ASTM D6047 - 17 (2025) 乙烯-丙烯-二烯共聚三聚物 (EPDM) 中5-ENB或双环戊二烯 (DCPD) 生橡胶测定的标准试验方法

VIP免费

那山那人那狗 2026-07-27 12 380.96KB 8 页 20星币

Designation: D6047 −17 (Reapproved 2025)
Standard Test Methods for
Rubber, Raw—Determination of 5-Ethylidenenorbornene
(ENB) or Dicyclopentadiene (DCPD) in Ethylene-Propylene-
Diene (EPDM) Terpolymers
1
This standard is issued under the ﬁxed designation D6047; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 These test methods cover the determination of the
content of 5-ethylidenenorbornene (ENB) or Dicyclopentadi-
ene (DCPD) in ethylene-propylene-diene (EPDM) terpoly-
mers. They are applicable to diene contents in the 0.1 to 10
mass % range.
1.2 ENB and DCPD are dienes introduced in ethylene/
propylene rubbers to generate speciﬁc cure properties. Since
high precision for diene content determination has become
very important, a Fourier Transform Infrared Spectroscopic
(FTIR) method was developed. Diene determination was
performed in the past by a refractive index technique.
NOTE 1—The procedures for % ENB and % DCPD differ only in the
location in the infrared (IR) of the IR peak being quantiﬁed.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
standard.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
2
D297 Test Methods for Rubber Products—Chemical Analy-
sis
D1416 Test Methods for Rubber from Synthetic Sources—
Chemical Analysis (Withdrawn 1996)
3
D3568 Test Methods for Rubber—Evaluation of EPDM
(Ethylene Propylene Diene Terpolymers) Including Mix-
tures With Oil
D3900 Test Methods for Rubber—Determination of Ethyl-
ene Units in Ethylene-Propylene Copolymers (EPM) and
in Ethylene-Propylene-Diene Terpolymers (EPDM) by
Infrared Spectrometry
D4483 Practice for Evaluating Precision for Test Method
Standards in the Rubber and Carbon Black Manufacturing
Industries
E168 Practices for General Techniques of Infrared Quanti-
tative Analysis
E932 Practice for Describing and Measuring Performance of
Dispersive Infrared Spectrometers
E1421 Practice for Describing and Measuring Performance
of Fourier Transform Mid-Infrared (FT-MIR) Spectrom-
eters: Level Zero and Level One Tests
2.2 ANCHA Document:
4
Speciﬁcation for Evaluation of Research Quality Analysis
of Infrared Spectra
3. Summary of Test Methods
3.1 The test specimen is molded between two PTFE-coated
aluminum or Mylar sheets. The ENB content is determined
from its infrared absorbance at 1681–1690 cm
−1
, a measure of
ENB’s exocyclic double bond. The DCPD content is deter-
mined from its infrared absorbance at 1605–1610 cm
−1
, a
measure of DCPD’s monocyclic double bond.
3.2 The second derivative of the absorbance is calculated
and ratioed to an internal thickness gage. For ENB the resulting
second derivative peak near 1690 cm
−1
is related to ENB mass
fraction by calibrating the instrument with known EPDM
1
These test methods are under the jurisdiction of Committee D11 on Rubber and
Rubber-like Materials and are the direct responsibility of Subcommittee D11.11 on
Chemical Analysis.
Current edition approved Nov. 1, 2025. Published December 2025. Originally
approved in 1996. Last previous edition approved in 2021 as D6047 – 17 (2021).
DOI: 10.1520/D6047-17R25.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at www.astm.org/contact. For Annual Book of
ASTM Standards volume information, refer to the standard’s Document Summary
page on the ASTM website.
3
The last approved version of this historical standard is referenced on
www.astm.org.
4
“Speciﬁcation for Evaluation of Research Quality Analysis of Infrared
Spectra,” Analytical Chemistry, ANCHA, Vol 47, No. 11, p. 94a.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
1

