ASTM E2744-10(2015)
(Test Method)Standard Test Method for Pressure Calibration of Thermal Analyzers
Standard Test Method for Pressure Calibration of Thermal Analyzers
SIGNIFICANCE AND USE
5.1 Most thermal analysis experiments are conducted under ambient pressure conditions using isothermal or temperature time rate of change conditions where time or temperature is the independent parameter. Some experiments, however, are conducted under reduced or elevated pressure conditions where pressure is an independent experimental parameter (Test Method E537). Oxidation Induction Times (Test Methods D5483, D5885, D6186, and E1858), Oxidation Onset Temperature (Test Method E2009), and the Vapor Pressure (Test Method E1782) are other examples of experiments conducted under elevated or reduced pressure (vacuum) conditions. Since in these cases pressure is an independent variable, the measurement system for this parameter shall be calibrated to ensure interlaboratory reproducibility.
5.2 The dependence of experimental results on pressure is usually logarithmic rather than linear.
SCOPE
1.1 This test method describes the calibration or performance confirmation of the electronic pressure signals from thermal analysis apparatus.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 There is no ISO standard equivalent to this test method.
1.4 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.
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Designation: E2744 − 10(Reapproved 2015)
Standard Test Method for
Pressure Calibration of Thermal Analyzers
This standard is issued under the fixed designation E2744; 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 E1782 Test Method for Determining Vapor Pressure by
Thermal Analysis
1.1 This test method describes the calibration or perfor-
E1858 Test Method for Determining Oxidation Induction
mance confirmation of the electronic pressure signals from
Time of Hydrocarbons by Differential Scanning Calorim-
thermal analysis apparatus.
etry
1.2 The values stated in SI units are to be regarded as
E2009 Test Methods for Oxidation Onset Temperature of
standard. No other units of measurement are included in this
Hydrocarbons by Differential Scanning Calorimetry
standard.
E2161 Terminology Relating to Performance Validation in
1.3 There is no ISO standard equivalent to this test method. Thermal Analysis
1.4 This standard does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 3.1 Definitions:
priate safety and health practices and determine the applica-
3.1.1 The technical terms used in this test method are
bility of regulatory limitations prior to use. defined in Terminologies E473, E1142, and E2161, including
calibration, Celsius, differential scanning calorimetry, high
2. Referenced Documents
pressure, linearity, oxidative induction time, thermal analysis,
and vapor pressure.
2.1 ASTM Standards:
D5483 Test Method for Oxidation Induction Time of Lubri-
3.2 Definitions of Terms Specific to This Standard:
catingGreasesbyPressureDifferentialScanningCalorim-
3.2.1 absolute pressure, n—pressure measured relative to
etry
zero pressure corresponding to empty space.
D6186 Test Method for Oxidation Induction Time of Lubri-
3.2.1.1 Discussion—Absolute pressure is atmospheric pres-
cating Oils by Pressure Differential Scanning Calorimetry
sure plus gage pressure.
(PDSC)
3.2.2 atmospheric pressure, n—the pressure due to the
D5720 Practice for Static Calibration of Electronic
weight of the atmosphere.
Transducer-Based Pressure Measurement Systems for
3.2.2.1 Discussion—Atmospheric pressure varies with el-
Geotechnical Purposes
evation above sea level, acceleration due to gravity and
D5885 Test Method for Oxidative Induction Time of Poly-
weather conditions. Standard atmospheric pressure is
olefin Geosynthetics by High-Pressure Differential Scan-
101.325 kPa.
ning Calorimetry
3.2.3 barometer, n—an instrument for measuring atmo-
E473 Terminology Relating to Thermal Analysis and Rhe-
spheric pressure.
ology
E537 Test Method for The Thermal Stability of Chemicals 3.2.4 gage pressure, n—pressure measured relative to atmo-
by Differential Scanning Calorimetry spheric pressure.
E1142 Terminology Relating to Thermophysical Properties 3.2.4.1 Discussion—Zero gage pressure is equal to atmo-
spheric pressure. Gage pressure is the difference between
absolute pressure and atmospheric pressure.
ThistestmethodisunderthejurisdictionofASTMCommitteeE37onThermal
3.2.5 pressure, n—the force exerted to a surface per unit
Measurements and is the direct responsibility of Subcommittee E37.10 on
area.
Fundamental, Statistical and Mechanical Properties.
Current edition approved March 1, 2015. Published March 2015. Originally
3.2.6 vacuum, n—pressure less than atmospheric pressure.
approved in 2010. Last previous edition approved in 2010 as E2744 – 10.
