ASTM D3530-20

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 mass percent of composite material prepregs. This standard focuses on composites with thermosetting resins, which 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 (572 °F).  
1.3 Use of this test method is limited to temperatures below which the matrix flows from the reinforcement.  
1.4 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 8.  
1.6 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.

General Information

• Status: Published
• Publication Date: 31-Aug-2020
• ICS: 59.100.30 - Aramide materials
• ICS: 71.040.40 - Chemical analysis
• Technical Committee: D30 - Composite Materials
• Drafting Committee: D30.03 - Constituent/Precursor Properties

Relations

• Refers: ASTM D883-24 - Standard Terminology Relating to Plastics
• Effective Date: 01-Feb-2024
• Refers: ASTM D883-23 - Standard Terminology Relating to Plastics
• Effective Date: 01-Nov-2023
• Refers: ASTM D883-20 - Standard Terminology Relating to Plastics
• Effective Date: 01-Jan-2020
• Refers: ASTM D3878-19a - Standard Terminology for Composite Materials
• Effective Date: 15-Oct-2019
• Refers: ASTM D883-19c - Standard Terminology Relating to Plastics
• Effective Date: 01-Aug-2019
• Refers: ASTM D3878-19 - Standard Terminology for Composite Materials
• Effective Date: 15-Apr-2019
• Refers: ASTM D883-19a - Standard Terminology Relating to Plastics
• Effective Date: 15-Apr-2019
• Refers: ASTM D883-19 - Standard Terminology Relating to Plastics
• Effective Date: 01-Feb-2019
• Refers: ASTM D883-18a - Standard Terminology Relating to Plastics
• Effective Date: 01-Dec-2018
• Refers: ASTM D883-18 - Standard Terminology Relating to Plastics
• Effective Date: 01-Nov-2018
• Refers: ASTM D3878-18 - Standard Terminology for Composite Materials
• Effective Date: 01-Apr-2018
• Refers: ASTM D883-17 - Standard Terminology Relating to Plastics
• Effective Date: 15-Aug-2017
• Refers: ASTM D3878-16 - Standard Terminology for Composite Materials
• Effective Date: 01-Aug-2016
• Refers: ASTM D3878-15 - Standard Terminology for Composite Materials
• Effective Date: 01-Jul-2015
• Refers: ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2014

Overview

ASTM D3530-20: Standard Test Method for Volatiles Content of Composite Material Prepreg specifies a widely recognized test method for determining the volatiles content in composite material prepregs. This standard focuses on composite materials with thermosetting resins and measures the percentage of volatiles lost when samples are exposed to elevated temperatures, particularly during the nominal cure or consolidation process. Understanding the volatiles content in prepregs is essential for optimizing manufacturing processes, ensuring product quality, and achieving consistent composite material properties.

Key Topics

• Purpose: The standard provides a reliable method to determine volatiles content (by mass percentage) in prepreg materials. Typical volatiles include moisture, solvents, and low molecular weight compounds that evaporate when heated.
• Scope: ASTM D3530-20 applies to composite prepregs with thermosetting resins and is limited to circulating air ovens with a maximum temperature of approximately 300 °C (572 °F). It should only be used at temperatures below the resin matrix’s flow point.
• Units: Results are reported in SI units, with values in parentheses provided for reference only.
• Safety: The standard highlights the need for safe handling practices, ventilation, and compliance with applicable regulations, especially where toxic or flammable volatiles may be present.
• Precision and Limitations: The measured volatiles can vary depending on oven airflow, sample geometry, placement, and exposure time. The method requires careful specimen preparation and standardized oven conditions for repeatable results.

Applications

ASTM D3530-20 is fundamental in the composites manufacturing industry, especially for companies developing or processing fiber-reinforced polymer-matrix composite materials. Understanding and controlling the volatiles content is crucial for:

• Process Optimization: Accurate measurement of volatiles helps manufacturers fine-tune curing schedules and storage conditions, reducing defects such as porosity or incomplete curing in the final product.
• Quality Assurance: Consistent volatiles content is key to ensuring batch-to-batch uniformity and meeting customer or regulatory requirements for prepreg materials.
• Research and Development: Material developers use this method to compare new resin formulations, optimize prepreg shelf life, and tailor prepreg performance characteristics.
• Industry Compliance: The test method supports compliance with international product quality standards for composite materials used in aerospace, automotive, marine, and industrial applications.

