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ASTM F2625-07

(Test Method)

Standard Test Method for Measurement of Enthalpy of Fusion, Percent Crystallinity, and Melting Point of Ultra-High-Molecular Weight Polyethylene by Means of Differential Scanning Calorimetry

Standard Test Method for Measurement of Enthalpy of Fusion, Percent Crystallinity, and Melting Point of Ultra-High-Molecular Weight Polyethylene by Means of Differential Scanning Calorimetry

SIGNIFICANCE AND USE
The crystallinity of UHMWPE will influence its mechanical properties, such as creep and stiffness. The reported crystallinity will depend on the integration range used to determine the heat of fusion, and the theoretical heat of fusion of 100 % crystalline polyethylene used to calculate the percent crystallinity in an unknown specimen. Differential scanning calorimetry is an effective means of accurately measuring both heat of fusion and melting temperature.
This test method is useful for both process control and research.
SCOPE
1.1 This test method discusses the measurement of the heat of fusion and the melting point of ultra-high-molecular weight polyethylene (UHMWPE), and the subsequent calculation of the percentage of crystallinity.
1.2 This test method can be used for UHMWPE in powder form, consolidated form, finished product, or a used product. It can also be used for irradiated or chemically-crosslinked UHMWPE.
1.3 This test method does not suggest a desired range of crystallinity or melting points for specific applications.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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.

General Information

Status
Historical
Publication Date
31-Jan-2007
ICS
07.030 - Physics. Chemistry
17.200.10 - Heat. Calorimetry
Technical Committee
F04 - Medical and Surgical Materials and Devices
Drafting Committee
F04.15 - Material Test Methods
Current Stage
Ref Project

Relations

Replaced By
ASTM F2625-10 - Standard Test Method for Measurement of Enthalpy of Fusion, Percent Crystallinity, and Melting Point of Ultra-High-Molecular Weight Polyethylene by Means of Differential Scanning Calorimetry
Effective Date
01-Dec-2010

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ASTM F2625-07 - Standard Test Method for Measurement of Enthalpy of Fusion, Percent Crystallinity, and Melting Point of Ultra-High-Molecular Weight Polyethylene by Means of Differential Scanning CalorimetryASTM F2625-07 - Standard Test Method for Measurement of Enthalpy of Fusion, Percent Crystallinity, and Melting Point of Ultra-High-Molecular Weight Polyethylene by Means of Differential Scanning Calorimetry
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ASTM F2625-07 - Standard Test Method for Measurement of Enthalpy of Fusion, Percent Crystallinity, and Melting Point of Ultra-High-Molecular Weight Polyethylene by Means of Differential Scanning Calorimetry
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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:F2625–07
Standard Test Method for
Measurement of Enthalpy of Fusion, Percent Crystallinity,
and Melting Point of Ultra-High-Molecular Weight
1
Polyethylene by Means of Differential Scanning Calorimetry
This standard is issued under the fixed designation F2625; 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 (ϵ) indicates an editorial change since the last revision or reapproval.
1. Scope E967 Test Method for Temperature Calibration of Differen-
tial Scanning Calorimeters and Differential Thermal Ana-
1.1 This test method discusses the measurement of the heat
lyzers
of fusion and the melting point of ultra-high-molecular weight
E968 Practice for Heat Flow Calibration of Differential
polyethylene (UHMWPE), and the subsequent calculation of
Scanning Calorimeters
the percentage of crystallinity.
E1953 Practice for Description of Thermal Analysis and
1.2 This test method can be used for UHMWPE in powder
Rheology Apparatus
form, consolidated form, finished product, or a used product. It
can also be used for irradiated or chemically-crosslinked
3. Terminology
UHMWPE.
3.1 Symbols:
1.3 This test method does not suggest a desired range of
3.1.1 ∆H ,n—theoreticalheatoffusionof100 %crystalline
f
crystallinity or melting points for specific applications.
material (J/g).
1.4 The values stated in SI units are to be regarded as
3.1.2 ∆H , n—mass normalized heat of fusion of the test
s
standard. No other units of measurement are included in this
sample (J/g).
standard.
3.1.3 T , n—melting temperature at the peak of the melting
p
1.5 This standard does not purport to address all of the
endotherm (°C).
safety concerns, if any, associated with its use. It is the
3.1.4 T , n—onset temperature of the melting endotherm
o
responsibility of the user of this standard to establish appro-
(°C).
priate safety and health practices and determine the applica-
3.1.5 %X, n—percentage of crystallinity of material.
bility of regulatory limitations prior to use.
4. Summary of Test Method
2. Referenced Documents
2 4.1 This test method consists of placing a known mass of
2.1 ASTM Standards:
UHMWPE in a sample pan and heating the sample pan at a
D3418 Test Method for Transition Temperatures and En-
controlled temperature while measuring the heat flow to the
thalpies of Fusion and Crystallization of Polymers by
sample pan and an empty reference pan. The area under the
Differential Scanning Calorimetry
melting endotherm, indicative of the enthalpy of melting, is
E793 Test Method for Enthalpies of Fusion and Crystalli-
normalized with the sample mass. This value is then normal-
zation by Differential Scanning Calorimetry
ized with the theoretical enthalpy of melting of 100 % crystal-
linepolyethylenetodeterminethepercentageofcrystallinityin
the test sample.
1
This test method is under the jurisdiction ofASTM Committee F04 on Medical
and Surgical Materials and Devices and is the direct responsibility of Subcommittee
5. Significance and Use
F04.15 on Material Test Methods.
5.1 The crystallinity of UHMWPE will influence its me-
Current edition approved Feb. 1, 2007. Published February 2007. DOI: 10.1520/
F2625-07.
chanical properties, such as creep and stiffness. The reported
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
crystallinity will depend on the integration range used to
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
determine the heat of fusion, and the theoretical heat of fusion
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. of 100 % crystalline polyethylene used to calculate the percent
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
F2625–07
crystallinity in an unknown specimen. Differential scanning material. Both onset of the melting endotherm of the reference
calorimetry is an effective means of accurately measuring both standard and the heat of fusion shall be reported and compared
3
heat of fusion and melting temperature. with published values (T = 156.6°C, ∆H = 28.57 J/g). The
o f
5.2 This test method is useful for both process control and DSC calibration should be verified on at least a monthly basis.
research.
NOTE 3—The value of the ∆H will vary with the lot of the indium by
f
as much as 3 %. Users should refer to the certificate of analysis for the
6. Interferences
∆H of their specific lot of indium.
f
6.1 As machining processes can affect the crystalline struc-
11. Procedure
ture of UHMWPE, care should be taken to obtain a represen-
tative sample away from t
...

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