ASTM D3222-05(2015)
(Specification)Standard Specification for Unmodified Poly(Vinylidene Fluoride) (PVDF) Molding Extrusion and Coating Materials
Standard Specification for Unmodified Poly(Vinylidene Fluoride) (PVDF) Molding Extrusion and Coating Materials
ABSTRACT
This specification covers melt processable unmodified poly(vinylidene fluoride) (PVDF) molding, extrusion and coating materials. This specification covers only virgin homopolymer prepared from vinylidene fluoride supplied in form of pellet or powder and shall be free of foreign matter. Two types covered by this specification are type I PVDF fluoroplastics and type II PVDF fluoroplastics. Detailed requirements that shall conform to this specification include peak melting endotherm, specific gravity, refractive index, limiting oxygen index, flow rate, rheological properties, tensile properties, flexural properties, impact resistance, D-C resistance, dielectric strength, dielectric constant, and dissipation factor. Preparation of compression molded specimen shall be in accordance to this specification.
SCOPE
1.1 This specification covers melt processable molding and extrusion materials, as well as coating materials of poly(vinylidene fluoride) fluoroplastic, commonly abbreviated PVDF (or PVF2 in scientific literature). This specification covers thermoplastic resin materials supplied in pellet or powder form.
1.2 This specification applies only to the virgin homopolymer prepared from vinylidene fluoride, not copolymers, reinforced, filled grades or special grades with additives or treatments for modification of attributes.
1.3 The tests involved are intended to provide information for specification of unmodified PVDF homopolymer resins. It is not the purpose of this specification to provide engineering data for design purposes.
1.4 PVDF fluoroplastics melt between 156 and 180°C (312 and 356°F) and are thermally stable up to about 370°C (698°F). (Warning—Evolution of corrosive and toxic hydrogen fluoride can occur under certain conditions.)
1.5 The values stated in SI units, as detailed in IEEE/ASTM S-10, are to be regarded as the standard. The values given in parentheses are for information only.
Note 1: PVDF exhibits polymorphism.2 The type and extent of crystalline structure varies with the thermomechanical history of the sample. Specimens prepared by techniques different than prescribed in this specification can have properties that vary from the values specified.
1.6 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 10.
Note 2: There is no equivalent ISO standard for this specification. Information in this specification is technically equivalent to related information in ISO 12086-1 and ISO 12086-2.
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Designation:D3222 −05 (Reapproved 2015)
Standard Specification for
Unmodified Poly(Vinylidene Fluoride) (PVDF) Molding
Extrusion and Coating Materials
This standard is issued under the fixed designation D3222; 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.
NOTE 2—There is no equivalent ISO standard for this specification.
1. Scope
Information in this specification is technically equivalent to related
1.1 This specification covers melt processable molding and
information in ISO 12086-1 and ISO 12086-2.
extrusion materials, as well as coating materials of poly(vi-
2. Referenced Documents
nylidene fluoride) fluoroplastic, commonly abbreviated PVDF
(or PVF in scientific literature). This specification covers
2.1 ASTM Standards:
thermoplastic resin materials supplied in pellet or powder
D149Test Method for Dielectric Breakdown Voltage and
form.
DielectricStrengthofSolidElectricalInsulatingMaterials
at Commercial Power Frequencies
1.2 This specification applies only to the virgin homopoly-
D150Test Methods forAC Loss Characteristics and Permit-
mer prepared from vinylidene fluoride, not copolymers,
tivity (Dielectric Constant) of Solid Electrical Insulation
reinforced, filled grades or special grades with additives or
D256Test Methods for Determining the Izod Pendulum
treatments for modification of attributes.
Impact Resistance of Plastics
1.3 The tests involved are intended to provide information
D257Test Methods for DC Resistance or Conductance of
for specification of unmodified PVDF homopolymer resins. It
Insulating Materials
is not the purpose of this specification to provide engineering
D542Test Method for Index of Refraction of Transparent
data for design purposes.
Organic Plastics
1.4 PVDF fluoroplastics melt between 156 and 180°C (312
D618Practice for Conditioning Plastics for Testing
and356°F)andarethermallystableuptoabout370°C(698°F).