Related Standards

Several related ASTM and industry standards complement ASTM D3530-20:

• ASTM D883: Terminology Relating to Plastics - Provides definitions that support understanding of the terminology used within D3530-20.
• ASTM D3878: Terminology for Composite Materials - Reference for standardized composite material terms.
• ASTM E177: Practice for Use of the Terms Precision and Bias in ASTM Test Methods - Used for describing statistical parameters in test methods.
• ASTM E1309: Guide for Identification of Fiber-Reinforced Polymer-Matrix Composite Materials in Databases (Withdrawn 2015) - Formerly provided guidelines for material identification.
• NFPA 86: Standard for Ovens and Furnaces - Offers critical safety guidelines for operating ovens during volatile content determination.

Keywords: composite materials, prepreg, volatiles content, thermosetting resins, ASTM D3530-20, composites manufacturing, quality assurance, composites testing, international standards.

By utilizing ASTM D3530-20, manufacturers, laboratories, and quality control professionals can ensure precise assessment of volatiles content, supporting high-quality composite product outcomes and regulatory compliance.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D3530 − 20
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 E177Practice for Use of the Terms Precision and Bias in
ASTM Test Methods
1.1 This test method covers the determination of the vola-
tiles content, in mass percent of composite material prepregs. 2.2 NFPA Standard:
Thisstandardfocusesoncompositeswiththermosettingresins, NFPA 86Standard for Ovens and Furnaces
which tend to lose a few percent of the matrix mass when
heated due to loss of both retained water and low molecular
3. Terminology
weight matrix constituents that volatilize during heating.
3.1 Definitions—Terminology D3878 defines terms relating
1.2 Use of this test method is limited to maximum tempera-
to composite materials. Terminology D883 defines terms
ture of circulating air ovens, approximately 300°C (572°F). relating to plastics. Practice E177 defines terms relating to
statistics.Intheeventofaconflictbetweenterms,Terminology
1.3 Use of this test method is limited to temperatures below
D3878 shall have precedence over other documents.
which the matrix flows from the reinforcement.
3.1.1 prepreg, n—the admixture of fibrous reinforcement
1.4 Units—The values stated in SI units are to be regarded
andpolymericmatrixusedtofabricatecompositematerials;its
as standard. The values given in parentheses after SI units are
form may be sheet, tape, or tow.
providedforinformationonlyandarenotconsideredstandard.
3.1.1.1 Discussion—For thermosetting matrices, it has been
1.5 This standard does not purport to address all of the
partially cured to a controlled viscosity called “B stage.” See
safety concerns, if any, associated with its use. It is the
Terminology D3878.
responsibility of the user of this standard to establish appro-
3.2 Definitions of Terms Specific to This Standard:
priate safety, health, and environmental practices and deter-
3.2.1 volatiles, n—the solvent(s), water, low molecular
mine the applicability of regulatory limitations prior to use.
weight matrix components, and other constituents that volatil-
Specific precautionary statements are given in Section 8.
ize or evaporate during heating.
1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard-
3.2.2 volatiles content, n—theamountofvolatilespresentin
ization established in the Decision on Principles for the
a prepreg expressed as a mass percent.
Development of International Standards, Guides and Recom-
3.3 Symbols:
mendations issued by the World Trade Organization Technical
M—the final mass of the sample, after oven exposure.
f
Barriers to Trade (TBT) Committee.
M—the initial mass of the sample, before oven exposure.
i
V —the mass percent volatiles content.
2. Referenced Documents c
2.1 ASTM Standards:
4. Summary of Test Method
D883Terminology Relating to Plastics
4.1 Specimens of prepreg are cut and weighed gravimetri-
D3878Terminology for Composite Materials
cally (M). These specimens are then exposed to elevated
i
temperature for a specified time, equal to the nominal cure or
consolidation temperature of the material, in an air-circulating
This test method is under the jurisdiction of ASTM Committee D30 on
Composite Materials and is the direct responsibility of Subcommittee D30.03 on
oventoremovethevolatiles.Afteraspecifiedtimeintheoven,
Constituent/Precursor Properties.
the specimens are removed and reweighed (M). The percent
f
Current edition approved Sept. 1, 2020. Published November 2020. Originally
change in mass is expressed as volatiles content.
approved in 1976. Last previous edition approved in 2015 as D3530–97(2015).
DOI: 10.1520/D3530-20.
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 Available from National Fire Protection Association (NFPA), 1 Batterymarch
the ASTM website. Park, Quincy, MA 02269-9101.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3530 − 20
5. Significance and Use 7.8 Tong/tweezer or other proper tools for handling hot
items, or a combination thereof.
5.1 This test method is used to obtain the volatiles content
of composite material prepreg. Knowledge of the volatiles
7.9 Release agent.
content is useful in developing optimum manufacturing pro-
cesses.
8. Hazards
5.2 Thevolatilescontentisdeterminedafterexposuretothe
8.1 Some materials contain flammable or toxic solvents as
nominal cure or consolidation temperature.
partofthematrix.Thesematerialscouldbuilduptodangerous
concentrations of vapor in the oven. NFPA86 provides safety
6. Interferences
guidelines on amount of flammable materials that may be
safely placed in an oven and proper ventilation.
6.1 Airflow—The amount of measured volatiles may be
increased or decreased by changing the velocity of airflow.
9. Test Specimens
Since airflow in most ovens is not linear in each part, a
velometer should be used to measure airflow where samples
9.1 The minimum number of recommended test specimens
are placed. Samples should be placed only in positions of
is three.
known airflow so that results may be repeatable. Use of baffles
9.2 The specimen size shall be a minimum of 1600 mm
has been found to even airflow between samples.
(2.48in. ) by material thickness. Ribbon, braid, and fabric
6.2 Sample Exposure—Thegeometricshapeandpositioning
forms that do not drip resin shall be suspended from the rack.
of the sample have an effect on the measured volatiles content.
Ribbon shall be looped in close proximity so that in
...

