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ASTM E928-08(2014)

(Test Method)

Standard Test Method for Purity by Differential Scanning Calorimetry

Standard Test Method for Purity by Differential Scanning Calorimetry

SIGNIFICANCE AND USE
5.1 The melting temperature range of a compound broadens as the impurity level rises. This phenomenon is described approximately by the van’t Hoff equation for melting point depressions. Measuring and recording the instantaneous heat flow into the specimen as a function of temperature during such a melting process is a practical way for the generation of data suitable for analysis by the van’t Hoff equation.  
5.2 The results obtained include: sample purity (expressed as mole percent); enthalpy of fusion (expressed as joules per mole); and the melting temperature (expressed in Kelvin) of the pure form of the major component.  
5.3 Generally, the repeatability of this test method decreases as the purity level decreases. This test method is ordinarily considered unreliable when the purity level of the major component of the mixture is less than 98.5 mol % or when the incremental enthalpy correction (c) exceeds 20 % of the original detected enthalpy of fusion.  
5.4 This test method is used for quality control, specification acceptance, and research.
SCOPE
1.1 This test method describes the determination of purity of materials greater than 98.5 mole percent purity using differential scanning calorimetry and the van’t Hoff equation.  
1.2 This test method is applicable to thermally stable compounds with well-defined melting temperatures.  
1.3 Determination of purity by this test method is only applicable when the impurity dissolves in the melt and is insoluble in the crystal.  
1.4 There is no ISO method equivalent to this test method.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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.

General Information

Status
Historical
Publication Date
14-Aug-2014
ICS
17.200.10 - Heat. Calorimetry
Technical Committee
E37 - Thermal Measurements
Drafting Committee
E37.01 - Calorimetry and Mass Loss
Current Stage
Ref Project

Relations

Replaces
ASTM E928-08 - Standard Test Method for Determination of Purity by Differential Scanning Calorimetry
Effective Date
15-Aug-2014
Replaced By
ASTM E928-19 - Standard Test Method for Purity by Differential Scanning Calorimetry
Effective Date
01-May-2019
Referred By
ASTM E2069-19 - Standard Test Method for Temperature Calibration on Cooling of Differential Scanning Calorimeters
Effective Date
15-Aug-2014

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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: E928 − 08 (Reapproved 2014)
Standard Test Method for
1
Purity by Differential Scanning Calorimetry
This standard is issued under the fixed designation E928; 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.
1. Scope E1970PracticeforStatisticalTreatmentofThermoanalytical
Data
1.1 Thistestmethoddescribesthedeterminationofpurityof
materials greater than 98.5 mole percent purity using differen-
3. Terminology
tial scanning calorimetry and the van’t Hoff equation.
3.1 Definitions—The definitions relating to thermal analysis
1.2 This test method is applicable to thermally stable
appearing in Terminology E473 shall be considered applicable
compounds with well-defined melting temperatures.
to this test method.
1.3 Determination of purity by this test method is only
4. Summary of Test Method
applicable when the impurity dissolves in the melt and is
3
insoluble in the crystal.
4.1 Thistestmethodisbaseduponthevan’tHoffequation:
1.4 There is no ISO method equivalent to this test method. 2
T 5 T 2 ~RT χ!/~HF! (1)
s o o
1.5 The values stated in SI units are to be regarded as
where:
standard. No other units of measurement are included in this
T = specimen temperature, K
s
standard.
T = melting temperature of 100% pure material, K
o
−1 −1
1.6 This standard does not purport to address all of the
R = gas constant (= 8.314 J mol K ),
safety concerns, if any, associated with its use. It is the χ = mole fraction of impurity,
−1
responsibility of the user of this standard to establish appro- H = heat of fusion, J mol , and
F = fraction melted.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4.2 This test method consists of melting the test specimen
that is subjected to a temperature-controlled program while
2. Referenced Documents
recording the heat flow into the specimen as a function of
2
2.1 ASTM Standards:
temperature.Theresultingmeltingendothermareaismeasured
E473Terminology Relating to Thermal Analysis and Rhe- to yield the enthalpy of fusion, H.The melting endotherm area
ology
is then partitioned into a series of fractional areas (about ten,
E793Test Method for Enthalpies of Fusion and Crystalliza- comprisingthefirst10to50%ofthetotalarea).Thefractional
tion by Differential Scanning Calorimetry
area, divided by the total area, yields the fraction melted, F.
E794TestMethodforMeltingAndCrystallizationTempera- Each fractional area is assigned a temperature, T .
s
tures By Thermal Analysis
4.3 Eq1hastheformofY=mX+bwhereY= T,X=1/F,
s
E967Test Method for Temperature Calibration of Differen- 2
m=−(RT χ)/ H, and b = T . A plot of Y versus X should
o o
tial Scanning Calorimeters and Differential ThermalAna-
produce a straight line with slope m and intercept b.
lyzers
4.4 In practice, however, the resultant plot of T versus 1 /F
s
E968Practice for Heat Flow Calibration of Differential
is seldom a straight line. To linearize the plot, an incremental
Scanning Calorimeters
amount of area is added to the total area and to each fractional
area to produce a revised value for F. The process of
incremental addition of area is continued until a straight line is
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
Measurements and is the direct responsibility of Subcommittee E37.01 on Calo- obtained.
rimetry and Mass Loss.
F 5 ~A 1c!/~A 1c! (2)
part total
Current edition approved Aug. 15, 2014. Published September 2014. Originally
approved in 1983. Last previous edition approved in 2008 as E928–08. DOI:
10.1520/E0928-08R14.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Brennan, W. P., DiVito, M. P., Fynas, R. L., Gray,A. P., “An Overview of the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Calorimetric Purity Measurement”, in Purity Determinations by Thermal Methods,
Standards volume information, refer to the standard’s Document Summary page on R. L. Blaine and C. K. Schoff (Eds.), Special Technical Publication 838,American
the ASTM website. Society for Testing and Materials, West Conshohocken, PA, 1984, pp. 5–15.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E928 − 08 (2014)
where: 6.2.2 Thesolubilityoftheimpurityinthesolidofthemajor
constituent is negligible; and
A = area of fraction melted, mJ
part
6.2.3 The major constituent displays a single well-defined
A = total area, mJ and
total
c = incremental area, mJ. meltingendotherminthetemperaturerangeofinterest.Micro-
NOTE 1
...