D638Test Method for Tensile Properties of Plastics
(Warning—Evolution of corrosive and toxic hydrogen fluo-
D790Test Methods for Flexural Properties of Unreinforced
ride can occur under certain conditions.)
and Reinforced Plastics and Electrical Insulating Materi-
als
1.5 ThevaluesstatedinSIunits,asdetailedinIEEE/ASTM
D792Test Methods for Density and Specific Gravity (Rela-
S-10, are to be regarded as the standard. The values given in
tive Density) of Plastics by Displacement
parentheses are for information only.
D883Terminology Relating to Plastics
NOTE 1—PVDF exhibits polymorphism. The type and extent of
D1238Test Method for Melt Flow Rates of Thermoplastics
crystalline structure varies with the thermomechanical history of the
by Extrusion Plastometer
sample. Specimens prepared by techniques different than prescribed in
D2863Test Method for Measuring the Minimum Oxygen
this specification can have properties that vary from the values specified.
Concentration to Support Candle-Like Combustion of
1.6 This standard does not purport to address all of the
Plastics (Oxygen Index)
safety concerns, if any, associated with its use. It is the
D3418Test Method for Transition Temperatures and En-
responsibility of the user of this standard to establish appro-
thalpies of Fusion and Crystallization of Polymers by
priate safety and health practices and determine the applica-
Differential Scanning Calorimetry
bility of regulatory limitations prior to use. Specific precau-
D3835Test Method for Determination of Properties of
tionary statements are given in Section 10.
Polymeric Materials by Means of a Capillary Rheometer
D3892Practice for Packaging/Packing of Plastics
This specification is under the jurisdiction of ASTM Committee D20 on
IEEE/ASTM S-10Use of the International System of Units
Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic
Materials.
Current edition approved May 1, 2015. Published June 2015. Originally
approved in 1973. Last previous edition approved in 2010 as D3222-05(2010). For referenced ASTM standards, visit the ASTM website, www.astm.org, or
DOI: 10.1520/D3222-05R15. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Lovinger, A. J., “Poly(Vinylidene Fluoride)” Developments in Crystalline Standards volume information, refer to the standard’s Document Summary page on
Polymers, Vol 1, Chapter 5, D. C. Bassett, Ed., Applied Science, London, 1982. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3222−05 (2015)
TABLE 1 Classification of PVDF Resins
Typical Values or Ranges
Property Type I Type II
Grade 1 Grade 2
Specific Gravity Gms/cc 1.75-1.79 1.75-1.79 1.76-1.79
Peak Melting Endotherm °C 156-162 162-170 164-180
Melt Flow Rate g/10 min (wt in Kg)
A
Ultra High Viscosity . . 0.5-10
A B C
High Viscosity 0.5-8 5-8 0.5-10
A B D
Medium Viscosity 4-18 5-36 0.5-30
E F
Low Viscosity . 3.5-45 0.5-60
G
Apparent Melt Viscosity Pa’s:
High Viscosity 2800-3800 2800-3700 2500-4000
Medium Viscosity 2300-2800 1300-2800 1300-2500
Low Viscosity . 350-1300 250-1300
Note: For measuring MFR values of PVDF, the load must be selected based on the viscosity as follows:
A
= 21.6 Kg
B
= 12.5 Kg
C
= 10.0 Kg
D
=5Kg
E
=3.8Kg
F
= 2.16 Kg
G −1
Reported for a shear rate of 100 s determined by capillary rheometry at 232°C (450°F) using 0.027 radian (60°) entrance angle die with L/D of 15 and in accordance
with procedures of Test Method D3835. Multiply the pascal second values by ten to obtain poise values.
(SI): The Modern Metric System resin grades available from several sources and are provided
2.2 IEC and ISO Standards: for information purposes only.
4.1.2 Type II—PVDF fluoroplastics are polymerized in sus-
ISO 12086-1 Plastics—Fluoropolymer Dispersion and
Moulding and Extrusion Materials—Part 1: Designation pension. Peak melting temperatures of these resins range from
164 to 180°C. The particles isolated from suspension are
and Basis for Specification
ISO 12086-2 Plastics—Fluoropolymer Dispersion and spherical and range typically from 20 to 150 µm in diameter.
4.1.2.1 Type II resins are available commercially, and the
Molding and Extrusion Materials—Part 2: Preparation of
data of
Test Specimens and Determination of Properties Table 1 reflect ranges encompassing values typical for
the properties of available grades.
3. Terminology
4.2 The system uses predefined cells to refer to specific
3.1 Definitions:
aspects of this specification, as illustrated below.
