24):
12.2.8 Chlorosulfonated Polyethylene (see Figs. 17 and
Wavelength, µm Wavenumber, cm−1 Intensity
18):
Wavelength, µm Wavenumber, cm−1 Intensity 4.5 2220 strong
10.4 962 very strong
11.0 909 strong 11.0 909 medium
10.4 962 medium
10.1 990 medium Reported diagnostic absorptions and related spectra refer to
12.3 813 weak acrylonitrile-butadiene rubber with an acrylonitrile content of
13.5 741 medium
13.9 720 weak
about 33 %.
14.4 695 weak 13.2.4 Chloroprene Rubber (see Figs. 25 and 26):
Wavelength, µm Wavenumber, cm−1 Intensity
Some of the principal absorptions in the spectrum obtained
from the pyrolyzate of chlorosulfonated polyethylene are 6.0 1665 very strong
closely similar both in frequency and intensity to those found 7.6 1315 medium
9.0 1110 strong
in the spectrum of polybutadiene pyrolyzate, and the result of 12.2 820 strong
the test for chlorine should be taken into account when
deciding between these two polymers. The table above in- 13.2.5 Butyl Rubber (see Figs. 27 and 28):
cludes some absorptions common to both, but the bands at 12.3 Wavelength, µm Wavenumber, cm−1 Intensity
and 13.5 µm (813 and 741 cm−1) although not particularly 7.3 1370 very strong
strong, are indicative of chlorosulfonated polyethylene. Par- 7.2 1390 very strong
ticular care should be exercised in the interpretation of spectra 8.1 1235 very strong
from vulcanizates. 13.2.6 Polybutadiene Rubber (see Figs. 29 and 30):
Wavelength, µm Wavenumber, cm−1 Intensity
13. Diagnostic Absorptions for Films
13.5 741 very strong
13.1 The following absorptions, when they occur, are of no 11.0 909 medium
diagnostic value and should not be used for rubber identifica- 10.4 962 medium
tion: 10.1 990 medium

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 D 3677 – 00 (2004)
Reported diagnostic absorptions and related spectra refer to 13.2.8 Chlorosulfonated Polyethylene (see Figs. 33 and 34):
polybutadiene rubber with high cis content. Relative intensities Wavelength, µm Wavenumber, cm−1 Intensity
of absorptions depend on the ratio of isomers in vulcanizates.
7.3 1370 strong
13.2.7 Ethylene-Propylene Rubber (see Figs. 31 and 32): 7.9 1265 medium
Wavelength, µm Wavenumber, cm−1 Intensity 8.6 1150 strong
13.7 730 medium
7.3 1370 strong
8.7 1145 medium In vulcanizates, the absorption, depending on the chlorosul-
13.0 and 14.0 760 and 710 medium fonic groups, strongly decreases.

