100% found this document useful (2 votes)
53 views7 pages

Thermal Conductivity and Thermal Diffusivity by Modulated Temperature Differential Scanning Calorimetry

Uploaded by

Tatiana Vianna
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
100% found this document useful (2 votes)
53 views7 pages

Thermal Conductivity and Thermal Diffusivity by Modulated Temperature Differential Scanning Calorimetry

Uploaded by

Tatiana Vianna
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 7

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: E1952 − 23

Standard Test Method for


Thermal Conductivity and Thermal Diffusivity by Modulated
Temperature Differential Scanning Calorimetry1
This standard is issued under the fixed designation E1952; 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 Scope Scanning Calorimeters (Withdrawn 2023)3


1.1 This test method describes the determination of thermal E1142 Terminology Relating to Thermophysical Properties
conductivity of homogeneous, non-porous solid materials in E1231 Practice for Calculation of Hazard Potential Figures
the range of 0.10 W/(K·m) to 1.0 W ⁄(K·m) by modulated of Merit for Thermally Unstable Materials
temperature differential scanning calorimeter. This range in- E2161 Terminology Relating to Performance Validation in
cludes many polymeric, glass, and ceramic materials. Thermal Thermal Analysis and Rheology
diffusivity, which is related to thermal conductivity through
3. Terminology
specific heat capacity and density, may also be derived.
Thermal conductivity and diffusivity can be determined at one 3.1 Definitions:
or more temperatures over the range of 0 °C to 90 °C. 3.1.1 Specific technical terms used in this test method are
defined in Terminologies E473, E1142, and E2161 including
1.2 The values stated in SI units are to be regarded as
calibration, differential scanning calorimetry, heat capacity,
standard.
modulated temperature, precision, reference material, relative
1.3 This standard does not purport to address all of the standard deviation, repeatability, reproducibility, specific heat
safety concerns, if any, associated with its use. It is the capacity, standard deviation, thermal analysis, thermal
responsibility of the user of this standard to establish appro- conductance, and thermal conductivity.
priate safety, health, and environmental practices and deter- 3.2 Definitions of Terms Specific to This Standard:
mine the applicability of regulatory limitations prior to use. 3.2.1 modulated temperature differential scanning
1.4 This international standard was developed in accor- calorimeter—a version of differential scanning calorimetry that
dance with internationally recognized principles on standard- provides a sinusoidally varying temperature program to the test
ization established in the Decision on Principles for the specimen in addition to the traditional isothermal or tempera-
Development of International Standards, Guides and Recom- ture ramp programs. Results from analysis shall include
mendations issued by the World Trade Organization Technical apparent and specific heat capacity.
Barriers to Trade (TBT) Committee.
4. Summary of Test Method
2. Referenced Documents
4.1 The heat capacity of a test specimen may be determined
2.1 ASTM Standards:2 using the modulated temperature approach in which an oscil-
E473 Terminology Relating to Thermal Analysis and Rhe- latory or periodically repeating temperature program (around
ology an average temperature) is imposed upon a test specimen
E967 Test Method for Temperature Calibration of Differen- producing an oscillatory (periodic) heat flow into or out of the
tial Scanning Calorimeters and Differential Thermal Ana- specimen. The heat capacity of the test specimen may be
lyzers obtained from the amplitude of the resultant heat flow divided
E968 Practice for Heat Flow Calibration of Differential by the amplitude of the oscillatory (periodic) temperature that
produces it. Specific heat capacity is obtained by normalizing
1
the heat capacity to specimen mass.
This test method is under the jurisdiction of Committee E37 on Thermal
Measurements and is the direct responsibility of Subcommittee E37.10 on 4.1.1 The accuracy of the heat capacity thus obtained
Fundamental, Statistical and Mechanical Properties. depends upon experimental conditions. When a thin test
Current edition approved June 1, 2023. Published June 2023. Originally specimen encapsulated in a specimen pan of high thermal
approved in 1998. Last previous edition approved in 2017 as E1952 – 17. DOI:
conductivity is treated with temperature oscillations of long
10.1520/E1952-23.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG6HS*07