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.
Designation: D3530 − 97 (Reapproved 2015) D3530 − 20
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.
1. Scope
1.1 This test method covers the determination of the volatiles content, in weightmass percent of composite material prepregs. This
standard focuses on composites with thermosetting resins thatresins, which 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).ovens,
approximately 300 °C (572 °F).
1.3 Use of this test method is limited to temperatures below which the matrix flows from the reinforcement.
1.4 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided
for information only and are not considered 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 8.
1.6 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.
2. Referenced Documents
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
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
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 Nov. 1, 2015Sept. 1, 2020. Published December 2015November 2020. Originally approved in 1976. Last previous edition approved in 20082015
ϵ2
as D3530/D3530M – 97D3530 – 97(2008)(2015). . DOI: 10.1520/D3530_D3530M-97R15.10.1520/D3530-20.
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.
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 − 20
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. Itsmaterials;
its form may be sheet, tape, or tow. See Terminology D3878.
3.1.1.1 Discussion—
For thermosetting matrices, it has been partially cured to a controlled viscosity called “B stage.” See Terminology D3878.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 volatiles, n—the solvent(s), water, low molecular weight matrix components, and other constituents that volatilize or
evaporate during heating.
3.2.2 Volatiles Content,volatiles content, n—the amount of volatiles present in a prepreg expressed as a weightmass 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
3.3 Symbols:
M —the final mass of the sample, after oven exposure.
f
M —the initial mass of the sample, before oven exposure.
i
V —the mass percent volatiles content.
c
4. Summary of Test Method
4.1 Specimens of prepreg are weighed and cut and weighed gravimetrically (M ). These specimens are then exposed to elevated
i
temperature, temperature for a specified time, equal to the nominal cure or consolidation temperature of the material, in an air
circulating air-circulating oven to remove the volatiles. The exposed samples are reweighed andAfter a specified time in the oven,
the specimens are removed and reweighed (M the). The percent change in weight mass is expressed as volatiles content.
f
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 (6 in.) diameter hoop may give slightly different results than the same ribbon wound in a 50 mm50 mm (2 in.)
diameter hoop. A thinner sample will be exposed to more airflow at its surface than a thicker sample.
6.3 Time of Exposure—Exposure in Oven—For any given temperature, sample placement, and airflow, the sample will lose
D3530 − 20
volatiles at a set initial rate,rate that decreases over time. After some timea certain period, volatiles lost in the test will approach
the true volatiles content of the sample. If the time period is not sufficient to show athe true volatiles content of the material, the
volatiles content is representative of o
...