TEST METHOD B SEMI-QUANTITATIVE ANALYSIS

14. Scope 15.2.1 A milled vulcanizate is digested with a hot solution

14.1 These test methods describe the semiquantitative de- of sulfuric and chromic acid and the residue is dissolved in
tection of certain rubbers in blends. boiling dichloromethane. An infrared spectrum of a film, cast
14.1.1 Polyisoprene (IR and NR), BR, and SBR are esti- on a salt plate from dichloromethane, provides a means of
mated when di-blends or tri-blends are present. The percentage determining the presence or absence of saturated rubbers in
of a single component of the blend is accurate to approximately unsaturated rubbers.
65 % of the total rubber content. See 15.1 and Sections 16-22. 15.2.2 The acid mixture decomposes unsaturated rubbers
14.1.2 Saturated rubbers (IIR or EPDM) (see Note 6) are such as NR, IR, BR, and SBR. Because EPDM and IIR are
detected in the presence of unsaturated rubbers (NR, IR, BR, highly saturated, they are virtually unattacked by the acid
SBR, and CR). Approximately 3 to 6 % of EPDM or IIR alone mixture. Furthermore, IIR and EPDM are only partially vul-
can be found in blends of unsaturated rubbers. When both canized in the presence of high levels of unsaturated rubbers
EPDM and IIR are present, the minimum detection limit is and may therefore be soluble in chlorinated solvents.
approximately 12 % of either rubber. See 15.2 and Sections 15.2.3 Any saturated polymer or rubber resistant to the acid
23-25.10 mixture, and also soluble in hot dichloromethane will appear in
the residue and consequently in the spectrum. Examples would
NOTE 2—For use in these test methods, the term “saturated rubbers” be low molecular mass polyethylene and polystyrene.
will be used to describe rubber containing no, or a small number of double
bonds, in the main rubber chain. For example, isobutylene rubber (IIR)
containing a small amount of an unsaturated material—isoprene. The term 16. Apparatus
“unsaturated rubbers” will be used to describe those rubbers containing 16.1 See Section 8 in addition to the following:
substantial numbers of double bonds in the main rubber chain, for 16.1.1 Grinding Mill, capable of grinding vulcanized rubber
example, IR, NR, SBR, BR, and CR. to 420 µm (40 mesh).11,5
14.1.3 References to IIR include chlorinated (CIIR) and 16.1.2 Magnetic Stirring Hot Plate, with controlled stirring
brominated (BIIR) versions of these rubbers. rates, capable of holding several 50-cm3 conical flasks.12,5
16.1.3 Magnetic Stirring Bars, covered with a chemical-
15. Summary of Test Methods resistant coating (see Note 3), approximately 25 mm long.
15.1 For estimation of NR, IR, BR, or SBR, or all of these, NOTE 3—Polytetrafluoroethylene has been found satisfactory.
in di-blends or tri-blends:
16.1.4 Büchner Funnel, for use with 5.5-cm filters.13,5
15.1.1 A milled, extracted test portion is ground to 420-µm
16.1.5 Glass Fiber Filters, 5.5 cm in diameter.14,5
(40-mesh) size, digested in hot 1,2-dichlorobenzene, and fil-
16.1.6 Vacuum Filtering Device. 15,5
tered to remove the carbon black. An infrared spectrum is made
16.1.7 Vacuum Oven. 16,5
on a film prepared from this solution.
16.1.8 Conical Flasks, 50-cm3 and 250-cm3 capacity, of
15.1.2 Absorbance ratio measurements at 1450 cm−1 and
heat-resistant glass.
other significant peaks found in the absorbance spectrum of the
rubbers listed in 14.1 are obtained next.
15.1.3 When the ratio values in accordance with 15.1.2 are
compared to those obtained from calibration data prepared 11
The sole source of supply of the grinding mill known to the committee at this
from all possible blends that the analyst expects to encounter of time is A. H. Thomas Co., Philadelphia, PA 19105, Wiley Intermediate Model.
12
The sole source of supply of the magnetic stirring hot plate known to the
NR, IR, BR, and SBR rubbers listed in 14.1.2, the composition
committee at this time is Cole-Parmer Instrument Co., Chicago, IL 60648, Model
of blends may be assessed. Magna-4.
15.2 For detection of EPDM or IIR in NR, IR, BR, SBR, or 13
The sole source of supply of the Büchner funnel known to the committee at
CR: this time is Fisher Scientific Co., Pittsburgh, PA 15219, Catalog No. 10-356B.
14
The sole source of supply of the glass fiber filters known to the committee at
this time is Reeve Angel Co., Clifton, NJ, No. 934AH.
15
The sole source of supply of the vacuum filtering device known to the
committee at this time is Fisher Scientific Co., Catalog No. 9-788, Fisher Filtrator.
10 16
Based upon Anderson, M., Uniroyal Tire Co., “Detecting Traces of EPDM or The sole source of supply of the vacuum oven known to the committee at this
IIR in Blends,” Elastomerics, October 1978, p. 40. time is National Appliance Co., Portland, OR.