3.1.1 For definitions of plastics terms used in this
Specification
specification, see Terminology D883.
Special
Standard Number Block Type Grade Class
Notes
3.1.2 lot, n—one production run or a uniform blend of two
Example: Specification
or more production runs.
D3222 – 05 I 2 . .
For this example (D3222–05, I2), the line callout describes
4. Classification
a PVDF resin polymerized in emulsion, having a specific
4.1 This specification covers two types of natural, unmodi-
gravity between 1.75 and 1.79, and a peak melting endotherm
fied PVDF fluoroplastics supplied in pellet form for molding
between 162 to 170°C. A comma is used as the separator
andextrusion,andinpowderformforsolutions,dispersions,or
betweentheStandardNumberandtheType.Separatorsarenot
coatings.
needed between the Type, Grade, and Class. Provision for
4.1.1 Type I—PVDFfluoroplasticsarepolymerizedinemul-
Special Notes is included so that other information, such as a
sion. Depending upon the polymerization conditions, the peak
preferred viscosity range, can be provided when required.
melting point of the resin can be varied between 156 and
When special notes are used, they shall be preceded by a
170°C. The diameter of the primary particle isolated from the
comma.
emulsion is typically less than 1 µm; the dried powder has an
average agglomerate diameter range of 3 to 15 µm.
5. General Requirements
4.1.1.1 Two distinctly different Type I emulsion PVDF
5.1 Thematerialshallbeofuniformcompositionandfreeof
resins are available commercially. These are differentiated by
foreign matter.
peak melting endotherm values, as shown in Table 1, and this
differenceisthebasisforsubdividingTypeIresinsintoGrades
6. Detail Requirements
1and2.Table1showsthemeltviscosityrangesencompassing
6.1 General Attributes:
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org.
5 6
Dohany, J. E., and Robb, L. E., “Poly(Vinylidene Fluoride)” Kirk-Othmer See the ASTM Form and Style for ASTM Standards, available from ASTM
Encyclopedia of Chemical Technology, Vol 11, 3rd Edition, 1980, pp. 64–74. Headquarters.
D3222−05 (2015)
6.1.1 Peak Melting Endotherm—The material covered by ture is 30 to 60°C higher than the upper peak melting
this specification shall have a minimum peak melting endo- endotherm value depending on the grade. Mold temperature is
therm for the type and class as shown in Table 1 when tested 120 610°F.
in accordance withTest Method D3418. ForType I resins, this
6.3.2 Flexural Properties—The material covered in this
shall involve heating a solid specimen of 5 61 mg from room
specification shall have a minimum flexural modulus of 1.38
temperature to 200°C at 10°C/min, maintaining the tempera-
GPa (190×10 psi) when tested in accordance with Method I
ture at 200°C for 5 min, followed by cooling at a controlled
of Test Methods D790, using 6.4-mm (0.25-in.) thick speci-
rate of 10°C/min to about 30°C, then reheating at 10°C/min to
menspreparedbyinjectionmoldingunderconditionsspecified
200°C. Record the peak melting endotherm during the second
by the resin supplier. Alternatively, compression-molded
melting cycle.
samples are used (see Section 8) and tested after the 16-h
conditioning period.
6.1.1.1 Temperature—Test Type II resins likewise except
that the maximum is 250°C.
6.3.3 Impact Resistance—Type I material covered in this
6.1.2 Specific Gravity—A solid specimen of the material specificationshallhaveaminimumimpactstrengthof80.0J/m
(1.50 ft·lbf/in.) determined by Test Methods D256 using
covered by this specification shall have the minimum specific
gravity indicated in Table 1 (1.75 for Type I, Class 1 and 1.76 6.4-mm(0.25-in.)thickspecimenspreparedbyinjectionmold-
ing under conditions specified by the manufa
...
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: D3222 − 05 (Reapproved 2010) D3222 − 05 (Reapproved 2015)
Standard Specification for
Unmodified Poly(Vinylidene Fluoride) (PVDF) Molding
Extrusion and Coating Materials
This standard is issued under the fixed designation D3222; 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 specification covers melt processable molding and extrusion materials, as well as coating materials of poly(vinylidene
fluoride) fluoroplastic, commonly abbreviated PVDF (or PVF in scientific literature). This specification covers thermoplastic resin
materials supplied in pellet or powder form.
