Designation: D 3677 – 00

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 3.2 This test method provides such composition analysis

1.1 These test methods, based on infrared examination of utilizing an infrared technique.
pyrolysis products (pyrolyzates) and films can be used for 4. Reagents
rubber identification.
1.2 These test methods are applicable to rubbers in the raw 4.1 Purity of Reagents—Reagent grade chemicals shall be
state and, when compounded, both in the cured and uncured used in all tests. Unless otherwise indicated, it is intended that
state. all reagents shall conform to the specifications of the Commit-
1.3 The values stated in SI units are to be regarded as tee on Analytical Reagents of the American Chemical Society,
standard. where such specifications are available.4 Other grades may be
1.4 This standard does not purport to address all of the used, provided it is first ascertained that the reagent is of
safety concerns, if any, associated with its use. It is the sufficiently high purity to permit its use without lessening the
responsibility of the user of this standard to establish appro- accuracy of the determination.
priate safety and health practices and determine the applica- 4.2 Acetone.
bility of regulatory limitations prior to use. Specific precau- 4.3 Alcohol, specially denatured (Formula 2-B or 30 is
tionary statements are given in Section 17. satisfactory).
4.4 2-Butanone.
2. Referenced Documents 4.5 Chloroform.
2.1 ASTM Standards: 4.6 Congo Red Paper.
D 297 Test Methods for Rubber Products—Chemical 4.7 Diatomaceous Filter Aid5—Some grades are quite un-
Analysis2 satisfactory in that they will not sufficiently absorb carbon
D 1418 Practice for Rubber and Rubber Latices— black.
Nomenclature2 4.8 1,2-Dichlorobenzene6—A check on suitability may be
D 3452 Practice for Rubber—Identification by Pyrolysis- made by evaporating 50 cm3 to dryness and making an infrared
Gas Chromatography2 spectrum of the residue. Any substantial absorbance at posi-
E 168 Practices for General Techniques of Infrared Quanti- tions near those wavenumbers that will be used for rubber
tative Analysis3 analysis, indicates that the 1,2-dichlorobenzene is unsuitable
for use.
3. Significance and Use 4.9 Dry Compressed Air and Nitrogen, in cylinders, or
3.1 For research, development, and quality control pur- provided as a laboratory service.
poses, it is advantageous to determine the composition of 4.10 Sodium Sulfate, anhydrous.
rubbers in cured, compounded products. 4.11 Toluene.

4
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
1
These test methods are under the jurisdiction of ASTM Committee D11 on listed by the American Chemical Society, see Analar Standards for Laboratory
Rubber and are the direct responsibility of Subcommittee D11.11 on Chemical Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Analysis. and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Current edition approved Nov. 10, 2000. Published December 2000. Originally MD.
published as D 3677 – 78. Last previous edition D 3677 – 90 (1995)e1 5
Fisher Scientific, Catalog No. C211 (Celite) is satisfactory.
2 6
Annual Book of ASTM Standards, Vol 09.01. J. T. Baker Chemical Co., Phillipsburg, NJ 08865, Catalog No. 9217 has been
3
Annual Book of ASTM Standards, Vol 03.06. found satisfactory.

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

1
 D 3677 – 00
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

PART 1 QUALITATIVE ANALYSIS

5. Scope 6.1.6 Polybutadiene Rubber (High cis):

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

2
 D 3677 – 00

F electric, thermoregulated furnace

H aluminum block, bored to hold tubes
P glass tube for sample container
S ground-glass taper
T collecting tube
FIG. 2 Temperature Controlled Pyrolysis Apparatus

FIG. 1 Extraction Apparatus with Glass Condenser 8.8 High-Resolution Infrared Spectrophotometer, double
and Ground Glass Joint 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
7.2.2 A small quantity of extracted and dried rubber is
exceed 2 cm−1 over 80 % of the wavenumber range and at no
subjected to mild thermal degradation at 200 6 5°C for a short
place should it exceed 5 cm −1.) Any spectrophotometer
time. The degraded sample is dissolved in trichloroethylene
complying with these requirements may be used. The equip-
then chloroform, and a film cast on a salt plate. This film is
ment shall be operated by an experienced analyst according to
used as in 7.1.4.
the manufacturer’s directions for optimum performance.9
8. Apparatus
9. Preparation of Test Portion
8.1 Extraction Apparatus:
9.1 Temperature Controlled Pyrolysis in a Stream of Nitro-
8.1.1 The extraction apparatus used shall be of the general
gen (Fig. 2; Preferred Method):
type and dimensions shown in Fig. 1.
9.1.1 Prepare the test portion by milling into a thin sheet on
8.2 Test Tubes, small, and other necessary glassware suffi-
a laboratory mill or cutting into cubes about 2 mm wide and
cient to carry out the test as written.
wrap approximately 0.5 g in filter paper or nylon cloth. Extract
8.3 Pyrolysis Apparatus (Fig. 2)—The pyrolysis apparatus
the wrapped test portion in an extraction cup in accordance
consists of a glass tube (P) having inward projections to
with Section 18 of Test Methods D 297, for a minimum of 4 h
prevent the sample from falling to the bottom of the tube and
with methanol, ethanol, or 2-propanol. A vulcanizate may be
a lateral condenser tube. The tube (P) has a ground-glass
extracted with acetone or 2-butanone, in addition to the above
standard taper (S) which carries a small glass adductor tube. A
alcohols. Alternatively, the rapid reflux procedure may be used
collecting tube (T) is placed under the condenser tube. An
for 1 h in accordance with Section 25 of Test Methods D 297.
electric, thermoregulated furnace (F) accommodates an alumi-
9.1.2 Remove the extracted rubber from the apparatus and
num block (H) with holes for one or more tubes (P).
dry at 100°C until free of solvent. One to two hours is usually
8.4 Capillary Pipets.
required.
8.5 Oven, capable of maintaining a temperature of 200 6
9.1.3 Introduce a small amount of anhydrous sodium sulfate
5°C for use in 10.2.
into the collecting tube (T) to absorb water produced during
8.6 Water Bath, for use in 10.2.
pyrolysis.
8.7 Salt Plates, polished (sodium chloride or potassium
bromide), 4 by 25 mm, to serve as windows for the spectro-
photometer.7
8
High resolution is defined in “Specification for Evaluation of Research Quality
Analysis of Infrared Spectra, Analytical Chemistry, ANCHA, Vol 47, No. 11, p.
94A.
7 9
Barnes Engineering Co., Stamford, CT 06902, Catalog No. 7000-316 has been Perkin-Elmer, Model 283, Perkin-Elmer Corp., Norwalk, CT 96856, has been
found satisfactory. found satisfactory.