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 D 3677 – 00 (2004)
NOTE 4—Borosilicate glass has been found satisfactory. For NR/BR: 1375, 965, 910, 835, and 735 cm−1
For NR/SBR: 1375, 965, 910, 835, 735, and 699 cm−1
16.1.9 Pipet, Pasteur type, disposable17,5 (or equivalent). For NR/BR/SBR: 1375, 835, 735, and 699 cm−1
16.1.10 Usual Laboratory Glassware, necessary for carry- For BR/SBR: 910, 735, and 699 cm−1
ing out the test method as written. 19.5 Inaccurate results will be obtained if absorbance ratios
from di-blends are compared to ratios from tri-blends.
17. Safety Precautions
17.1 Because of the toxicity of the solvents used in this test 20. Procedure
method, a well-ventilated fume hood shall be used and the skin 20.1 Dry the extracted test portion thoroughly and grind in
and eyes suitably protected during this analysis. the mill (16.1.1) to 420 µm.
17.2 Although not outlined in this test method, all recog-
20.2 Divide the test portion into approximately equal por-
nized health and safety precautions shall be observed when
tions and place in three 50-cm3 conical flasks.
following this test method.
20.3 Place a stirring bar in each of the flasks, fill it nearly
18. Preparation of Test Portion full with 1,2-dichlorobenzene, and cover with a watch glass.
20.4 Place the flasks on the stirring hot plate, set for a
18.1 If the test portion is vulcanized, sheet it out on a cool temperature a few degrees below boiling (approximately
mill and weigh approximately 2.2 g. 175°C), and stir vigorously for 2 to 8 h, until digestion is
18.2 If the test portion is unvulcanized, vulcanize it and complete.
sheet it out on a cool mill. Weigh approximately 2.2 g.
20.4.1 It is imperative that digestion be complete so that all
18.2.1 Test portions must be vulcanized; otherwise, the of the rubber is in solution. Completeness of digestion is
intensity of the unsaturation bands will be variable. evident when the flask is shaken, held up to a strong light, and
18.3 Extract the vulcanized sheet overnight with alcohol the solution exhibits a deep purplish-brown color with no
(4.3), using the apparatus in accordance with 8.1. undigested particles floating on the surface.
18.4 Extraction for 2 h with acetone or 2-butanone may also 20.5 Prepare a filter bed by placing a glass fiber filter in a
be effective. Büchner funnel, wetting it with chloroform, then filling the
18.4.1 The object of extraction is to remove, as much as funnel with diatomaceous filter aid (4.7), and saturating this
possible, all the additives in the compound. The choice of with chloroform from a wash bottle.
solvent is left to the discretion of the analyst, whose prior
20.6 With the Büchner funnel in place on the vacuum
knowledge of the vulcanizate composition will dictate the most
filtering device (16.1.6) and a 250-cm3 beaker placed to receive
suitable solvent for extraction.
the filtrate, pour the hot solution from the flask into the funnel,
and at the same time turn on the vacuum.
19. Calibration
20.7 Wash the solution through the funnel with boiling
19.1 Prepare sets of standard, vulcanized compounds con- chloroform until the filtrate comes through colorless.
taining blends of the rubbers of interest over ranges of expected 20.7.1 Filtering requires some experience. If a black filtrate
ratios (for example, 80/20 NR/BR, 70/30, 60/40, 50/50) with comes through the filter (or anything darker than a golden-
blends of two or three rubbers. yellow) it will be necessary to refilter the solution, while hot,
19.1.1 Prepare separate standard blends for emulsion SBR, through the filter until the filtrate is clear.
solution SBR, and high-styrene SBR, and for cis-BR and
20.7.2 Stirring the filter bed with a spatula during filtration
high-trans emulsion BR.
can improve the intimate contact between the filter aid and the
19.1.2 NR and IR give essentially the same values; there- liquid.
fore, one set of standards with either IR or NR should be
20.8 Evaporate the liquid in the beaker to near dryness on an
sufficient.
electric hot plate, at the same temperature as in 20.4, using a
19.2 Carry out the preparation and procedure as outlined in
stream of dry air.
Sections 18 and 20 for all blends. Use the same infrared
instrument for sample measurement as for standard calibration 20.9 Add a few drops of toluene to the dried residue of 20.8,
measurements. and with a Pasteur pipet (16.1.9), transfer a few drops of the
solution to the sodium chloride or potassium bromide plate
19.3 On linear graph paper, plot the absorbance ratios for
(8.7) that has been placed on a watch glass.
each peak in each blend against the known rubber content of
each rubber, in percent of total rubber. 20.10 Place the prepared plate in a vacuum oven under
19.3.1 For BR blends at 735 cm−1, make separate calibra- strong vacuum with a slight intake of air at about 50°C for 1 h
tion curves for high SBR and high NR content. to dry the film completely. Make the film even by smoothing it
with a rotating motion of the side of the Pasteur pipet. The
19.4 Use the following peak absorbance and that at 1450
thickness of the film shall be such that when placed in the
cm−1 to obtain the necessary ratios:
sample beam of the spectrophotometer and measured against
air in the reference beam, an absorbance of 0.04 to 0.10 is
obtained at 4000 cm−1, and 0.35 to 0.45 absorbance at the peak
17
The sole source of supply of the pipet known to the committee at this time is around 1450 cm−1. This corresponds to about 80 to 90 % and
Fisher Scientific Co., Catalog No. 13-678-6A. 35 to 45 % transmittance respectively.