standards. For DCPD, the resulting second derivative peak near
1610 cm
−1
is related to DCPD mass fraction by calibrating the
instrument with known EPDM standards.
3.3 Two main steps are performed in this procedure: auto-
matic determination of ﬁlm thickness and quantiﬁcation of
diene.
3.4 For oil-extended polymers, the oil must be extracted
before diene is determined. Test Methods D1416, Sections 67
through 74 and Test Methods D297 can be used for this
purpose.
4. Apparatus
4.1 Press, Carver-type, capable of pressing ﬁlms at 150°C
and 10 MPa or higher.
4.1.1 Primary Mold—A stainless steel (SS) mold, approxi-
mately 400 µm thick, with an opening sized appropriately for
the specimen ﬁlm holder described in 4.4 (typically 2 by 2 cm).
The mold should have approximately the same dimensions as
the press platens.
4.1.2 Alternate Mold—A thinner mold may be used;
however, precision may be adversely affected at low diene
levels. Test precision should be determined when thinner ﬁlms
are utilized. Example: a 127-µm (0.005-in) SS shim with a 15-
by 35-mm opening may be used for the simultaneous determi-
nation of ethylene (Test Methods D3900) and diene.
4.1.3 Alternative Mold for Low Molecular Weight (Liquid)
EPDM Terpolymers—For liquid EPDM a ring washer 22 mm
OD by 16 mm ID (7/8 in OD by 5/8 inch in ID) 400 µm thick
is used as a apacer between salt plates (NaBr, NaCl) to set a
ﬁxed path length. The spacer is sized to cover only the outer
edge of the salt plate.
4.2 Sheets for Molding, either PTFE-coated aluminum
sheets or Mylar, Type A, 36 µm thick or less.
4.3 Specimen Film Holders—Films may be molded, cut, and
transferred to a ﬁlm holder. Magnetic ﬁlm holders are ideal.
Alternatively, a mold sized to ﬁt in the spectrometer specimen
compartment, with an appropriate size opening may be used to
support the ﬁlm without removal after pressing.
4.4 Infrared Fourier Transform Spectrophotometer—An in-
strument capable of measuring absorbances in the range 400 to
6000 cm
−1
with a transmittance speciﬁcation (accuracy) of 6
1 % Tor better. The instrument should be capable of spectral
resolution of 2 cm
−1
(see “Speciﬁcation for Evaluation of
Research Quality Analysis of Infrared Spectra”). A deuterated
triglycine sulfate (DTGS) detector should be used. The instru-
ment must be operating in accordance with Practices E168.
Practices E932 and E1421 are other important references.
4.4.1 The instrument should be capable of spectral
accumulation, averaging, and subtracting capabilities. Water is
the primary source of interference in this method. Methods,
physical and electronic, that minimize moisture level and
variation are required to obtain the highest precision. The
preferred method is use of an instrument equipped with a dry
gas purge and a specimen shuttle, which permits alternating
and repetitive collection of single beam specimen and back-
ground spectra (see Section 6). Alternatively, should a speci-
men shuttle be unavailable, careful purging of the sample
compartment with dry nitrogen can yield satisfactory results.
High precision of calibration standard data is indicative of
adequate purging. When moisture interference is not removed
by purging, spectral subtraction of water vapor may be used. A
procedure for further method development is described in
Appendix X1.
5. Test Specimen Preparation
5.1 Primary Method—Place an appropriate amount of the
test specimen to ﬁll the mold opening (typically 0.2 to 0.5 g)
between two PTFE-coated aluminum or Mylar sheets in the
mold. Place the mold between the press platens heated to 125
65°C and apply approximately 10 MPa or higher pressure for
60 610 s.
NOTE 2—High molecular weight polymers may require higher tempera-
tures and pressures to obtain a good test specimen.
5.1.1 Cool the specimen to ambient temperature. Cut, if
necessary, a piece of ﬁlm to the appropriate size to cover the
specimen holder window. Detach the specimen ﬁlm from the
aluminum or Mylar and position it on the spectrophotometer
sample holder window.
5.2 Alternate Method—When using the thinner mold de-
scribed in 4.1.2, place a small piece (0.04–0.06 g) of test
specimen in the mold opening between two Mylar sheets and
press as in 5.1. Remove the mold from the press, turn it over
and press it again, then remove the mold from the press and
cool it to ambient temperature. When cool, carefully remove
the Mylar sheets, allowing the specimen ﬁlm to remain
attached to the mold.
5.3 Alternate Method for Liquid Sample Film Preparation—
Place a washer (described in 4.1.3) on top of a salt plate. Place
a small amount (about 0.3 g) of liquid EPDM polymer in the
center of the washer ﬁlling the hole completely. Place a second
salt plate on top of the ﬁlled washer. Gently place a 1 kg weight
on top of the salt plate/washer assembly and allow the
weighted assembly to sit for 2 to 3 min. (For viscous samples
it may be necessary to warm the sample prior to pressing.)
Remove the weight and allow to cool, if necessary. Wipe off
any excess material that may have been pressed out of the
assembly. Hold the assembly up to the light and inspect for
bubbles or voids, or both. Should there be imperfections, repeat
the sample preparation with a larger amount of sample.
6. Spectral Acquisition
6.1 With a specimen shuttle:
6.1.1 Data acquisition parameters:
6.1.1.1 Resolution: 2 cm
−1
.
6.1.1.2 Scans/Scan time: Total scan time required, split
between specimen and background, is about 90 s.
6.1.2 Place the test specimen in the specimen compartment,
allow purge to reestablish, and in alternating fashion, collect
single beam specimen (P) and “empty specimen compartment”
(P
0
) spectra. Eight passes of the shuttle should be sufficient
(eight specimen and eight empty compartment collections),
collecting four scans at each position.
D6047 − 17 (2025)
2