1.2 This specification applies only to the virgin homopolymer prepared from vinylidene fluoride, not copolymers, reinforced,
filled grades or special grades with additives or treatments for modification of attributes.
1.3 The tests involved are intended to provide information for specification of unmodified PVDF homopolymer resins. It is not
the purpose of this specification to provide engineering data for design purposes.
1.4 PVDF fluoroplastics melt between 156 and 180°C (312 and 356°F) and are thermally stable up to about 370°C (698°F).
(Warning—Evolution of corrosive and toxic hydrogen fluoride can occur under certain conditions.)
1.5 The values stated in SI units, as detailed in IEEE/ASTM S-10, are to be regarded as the standard. The values given in
parentheses are for information only.
NOTE 1—PVDF exhibits polymorphism. The type and extent of crystalline structure varies with the thermomechanical history of the sample.
Specimens prepared by techniques different than prescribed in this specification can have properties that vary from the values specified.
1.6 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 10.
NOTE 2—There is no equivalent ISO standard for this specification. Information in this specification is technically equivalent to related information
in ISO 12086-1 and ISO 12086-2.
2. Referenced Documents
2.1 ASTM Standards:
D149 Test Method for Dielectric Breakdown Voltage and Dielectric Strength of Solid Electrical Insulating Materials at
Commercial Power Frequencies
D150 Test Methods for AC Loss Characteristics and Permittivity (Dielectric Constant) of Solid Electrical Insulation
D256 Test Methods for Determining the Izod Pendulum Impact Resistance of Plastics
D257 Test Methods for DC Resistance or Conductance of Insulating Materials
D542 Test Method for Index of Refraction of Transparent Organic Plastics
D618 Practice for Conditioning Plastics for Testing
D638 Test Method for Tensile Properties of Plastics
D790 Test Methods for Flexural Properties of Unreinforced and Reinforced Plastics and Electrical Insulating Materials
D792 Test Methods for Density and Specific Gravity (Relative Density) of Plastics by Displacement
D883 Terminology Relating to Plastics
D1238 Test Method for Melt Flow Rates of Thermoplastics by Extrusion Plastometer
This specification is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials.
Current edition approved Nov. 1, 2010May 1, 2015. Published March 2011June 2015. Originally approved in 1973. Last previous edition approved in 20052010 as
D3222 - 05.D3222 - 05(2010). DOI: 10.1520/D3222-05R10.10.1520/D3222-05R15.
Lovinger, A. J., “Poly(Vinylidene Fluoride)” Developments in Crystalline Polymers, Vol 1, Chapter 5, D. C. Bassett, Ed., Applied Science, London, 1982.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3222 − 05 (2015)
TABLE 1 Classification of PVDF Resins
Typical Values or Ranges
Property Type I Type II
Grade 1 Grade 2
Specific Gravity Gms/cc 1.75-1.79 1.75-1.79 1.76-1.79
Peak Melting Endotherm °C 156-162 162-170 164-180
Melt Flow Rate g/10 min (wt in Kg)
A
Ultra High Viscosity . . 0.5-10
A B C
High Viscosity 0.5-8 5-8 0.5-10
A B D
Medium Viscosity 4-18 5-36 0.5-30
E F
Low Viscosity . 3.5-45 0.5-60
G
Apparent Melt Viscosity Pa’s:
High Viscosity 2800-3800 2800-3700 2500-4000
Medium Viscosity 2300-2800 1300-2800 1300-2500
Low Viscosity . 350-1300 250-1300
Note: For measuring MFR values of PVDF, the load must be selected based on the viscosity as follows:
A
= 21.6 Kg
B
= 12.5 Kg
C
= 10.0 Kg
D
= 5 Kg
E
= 3.8 Kg
F
= 2.16 Kg
G −1
Reported for a shear rate of 100 s determined by capillary rheometry at 232°C (450°F) using 0.027 radian (60°) entrance angle die with L/D of 15 and in accordance
with procedures of Test Method D3835. Multiply the pascal second values by ten to obtain poise values.