8
 D 3677 – 00 (2004)
20.11 Scan the spectrum of the prepared film (20.10) from 835 propenyl —C=CH—
approximately 4000 to 600 cm−1 with an instrument setting ?
CH3
suitable for quantitative analysis, in the absorbance mode, if 699 5 adjacent hydrogens of monosubstituted benzene ring
possible. (for example, phenyl) of styrene
735 cis C=C
NOTE 5—On the Perkin-Elmer, Model 283, suitable settings are: scan
time 12 min, response 1, absorbance mode, program N(6), abscissa and 22. Precision and Bias
ordinate expansion 1, with suppression.
22.1 Precision—No work has been done to test the preci-
20.11.1 The spectrophotometer shall be adjusted according sion of this test method, however, the results obtained by this
to the manufacturer’s directions for optimum performance. test method have been verified on an NR/SBR blend, using Test
Since instruments vary widely in settings and display, the Methods D 297, Section 52, for Polyisoprene Content, and
optimum settings are left to the discretion of the analyst. Refer Section 56, for SBR Content, and the results have been found
to Practice E 168 for further recommendations on the use of to be consistent within 65 %.
infrared spectrophotometers. 22.2 Bias—Under the best conditions, accuracy is 65 % of
20.11.2 If only a transmittance mode is possible with the the rubber content for detection of EPDM or IIR in NR, IR,
instrument being used, the spectrum shall be scanned in that BR, SBR, or CR. For example, in a 70/30 NR/BR blend, the
mode. outlined procedure would give 70 6 5 % NR and 30 6 5 %
20.12 Draw baselines with a straightedge, preferably to BR.
approximately the following wavenumbers (all values are in
23. Apparatus
reciprocal centimetres):
1390–1510 for the 1450 peak
23.1 Usual laboratory glassware necessary for carrying out
1340–1390 for the 1375 peak the test method as written and in addition to apparatus in 8.7
930–990 for the 965 peak and 8.8 are the following:
790–870 for the 835 peak
650–790 for the 735 peak
23.2 Stainless Steel Sieve, 18,5 420 µm (40 mesh) or finer.
660–710 for the 699 peak 23.3 Electric Hot Plate.
20.12.1 Although other baselines can be used, experience 24. Reagents
has shown that short baselines are preferred. In any case, the
24.1 Chromic Acid Digestion Mixture—Dissolve 200 g of
analyst must draw the baselines for the standards in the same
chromic acid (CrO3) in 500 cm3 of water, Cautiously add 150
manner as was done for the samples.
cm3 of H2SO4(density 1.84 mg/m3), and mix well.
20.13 On the spectrum, subtract the absorbance at a point on 24.2 Acetone, Reagent Grade.
the baseline directly below each peak of interest, from the peak 24.3 Dichloromethane, Reagent Grade, with a residue on
absorbance, to give the corrected absorbance. evaporation not over 0.0002 %.
20.13.1 When the percent transmittance mode is used, 24.4 Wetting Agent—A saturated solution of dioctyl sodium
divide the percent transmittance at a point on the baseline sulfosuccinate (aerosol OT) is satisfactory.
directly above the peak by the percent transmittance of the
peak and take the log10 of the quotient. 25. Procedure
20.14 Obtain absorbance ratios by dividing the corrected 25.1 Weigh about 1 g of milled vulcanizate and place in a
absorbance of each of the peaks at 1375, 965, 910, 835, 735, 400-cm3 beaker, then add about 200 cm3 of acetone. (Uncured
and 699 cm−1 as are of interest, by the corrected absorbance at compounds should be vulcanized by any appropriate method,
1450 cm−1. before milling.)
20.15 Take the mean for the three test portions as the 25.2 Heat the beaker on a hot plate, so that it boils for about
absorbance ratio in each case. 1 min, then decant the acetone. This short solvent treatment
20.16 Using the data obtained in 20.14 and 20.15, refer to will remove most of the compounding and extender oils,
the calibration curves prepared in accordance with Section 19 should any be present.
and determine the percent of each rubber in the mixture. 25.3 Dry the beaker and contents until all of the acetone has
20.17 If the readings from different peaks disagree, give evaporated, then add 50 cm3 of the acid digestion solution (see
precedence to the 1375 and 699 cm−1 peaks as the most 24.1) and one drop of wetting agent (see 24.4).
accurate, 835 and 735 cm−1 peaks as second in accuracy, and 25.4 Cover the beaker with a watch glass and place on a
965 and 910 cm−1 peaks as the least accurate. steam plate or steam bath (not an electric hot plate) and observe
the start of the reaction, as evidenced by bubbles. Remove the
21. Absorbance Peaks and Their Assignments beaker just 15 min after bubbles start to appear.
25.5 Pour the warm solution through the sieve (see 23.2),
21.1 The absorbance peaks and their assignments are: wash the residue copiously with hot water, then with a few
cm−1 cubic centimetres of acetone.
1450 methylene —CH2—
1375 methyl —CH3
965 trans C=C 18
The sole source of supply of the stainless steel sieve known to the committee
910 vinyl C=C at this time is W. S. Tyler Co., Mentor, OH 44060.