1
'RZQORDGHGSULQWHGE\
0&7 0LQLVWHULRGD&LHQFLDH7HFQRORJLDSXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
E1952 − 23
period (low frequency), the test specimen is assumed to environment of inert nitrogen purge gas at a rate of
achieve a uniform temperature distribution and the resultant 50 mL ⁄min 6 10 mL ⁄min.
heat capacity information will be comparable with those of 7.1.2 A Temperature Controller, capable of executing a
other non-oscillatory test methods. specific temperature program by (1) operating the furnace
4.1.2 When one end of a thick test specimen is exposed to between selected temperature limits at a rate of temperature
the temperature oscillations of short period (high frequency), change of 1 °C ⁄min, (2) holding at an isothermal temperature
the test specimen will achieve a temperature distribution over over the temperature range of 0 °C to 90 °C within 60.1 °C,
its length related to its thermal diffusivity. and (3) sinusoidal varying temperature with an amplitude of
4.1.3 The apparent heat capacity information thus obtained 60.2 °C to 0.7 °C and a period of 60 s to 100 s (frequency of
is lower than that of the uniform temperature distribution case 10 mHz to 16 mHz).
described above and is proportional to the square root of
NOTE 1—The upper thermal conductivity achievable by this method is
thermal conductivity of the test specimens (1).4 The thermal
extended to 4 W (K·m) for instruments capable of 20 s periods (frequency
conductivity of the test specimen may be derived from the of 50 mHz) (2).
apparent heat capacity of a thick specimen, the actual heat
capacity of a thin specimen, and a series of geometric and 7.1.3 A Calculating Device, capable of transforming the
experimental constants. experimentally determined modulated temperature and modu-
lated specimen heat flow signals into the required continuous
4.2 If the thermal conductivity of the test specimen is low, output forms of heat capacity (preferably in units of mJ/K),
approaching that of the purge gas surrounding it, a correction specific heat capacity (preferably in units of J/(g·K)), and
to the measured thermal conductivity is required to compensate average test temperature to the required accuracy and preci-
for heat losses from the thick test specimen. sion.
4.3 Thermal diffusivity is derived from the determined 7.1.4 A Data Collecting Device, to provide a means of
thermal conductivity, specific heat capacity, and density of the acquiring, storing, and displaying measured or calculated
test specimen. signals, or both. The minimum output signals required are heat
flow, temperature, time, heat capacity, specific heat capacity,
5. Significance and Use and average temperature with a sensitivity of 0.001 mJ ⁄K for
5.1 Thermal conductivity is a useful design parameter for heat capacity, 0.001 J ⁄(g·K) for specific heat capacity, 0.01 °C
the rate of heat transfer through a material. for average temperature, and 0.1 min for time.
7.1.5 A Coolant System, to provide oscillatory heating and
5.2 The results of this test method may be used for design
cooling rates of at least 3 °C ⁄min.
purposes, service evaluation, manufacturing control, research
and development, and hazard evaluation. (See Practice E1231.) 7.1.6 Inert Nitrogen, or other low conductivity purge gas
flowing at a rate of 50 mL ⁄min (see 7.1.1).
6. Interferences NOTE 2—Helium, a commonly used purge gas, is unacceptable for this
6.1 Because the specimen size used in thermal analysis is on purpose, due to its very high thermal conductivity which results in reduced
range, precision, and accuracy.
the order of 10 mg to 100 mg, care must be taken to ensure it
is homogeneous or representative of the material, or both. 7.2 A Balance, with a range of at least 200 mg to weigh
6.2 The calculation of thermal conductivity requires knowl- specimens or containers, or both, (pans, crucibles, etc.) to
edge of this specimen geometry. This test method requires a 60.01 mg.
specific specimen size and shape. Other geometries may be 7.3 Calipers or other length-measuring device with a range
used with the appropriate modifications to the calculating greater than 4 mm, readable to 0.01 mm.
equations.
7.4 Sapphire Disk Calibration Material, 20 mg to 30 mg.
7. Apparatus 7.5 Polystyrene Thermal Conductivity Calibration Material,
7.1 A modulated temperature differential scanning calorim- of known thermal conductivity and specific heat capacity, in
eter consisting of: the shape of a right circular cylinder, 6.3 mm 6 0.2 mm in
7.1.1 A Differential Scanning Calorimetry (DSC) Test diameter and 3.5 mm 6 0.3 mm thickness.
Chamber, of (1) a furnace to provide uniform controlled 7.5.1 Polystyrene Specific Heat Capacity Reference
heating/cooling of a specimen and reference to a constant Material, composed of the same material as the thermal
temperature or at a constant rate within the applicable range of conductivity calibration material, in the shape of a right
this test method; (2) a temperature sensor (or other signal circular cylinder or disk, 6.3 mm 6 0.2 mm in diameter and
source) to provide an indication of the specimen temperature 0.4 mm 6 0.1 mm in thickness.
readable to 0.01 °C; (3) a differential sensor to detect a heat 7.6 Circular Aluminum Disk, 6.3 mm in diameter and
flow difference between the specimen and reference equivalent 0.01 mm or thinner in thickness.
to 0.001 mW; and (4) a means of sustaining a test temperature
7.7 Containers (pans, crucibles, etc.) that are inert to the
specimen and are of suitable structural shape and integrity to
4
The boldface numbers in parentheses refer to a list of references at the end of contain the specimen in accordance with the specific require-
this standard. ments of this test method.