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: E928 − 08 E928 − 08 (Reapproved 2014)
Standard Test Method for
1
Purity by Differential Scanning Calorimetry
This standard is issued under the fixed designation E928; 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 This test method describes the determination of purity of materials greater than 98.5 mole percent purity using differential
scanning calorimetry and the van’tvan’t Hoff equation.
1.2 This test method is applicable to thermally stable compounds with well-defined melting temperatures.
1.3 Determination of purity by this test method is only applicable when the impurity dissolves in the melt and is insoluble in
the crystal.
1.4 There is no ISO method equivalent to this test method.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.
1.6 There is no ISO method equivalent to this test method.
2. Referenced Documents
2
2.1 ASTM Standards:
E473 Terminology Relating to Thermal Analysis and Rheology
E793 Test Method for Enthalpies of Fusion and Crystallization by Differential Scanning Calorimetry
E794 Test Method for Melting And Crystallization Temperatures By Thermal Analysis
E967 Test Method for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal Analyzers
E968 Practice for Heat Flow Calibration of Differential Scanning Calorimeters
E1970 Practice for Statistical Treatment of Thermoanalytical Data
3. Terminology
3.1 Definitions—The definitions relating to thermal analysis appearing in Terminology E473 shall be considered applicable to
this test method.
4. Summary of Test Method
3
4.1 This test method is based upon the van’t Hoff equationequation: :
2
T 5 T 2 ~RT χ!/~H F! (1)
s o o
where:
T = specimen temperature, K
s
T = melting temperature of 100 % pure material, K
o
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.01 on Calorimetry
and Mass Loss.
Current edition approved Sept. 1, 2008Aug. 15, 2014. Published November 2008 September 2014. Originally approved in 1983. Last previous edition approved in
20032008 as E928 – 03.E928 – 08. DOI: 10.1520/E0928-08.10.1520/E0928-08R14.
2
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.
3
Brennan, W. P., DiVito, M. P., Fynas, R. L., Gray, A. P., “An Overview of the Calorimetric Purity Measurement”, in Purity Determinations by Thermal Methods, R. L.
Blaine and C. K. Schoff (Eds.), Special Technical Publication 838, American Society for Testing and Materials, West Conshohocken, PA 1984, pp. 5 - 15.Brennan, W. P.,
DiVito, M. P., Fynas, R. L., Gray, A. P., “An Overview of the Calorimetric Purity Measurement”, in Purity Determinations by Thermal Methods, R. L. Blaine and C. K. Schoff
(Eds.), Special Technical Publication 838, American Society for Testing and Materials, West Conshohocken, PA, 1984, pp. 5–15.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E928 − 08 (2014)
−1 − 1
R = gas constant (= 8.314 J mol K ),
χ = mole fraction of impurity,
− 1
H = heat of fusion, J mol , and
F = fraction melted.
4.2 This test method consists of melting the test specimen that is subjected to a temperature-controlled program while recording
the heat flow into the specimen as a function of temperature. The resulting melting endotherm area is measured to yield the
enthalpy of fusion, H. The melting endotherm area is then partitioned into a series of fractional areas (about ten, comprising the
first 10 to 50 % of the total area). The fractional area, divided by the total area, yields the fraction melted, F. Each fractional area
is assigned a temperature, T .
s
2
4.3 Eq 1 has the form
...

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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.

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  • Standard
    4 pages
    English language
    sale 15% off