D2863 Test Method for Measuring the Minimum Oxygen Concentration to Support Candle-Like Combustion of Plastics
(Oxygen Index)
D3418 Test Method for Transition Temperatures and Enthalpies of Fusion and Crystallization of Polymers by Differential
Scanning Calorimetry
D3835 Test Method for Determination of Properties of Polymeric Materials by Means of a Capillary Rheometer
D3892 Practice for Packaging/Packing of Plastics
IEEE/ASTM S-10 Use of the International System of Units (SI): The Modern Metric System
2.2 IEC and ISO Standards:
ISO 12086-1 Plastics—Fluoropolymer Dispersion and Moulding and Extrusion Materials—Part 1: Designation and Basis for
Specification
ISO 12086-2 Plastics—Fluoropolymer Dispersion and Molding and Extrusion Materials—Part 2: Preparation of Test
Specimens and Determination of Properties
3. Terminology
3.1 Definitions:
3.1.1 For definitions of plastics terms used in this specification, see Terminology D883.
3.1.2 lot, n—one production run or a uniform blend of two or more production runs.
4. Classification
4.1 This specification covers two types of natural, unmodified PVDF fluoroplastics supplied in pellet form for molding and
extrusion, and in powder form for solutions, dispersions, or coatings.
4.1.1 Type I—PVDF fluoroplastics are polymerized in emulsion. Depending upon the polymerization conditions, the peak
melting point of the resin can be varied between 156 and 170°C. The diameter of the primary particle isolated from the emulsion
is typically less than 1 μm; the dried powder has an average agglomerate diameter range of 3 to 15 μm.
4.1.1.1 Two distinctly different Type I emulsion PVDF resins are available commercially. These are differentiated by peak
melting endotherm values, as shown in Table 1, and this difference is the basis for subdividing Type I resins into Grades 1 and
2. Table 1 shows the melt viscosity ranges encompassing resin grades available from several sources and are provided for
information purposes only.
4.1.2 Type II—PVDF fluoroplastics are polymerized in suspension. Peak melting temperatures of these resins range from 164
to 180°C. The particles isolated from suspension are spherical and range typically from 20 to 150 μm in diameter.
4.1.2.1 Type II resins are available commercially, and the data of Table 1 reflect ranges encompassing values typical for the
properties of available grades.
4.2 The system uses predefined cells to refer to specific aspects of this specification, as illustrated below.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
Dohany, J. E., and Robb, L. E., “Poly(Vinylidene Fluoride)” Kirk-Othmer Encyclopedia of Chemical Technology, Vol 11, 3rd Edition, 1980, pp. 64–74.
D3222 − 05 (2015)
Specification
Special
Standard Number Block Type Grade Class
Notes
Example: Specification
D3222 – 05 I 2 . .
For this example (D3222 – 05, I2), the line callout describes a PVDF resin polymerized in emulsion, having a specific gravity
between 1.75 and 1.79, and a peak melting endotherm between 162 to 170°C. A comma is used as the separator between the
Standard Number and the Type. Separators are not needed between the Type, Grade, and Class. Provision for Special Notes is
included so that other information, such as a preferred viscosity range, can be provided when required. When special notes are
used, they shall be preceded by a comma.
5. General Requirements
5.1 The material shall be of uniform composition and free of foreign matter.
6. Detail Requirements
6.1 General Attributes:
6.1.1 Peak Melting Endotherm—The material covered by this specification shall have a minimum peak melting endotherm for
the type and class as shown in Table 1 when tested in accordance with Test Method D3418. For Type I resins, this shall involve
heating a solid specimen of 5 6 1 mg from room temperature to 200°C at 10°C/min, maintaining the temperature at 200°C for 5
min, followed by cooling at a controlled rate of 10°C/min to about 30°C, then reheating at 10°C/min to 200°C. Record the peak
melting endotherm during the second melting cycle.
6.1.1.1 Temperature—Test Type II resins likewise except that the maximum is 250°C.
6.1.2 Specific Gravity—A solid specimen of the material covered by this specification shall have the minimum specific gravity
indicated in Table 1 (1.75 for Type I, Class 1 and 1.76 for all others) when tested in accordance with Test Method D792.
NOTE 3—Test attached to the specimen upon immersion. Dipping the specimens in a very dilute solution (less than 0.1 weight percent) of an ammonium
perfluorooctanoate surfactant minimizes this problem.
6.1.3 Refractive Index—The material covered in this specification shall have a refractive index of 1.42 when measured at the
sodium D line at 25°C (77°F) in accordance with the refractometer procedure in Test Methods D542, using specimens that have
not been subjected to any processes which induce orientation of the polymer chains or crystal-lites. Compression-molded
specimens at least 2-mm (0.079-in.) thick that have been quenched rapidly in water are preferred.
6.1
...
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