3
 D 3677 – 00
9.1.4 Place a strip of moistened Congo red paper across the 10.1.3 Place 1 g of the prepared rubber (9.1.1 and 9.1.2) and
mouth of the tube, as a test for chlorine (a change from red to 50 cm3 of 1,2-dichlorobenzene in a 100-cm3 flask fitted with a
blue). reflux condenser. Boil until the rubber is dispersed or dis-
9.1.5 If alternative chlorine determining methods are em- solved.
ployed, this procedure must be suitably modified. 10.1.3.1 The time required for dissolution varies with the
9.1.6 Bring the electrical furnace ( F) to 450 to 500°C and rubber. Natural rubber requires 3 to 4 h, while chloroprene
hold at this temperature. This range is recommended to obtain requires more than 24 h. Some rubbers never completely
fast pyrolysis, without excessive degradation and carboniza- dissolve.
tion. Temperatures below this range should be avoided. 10.1.3.2 Discontinue refluxing at the end of 48 h to mini-
9.1.7 Pass a slow stream of nitrogen through the pyrolysis mize the risk of altering the molecular structure of the rubber.
tube and introduce the tube into a hole of the aluminum block 10.1.3.3 Even though complete dissolution is not effected in
( H). The nitrogen serves to displace air, prevent oxidation, and 48 h, enough rubber has usually dissolved to provide a good
facilitate transfer of the pyrolysis products to the collecting spectrum.
tube ( T).
10.1.4 Cool the mixture and transfer to a beaker with 50 cm3
9.1.8 Carry on heating to complete distillation, which re- of toluene.
quires approximately 15 min.
10.1.5 If the compound does not contain carbon black,
9.1.9 Transfer a few drops of the pyrolyzate from the tube to
centrifuge to eliminate mineral fillers.
a sodium chloride or potassium bromide plate, using a capillary
pipet. 10.1.6 If the compound contains carbon black, add 10 to 20
9.1.10 Place a spacer of suitable thickness in position, close g of filter aid (4.7) to facilitate filtration through filter paper.
the cell with a second plate of the same material, and mount the 10.1.7 If the filtrate from 10.1.6 still contains carbon black,
cell in the infrared spectrophotometer. repeat the filtration with additional filter aid.
9.1.11 Record the spectrum over the wavelength range from 10.1.8 Concentrate the centrifuged or filtered solution to a
2.5 to 15 µm. small volume under vacuum in a stream of nitrogen.
9.1.12 Spectra should be obtained immediately after pyroly- 10.1.9 Evaporate a few drops of the concentrated solution
sis to minimize further change in the pyrolysis products. on a salt plate to give a film thickness with 10 to 20 %
9.2 Gas Flame Pyrolysis (Alternative Test Method): transmittance at 6.9 µm.
9.2.1 Prepare the extract, dry 2 g of test portion (9.1.1 and 10.1.10 Record the spectrum over the 2.5 to 15-µm wave-
9.1.2), and place 0.1 to 0.2 g of the test portion in the bottom length region.
of a small glass test tube. Place a strip of moistened Congo red 10.2 Mild Thermal Degradation for Vulcanizates:
paper across the mouth of the tube. Hold the tube horizontally, 10.2.1 Prepare, extract, and dry about 2 g of rubber in
and quickly bring the lower end containing the test portion into accordance with 9.1.1 and 9.1.2.
the hot zone of a gas burner, so that the rubber is rapidly
10.2.2 Place the dried rubber in a test tube capped with glass
pyrolyzed and charring is kept to a minimum. Note any color
change in the Congo red paper, from red to blue, indicating the wool and heat to 200 6 5°C in the oven (8.5) for approxi-
presence of chlorine. mately 10 min.
9.2.2 Maintain the heating until the pyrolyzate condenses in 10.2.3 Transfer the rubber to a beaker and add 50 cm 3 of
the cool end of the tube, withdraw the test tube from the flame, trichloroethylene.
and cool while holding horizontally. 10.2.4 Allow the beaker and contents to stand on a water
9.2.3 Alternatively, the sample may be placed in a small bath for approximately 30 min with occasional stirring to effect
glass tube and the end of the tube drawn out to a “retort” shape dissolution of the degraded rubber.
with a blast lamp. Pyrolysis is carried out as described in 9.2.1. 10.2.5 Filter the mixture (10.2.4) through filter paper to
Care should be taken to keep the delivery end of the pyrolysis remove any undissolved vulcanizate or fillers.
tube warm enough so that pyrolysis products do not condense 10.2.6 If free carbon is released by the vulcanizate (some-
and block the opening, causing the tube to explode. The times found with polyisoprene and butyl rubbers), add a small
condensate can be collected in a small test tube containing amount of filter aid (4.7) to the solution before filtering.
anhydrous sodium sulfate to remove moisture. Proceed in 10.2.7 Remove the trichloroethylene by evaporation, distil-
accordance with 9.1.9-9.1.12. lation, or by the use of a rotary evaporator with vacuum. In no
9.2.4 If alternative chlorine detecting methods are em- case should the solution be heated to over 80°C.
ployed, this procedure must be suitably modified.
10.2.8 Dissolve the residue in a small amount of chloro-
form.
10. Sample Preparation for Films
10.2.9 If the analyst suspects that the filtrate from 10.2.6
10.1 Dissolution for Vulcanizates: contains material other than rubber, which might interfere in
10.1.1 Prepare a test portion in accordance with 9.1.1 and interpretation of the final infrared spectrum, the polymer
9.1.2. should be precipitated from the solution of 10.2.5 or 10.2.6 by
10.1.2 Pyrolyze and test for chlorine in accordance with methanol. Filter the recovered polymer and dissolve in chlo-
9.1.4 and 9.1.5 or 9.2.1-9.2.4. roform.