6.1.3 Calculate the specimen absorbance spectrum as minus
the log
10
of the ratio of the accumulated single beam specimen
spectrum to the single beam empty specimen compartment
spectrum:
A5 2log
10
~
P/P
0
!
(1)
6.2 Without a specimen shuttle:
6.2.1 Data acquisition parameters:
6.2.1.1 Resolution: 2 cm
−1
.
6.2.1.2 Scans/Scan Time: Background scan: 32 scans, 20 s
total; specimen scan: 32 scans, 20 s total.
6.2.2 Establish dry atmosphere inside empty specimen com-
partment and collect “empty specimen compartment” (P
0
)
spectra.
6.2.3 Place test specimen in the specimen compartment and
re-establish a dry atmosphere inside the specimen compart-
ment. Collect single beam specimen spectra (P) and calculate
the specimen absorption spectra (A) as described in 6.1.3.
7. Calibration of the Spectrophotometer
7.1 Obtain a series of known standards covering the 0–10
mass % diene range. Calibration may be based on secondary
standards qualiﬁed by other laboratories using this method or,
more generally, by primary standards whose diene content is
well known. Primary standards may be established via use of
1
H Nuclear Magnetic Resonance (NMR), in conjunction with
other techniques. The calibration standards employed in the
development of this method were determined by a combination
of refractive index and
1
H NMR (utilizing samples dissolved in
deuterated o-dichlorobenzene at 120°C; the ENB assignment
was based exclusively on the exocyclic oleﬁnic protons of
ENB). The use of four standards at the 0 (copolymer), 2, 5, and
10 mass % levels are the minimum recommended.
5
7.2 Using the procedures in Section 6, acquire a minimum
of ﬁve absorbance spectra for each of the calibration standards
described in 7.1. Several repetitions on separate specimens of
each standard may be averaged to improve the accuracy of the
calibration.
7.3 Using the procedures in Section 8, calculate the ratio of
the second derivative diene peak height to the internal thick-
ness gage for each of the spectra acquired.
7.4 Calculate a linear calibration line (diene peak ratio
versus assigned values of the standards in mass % diene) by
computing a slope and intercept using standard least squares
linear regression techniques.
8. Diene Determination
8.1 Prepare the specimen ﬁlm as described in Section 5.
8.2 Collect a single absorbance spectrum based on the
procedure in Section 6.
8.3 Determination of Film Thickness:
8.3.1 Correct the offset of the spectrum by bringing the
lowest point of the spectrum to zero (that is, determine the
minimum absorbance in the spectrum and offset the spectrum
to bring the absorbance to zero).
8.3.2 To determine the ﬁlm thickness automatically, calcu-
late the difference of the absorbance at the basepoint near 2703
cm
−1
minus the absorbance at the basepoint near 2750 cm
−1
. If
the net difference is positive, the sample belongs to Group 1.
Otherwise, it belongs to Group 2 (see Fig. 1).
8.3.2.1 Group 1: Thickness gage is the net absorbance
difference between 2708 cm
−1
(isooptic point) and 2450 cm
−1
(anchor point) (see Fig. 2).
8.3.2.2 Group 2: Thickness gage is the net absorbance
difference between 2668 cm
−1
(isooptic point) and 2450 cm
−1
(anchor point) (see Fig. 3).
8.4 Diene Quantitation:
8.4.1 Normalize the total spectrum to one optical density
(OD) by multiplying the total spectrum by 1/A, where Ais the
net absorbance at thickness gage.
8.4.2 ENB Calculation—Calculate the peak height (in OD)
of the second derivative (the second derivative algorithm
should use at least nine point smoothing) between 1681 and
1690 cm
−1
by applying the following formula:
Peak Ht 5A
1681
2
~
0.75 A
1688
10.25 A
1689
!
(2)
This will be called the ENB peak height throughout this
procedure. Fig. 4 gives a visual impression of a typical second
derivative spectrum of EPDM.
8.4.3 Use the calibration developed in Section 8.4.2 to
compute a mass % ENB for the sample, employing the
principle that only interpolation (and not extrapolation) is used.
If the ENB peak height determined in 8.4.5 is lower than the
ENB peak height of the lowest, or higher than the ENB peak
height of the highest calibration standard, then the ENB mass
% should be reported as “out of range for the calibration
employed.”
8.4.4 DCPD Calculation—Calculate the peak height (in
OD) of the second derivative (the second derivative algorithm
should use nine point smoothing) between 1601 and 1620 cm
−1
by applying the following formula:
Peak Ht 5
~
A
1601
2A
1610
!
(3)
This will be called the DCPD peak height throughout this
procedure.
8.4.5 Use the calibration developed in Section 8.4.4 to
compute a mass % DCPD for the sample, employing the
principle that only interpolation (and not extrapolation) is used.
If the DCPD peak height determined in 8.4.5 is lower than the
DCPD peak height of the lowest, or higher than the DCPD
peak height of the highest calibration standard, then the DCPD
mass % should be reported as “out of range for the calibration
employed.”
9. Report
9.1 Report the following information:
9.1.1 ENB or DCP content to the nearest tenth.
ENB 5xx.x mass %
5
The sole source of supply for the ENB standards known to the committee at this
time is ExxonMobil Chemical Polymer Laboratories, P.O. Box 5200, Baytown, TX
77520. The sole source of supply for the DCPD standards known to the committee
at this time is UniRoyal Chemical Company, Chemical Characterization Lab,
Benson Road, Middlebury, CT 06749. If you are aware of alternative suppliers,
please provide this information to ASTM Headquarters. Your comments will receive
careful consideration at a meeting of the responsible technical committee,
1
which
you may attend.
D6047 − 17 (2025)
3