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 D 3677 – 00 (2004)
TABLE 1 Determination of Saturated Rubbers in the Presence of Unsaturated Rubbers
Results found by laboratory
Sample Known
Lab. 1 Lab. 2 Lab. 3 Lab. 4
A 424 29 % CIIR, 3 % EPDM, 13 % NR, 10 % SBR IIR IIR IIR IIR
A 425 12 % CIIR, 12 % EPDM, 15 % NR, 15 % SBR IIR + EPDM IIR + EPDM IIR + EPDM IIR + EPDM
A 426 5 % IIR, 10 % NR, 5 % BR, 29 % SBR, 5 % CR IIR + EPDM IIR + EPDM IIR IIR + EPDM
A 427 5 % EPDM, 10 % NR, 5 % BR, 29 % SBR, 5 % CR EPDM ... IIR + EPDM EPDM
A 428 3 % IIR, 13 % NR, 5 % BR, 29 % SBR, 5 % CR IIR EPDM IIR IIR + EPDM
A 429 3 % EPDM, 13 % NR, 5 % BR, 39 % SBR, 5 % CR EPDM EPDM IIR + EPDM EPDM

25.6 If there is no rubber residue on the sieve at this point, 25.11 Compare the spectrum obtained with Fig. 28 and Fig.
then IIR or EPDM is absent, and the test should be discontin- 32 or preferably to one’s own spectra of purified IIR or EPDM.
ued. NOTE 7—Purified rubbers may be prepared by pouring a hot toluene
25.7 If there is residue on the sieve, collect it in a beaker, solution of the rubber into about four times as much methanol to coagulate
dry off most of the acetone and add 30 cm3 of dichloromethane, it, then dissolving it in dichloromethane and scanning in the same manner
cover the beaker with a watch glass and boil the dichlo- as for the unknowns.
romethane on a hot plate at high heat until a volume of about 25.12 Note the following diagnostic bands and their con-
10 cm3 is reached. figurations: 1390, 1370, and 1230 cm−1 for IIR and 1380 and
NOTE 6—If a large amount of solid particles are present, filter the 721 cm−1 for EPDM. Since the 1380-cm−1 band might be
solution into a beaker through a loose filter such as a glass fiber pad or caused by NR contamination, look for the accompanying NR
glass wool. However, this filtration may not be necessary. band at 836 cm−1 to verify this contamination.
25.8 Pour the solution into a 50-cm3 beaker and evaporate 26. Precision and Bias
to 1 to 2 cm3. 26.1 See 14.1.2.
25.9 Apply enough drops of the solution from 25.8 to a salt 26.2 A task group composed of four laboratories, testing six
plate window to make a good film. Evaporate the dichlo- vulcanizates (both black and white stocks) obtained the fol-
romethane with gentle heat (for example in a vacuum oven at lowing results with this test method: see Table 1.
50°C). If the residue was quite small, apply all of it to the salt
plate. 27. Keywords
25.10 With the salt plate in the sample beam of the infrared 27.1 acrylonitrile-butadiene rubber; balata; butyl rubber;
spectrophotometer and air in the reference beam, scan the chloroprene; ethylene-propylene rubber; ethylene-propylene-
spectrum from 4000 to 600 cm−1 or lower. If the spectrum is diene rubber; gutta percha; infrared spectrometry; polybutadi-
weak, expand it 5 or 10 times in the ordinate direction, if the ene; polyisoprene; nitrile rubber; styrene-butadiene rubber
instrument permits.

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 D 3677 – 00 (2004)

FIG. 3 IR Pyrolyzate from Raw Rubber

FIG. 4 IR Pyrolyzate from a Vulcanizate

FIG. 5 SBR Pyrolyzate from Raw Rubber

11
 D 3677 – 00 (2004)

FIG. 6 SBR Pyrolyzate from a Vulcanizate

FIG. 7 NBR Pyrolyzate from Raw Rubber

FIG. 8 NBR Pyrolyzate from a Vulcanizate

12
 D 3677 – 00 (2004)

FIG. 9 CR Pyrolyzate from Raw Rubber

FIG. 10 CR Pyrolyzate from a Vulcanizate

FIG. 11 IIR Pyrolyzate from Raw Rubber

13
 D 3677 – 00 (2004)

FIG. 12 IIR Pyrolyzate from a Vulcanizate

FIG. 13 BR Pyrolyzate from Raw Rubber

FIG. 14 BR Pyrolyzate from a Vulcanizate

14
 D 3677 – 00 (2004)

FIG. 15 EPM Pyrolyzate from Raw Rubber

FIG. 16 EPM Pyrolyzate from a Vulcanizate

FIG. 17 CSM Pyrolyzate from Raw Rubber

15
 D 3677 – 00 (2004)

FIG. 18 CSM Pyrolyzate from a Vulcanizate

FIG. 19 IR Film from Raw Rubber

FIG. 20 IR Film from a Vulcanizate

16
 D 3677 – 00 (2004)

FIG. 21 SBR Film from Raw Rubber

FIG. 22 SBR Film from a Vulcanizate

FIG. 23 NBR Film from Raw Rubber

17
 D 3677 – 00 (2004)

FIG. 24 NBR Film from a Vulcanizate

FIG. 25 CR Film from Raw Rubber

FIG. 26 CR Film from a Vulcanizate

18
 D 3677 – 00 (2004)

FIG. 27 IIR Film from Raw Rubber

FIG. 28 IIR Film from a Vulcanizate

FIG. 29 BR Film from Raw Rubber

19
 D 3677 – 00 (2004)

FIG. 30 BR Film from a Vulcanizate

FIG. 31 EPM Film from Raw Rubber

FIG. 32 EPM Film from a Vulcanizate

20
 D 3677 – 00 (2004)

FIG. 33 CSM Film from Raw Rubber

FIG. 34 CSM Film from a Vulcanizate

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21