4
 D 3677 – 00
10.2.10 Cast a film having 10 to 20 % transmittance at 6.9 11.2.2 The table also serves to augment the reference
µm, on a salt plate (see 8.7). Record the infrared spectrum over spectra by drawing attention to absorptions that are absent,
the 2.5 to 15-µm wavelength region, using the infrared equip- thereby eliminating certain rubbers when ambiguity might
ment (8.8). arise.
10.3 Dissolution for Raw Rubbers: 11.2.3 In Sections 12 and 13, diagnostic absorptions are
10.3.1 Prepare a test portion in accordance with 9.1.1 and arranged in order from strong to weak. By “diagnostic value”
9.1.2, pyrolyze, and test for chlorine in accordance with 9.1.4 is meant those features of the absorption, subjectively assessed,
and 9.1.5 or 9.2.1-9.2.4. which a practiced spectroscopist recognizes as of significance
10.3.2 Place 1 g of the prepared rubber (9.1.1 and 9.1.2) and in rubber identification. Such absorptions are not necessarily
50 cm3 of chloroform in a 100-cm 3 flask fitted with a reflux specific nor necessarily very intense. They are, however,
condenser. Boil until the rubber dissolves. identifiable with certain compositional or structural features of
10.3.3 Cool and transfer to a beaker. the liquid pyrolyzates and films, and reproducible in the sense
10.3.4 Concentrate the solution to a small volume under that they are not seriously influenced by moderate variations in
vacuum in a stream of nitrogen. pyrolysis and dissolution conditions.
10.3.5 Cast a film on a salt plate and record the infrared 11.2.4 In general, it can be assumed with confidence that,
spectrum over the 2.5 to 15-µm wavelength region, taking care apart from exceptions stated, all the absorptions listed in
that the film has a thickness sufficient to give approximately 10 Sections 12 and 13 will appear in the spectrum of the
to 20 % transmittance at 6.9 µm. corresponding pyrolyzate or film, and if absent, it is inferred
that the rubber sought is absent.
11. Interpretation of Spectra
12. Diagnostic Absorptions for Pyrolyzates
11.1 Reference Spectra:
12.1 The following absorptions, when they occur, are of no
11.1.1 Because of the different modes of presentation of
diagnostic value and should not be used for rubber identifica-
spectra, it is strongly recommended that a set of reference
tion:
spectra on the same instrument should be prepared before
Wavelength, µm Wavenumber, cm−1
proceeding to unknown samples.
11.1.2 Reference spectra must be produced from test pieces 3.0 3330
of known composition following either Section 9 or 10. 3.5 2860
5.9 1700
11.1.3 Spectra of mixtures are not given because it is 6.9 1450
preferable for each laboratory to prepare its own set from test
NOTE 1—The SI unit for wavenumber is the reciprocal metre. Until
pieces of known composition. such units are used on instruments and graphs, the reciprocal centimetre
11.1.4 Small, but unavoidable variations in experimental will be retained in this standard.
conditions and instrument characteristics may give rise to
12.2 The principal absorptions in order of diagnostic value
slight differences in spectra. Spectra produced at different times
are as follows:
may not be identical in terms of peak height (intensity of
12.2.1 Isoprene Rubber (see Fig. 3 and Fig. 4):
absorption) or absorption wavelength. The experienced spec-
Wavelength, µm Wavenumber, cm−1 Intensity
troscopist will recognize this.
11.1.5 Vulcanizates may give slightly different liquid pyro- 11.3 885 very strong
lyzate and film spectra than those prepared from corresponding 7.3 1370 strong
12.5 800 medium
raw rubber, and the interpretation of such spectra requires 6.1 1640 medium
particular care, when strong characteristic features are lacking. 11.0 909 shoulder
11.1.6 The precautions of 11.1.4 and 11.1.5 are cited to alert In vulcanizates the absorption at 12.5 µm (800 cm −1) may
the spectroscopist to difficulties that may arise from the use of sometimes decrease in intensity with the appearance of a
this method and to encourage the practice of maintaining a broader, less intense absorption at 12.3 µm (813 cm−1).
reference file of films and pyrolyzates of all the rubbers that 12.2.2 Styrene-Butadiene Rubber (see Fig. 5 and Fig. 6):
may require identification.
Wavelength, µm Wavenumber, cm−1 Intensity
11.1.7 In all cases, spectra must be interpreted in the light of
the test for chlorine. If the test for chlorine is negative, then the 14.3 699 very strong
rubber is characterized as a hydrocarbon or nitrile type. 12.9 775 strong
6.7 1490 medium
11.2 Diagnostic Absorptions: 11.0 909 strong
11.2.1 The tables of diagnostic absorptions (Sections 12 and 10.1 990 fairly strong
10.4 962 medium
13) should be used only in conjunction with the reference
spectra. Their purpose is to indicate the principal absorptions The relative intensities of absorptions at 11.0 µm (909 cm−1),
by which the spectra may be related to films and pyrolyzates, 10.1 µm (990 cm−1), and 10.4 µm (962 cm−1) depend on the
such as the specific nature of certain peaks, their relationship ratio of isomers in the polybutadiene component and, therefore,
with neighboring peaks or other regions of the spectrum, etc. may vary.