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG6HS*07


2
'RZQORDGHGSULQWHGE\
0&7 0LQLVWHULRGD&LHQFLDH7HFQRORJLDSXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
E1952 − 23
7.8 Silicone Heat Transfer Fluid, with no thermal transi- 10.3 Determine the thermal conductivity calibration factor,
tions over the temperature range from –10 °C to 100 °C. D.
NOTE 3—Silicone oil with a viscosity of about 1 Pa·s (10 poise) has 10.3.1 Weigh the thin (0.4 mm) polystyrene (or other)
been found satisfactory for this application. calibration disk (from 7.5.1); record the mass as m1. Enter it as
7.9 While not required, users may find the following op- an experimental parameter into the apparatus calculator. En-
tional apparatus and materials useful for this determination. capsulate the thin polystyrene calibration disk in a standard
7.9.1 Polymeric Thermal Conductivity Performance aluminum sample container with lid.
Material, a right circular cylinder, 6.3 mm 6 0.2 mm in diam- 10.3.2 Place the encapsulated test specimen in the DSC on
eter and 3.5 mm 6 0.3 mm in length. the specimen sensor. Use an empty aluminum container and lid
7.9.2 Polymeric Specific Heat Capacity Reference Material, on the reference side.
composed of the same material as the thermal conductivity NOTE 5—Matching the combined weights of the reference container
standard reference material, a right circular cylinder or disk, and lid to those of the specimen container and lid within 60.1 mg
6.3 mm 6 0.2 mm in diameter and 0.4 mm 6 0.1 mm in thick- produces the best results.
ness. 10.3.3 Measure the heat capacity of the thin polystyrene
8. Sampling calibration material using the conditions of 10.2.1. Record the
specific heat capacity (cp) in units of J/(g·K).
8.1 Select two right circular cylinders, both nominally
6.3 mm in diameter. The first of these test specimens is NOTE 6—This value for the specific heat capacity of polystyrene may be
nominally 0.4 mm thick and the second is nominally 3.5 mm compared against the literature values listed in Table 1 as a performance
thick. These test specimens are most conveniently obtained by criteria test.
cutting from 0.25-in. diameter rod, a common material form. 10.3.4 Weigh the thick (3.5 mm) polystyrene calibration
NOTE 4—Other fabrication techniques, such as cutting from sheet stock
disk (from 7.5); record the mass as m2; and enter it into the
using cork borers, machining from stock, or molding may also be used. experimental parameters screen on the measuring apparatus.
8.1.1 Polish the circular end surfaces of the test specimens 10.3.5 Measure and record the diameter (d) and length (L)
smooth and parallel to within 630 µm with 600 grit emery of the polystyrene calibration test specimen.
paper. 10.3.6 Moisten the DSC sample and reference sensors with
