ASTM D3530-97(2015)

Standard Test Method for Volatiles Content of Composite Material Prepreg

SIGNIFICANCE AND USE
5.1 This test method is used to obtain the volatiles content of composite material prepreg. Knowledge of the volatiles content is useful in developing optimum manufacturing processes.  
5.2 The volatiles content is determined after exposure to the nominal cure or consolidation temperature.
SCOPE
1.1 This test method covers the determination of the volatiles content, in weight percent of composite material prepregs. This standard focuses on composites with thermosetting resins that tend to lose a few percent of the matrix mass when heated due to loss of both retained water and low molecular weight matrix constituents that volatilize during heating.  
1.2 Use of this test method is limited to maximum temperature of circulating air ovens (approximately 300°C).  
1.3 Use of this test method is limited to temperatures below which the matrix flows from the reinforcement.  
1.4 The values stated in SI units are to be regarded as standard.  
1.5 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 appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 8.

General Information

• Status: Historical
• Publication Date: 31-Oct-2015
• ICS: 59.100.30 - Aramide materials
• ICS: 71.040.40 - Chemical analysis
• Technical Committee: D30 - Composite Materials
• Drafting Committee: D30.03 - Constituent/Precursor Properties

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D3530 − 97 (Reapproved 2015)
Standard Test Method for
Volatiles Content of Composite Material Prepreg
This standard is issued under the fixed designation D3530; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope 2.2 NFPA Standard:
NFPA 86Standard for Ovens and Furnaces
1.1 This test method covers the determination of the vola-
tilescontent,inweightpercentofcompositematerialprepregs.
3. Terminology
This standard focuses on composites with thermosetting resins
3.1 Definitions—Terminology D3878 defines terms relating
that tend to lose a few percent of the matrix mass when heated
to composite materials. Terminology D883 defines terms
due to loss of both retained water and low molecular weight
relating to plastics. Practice E177 defines terms relating to
matrix constituents that volatilize during heating.
statistics.Intheeventofaconflictbetweenterms,Terminology
1.2 Use of this test method is limited to maximum tempera-
D3878 shall have precedence over other documents.
ture of circulating air ovens (approximately 300°C). 3.1.1 prepreg, n—the admixture of fibrous reinforcement
andpolymericmatrixusedtofabricatecompositematerials.Its
1.3 Use of this test method is limited to temperatures below
form may be sheet, tape, or tow. See Terminology D3878.
which the matrix flows from the reinforcement.
3.2 Definitions of Terms Specific to This Standard:
1.4 The values stated in SI units are to be regarded as
3.2.1 Volatiles Content, n—the amount of volatiles present
standard.
in a prepreg expressed as a weight percent.
1.5 This standard does not purport to address all of the
3.3 Symbols:
safety concerns, if any, associated with its use. It is the
3.3.1 M—the initial mass of the sample.
i
responsibility of the user of this standard to establish appro-
3.3.2 M—the mass of the sample after oven exposure.
f
priate safety and health practices and determine the applica-
3.3.3 V —the weight percent volatiles content.
bility of regulatory limitations prior to use. Specific precau- c
tionary statements are given in Section 8.
4. Summary of Test Method
4.1 Specimens of prepreg are weighed and then exposed to
2. Referenced Documents
elevated temperature, equal to the nominal cure or consolida-
2.1 ASTM Standards:
tion temperature of the material, in an air circulating oven to
D3878Terminology for Composite Materials
remove the volatiles. The exposed samples are reweighed and
E177Practice for Use of the Terms Precision and Bias in
the percent change in weight expressed as volatiles content.
ASTM Test Methods
E1309 Guide for Identification of Fiber-Reinforced 5. Significance and Use
Polymer-Matrix Composite Materials in Databases(With-
5.1 This test method is used to obtain the volatiles content
drawn 2015)
of composite material prepreg. Knowledge of the volatiles
content is useful in developing optimum manufacturing pro-
cesses.
This test method is under the jurisdiction of ASTM Committee D30 on
5.2 Thevolatilescontentisdeterminedafterexposuretothe
Composite Materials and is the direct responsibility of Subcommittee D30.03 on
nominal cure or consolidation temperature.
Constituent/Precursor Properties.
Current edition approved Nov. 1, 2015. Published December 2015. Originally
6. Interferences
approved in 1976. Last previous edition approved in 2008 as D3530/
ϵ2
D3530M–97(2008) . DOI: 10.1520/D3530_D3530M-97R15.
6.1 Airflow—The amount of measured volatiles may be
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
increased or decreased by changing the velocity of airflow.
contactASTM Customer Service at [e-mail]. ForAnnual Book ofASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3 4
The last approved version of this historical standard is referenced on Available from National Fire Protection Association (NFPA), 1 Batterymarch
www.astm.org. Park, Quincy, MA 02269-9101.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3530 − 97 (2015)
Since airflow in most ovens is not linear in each part, a drip resin shall be suspended from the rack. Ribbon shall be
velometer should be used to measure airflow where samples looped in close proximity so that individual strands are not
are placed. Samples should be placed only in positions of clumped together. Other forms may be placed horizontally on
known airflow so that results may be repeatable. Use of baffles the rack.
has been found to even airflow between samples.
10. Calibration and Standardization
6.2 Sample Exposure—Thegeometricshapeandpositioning
10.1 All measuring equipment shall have certified calibra-