5
 D 3677 – 00

FIG. 3 IR Pyrolyzate from Raw Rubber

FIG. 4 IR Pyrolyzate from a Vulcanizate

12.2.3 Acrylonitrile-Butadiene Rubber (see Fig. 7 and Fig. while the stronger absorptions at 11.3 µm (885 cm−1) and 14.3
8): µm (699 cm−1) are common in some degree to all the other
Wavelength, µm Wavenumber, cm−1 Intensity polymers.
4.5 2220 medium strong 12.2.5 Butyl Rubber (see Fig. 11 and Fig. 12):
10.4 962 medium Wavelength, µm Wavenumber, cm−1 Intensity
6.2 1610 medium
6.3 1590 medium 7.3 1370 strong
11.0 909 medium 7.2 1390 strong
11.3 885 strong
12.2.4 Chloroprene Rubber (see Fig. 9 and Fig. 10): 8.0 to 8.2 1250 to 1220 medium doublet, some-
Wavelength, µm Wavenumber, cm−1 Intensity times absent
13.8 727 very weak, sometimes
12.2 820 medium absent
13.4 747 weak, sometimes absent
13.0 769 weak, sometimes absent 12.2.6 Polybutadiene Rubber (see Fig. 13 and Fig. 14):
11.3 885 medium Wavelength, µm Wavenumber, cm−1 Intensity
14.3 699 medium
11.0 909 strong
The pyrolyzate of chloroprene rubber can give a variable 10.4 962 strong
spectrum that also tends to be lacking in characteristic features. 10.1 990 medium
The most useful absorption is that at 12.2 µm (820 cm−1), but 12.3 813 weak
14.4 695 weak
this is rather broad and often not very intense. A weak
absorption at 13.4 µm (747 cm−1) sometimes fails to appear,

6
 D 3677 – 00

FIG. 5 SBR Pyrolyzate from Raw Rubber

FIG. 6 SBR Pyrolyzate from a Vulcanizate

FIG. 7 NBR Pyrolyzate from Raw Rubber

12.2.6.1 Some of the principal absorptions in the spectrum and the result of the test for chlorine should be taken into
obtained from the pyrolyzate of polybutadiene rubber are account when deciding between these two rubbers (see also
closely similar both in frequency and intensity to those found 12.2.8). Particular care should be exercised in the interpretation
in the spectrum of chlorosulfonated polyethylene pyrolyzate of spectra from vulcanizates, and the 12 to 15-µm (833 to

7
 D 3677 – 00

FIG. 8 NBR Pyrolyzate from a Vulcanizate

FIG. 9 CR Pyrolyzate from Raw Rubber

667-cm −1) region should be well scrutinized for small, but Wavelength, µm Wavenumber, cm−1 Intensity
diagnostically significant absorptions.
11.0 909 strong
12.2.6.2 Polybutadiene rubbers having different isomer ra- 10.4 962 medium
tios may, on pyrolysis, show absorptions of differing relative 10.1 990 medium
intensities, notably those at 10.4 and 11.0 µm (962 and 909 12.3 813 weak
13.5 741 medium
cm−1). 13.9 720 weak
12.2.6.3 The spectrum of the polybutadiene pyrolyzate dif- 14.4 695 weak
fers from that of the styrene–butadiene pyrolyzate in that the
absorptions due to aromatic constituents are absent or much Some of the principal absorptions in the spectrum obtained
reduced. from the pyrolyzate of chlorosulfonated polyethylene are
12.2.7 Ethylene Propylene Rubber (see Fig. 15 and Fig. closely similar both in frequency and intensity to those found
16): in the spectrum of polybutadiene pyrolyzate, and the result of
Wavelength, µm Wavenumber, cm−1 Intensity the test for chlorine should be taken into account when
deciding between these two polymers. The table above in-
7.3 1370 strong
11.0 909 strong
cludes some absorptions common to both, but the bands at 12.3
11.3 885 strong and 13.5 µm (813 and 741 cm −1) although not particularly
10.4 962 medium strong, are indicative of chlorosulfonated polyethylene. Par-
13.8 725 medium
ticular care should be exercised in the interpretation of spectra
12.2.8 Chlorosulfonated Polyethylene (see Fig. 17 and Fig. from vulcanizates.
18):

8
 D 3677 – 00

FIG. 10 CR Pyrolyzate from a Vulcanizate

FIG. 11 IIR Pyrolyzate from Raw Rubber

13. Diagnostic Absorptions for Films 13.2.2 Styrene-Butadiene Rubber (see Fig. 21 and Fig. 22):
13.1 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- 14.3 699 very strong
tion: 13.2 758 strong
Wavelength, µm Wavenumber, cm−1 6.7 1490 medium
11.0 909 strong
3.0 3330 10.4 962 very strong
3.5 2860
5.9 1700 Reported diagnostic absorptions and related spectra refer to
6.9 1450 styrene-butadiene rubber with a styrene content of about
13.2 The principal absorptions in the order of diagnostic 23.5 %, produced by emulsion polymerization. Other copoly-
value are as follows: mers having different monomer ratios or copolymers produced
13.2.1 Isoprene Rubber (see Fig. 19 and Fig. 20): by solution polymerization may have slightly different diag-
Wavelength, µm Wavenumber, cm−1 Intensity nostic absorption and spectra.
12.0 833 strong
13.2.3 Acrylonitrile-Butadiene Rubber (see Fig. 23 and
7.3 1370 strong Fig. 24):
6.0 1665 medium Wavelength, µm Wavenumber, cm−1 Intensity
11.3 885 weak
4.5 2220 strong
Reported diagnostic absorptions and related spectra for
10.4 962 very strong
natural rubber and synthetic polyisoprene are tabulated above. 11.0 909 medium
Gutta percha and balata have different diagnostic absorptions
and spectra.

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FIG. 12 IIR Pyrolyzate from a Vulcanizate

FIG. 13 BR Pyrolyzate from Raw Rubber

FIG. 14 BR Pyrolyzate from a Vulcanizate

Reported diagnostic absorptions and related spectra refer to 13.2.4 Chloroprene Rubber (see Fig. 25 and Fig. 26):
acrylonitrile-butadiene rubber with an acrylonitrile content of
about 33 %.

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FIG. 15 EPM Pyrolyzate from Raw Rubber

FIG. 16 EPM Pyrolyzate from a Vulcanizate

FIG. 17 CSM Pyrolyzate from Raw Rubber

Wavelength, µm Wavenumber, cm−1 Intensity 13.2.5 Butyl Rubber (see Fig. 27 and Fig. 28):
6.0 1665 very strong
7.6 1315 medium
9.0 1110 strong
12.2 820 strong

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FIG. 18 CSM Pyrolyzate from a Vulcanizate

FIG. 19 IR Film from Raw Rubber

FIG. 20 IR Film from a Vulcanizate

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FIG. 21 SBR Film from Raw Rubber

FIG. 22 SBR Film from a Vulcanizate

Wavelength, µm Wavenumber, cm−1 Intensity Wavelength, µm Wavenumber, cm−1 Intensity

7.3 1370 very strong 7.3 1370 strong

7.2 1390 very strong 8.7 1145 medium
8.1 1235 very strong 13.0 and 14.0 760 and 710 medium

13.2.6 Polybutadiene Rubber (see Fig. 29 and Fig. 30): 13.2.8 Chlorosulfonated Polyethylene (see Fig. 33 and Fig.
Wavelength, µm Wavenumber, cm−1 Intensity 34):
13.5 741 very strong Wavelength, µm Wavenumber, cm−1 Intensity
11.0 909 medium
10.4 962 medium 7.3 1370 strong
10.1 990 medium 7.9 1265 medium
8.6 1150 strong
Reported diagnostic absorptions and related spectra refer to 13.7 730 medium
polybutadiene rubber with high cis content. Relative intensities
In vulcanizates, the absorption, depending on the chlorosul-
of absorptions depend on the ratio of isomers in vulcanizates.
fonic groups, strongly decreases.
13.2.7 Ethylene-Propylene Rubber (see Fig. 31 and Fig.
32):

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FIG. 23 NBR Film from Raw Rubber

FIG. 24 NBR Film from a Vulcanizate

PART 2 SEMI-QUANTITATIVE ANALYSIS

14. Scope EPDM and IIR are present, the minimum detection limit is
approximately 12 % of either rubber. See 15.2 and Sections
14.1 These test methods describe the semiquantitative de-
23-25.10
tection of certain rubbers in blends.
14.1.1 Polyisoprene (IR and NR), BR and SBR are esti- NOTE 2—For use in these test methods, the term “saturated rubbers”
will be used to describe rubber containing no, or a small number of double
mated when di-blends or tri-blends are present. The percentage bonds, in the main rubber chain. For example, isobutylene rubber (IIR)
of a single component of the blend is accurate to approximately containing a small amount of an unsaturated material—isoprene. The term
65 % of the total rubber content. See 15.1 and Sections 16-22. “unsaturated rubbers” will be used to describe those rubbers containing
14.1.2 Saturated rubbers (IIR or EPDM) (see Note 3) are
detected in the presence of unsaturated rubbers (NR, IR, BR,
SBR and CR). Approximately 3 to 6 % of EPDM or IIR alone 10
Based upon “Detecting Traces of EPDM or IIR in Blends,” by Malcolm
can be found in blends of unsaturated rubbers. When both Anderson, Uniroyal Tire Co., Elastomerics, October 1978, p. 40.

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 D 3677 – 00

FIG. 25 CR Film from Raw Rubber

FIG. 26 CR Film from a Vulcanizate

FIG. 27 IIR Film from Raw Rubber

substantial numbers of double bonds in the main rubber chain, for example, IR, NR, SBR, BR and CR.

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FIG. 28 IIR Film from a Vulcanizate

FIG. 29 BR Film from Raw Rubber

FIG. 30 BR Film from a Vulcanizate

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FIG. 31 EPM Film from Raw Rubber

FIG. 32 EPM Film from a Vulcanizate

FIG. 33 CSM Film from Raw Rubber

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FIG. 34 CSM Film from a Vulcanizate

14.1.3 References to IIR include chlorinated (CIIR) and 16.1.1 Grinding Mill, capable of grinding vulcanized rubber
brominated (BIIR) versions of these rubbers. to 420 µm (40 mesh).11
16.1.2 Magnetic Stirring Hot Plate, with controlled stirring
15. Summary of Test Methods rates, capable of holding several 50-cm3 conical flasks.12
15.1 For estimation of NR, IR, BR, or SBR, or all of these, 16.1.3 Magnetic Stirring Bars, covered with a chemical-
in di-blends or tri-blends: resistant coating,13 approximately 25 mm long.
15.1.1 A milled, extracted test portion is ground to 420-µm 16.1.4 Büchner Funnel, for use with 5.5-cm filters.14
(40-mesh) size, digested in hot 1,2-dichlorobenzene, and fil- 16.1.5 Glass Fiber Filters, 5.5 cm in diameter.15
tered to remove the carbon black. An infrared spectrum is made 16.1.6 Vacuum Filtering Device. 16
on a film prepared from this solution. 16.1.7 Vacuum Oven. 17
15.1.2 Absorbance ratio measurements at 1450 cm−1 and 16.1.8 Conical Flasks, 50-cm3 and 250-cm3 capacity, of
other significant peaks found in the absorbance spectrum of the heat-resistant glass.18
rubbers listed in 14.1 are obtained next. 16.1.9 Pipet, Pasteur type, disposable19 (or equivalent).
15.1.3 When the ratio values in accordance with 15.1.2 are 16.1.10 Usual Laboratory Glassware, necessary for carry-
compared to those obtained from calibration data prepared ing out the test method as written.
from all possible blends which the analyst expects to encounter 17. Safety Precautions
of NR, IR, BR, and SBR rubbers listed in 14.1.2, the
composition of blends may be assessed. 17.1 Because of the toxicity of the solvents used in this test
15.2 For detection of EPDM or IIR in NR, IR, BR, SBR or method, a well-ventilated fume hood shall be used and the skin
CR: and eyes suitably protected during this analysis.
15.2.1 A milled vulcanizate is digested with a hot solution 17.2 Although not outlined in this test method, all recog-
of sulfuric and chromic acid and the residue is dissolved in nized health and safety precautions shall be observed when
boiling dichloromethane. An infrared spectrum of a film, cast following this test method.
on a salt plate from dichloromethane, provides a means of 18. Preparation of Test Portion
determining the presence or absence of saturated rubbers in
18.1 If the test portion is vulcanized, sheet it out on a cool
unsaturated rubbers.
mill and weigh approximately 2.2 g.
15.2.2 The acid mixture decomposes unsaturated rubbers
such as NR, IR, BR and SBR. Because EPDM and IIR are
highly saturated, they are virtually unattacked by the acid 11
A. H. Thomas Co., Philadelphia, PA 19105, Wiley Intermediate Model is
mixture. Furthermore, IIR and EPDM are only partially vul- satisfactory.
12
Cole-Parmer Instrument Co., Chicago, IL 60648, Model Magna-4 has been
canized in the presence of high levels of unsaturated rubbers found satisfactory.
and may therefore be soluble in chlorinated solvents. 13
Polytetrafluoroethylene has been found satisfactory.
15.2.3 Any saturated polymer or rubber resistant to the acid 14
Fisher Scientific Co., Pittsburgh, PA 15219, Catalog No. 10-356B has been
mixture, and also soluble in hot dichloromethane will appear in found satisfactory.
15
Reeve Angel Co., Clifton, NJ, No. 934AH has been found satisfactory.
the residue and consequently in the spectrum. Examples would 16
Fisher Scientific Co., Catalog No. 9-788, Fisher Filtrator, has been found
be low molecular mass polyethylene and polystyrene. satisfactory.
17
One supplied by National Appliance Co., Portland, OR, has been found
16. Apparatus satisfactory.
18
Borosilicate glass has been found satisfactory.
16.1 See Section 8 in addition to the following: 19
Fisher Scientific Co., Catalog No. 13-678-6A has been found satisfactory.

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 D 3677 – 00
18.2 If the test portion is unvulcanized, vulcanize it and 20.5 Prepare a filter bed by placing a glass fiber filter in a
sheet it out on a cool mill. Weigh approximately 2.2 g. Büchner funnel, wetting it with chloroform, then filling the
18.2.1 Test portions must be vulcanized; otherwise the funnel with diatomaceous filter aid (4.7), and saturating this
intensity of the unsaturation bands will be variable. with chloroform from a wash bottle.
18.3 Extract the vulcanized sheet overnight with alcohol 20.6 With the Büchner funnel in place on the vacuum
(4.3), using the apparatus in accordance with 8.1. filtering device (16.1.6) and a 250-cm3 beaker placed to receive
18.4 Extraction for 2 h with acetone or 2-butanone may also the filtrate, pour the hot solution from the flask into the funnel,
be effective. and at the same time turn on the vacuum.
18.4.1 The object of extraction is to remove, as much as 20.7 Wash the solution through the funnel with boiling
possible, all the additives in the compound. The choice of chloroform until the filtrate comes through colorless.
solvent is left to the discretion of the analyst, whose prior 20.7.1 Filtering requires some experience. If a black filtrate
knowledge of the vulcanizate composition will dictate the most comes through the filter (or anything darker than a golden-
suitable solvent for extraction. yellow) it will be necessary to refilter the solution, while hot,
through the filter until the filtrate is clear.
19. Calibration 20.7.2 Stirring the filter bed with a spatula during filtration
19.1 Prepare sets of standard, vulcanized compounds con- can improve the intimate contact between the filter aid and the
taining blends of the rubbers of interest over ranges of expected liquid.
ratios (for example, 80/20 NR/BR, 70/30, 60/40, 50/50) with 20.8 Evaporate the liquid in the beaker to near dryness on an
blends of two or three rubbers. electric hot plate, at the same temperature as in 20.4, using a
19.1.1 Prepare separate standard blends for emulsion SBR, stream of dry air.
solution SBR and high-styrene SBR, and for cis-BR and 20.9 Add a few drops of toluene to the dried residue of 20.8,
high-trans emulsion BR. and with a Pasteur pipet, (16.1.9) transfer a few drops of the
19.1.2 NR and IR give essentially the same values; there- solution to the sodium chloride or potassium bromide plate
fore, one set of standards with either IR or NR should be (8.7), that has been placed on a watch glass.
sufficient. 20.10 Place the prepared plate in a vacuum oven under
19.2 Carry out the preparation and procedure as outlined in strong vacuum with a slight intake of air at about 50°C for 1 h
Sections 18 and 20 for all blends. Use the same infrared to dry the film completely. Make the film even by smoothing it
instrument for sample measurement as for standard calibration with a rotating motion of the side of the Pasteur pipet. The
measurements. thickness of the film shall be such that when placed in the
19.3 On linear graph paper, plot the absorbance ratios for sample beam of the spectrophotometer and measured against
each peak in each blend against the known rubber content of air in the reference beam, an absorbance of 0.04 to 0.10 is
each rubber, in percent of total rubber. obtained at 4000 cm−1, and 0.35 to 0.45 absorbance at the peak
19.3.1 For BR blends at 735 cm−1, make separate calibra- around 1450 cm−1. This corresponds to about 80 to 90 % and
tion curves for high SBR and high NR content. 35 to 45 % transmittance respectively.
19.4 Use the following peak absorbance and that at 1450 20.11 Scan the spectrum of the prepared film (20.10) from
cm−1 to obtain the necessary ratios: approximately 4000 to 600 cm−1 with an instrument setting
For NR/BR: 1375, 965, 910, 835, and 735 cm−1 suitable for quantitative analysis,20 in the absorbance mode, if
For NR/SBR: 1375, 965, 910, 835, 735, and 699 cm−1 possible.
For NR/BR/SBR: 1375, 835, 735, and 699 cm−1
For BR/SBR: 910, 735, and 699 cm−1
20.11.1 The spectrophotometer shall be adjusted according
to the manufacturer’s directions for optimum performance.
19.5 Inaccurate results will be obtained if absorbance ratios Since instruments vary widely in settings and display, the
from di-blends are compared to ratios from tri-blends. optimum settings are left to the discretion of the analyst. Refer
to Practice E 168 for further recommendations on the use of
20. Procedure infrared spectrophotometers.
20.1 Dry the extracted test portion thoroughly and grind in 20.11.2 If only a transmittance mode is possible with the
the mill (16.1.1) to 420 µm. instrument being used, the spectrum shall be scanned in that
20.2 Divide the test portion into approximately equal por- mode.
tions and place in three 50-cm3 conical flasks. 20.12 Draw baselines with a straightedge, preferably to
20.3 Place a stirring bar in each of the flasks, fill it nearly approximately the following wavenumbers (all values are in
full with 1,2-dichlorobenzene, and cover with a watch glass. reciprocal centimetres):
20.4 Place the flasks on the stirring hot plate, set for a 1390–1510 for the 1450 peak
temperature a few degrees below boiling (approximately 1340–1390 for the 1375 peak
175°C), and stir vigorously for 2 to 8 h, until digestion is 930–990 for the 965 peak
790–870 for the 835 peak
complete. 650–790 for the 735 peak
20.4.1 It is imperative that digestion be complete so that all
of the rubber is in solution. Completeness of digestion is
evident when the flask is shaken, held up to a strong light, and 20
On the Perkin-Elmer, Model 283, suitable settings are: scan time 12 min,
the solution exhibits a deep purplish-brown color with no response 1, absorbance mode, program N(6), abscissa and ordinate expansion 1,
undigested particles floating on the surface. with suppression.