DOI:101520/E2744-10R15.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 4. Summary of Test Method
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
4.1 The pressure (vacuum) signal generated by a thermal
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. analyzer is compared to a gage whose performance is known
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2744 − 10 (2015)
and traceable to a national metrology institute. The thermal pressure. Pressure relief shall be provided at pressures no
analyzer may be said to be in conformance if the performance greater than 1.2 times the maximum allowable working pres-
is within established limits. Alternately, the pressure signal sure.
may be calibrated using a two-point calibration method.
8. Preparation of Apparatus
5. Significance and Use 8.1 Assemble the apparatus so that the calibration pressure
gageisconnectedinparallelwiththepressuretransducerofthe
5.1 Most thermal analysis experiments are conducted under
apparatus.Thatis,theinstrumenttransducerandthecalibration
ambient pressure conditions using isothermal or temperature
gage shall see the same static pressure (see Fig. 1). Equilibrate
timerateofchangeconditionswheretimeortemperatureisthe
the thermal analysis apparatus pressure container, reference
independent parameter. Some experiments, however, are con-
pressure gage and instrument transducer at ambient tempera-
ducted under reduced or elevated pressure conditions where
ture.
pressure is an independent experimental parameter (Test
Method E537). Oxidation Induction Times (Test Methods
9. Calibration
D5483, D5885, D6186, and E1858), Oxidation Onset Tem-
9.1 Perform any pressure signal calibration procedures rec-
perature (Test Method E2009), and the Vapor Pressure (Test
ommended by the manufacturer of the thermal analyzer as
Method E1782) are other examples of experiments conducted
described in the Operator’s Manual.
under elevated or reduced pressure (vacuum) conditions. Since
in these cases pressure is an independent variable, the mea-
10. Procedure
surementsystemforthisparametershallbecalibratedtoensure
10.1 Electronic pressure signals associated with thermal
interlaboratory reproducibility.
analysis apparatus measure gage pressure relative to atmo-
5.2 The dependence of experimental results on pressure is
spheric pressure. However, absolute pressure is most often
usually logarithmic rather than linear.
required for thermal analysis experiments.Absolute pressure is
the sum of gage pressure and atmospheric pressure. So
6. Apparatus
knowledge of atmospheric pressure is required to obtain
absolute pressure.
6.1 Reference pressure gage with a range 1.2 times the
maximumvaluetobecalibratedreadabletowithin0.1 %ofthe
10.2 Using a laboratory barometer, measure and record the
full range and performance of which has been verified using
atmospheric pressure (Patm) within one hour of the pressure
standards and procedures traceable to a national metrology
calibration in steps 10.4 – 10.6.
institute (such as the National Institute of Standards and
NOTE 5—Should a laboratory barometer be unavailable, local pressure
Technology (NIST)).
may often be obtained by contacting the local weather service. This
approach is not suitable for laboratories operating under negative gage
NOTE 1—To ensure an accurate pressure measurement, the reference
pressure.
pressure gage shall be placed as close as practical to the thermal analysis
10.3 Assemble the instrument to be calibrated, the reference
apparatus to be calibrated and connected to the thermal analysis apparatus
with large diameter tubing such a
...
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: E2744 − 10 E2744 − 10 (Reapproved 2015)
Standard Test Method for
Pressure Calibration of Thermal Analyzers
This standard is issued under the fixed designation E2744; 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 calibration or performance confirmation of the electronic pressure signals from thermal
analysis apparatus.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 There is no ISO standard equivalent to this test method.
1.4 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.
2. Referenced Documents
2.1 ASTM Standards:
D5483 Test Method for Oxidation Induction Time of Lubricating Greases by Pressure Differential Scanning Calorimetry
D6186 Test Method for Oxidation Induction Time of Lubricating Oils by Pressure Differential Scanning Calorimetry (PDSC)
D5720 Practice for Static Calibration of Electronic Transducer-Based Pressure Measurement Systems for Geotechnical Purposes
D5885 Test Method for Oxidative Induction Time of Polyolefin Geosynthetics by High-Pressure Differential Scanning
Calorimetry
E473 Terminology Relating to Thermal Analysis and Rheology
E537 Test Method for The Thermal Stability of Chemicals by Differential Scanning Calorimetry
E1142 Terminology Relating to Thermophysical Properties
E1782 Test Method for Determining Vapor Pressure by Thermal Analysis
E1858 Test Method for Determining Oxidation Induction Time of Hydrocarbons by Differential Scanning Calorimetry
E2009 Test Methods for Oxidation Onset Temperature of Hydrocarbons by Differential Scanning Calorimetry
E2161 Terminology Relating to Performance Validation in Thermal Analysis
3. Terminology
3.1 Definitions:
3.1.1 The technical terms used in this test method are defined in Terminologies E473, E1142, and E2161, including calibration,
Celsius, differential scanning calorimetry, high pressure, linearity, oxidative induction time, thermal analysis, and vapor pressure.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 absolute pressure, n—pressure measured relative to zero pressure corresponding to empty space.