of the sample have an effect on the measured volatiles content.
tions that are current at the time of use of the equipment. The
Samples placed horizontally in a rack will not be exposed to
calibration documentation shall be available for inspection.
the same amount of airflow as samples hung vertically. A
ribbon wound in a 150 mm diameter hoop may give slightly
11. Conditioning
different results than the same ribbon wound in a 50 mm
diameter hoop. A thinner sample will be exposed to more
11.1 Store carbon fiber-epoxy prepreg at low temperatures
airflow at its surface than a thicker sample.
as recommended by the manufacturer (typically approxi-
mately−18°C).Allow sealed packages of material to warm as
6.3 Time of Exposure—For any given temperature, sample
recommended by manufacturer or controlling specification
placement, and airflow, the sam
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´2
Designation: D3530 − 97 (Reapproved 2008) D3530 − 97 (Reapproved 2015)
Standard Test Method for
Volatiles Content of Composite Material Prepreg
This standard is issued under the fixed designation D3530; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
ε NOTE—This standard was corrected to a single-designation standard editorially in October 2013.
ε NOTE—The designation of this standard was corrected editorially in November 2013.
1. Scope
1.1 This test method covers the determination of the volatiles content, in weight percent of composite material prepregs. This
standard focuses on composites with thermosetting resins that tend to lose a few percent of the matrix mass when heated due to
loss of both retained water and low molecular weight matrix constituents that volatilize during heating.
1.2 Use of this test method is limited to maximum temperature of circulating air ovens (approximately 300°C).
1.3 Use of this test method is limited to temperatures below which the matrix flows from the reinforcement.
1.4 The values stated in SI units are to be regarded as standard.
1.5 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 appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use. Specific precautionary statements are given in Section 8.
2. Referenced Documents
2.1 ASTM Standards:
D3878 Terminology for Composite Materials
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E1309 Guide for Identification of Fiber-Reinforced Polymer-Matrix Composite Materials in Databases (Withdrawn 2015)
2.2 NFPA Standard:
NFPA 86 Standard for Ovens and Furnaces
3. Terminology
3.1 Definitions—Terminology D3878 defines terms relating to composite materials. Terminology D883 defines terms relating
to plastics. Practice E177 defines terms relating to statistics. In the event of a conflict between terms, Terminology D3878 shall
have precedence over other documents.
3.1.1 prepreg, n—the admixture of fibrous reinforcement and polymeric matrix used to fabricate composite materials. Its form
may be sheet, tape, or tow. See Terminology D3878.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 Volatiles Content, n—the amount of volatiles present in a prepreg expressed as a weight percent.
3.3 Symbols:
3.3.1 M —the initial mass of the sample.
i
3.3.2 M —the mass of the sample after oven exposure.
f
3.3.3 V —the weight percent volatiles content.
c
This test method is under the jurisdiction of ASTM Committee D30 on Composite Materials and is the direct responsibility of Subcommittee D30.03 on
Constituent/Precursor Properties.
Current edition approved March 1, 2008Nov. 1, 2015. Published April 2008December 2015. Originally approved in 1976. Last previous edition approved in 20032008
ϵ2
as D3530/D3530M – 97(2003).(2008) . DOI: 10.1520/D3530_D3530M-97R08E02.10.1520/D3530_D3530M-97R15.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Available from National Fire Protection Association (NFPA), 1 Batterymarch Park, Quincy, MA 02269-9101.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3530 − 97 (2015)
4. Summary of Test Method
4.1 Specimens of prepreg are weighed and then exposed to elevated temperature, equal to the nominal cure or consolidation
temperature of the material, in an air circulating oven to remove the volatiles. The exposed samples are reweighed and the percent
change in weight expressed as volatiles content.
5. Significance and Use
5.1 This test method is used to obtain the volatiles content of composite material prepreg. Knowledge of the volatiles content
is useful in developing optimum manufacturing processes.
5.2 The volatiles content is determined after exposure to the nominal cure or consolidation temperature.
6. Interferences
6.1 Airflow—The amount of measured volatiles may be increased or decreased by changing the velocity of airflow. Since airflow
in most ovens is not linear in each part, a velometer should be used to measure airflow where samples are placed. Samples should
be placed only in positions of known airflow so that results may be repeatable. Use of baffles has been found to even airflow
between samples.
6.2 Sample Exposure—The geometric shape and positioning of the sample have an effect on the measured volatiles content.
Samples placed horizontally in a rack will not be exposed to the same amount of airflow as samples hung vertically. A ribbon
wound in a 150 mm diameter hoop may give slightly different results than the same ribbon wound in a 50 mm diameter hoop. A
thinner sample will be exposed to more airflow at its surface than a thicker sample.
6.3 Time of Exposure—For any given temperature, sample placement, and airflow, the sample will lose volatiles at a set initial
rate, that decreases over time. After some time period, volatiles lost in the test will approach the true volatiles content of the sample.
If the time period is not sufficient to show a true volatiles content of the material, the volatiles content is representative of only
the condition of the test.
6.4 Time of Ambient Exposure—Volatiles content varies due to prolonged exposure of temperatures exc
...