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 D 3677 – 00
21
660–710 for the 699 peak 23.2 Stainless Steel Sieve, 420 µm (40 mesh) or finer.
23.3 Electric Hot Plate.
20.12.1 Although other baselines can be used, experience
has shown that short baselines are preferred. In any case, the 24. Reagents
analyst must draw the baselines for the standards in the same 24.1 Chromic Acid Digestion Mixture—Dissolve 200 g of
manner as was done for the samples. chromic acid (CrO3) in 500 cm 3 of water, Cautiously add 150
20.13 On the spectrum, subtract the absorbance at a point on cm3 of H2SO4(density 1.84 Mg/m3), and mix well.
the baseline directly below each peak of interest, from the peak 24.2 Acetone, Reagent Grade.
absorbance, to give the corrected absorbance. 24.3 Dichloromethane, Reagent Grade, with a residue on
20.13.1 When the percent transmittance mode is used, evaporation not over 0.0002 %.
divide the percent transmittance at a point on the baseline 24.4 Wetting Agent— A saturated solution of dioctyl sodium
directly above the peak by the percent transmittance of the sulfosuccinate (aerosol OT) is satisfactory.
peak and take the log1 0 of the quotient.
20.14 Obtain absorbance ratios by dividing the corrected 25. Procedure
absorbance of each of the peaks at 1375, 965, 910, 835, 735, 25.1 Weigh about 1 g of milled vulcanizate and place in a
and 699 cm −1 as are of interest, by the corrected absorbance at 400-cm3 beaker, then add about 200 cm3 of acetone. (Uncured
1450 cm −1. compounds should be vulcanized by any appropriate method,
20.15 Take the mean for the three test portions as the before milling.)
absorbance ratio in each case. 25.2 Heat the beaker on a hot plate, so that it boils for about
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.
21.1 The absorbance peaks and their assignments are: 25.5 Pour the warm solution through the sieve (see 23.2),
cm−1
wash the residue copiously with hot water, then with a few
cubic centimetres of acetone.
1450 methylene —CH2— 25.6 If there is no rubber residue on the sieve at this point,
1375 methyl —CH3
965 trans C=C
then IIR or EPDM is absent, and the test should be discontin-
910 vinyl C=C ued.
835 propenyl —C=CH— 25.7 If there is residue on the sieve, collect it in a beaker,
?
CH3 dry off most of the acetone and add 30 cm3 of dichloromethane,
699 5 adjacent hydrogens of monosubstituted benzene ring cover the beaker with a watch glass and boil the dichlo-
(for example, phenyl) of styrene romethane on a hot plate at high heat until a volume of about
735 cis C=C
10 cm3 is reached.
22. Precision and Bias NOTE 3—If a large amount of solid particles are present, filter the
solution into a beaker through a loose filter such as a glass fiber pad or
22.1 Precision—No work has been done to test the preci- glass wool. However, this filtration may not be necessary.
sion of this test method, however, the results obtained by this
test method have been verified on an NR/SBR blend, using Test 25.8 Pour the solution into a 50-cm3 beaker and evaporate
Methods D 297, Section 52, for Polyisoprene Content, and to 1 to 2 cm3.
Section 56, for SBR Content, and the results have been found 25.9 Apply enough drops of the solution from 25.8 to a salt
to be consistent within6 5 %. plate window to make a good film. Evaporate the dichlo-
romethane with gentle heat (for example in a vacuum oven at
22.2 Bias—Under the best conditions, accuracy is 65 % of 50°C). If the residue was quite small, apply all of it to the salt
the rubber content for detection of EPDM or IIR in NR, IR, plate.
BR, SBR, or CR. For example, in a 70/30 NR/BR blend, the 25.10 With the salt plate in the sample beam of the infrared
outlined procedure would give 70 6 5 % NR and 30 6 5 % spectrophotometer and air in the reference beam, scan the
BR. spectrum from 4000 to 600 cm−1 or lower. If the spectrum is
weak expand it 5 or 10 times in the ordinate direction, if the
23. Apparatus instrument permits.
23.1 Usual laboratory glassware necessary for carrying out
the test method as written and in addition to apparatus in 8.7
and 8.8 are the following: 21
Those from W. S. Tyler Co., Mentor, OH 44060 are satisfactory.

20
 D 3677 – 00
25.11 Compare the spectrum obtained with Fig. 28 and Fig. 26.2 A task group composed of four laboratories, testing six
32 or preferably to one’s own spectra of purified IIR or EPDM. vulcanizates (both black and white stocks) obtained the fol-
NOTE 4—Purified rubbers may be prepared by pouring a hot toluene lowing results with this test method:
solution of the rubber into about four times as much methanol to coagulate
it, then dissolving it in dichloromethane and scanning in the same manner 27. Keywords
as for the unknowns.
27.1 acrylonitrile-butadiene rubber; balata; butyl rubber;
25.12 Note the following diagnostic bands and their con-
chloroprene; ethylene-propylene-diene rubber; ethylene-
figurations: 1390, 1370 and 1230 cm−1 for IIR and 1380 and
propylene rubber; gutta percha; infrared spectrometry; polyb-
721 cm −1 for EPDM. Since the 1380-cm−1 band might be
utadiene; polyisoprene; nitrile rubber; styrene-butadiene
caused by NR contamination, look for the accompanying NR
band at 836 −1 to verify this contamination. rubber

26. Precision and Bias

26.1 See 14.1.2.

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