silicone oil. Place a thin aluminum disk over each sensor.
9. Calibration Carefully place the thick sample (which has been moistened
9.1 Calibrate the temperature signal from the apparatus in with oil on the bottom side) on the aluminum disk covering the
accordance with Practice E967 using an indium reference sample sensor.
material and a heating rate of 1 °C ⁄min. NOTE 7—Ensure that silicone oil does not change the characteristics of
9.2 Calibrate the heat flow signal from the apparatus in the test specimen. It may leave a residue that must be cleaned before
accordance with Practice E968 using an indium reference alternative apparatus use. Xylene is a suitable solvent for cleaning.
material. NOTE 8—A cotton swab may be wetted with silicon oil and the pressed
between the fingers to remove any excess oil. The “moist” cotton swab
9.3 Calibrate the apparatus for heat capacity measurements may be passed once over the surface to “wet” it with the oil.
in accordance with the instructions of the manufacturer as 10.3.7 Measure the apparent heat capacity of the specimen
described in the instrument manual using isothermal tempera- in accordance with the conditions of 10.2.1. Record the
ture conditions (at the mid-point of the temperature range of apparent heat capacity (c) in the units of mJ/K.
interest), the sapphire calibration material (from 7.4) 60.5 °C
amplitude and 80 s period (12.5 mHz frequency).
10. Procedure
TABLE 1 Polystyrene Specific Heat CapacityA
10.1 Measure thermal conductivity under quasi-isothermal
Temperature Specific Heat CapacityB
conditions at an operator-selected temperature within the range (°C) (K) (J/(g • K))
from 0 °C to 90 °C. If measurements at additional temperatures 6.8 280.0 1.1326
are desired, repeat the procedure at those additional tempera- 16.8 290.0 1.1775
26.8 300.0 1.2230
tures. 36.8 310.0 1.2691
10.2 A common set of experimental conditions are used for 46.8 320.0 1.3156
50.0 323.2 1.3305
each measurement: 56.8 330.0 1.3626
10.2.1 Select the modulated mode on the DSC and record 66.8 340.0 1.4100
the heat capacity signal. Equilibrate the apparatus at the test 76.8 350.0 1.4577
86.8 360.0 1.5056
temperature selected by the operator. Modulate the temperature 96.8 370.0 1.5539
with an amplitude of 60.5 °C and a period (P) of 80 s A
Gaur, U., and Wunderlich, B., Journal of Physical and Chemical Reference Data,
(12.5 mHz). (See Note 5.) After 15 min equilibration time, Vol 11, No. 2, 1982, p. 313.
B
record the average test temperature (T) and the specific heat The values in this table were determined under special highly accurate test
conditions that are not attainable by or applicable to this test method. The actual
capacity (cp) or apparent heat capacity (c) as called for in the precision of this test method is given in Section 13.
appropriate section.

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG6HS*07


3
'RZQORDGHGSULQWHGE\
0&7 0LQLVWHULRGD&LHQFLDH7HFQRORJLDSXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
E1952 − 23
10.3.8 Using the values of P (from 10.2.1), cp (from 10.3.3); 10.4.9 Using the value for P (from 10.2.1), cp (from 10.4.4),
and m, L, and d (from 10.3.4 and 10.3.5), calculate the and M, L, and d (from 10.4.6 and 10.4.7), calculate the
observed thermal conductivity (λo) for polystyrene using Eq 1 observed thermal conductivity (λo) for the test specimen using
(see 11.1). Eq 1.
NOTE 9—An example calculation is presented in 11.5.1. NOTE 13—An example calculation is presented in 11.5.1.
10.3.9 Determine the value for thermal conductivity of 10.4.10 Using the value for λo (from 10.4.9) and the value of
polystyrene (λr) for the corresponding temperature (T) (from D (from 10.3.10), calculate the value for λ of the test specimen
10.2.1) from Table 2, linearly interpolating between values if using Eq 3.
necessary. NOTE 14—An example calculation is presented in 11.5.3.
10.3.10 Using the values for λo from 10.3.8 and the value
for λr from 10.3.9, calculate the thermal conductivity calibra- 10.4.11 Using the value for λ (from 10.4.10), the value of cp
tion constant (D) for temperature T using Eq 2. (from 10.4.4), and the values of m and L (from 10.4.6 and
10.4.7), calculate the thermal diffusivity (a) for the test
NOTE 10—An example calculation is presented in 11.5.2. specimen using Eq 4.
NOTE 11—Typical values for D range from approximately
10 mW ⁄(m·K) to 50 mW ⁄(m·K). NOTE 15—An example calculation is presented in 11.5.4.
10.4 Determine the thermal conductivity of the test speci- 10.4.12 Report values for thermal conductivity (λ) and
men. thermal diffusivity (a) at temperature (T) as the mean values of
10.4.1 Weigh the thin (0.4 mm) test specimen and record the duplicate determinations. Also report the range of measure-
mass as m3. Enter this value into the experimental parameters ments between the high and the low value.
screen of the apparatus. 10.5 Performance Criteria for Test Apparatus:
10.4.2 Encapsulate the thin specimen in a standard alumi- 10.5.1 The apparatus used for this test method is considered
num sample container with lid. adequate if the value for thermal conductivity for a suitable
10.4.3 Place the encapsulated test specimen on the DSC reference material is within 610 %.
sample sensor. Place an empty aluminum container and lid on 10.5.2 A suitable reference material is described in Section
the DSC reference sensor. 12.
NOTE 12—Matching the weights of the reference container and lid to
the specimen container and lid within 60.1 mg produces the best results. 11. Calculation
10.4.4 Measure the specific heat capacity of the thin test 11.1 Determine the observed thermal conductivity (λo) in
specimen using the conditions in 10.2.1. Record the specific accordance with Eq 1:
heat capacity (cp) in units J/(g·K). λ o 5 ~ 8 L c 2! / ~ c p m d 2 P ! (1)
10.4.5 Weigh the thick test specimen, recording its mass as
m4. where:
10.4.6 Measure and record the diameter (d) and length (L) λo = observed thermal conductivity (W/(K·m)),
of the test specimen. L = specimen length (mm),
10.4.7 Place a small drop of silicone oil on the DSC sample c = apparent heat capacity (mJ/K),
and reference sensors. Place a thin aluminum disk over each cp = specific heat capacity (J/(g·K),
drop of oil. Carefully position the thick test specimen (which m = thick specimen mass (mg),
has been wetted with oil on the bottom side) on the aluminum d = thick specimen diameter (mm), and
P = period (s).
disk covering the DSC sample sensor (see Note 6 and Note 7).
NOTE 16—When performing these calculations, retain all available
10.4.8 Measure the apparent heat capacity of the test speci- decimal places in the measured values and in intermediate values. The
men in accordance with the conditions in 10.2.1. Record the final result should be rounded to two significant places in the standard
apparent heat capacity (c) in units of mJ/K. deviation, as indicated in Section 13.
11.2 Calculate the thermal conductivity calibration constant
TABLE 2 Polystyrene Thermal ConductivityA (D) in W/(m·K) using Eq 2:
Temperature Thermal ConductivityB 1
(°C) (K) (W/(m·K)) D 5 ~ λ o λ r! 2 2 λ r (2)
–13 260 0.1480
0 273 0.1506 where:
7 280 0.1514
20 293 0.1529
λr = reference thermal conductivity (W/(m·K))
27 300 0.1539 11.3 Calculate the test specimen thermal conductivity (λ)
47 320 0.1562
67 340 0.1582 using Eq 3:
87 360 0.1605
97 370 0.1616 @λo 2 2 D1 ~ λ o 2 2 4 D λ o ! 2 #
1

λ5 (3)
A
Ho, C. Y., Desai, P. D., Wu, K. T., Havill, T. N., and Lee, T. Y., NBS Publication 2
GCR-77-83, 1977.
B
The values in this table were determined under special highly accurate steady-
11.4 Calculate thermal diffusivity (a) using Eq 4 (X1).
state conditions, which are not attainable by or applicable to this test method. The a 5 ~π λ d2 L!/~4 cp m! (4)
actual precision of this test method is given in Section 13.
11.5 Example Calculations:

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG6HS*07


4
'RZQORDGHGSULQWHGE\
0&7 0LQLVWHULRGD&LHQFLDH7HFQRORJLDSXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
E1952 − 23
11.5.1 If the following set of values were measured for a TABLE 3 Poly(methyl methacrylate) Specific Heat Capacity and
polystyrene thermal conductivity calibration material, the Thermal ConductivityA,B
Temperature Specific Heat Thermal
value for λo from Eq 1 becomes: Capacity ConductivityC
(°C) (K) (J/g·K)) (W/(m·K))
L = 3.45 mm, 7.2 280.0 1.2951 0.189
c = 61.65 mJ/K, 17.2 290.0 1.3353 0.190
cp = 1.20 J/(g·K), 27.2 300.0 1.3756 0.191
37.2 310.0 1.4158 0.193
m = 127.0 mg, 47.2 320.0 1.4561 0.194
d = 6.73 mm, and A
Gaur, U., Lau., S. F., Wunderlich, B. B., and Wunderlich, B., Journal of Physical
P = 80 s. and Chemical Reference Data, Vol 11, No. 4, 1982, p. 1065.
B
The values in this table were determined under special highly accurate steady-
then: state conditions, which are not attainable by or applicable to this test method. The
~ 8 × 3.45 mm × 61.65 mJ/K × 61.65 mJ/K ! actual precision of this test method is given in Section 13.
C
λo 5 Tye, R. P., and Salmon, D. R., “Thermal Conductivity Certified Reference
~ 1.20 J/ ~ g·K ! × 127.0 mg × 6.73 mm × 6.73 mm × 80 s ! Materials: Pyrex and Polymethylmethacrylate,” Thermal Conductivity 26: Thermal
Expansion 14, R. B. Dinwiddie and R. Mannello (eds), DEStech Publications,
recognizing that: Lancaster, PA, 2005, pp. 437–451.

1 W = 1 J/s
then:
13. Precision and Bias5
λo = 0.1900 W/(m·K) 13.1 An interlaboratory study (ILS) was conducted in 2000
11.5.2 If the thermal conductivity value of involving participation by 14 laboratories. Polystyrene (PS)
λr = 0.1552 W ⁄(m·K) is taken from Table 2 at 38.5 °C, and the was used as a calibration material. Each laboratory character-
value for λo is taken from 11.5.1, then Eq 2 is calculated to be: ized a polymethylmethacrylate (PMMA) certified thermal
conductivity performance standard obtained from the National
D = (0.1900 W/(m·K) × 0.1552 W/(m·K))0.5 – 0.1552 Physical Laboratory, the UK national standards laboratory. The
W/(m·K) results of this interlaboratory test are on file at ASTM Head-
= (0.1717 – 0.1552) W/(m·K) quarters
D = 0.0165 W/(m·K).
13.2 Precision:
11.5.3 If a value of the observed thermal conductivity for a 13.2.1 Within laboratory variability may be described using
test specimen is found to be: the repeatability value (r), obtained by multiplying the repeat-
ability standard deviation by 2.8. The repeatability value
λo = 0.2821 W/(m·K), then from Eq 3: estimates the 95 % confidence limit.
λ = [0.2821 W/(m·K) – (2 × 0.0165 W/(m·K)) + ({0.2821 13.2.1.1 Thermal conductivity repeatability (relative) stan-
W/(m·K) × 0.2821 W/(m·K)} – {4 × 0.0165 W/(m·K) × dard deviation values of 13 % and 8.7 % were obtained for PS
0.2821 W/(m·K)})0.5] / 2 and the PMMA performance standard, respectively. The pooled
λ = {0.2821 – 0.0330 + (0.07958 – 0.01862)0.5] W/(m·K) /
repeatability (relative) standard deviation for these two values
2
is 12 %.
λ = [0.2491 + 0.2469] W/(m·K) / 2
λ = 0.248 W/(m·K). 13.2.1.2 Specific heat capacity repeatability (relative) stan-
dard deviation values of 3.0 % and 1.9 % were obtained for PS
11.5.4 From Eq 4: and PMMA, respectively. The pooled repeatability (relative)
a 5 ~ 3.141 × 0.248 W/ ~ m·K ! × 6.73 mm × 6.73 mm × 3.45 mm! standard deviation for these three values is 2.7 %.
(5) 13.2.1.3 From the principle of propagation of uncertainties,
~ 4 × 1.20 J/ ~ g·K ! × 127.0 mg!
thermal diffusivity repeatability (relative) standard deviation is
where: estimated to be 12 %.
a = 0.200 mm2/s 13.2.2 Between laboratory variability may be described
using the reproducibility value (R) obtained by multiplying the
12. Performance Criteria reproducibility standard deviation by 2.8. The reproducibility
value estimates the 95 % confidence limit.
12.1 Poly(methyl methacrylate) or other material of known 13.2.2.1 Thermal conductivity reproducibility (relative)
thermal conductivity may be used to verify performance in this standard deviation values of 27 % and 10 % were obtained for
application. Specific heat capacity and thermal conductivity PS and PMMA performance standard, respectively. The pooled
values for a poly(methyl methacrylate) reference material (relative) standard deviation for these two values is 23 %.
(7.9.1 and 7.9.2) are presented in Table 3. 13.2.2.2 Specific heat capacity reproducibility (relative)
NOTE 17—Poly(methyl methacrylate), polyethylene and polyamide standard deviation values of 9.1 % and 5.8 % were obtained for
samples of known thermal conductivity are available from the National
Physical Laboratory, Teddington, Middlesex, TW11 0LW, England. Also
samples of borosilicate glass reference material are available from the 5
Supporting data have been filed at ASTM International Headquarters and may
Institute of Reference Materials and Measurements, Commission of the be obtained by requesting Research Report RR:E37-1026. Contact ASTM Customer
European Community, Retiessweg 2410, Geel, Belgium. Service at [email protected].

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG6HS*07


5
'RZQORDGHGSULQWHGE\
0&7 0LQLVWHULRGD&LHQFLDH7HFQRORJLDSXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
E1952 − 23
PS and PMMA, respectively. The pooled repeatability (rela- 13.3.5 The weighted bias for these two determinations of
tive) standard deviation of these three values is 8.2 %. specific heat capacity is 6.8 %.
13.2.2.3 From the principle of propagation of uncertainties,
thermal diffusivity reproducibility (relative) standard deviation 14. Report
is estimated to be 24 %.
14.1 Report the following information:
13.3 Bias:
14.1.1 Complete identification and description of the mate-
13.3.1 An estimation of bias is obtained by comparing the
rial tested, including source, manufacturer code, and any
mean values obtained for each performance standard to its
thermal or mechanical pretreatment.
certified or literature value. That is, bias = (mean value) –
(certified value). 14.1.2 Description of the instrumentation used for the test,
13.3.2 The mean thermal conductivity value for the PMMA such as manufacturer and model number.
performance standard at 47 °C is 0.185 W m-1K-1 with 28 de- 14.1.3 Description of calibration procedure, including val-
grees of freedom. The certified thermal conductivity value at ues for calibration constant(s) such as D.
this same temperature is 0.194 W m-1 K-1 (3). This represents 14.1.4 Test specimen dimensions, including diameter,
a bias of –0.009 W m-1 K-1 or –4.7 %. As this value is less than length, and mass.
the repeatability standard deviation, no bias is indicated. 14.1.5 Mean thermal conductivity (W/(m·K)) and thermal
13.3.3 The mean specific heat capacity value for PS at 47 °C diffusivity (mm2/s) at their measurement temperature.
is 1.403 J g-1 K-1 with 52 degrees of freedom. The literature
14.1.6 The specific dated version of this method used.
specific heat capacity value at this same temperature is
1.316 J g-1 K-1 (4). This represents a bias of 0.087 J g-1 K-1 or
6.6 %. 15. Keywords
13.3.4 The mean specific heat capacity value for PMMA at 15.1 ceramics; differential scanning calorimetry (DSC);
47 °C is 1.538 J g-1K-1 with 24 degrees of freedom. The glasses; modulated differential scanning calorimetry (MDSC);
literature specific heat value at this same temperature is modulated temperature differential scanning calorimetry; poly-
1.436 J g-1 K-1 (5). This represents a bias of 0.102 J g-1 K-1 or mers; thermal analysis; thermal conductivity; thermal diffusiv-
7.1 %. ity

APPENDIX

(Nonmandatory Information)

X1. DETERMINATION OF THERMAL DIFFUSIVITY

X1.1 Thermal diffusivity (a) of a material is related to its ρ 5 m/V (X1.2)


thermal conductivity (λ), a geometry specific property, through
the material’s specific heat capacity (cp), and density (ρ) by the X1.3 For a right cylinder, the volume is given by Eq X1.3:
Eq X1.1: V 5 π d 2 L/4 (X1.3)
a 5 λ/ ~ c p ρ ! (X1.1) X1.4 Substituting Eq X1.2 and Eq X1.3 into Eq X1.1 yields
Eq X1.4, the working Eq 4 of 11.4:
X1.2 By definition, density is mass (m) per unit volume (V)
as in Eq X1.2: a 5 ~π λ d2 L!/~4 Cp m! (X1.4)

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG6HS*07


6
'RZQORDGHGSULQWHGE\
0&7 0LQLVWHULRGD&LHQFLDH7HFQRORJLDSXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG
E1952 − 23
REFERENCES

(1) Marcus, S. M., and Blaine, R. L., Thermochimica Acta, Vol 243, 1994, TW11 0LW, England, 1993.
pp. 231–239. (4) Gaur, U., and Wunderlich, B., Journal of Physical and Chemical
(2) Verdonck, E., Blaine, R. L., and Dreezer, G., Thermal Conductivity Reference Data, Vol 11, No. 2, 1982, p. 313.
Measurements of Conducive Epoxy Adhesives by MDSC, Proceed- (5) Gaur, U., Lau, S. F., Wunderlich, B. B., and Wunderlich, B., Journal
ings of the 31st Conference of the North American Thermal Analysis of Physical and Chemical Reference Data, Vol 11, No. 4, 1982, p.
Society, 2003. 1065.
(3) Salmon, D. R., National Physical Laboratory, Teddington, Middlesex,

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or [email protected] (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/

&RS\ULJKWE\$670,QW O DOOULJKWVUHVHUYHG :HG6HS*07


7
'RZQORDGHGSULQWHGE\
0&7 0LQLVWHULRGD&LHQFLDH7HFQRORJLDSXUVXDQWWR/LFHQVH$JUHHPHQW1RIXUWKHUUHSURGXFWLRQVDXWKRUL]HG

You might also like