This test method is under the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.10 on Fundamental,
Statistical and Mechanical Properties.
Current edition approved March 15, 2010March 1, 2015. Published August 2010March 2015. DOI:101520/E2744-10.Originally approved in 2010. Last previous edition
approved in 2010 as E2744 – 10. DOI:101520/E2744-10R15.
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.
3.2.1.1 Discussion—
Absolute pressure is atmospheric pressure plus gage pressure.
3.2.2 atmospheric pressure, n—the pressure due to the weight of the atmosphere.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2744 − 10 (2015)
3.2.2.1 Discussion—
Atmospheric pressure varies with elevation above sea level, acceleration due to gravity and weather conditions. Standard
atmospheric pressure is 101.325 kPa.
3.2.3 barometer, n—an instrument for measuring atmospheric pressure.
3.2.4 gage pressure, n—pressure measured relative to atmospheric pressure.
3.2.4.1 Discussion—
Zero gage pressure is equal to atmospheric pressure. Gage pressure is the difference between absolute pressure and atmospheric
pressure.
3.2.5 pressure, n—the force exerted to a surface per unit area.
3.2.6 vacuum, n—pressure less than atmospheric pressure.
4. Summary of Test Method
4.1 The pressure (vacuum) signal generated by a thermal analyzer is compared to a gage whose performance is known and
traceable to a national metrology institute. The thermal analyzer may be said to be in conformance if the performance is within
established limits. Alternately, the pressure signal may be calibrated using a two-point calibration method.
5. Significance and Use
5.1 Most thermal analysis experiments are conducted under ambient pressure conditions using isothermal or temperature time
rate of change conditions where time or temperature is the independent parameter. Some experiments, however, are conducted
under reduced or elevated pressure conditions where pressure is an independent experimental parameter (Test Method E537).
Oxidation Induction Times (Test Methods D5483, D5885, D6186, and E1858), Oxidation Onset Temperature (Test Method
E2009), and the Vapor Pressure (Test Method E1782) are other examples of experiments conducted under elevated or reduced
pressure (vacuum) conditions. Since in these cases pressure is an independent variable, the measurement system for this parameter
shall be calibrated to ensure interlaboratory reproducibility.
5.2 The dependence of experimental results on pressure is usually logarithmic rather than linear.
6. Apparatus
6.1 Reference pressure gage with a range 1.2 times the maximum value to be calibrated readable to within 0.1 % of the full
range and performance of which has been verified using standards and procedures traceable to a national metrology institute (such
as the National Institute of Standards and Technology (NIST)).
NOTE 1—To ensure an accurate pressure measurement, the reference pressure gage shall be placed as close as practical to the thermal analysis apparatus
to be calibrated and connected to the thermal analysis apparatus with large diameter tubing such as 6.3 mm or larger especially for vacuum testing. Ensure
that there is no gas flow in the connection (for example, due to leaking) to provide a static pressure measurement.
NOTE 2—Additional information on pressure gages may be found in Practice D5720.
6.2 A source of pressurized inert gas, typically nitrogen, with a pressure regulator, capable of adjusting the pressure supplied
to the apparatus from zero to 100 % of the gage pressure range to be calibrated, commonly 7 MPa.
NOTE 3—Since the calibration is performed under static flow conditions, the pressurizing gas delivery system to the thermal analysis apparatus should
be of small diameter (such as 1.6 mm diameter tubing) for safety considerations.
NOTE 4—Do not use a reactive gas such as oxygen unless all apparatus, tubing and test gage have been cleaned and are rated for oxygen service.
6.3 The thermal analysis apparatus for which the pressure calibration is to be performed.
6.4 Barometer capable of measuring atmospheric pressure readable to 60.01 kPa (0.1 mm Hg).
7. Hazards
7.1 This test poses risks associated with high pressure operation. The thermal analysis apparatus, connecting tubing and
measurement gages shall be designed to contain pressures in excess of two times the maximum allowable working pressure.
Pressure relief shall be provided at pressures no greater than 1.2 times the maximum allowable working pressure.
8. Preparation of
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