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ASTM E968-99

(Practice)

Standard Practice for Heat Flow Calibration of Differential Scanning Calorimeters

Standard Practice for Heat Flow Calibration of Differential Scanning Calorimeters

SCOPE
1.1 This practice covers the heat flow calibration of differential scanning calorimeters over the temperature range from -130°C to +800°C.  
1.2 This practice may involve the use of hazardous materials, operations, and equipment. It is the responsibility of whoever uses this standard to establish appropriate safety practices, and to determine the applicability of regulatory limitations prior to use.  
1.3 Values given in SI units are to be regarded as the standard. Where appropriate, traditional values and units may appear in parenthesis following the SI designations.  
1.4 Computer or electronic based instruments, techniques or data manipulation equivalent to this practice may also be used.  
1.5 This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. See also Section 6.

General Information

Status
Historical
Publication Date
09-Mar-1999
ICS
17.200.10 - Heat. Calorimetry
Technical Committee
E37 - Thermal Measurements
Drafting Committee
E37.01 - Calorimetry and Mass Loss
Current Stage
Ref Project

Relations

Replaced By
ASTM E968-02 - Standard Practice for Heat Flow Calibration of Differential Scanning Calorimeters
Effective Date
10-Mar-2002

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ASTM E968-99 - Standard Practice for Heat Flow Calibration of Differential Scanning CalorimetersASTM E968-99 - Standard Practice for Heat Flow Calibration of Differential Scanning Calorimeters
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ASTM E968-99 - Standard Practice for Heat Flow Calibration of Differential Scanning Calorimeters
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Standards Content (Sample)

Designation: E 968 – 99
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Practice for
1
Heat Flow Calibration of Differential Scanning Calorimeters
This standard is issued under the fixed designation E 968; 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 (e) indicates an editorial change since the last revision or reapproval.
A
TABLE 1 Sapphire (a −Al O ) Specific Heat Capacity
1. Scope 2 3
Temperature, Specific Heat Specific Heat
1.1 This practice covers the heat flow calibration of differ-
Temperature, K
K Capacity, J/g·K Capacity, J/g·K
ential scanning calorimeters over the temperature range
140 0.2739 630 1.1184
from − 130°C to + 800°C.
150 3.3133 640 1.1228
1.2 Values given in SI units are to be regarded as the
160 0.3523 650 1.1272
170 0.3912 660 1.1313
standard.
180 0.4290 670 1.1353
1.3 Computer or electronic based instruments, techniques or
190 0.4659 680 1.1393
data manipulation equivalent to this practice may also be used.
200 0.5014 690 1.1431
210 0.5356 700 1.1467
1.4 This standard does not purport to address all of the
220 0.5684 710 1.1503
safety concerns, if any, associated with its use. It is the
230 0.6045 720 1.1538
responsibility of whoever uses this standard to consult and
240 0.6294 730 1.1572
250 0.6578 740 1.1604
establish appropriate safety and health practices and deter-
260 0.6846 750 1.1604
mine the applicability of regulatory limitations prior to use.
270 0.7102 760 1.1667
See also Section 7.
280 0.7344 770 1.1698
290 0.7574 780 1.1727
300 0.7792 790 1.1756
2. Referenced Documents
310 0.7999 800 1.1784
2.1 ASTM Standards:
320 0.8194 810 1.1811
2
330 0.8380 820 1.1839
E 473 Terminology Relating to Thermal Analysis
340 0.8555 830 1.1864
E 793 Test Method for Heats of Fusion and Crystallization
350 0.8721 840 1.1890
2
by Differential Scanning Calorimetry
360 0.8878 850 1.1914
370 0.9027 860 1.1939
E 967 Practice for Temperature Calibration of Differential
380 0.9168 870 1.1962
Scanning Calorimeters and Differential Thermal Analyz-
390 0.9302 880 1.1986
2
ers
400 0.9429 890 1.2008
410 0.9550 900 1.2031
420 0.9665 910 1.2053
3. Terminology
430 0.9775 920 1.2074
3.1 Definitions—Specific technical terms used in this prac-
440 0.9879 930 1.2095
450 0.9978 940 1.2115
tice are in accordance with Terminologies E 474 and E 1142.
460 1.0073 950 1.2135
3.2 Definitions of Terms Specific to This Standard:
470 1.0164 960 1.2153
3.2.1 coeffıcient of variation, n—a measure of relative 480 1.0250 970 1.2174
490 1.0332 980 1.2194
precision calculated as the standard deviation of a series of
500 1.0411 990 1.2212
values divided by their average. It is usually multiplied by 100
510 1.0436 1000 1.2230
and expressed as a percentage.
520 1.0379 1010 1.2249
530 1.0628 1020 1.2266
NOTE 1—The term quantitative differential thermal analysis refers to
540 1.0674 1030 1.2284
differential thermal analyzers that are designed to obtain quantitative or 550 1.0758 1040 1.2301
560 1.0819 1050 1.2318
semiquantitative heat flow results. This procedure may also be used to
570 1.0877 1060 1.2335
calibrate such apparatus.
580 1.0934 1070 1.2351
590 1.0988 1080 1.2364
4. Summary of Practice
600 1.1039 1090 1.2383
610 1.1090 1100 1.2400
4.1 Differential scanning calorimeters measure heat flow
620 1.1138
A
Archer, D.G., J. Phys. Chem. Ref. Data, Vol 22, No. 8, pp. 1441–1453 (1993).
1
This practice is under the jurisdiction of ASTM Committee E-37 on Thermal
Measurements and is the direct responsibility of Subcommittee E37.01 on Thermal
(power) into or out of a test specimen and provide a signal
Analysis Methods.
output proportional to this measurement. This signal often is
Current edition approved March 10, 1999. Published May 1999. Originally
recorded as a function of a second signal proportional to
published as E 968 – 83. Last previous edition E 968 – 83 (1993).
2
Annual Book of ASTM Standards, Vol 14.02. temperature or time. If this heat flow signal is integrated over
1

---------------------- Page: 1 ----------------------
E 968
time, the resultant value is proportional to energy (or enthalpy 6.1.1.4 A means of sustaining a test chamber environment,
or heat). To obtain the desired energy information, the observed of an inert purge gas at a purge gas rate of 10 to 100 mL/min
instrument response (such as the area under the curve scribed) 6 5 mL/min.
must be multiplied by a proportionality constant that converts
NOTE 3—Typically, 99.9+ % pure nitrogen, argon or helium are em-
the units of instrument output into the desired energy units.
ployed when oxidation in air is a concern. Unless effects of moisture are
This proportionality constant is called the instrument calibra-
to be studied, use of dry purge gas is recommended and is essentia
...

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