文档加载中……请稍候！
如果长时间未打开，您也可以点击刷新试试。

下载文档到电脑，查找使用更方便

亲，本站95%以上的标准规范都面向会员免费，办理VIP会员下载更省钱，平均每篇不到2元

立即下载 VIP免费下载

标签： #标准试验 #试验方法 #标准试验方法

摘要：

本页面提供ASTM D6047 - 17 (2025)标准试验方法的详细解读，该标准专门用于测定乙烯-丙烯-二烯共聚三聚物（EPDM）生橡胶中5-亚乙基-2-降冰片烯（5-ENB）或双环戊二烯（DCPD）的含量。通过红外光谱或化学滴定等指定技术，该方法确保对EPDM第三单体的精确量化，适用于橡胶原料质量控制、配方开发及产品一致性验证。内容涵盖测试原理、操作步骤、计算公式及数据解读要点，旨在帮助橡胶行业从业者准确掌握EPDM中二烯烃含量的测定规范，提升材料性能评估的可靠性。

展开>> 收起<<

ASTM D6047 - 17 (2025) 乙烯-丙烯-二烯共聚三聚物 (EPDM) 中5-ENB或双环戊二烯 (DCPD) 生橡胶测定的标准试验方法.pdf

共8页,预览3页

还剩页未读，继续阅读

声明：本文档系会员上传，若文档所含内容侵犯了您的版权或隐私，请立即通知，我们立即给予侵权申诉删除！

ASTM D6047 - 17 (2025) 乙烯-丙烯-二烯共聚三聚物 (EPDM) 中5-ENB或双环戊二烯 (DCPD) 生橡胶测定的标准试验方法

相关推荐

开通VIP享超值会员特权

相关内容

热门标签

举报选择: