Designation: E2253 − 16

Standard Test Method for

Temperature and Enthalpy Measurement Validation of
Differential Scanning Calorimeters1
This standard is issued under the fixed designation E2253; 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* E1860 Test Method for Elapsed Time Calibration of Ther-

1.1 This test method provides procedures for validating mal Analyzers
temperature and enthalpy measurements of differential scan- E1970 Practice for Statistical Treatment of Thermoanalytical
ning calorimeters (DSC) and analytical methods based upon Data
the measurement of temperature or enthalpy (or heat), or both, E2161 Terminology Relating to Performance Validation in
by DSC. Performance parameters determined include tempera- Thermal Analysis and Rheology
ture and calorimetric repeatability (precision), detection limit, 2.2 FDA Publications:3
quantitation limit, linearity, and bias. This test method is Q2B Validation of Analytical Procedures Methodology, 62
applicable to exothermic events. FR 27464, May 19, 1997
1.2 Validation of apparatus performance and analytical 3. Terminology
methods is requested or required for quality initiatives or where 3.1 Technical terms used in this standard are defined in
results may be used for legal purposes. Practice E177 and in Terminologies E473, E1142, and E2161
1.3 The values stated in SI units are to regarded as standard. including analyte, detection limit, differential scanning
No other units of measurement are included in this standard. calorimetry, enthalpy, extrapolated onset value (temperature),
1.4 This standard does not purport to address all of the linearity, mean, precision, quantitation limit, relative standard
safety concerns, if any, associated with its use. It is the deviation, repeatability, standard deviation, thermal curve, and
responsibility of the user of this standard to establish appro- validation.
priate safety and health practices and determine the applica- 4. Summary of Test Method
bility of regulatory limitations prior to use.
4.1 Temperature and time are the primary independent
2. Referenced Documents parameters and heat flow is the primary dependent experimen-
2.1 ASTM Standards:2 tal parameter provided by DSC. Integration of heat flow, as a
E177 Practice for Use of the Terms Precision and Bias in function of time, yields enthalpy (heat).
ASTM Test Methods 4.1.1 Time, measured by the DSC apparatus, shall conform
E473 Terminology Relating to Thermal Analysis and Rhe- to better than 0.1 % verified by Test Method E1860 and
ology reported.
E967 Test Method for Temperature Calibration of Differen- 4.1.2 Temperature is directly measured by a temperature
tial Scanning Calorimeters and Differential Thermal Ana- sensor that is an integral part of the differential scanning
lyzers calorimetry apparatus.
E968 Practice for Heat Flow Calibration of Differential 4.1.3 Heat flow, a measured value, is validated by its
Scanning Calorimeters integration over time to obtain the desired calorimetric (en-
E1142 Terminology Relating to Thermophysical Properties thalpic) information of interest.
4.2 Calorimetric validation of a differential scanning calo-
1
rimetric apparatus at a single temperature is performed using
This test method is under the jurisdiction of ASTM Committee E37 on Thermal
Measurements and is the direct responsibility of Subcommittee E37.10 on the indium metal melt as an analyte.
Fundamental, Statistical and Mechanical Properties.
4.3 Validation of a DSC method based upon enthalpic
Current edition approved April 1, 2016. Published April 2016. Originally
approved in 2003. Last previous edition approved in 2011 as E2253 – 11. DOI: measurement may be performed using the test specimen as the
10.1520/E2253-16. analyte.
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 Available from Food and Drug Administration (FDA), 10903 New Hampshire
the ASTM website. Ave., Silver Spring, MD 20993-0002, http://www.fda.gov.

*A Summary of Changes section appears at the end of this standard

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

1
 E2253 − 16
4.4 The enthalpy of three (or more) specimens (nominally 6.1.1.4 A means of sustaining a test chamber environment
representing the maximum, midpoint and minimum of the of an inert purge gas at a rate of 10 to 50 mL/min 6 10 %.
range of the test method) are measured in triplicate (or more). NOTE 2—Typically, 99+ % pure nitrogen (or other inert gas, such as
A fourth blank specimen, containing no analyte, is also argon or helium) is employed when oxidation in air is a concern. Unless
measured in triplicate. the effects of moisture are to be studied, the use of a dry purge gas is
recommended, especially for operation at subambient temperatures.
NOTE 1—Repeatability is determined by performing a sufficient number
of determinations to calculate statistically valid estimates of the standard 6.1.2 Temperature Controller, capable of executing a spe-
deviation or relative standard deviation of the measurement. cific temperature program by operating the furnace(s) between
4.4.1 Calorimetric linearity and bias are determined from selected temperature limits at a rate of temperature change
the best-fit (linear regression) straight-line correlation of the constant to 61 % or at an isothermal temperature constant to
results from measurements of the three (or more) specimens. 60.5°C.
4.4.2 Calorimetric detection limit and quantitation limit are 6.1.3 Data Collection Device, to provide a means of
determined from the standard deviation of the blank determi- acquiring, storing, and displaying measured or calculated
nation. signals, or both. The minimum output signals required for
4.4.3 Calorimetric repeatability is determined from the re- differential scanning calorimetry are heat flow, temperature,
peatability measurement of the three (or more) specimens. and time.
6.1.4 Containers, (pans, crucibles, vials, lids, closures,
4.5 The temperature validation of a differential scanning seals, etc.) that are inert to the specimen and reference
calorimetric apparatus is performed at three temperatures using materials and that are of suitable structural shape and integrity
indium, bismuth, and zinc metal melts as an analyte (see to contain the specimen and reference in accordance with the
Section 7). specific requirements of the test method.
4.5.1 The melting temperature of three (or more) materials
representing the maximum, midpoint, and minimum of the 6.2 Balance, of 100 mg or greater capacity to weigh
temperature range of the test method are measured in triplicate specimens and containers to 61 µg.
(or more) (see Note 1). NOTE 3—A balance of this high precision is required so that weighing
imprecision is not part of the overall method imprecision.
4.5.2 Temperature linearity and bias are determined from
the best-fit (linear regression) straight-line correlation of the 7. Reagents and Materials
results from the temperature measurements at the three (or
more) temperatures. 7.1 Indium (In) Metal, 99.99+ % purity, preferably a certi-
4.5.3 Temperature repeatability, detection limit and quanti- fied reference material for which the melting temperature and
tation limit are determined from the standard deviation of the enthalpy of fusion are known.
replicate temperature measurements. 7.2 Bismuth (Bi) Metal, 99.99+ % purity, preferably a cer-
tified reference material for which the melting temperature is
5. Significance and Use known.
5.1 This test method may be used to determine and validate 7.3 Zinc (Zn) Metal, 99.99+ % purity, preferably a certified
the performance of a particular DSC apparatus. reference material for which the melting temperature is known.
5.2 This test method may be used to determine and validate
8. Calibration and Standardization
the performance of a particular method based upon a DSC
temperature and enthalpic measurement, or both. 8.1 After turning the power on, allow the instrument to
equilibrate for at least one hour prior to any measurements.
5.3 This test method may be used to determine the repeat-
ability of a particular apparatus, operator, or laboratory. 8.2 Perform any cleaning and calibration procedures de-
scribed by the manufacturer in the apparatus Operator’s
5.4 This test method may be used for specification and
Manual.
regulatory compliance purposes.
8.3 If not previously established, perform temperature and
6. Apparatus heat flow calibrations according to Test Method E967 and
Practice E968 respectively, using the same purge gas, purge
6.1 Differential Scanning Calorimeter (DSC)—The essential
gas flow rate and heating rate (here 10°C/min) to be used for
instrumentation required to provide the minimum differential
validation experiments.
scanning calorimetric capability for this test method includes:
6.1.1 DSC Test Chamber, composed of: 8.4 If not previously established, obtain the instrument’s
6.1.1.1 Furnace(s), to provide uniform controlled heating or elapsed time conformance using Test Method E1860.
cooling of a specimen and reference to a constant temperature
or at a constant rate within the applicable temperature range of 9. Procedure for Determining Calorimetric Repeatability,
the test method. Detection Limit, Quantitation Limit, Linearity, and Bias
6.1.1.2 Temperature Sensor, to provide an indication of the 9.1 This process involves characterizing, in triplicate, a
specimen temperature to readability required. blank and three (or more) test specimens taken to represent the
6.1.1.3 Differential Sensor, to detect a heat flow difference low, medium and high extremes of the range over which
between the specimen and reference. performance is to be validated.

2
 E2253 − 16
NOTE 4—The details of this procedure are written using indium as an these two points as T1 and T2. Construct a linear baseline
analyte. For validation of an enthalpic method, test specimens represent- between the two points (see Fig. 1).
ing the range of that method shall be used, and steps 9.2 to 9.7 replaced
with the enthalpic method procedure. 9.9 Integrate, as a function of time, the heat flow described
9.2 Prepare three (or more) indium test specimens covering by the constructed baseline and the melting endotherm. Record
the enthalpy or mass range of the tests. Nominal mass values this value as enthalpy (∆Qmax(1), in mJ).
might be 1, 10, and 20 mg. Measure the mass of each of these 9.10 Repeat steps 9.3 through 9.9 for the medium mass test
specimens to the nearest 1 µg and record as Mmin, Mmid, and specimen from step 9.2. Use the same integration limits (T1 and
Mmax. Enclose each test specimen within clean specimen T2) determined in step 9.8. Record this value as enthalpy
containers and lids. Also prepare a blank specimen that (∆Qmid(1) , in mJ).
contains no analyte but otherwise is similar to the specimens NOTE 7—Loading and unloading of the specimen is required to
prepared above. determine analytical repeatability. If only instrumental repeatability is
NOTE 5—Most thermoanalytical methods cover 1.5 to 2 decades of being determined, the specimen may be left in place between determina-
range. The mass values selected should be approximately equally distrib- tions.
uted over the anticipated range. Other masses and mass ranges may be
used but shall be reported. 9.11 Repeat steps 9.3 through 9.9 for the small mass test
specimen from step 9.2. Use the same integration limits (T1 and
9.3 Load the largest specimen into the instrument chamber,
T2) determined in step 9.8. Record this value as enthalpy
purge the chamber with dry nitrogen (or other inert gas) at a
(∆Qmin(1), in mJ).
flow rate of 10 to 50 mL/min 6 10 % throughout the
experiment. An empty sample specimen container is loaded in 9.12 Repeat steps 9.3 through 9.9 for the blank test speci-
the reference position. men from step 9.2. Use the same integration limits (T1 and T2)
determined in step 9.8 (see Fig. 2). Record this value as
9.4 Erase any thermal history in the test specimen by
enthalpy (∆Qo(1), in mJ).
heating the specimen to 180°C, then cool at 5°C/min to 120°C.
NOTE 8—Observe and record the sign of the value for ∆ Qo. It may be
The thermal curve need not be recorded. positive or negative.
9.5 Equilibrate at 120°C for one minute. 9.13 Repeat steps 9.5 through 9.9 two more times for the
9.6 Heat the test specimen at 10°C/min through the indium large mass specimen. Remove the specimen from the DSC
melting transition to 180°C and record the thermal curve. sample chamber and reload it between each determination.
NOTE 6—Other heating rates may be used but shall be reported. Record these values as enthalpy (∆Qmax(2) and ∆Qmax(3), in
9.7 Cool the test specimen to 120°C at 5°C/min, then cool to mJ).
ambient temperature at any convenient rate. The thermal curve 9.14 Repeat steps 9.5 through 9.9 two more times for the
need not be recorded. medium mass specimen. Remove the specimen from the DSC
9.8 Construct a baseline for the melting endotherm by sample chamber and reload it between each determination.
selecting a point on the curve immediately before and another Record these values as enthalpy (∆Qmid(2) and ∆Qmid(3), in
immediately after the endotherm. Record the temperatures of mJ).

FIG. 1 Integration of Large Indium Melting Endotherm

3
 E2253 − 16

FIG. 2 Integration of Baseline

9.15 Repeat steps 9.5 through 9.9 two more times for the 9.22 Compare the slope (mean enthalpy of fusion) from step
low mass specimen. Remove the specimen from the DSC 9.20 to the accepted reference value for enthalpy of fusion as
sample chamber and reload it between each determination. in calculation of Eq 7 (see Practice E968). Report this
Record these values as enthalpy (∆Qmin(2) and ∆Qmin(3), in percentage value as the Calorimetric Bias (Bias).
mJ).
10. Procedure for Determining Temperature
9.16 Repeat steps 9.5 through 9.9 two more times for the
Repeatability, Detection Limit, Quantitation Limit,
blank specimen. Remove the specimen from the DSC sample
Linearity, and Bias
chamber and reload it between each determination. Record
these values as enthalpy (∆Qo(2) and ∆Qo(3), in mJ). 10.1 This process involves characterizing, in triplicate, three
(or more) test materials taken to represent the low, medium,
9.17 Calculate the mean (Q), standard deviation (s) and
and high extremes of the range over which performance is to be
relative standard deviation (RSD) for the enthalpy from the
validated.
replicate determinations made on each of the three mass
specimens (see Practice E1970). Record these values as Qmax, NOTE 10—The details of this procedure are written using indium,
Qmid, Qmin, smax, smid, smin, and RSDmax, RSDmid, and RSDmin, bismuth, and zinc as analytes. For validation of other temperature ranges,
test specimens representing the range of that method shall be used and
respectively. Calculate the mean and standard deviation for the 10.2 to 10.26 replaced with the temperature method procedure. Materials
enthalpy determination of the blank. Record these values as Qo with sufficiently high temperature accuracy are presented in Table 1. The
and so respectively. mass of reference materials shall be selected to approximate equal
enthalpies. Where practical, analytes with approximately equality tem-
9.18 Using the standard deviation for the enthalpy of the perature spaced transitions shall be used.
blank (so) from step 9.17, determine the instrument detection
limit (DL) and quantitation limit (QL) as in calculations 11.2 10.2 Prepare three (or more) indium test specimens.
and 11.3. Report DL and QL. 10.2.1 Into a tared specimen container, weigh a single 9 to
11 mg of the indium reference material. Seal the specimen
9.19 Calculate the pooled relative standard deviation for the container.
enthalpy of fusion from the RSDmax, RSDmid, and RSDmin,
obtained in step 9.17 (see Practice E1970). Report this value as
the Calorimetric Repeatability value (r). TABLE 1 Melting TemperaturesA
9.20 Using the three (or more) mass values from step 9.2 as Metal Symbol
Melting Temperature,
the independent (X) values and the three (or more) mean °C
Indium In 156.598
enthalpy values from step 9.17 as the dependent (Y) values, Tin Sn 231.928
determine the least square (linear regression) best fit values for Bismuth Bi 271.442
the slope (m) in mJ mg-1, and intercept (b) in mJ (see Practice Lead Pb 327.502
Zinc Zn 419.527
E1970). Aluminum Al 660.32B
NOTE 9—The units of mJ mg-1 for slope are equivalent to the units of A
Mangum, B.W., Furukawa, G.T., “Guidelines for Realizing the International
J g-1. Practical Temperature Scale of 1990 (ITS-90)”, United States National Institute of
9.21 Calculate the Percent Linearity (L) of the enthalpy of Technology (NIST) Technical Note 1265, 1990.
B
Should aluminum be used as a reference material, specimen containers other
fusion data from the values in step 9.20 and the calculation of than aluminum shall be used for all test materials.
Eq 5.

4
 E2253 − 16
10.2.2 Repeat 10.2.1 for two additional indium test speci- 10.9 Display the thermal curve for the melting endotherm
mens. with heat flow on the ordinate (Y-axis) and specimen tempera-
ture on the abscissa (X-axis). Determine the extrapolated onset
NOTE 11—The test 10 mg specimen from 9.2 may be used for this
purpose. temperature for the indium melting endotherm as T(In1) to two
places to the right of the decimal point.
10.3 Prepare three (or more) bismuth test specimens.
10.3.1 Into a tared specimen container, weigh a single 4.8 to 10.9.1 Construct a baseline by connecting a straight line
5.8 mg of the bismuth reference material. Seal the specimen from a point on the thermal curve immediately before and
container. another immediately after the melting endotherm.
10.3.2 Repeat 10.3 for two additional bismuth test speci- 10.9.2 Construct a tangent at the point of maximum rate of
mens. change on the leading edge of the melting endotherm. Extrapo-
late this line to the baseline in 10.9.1.
10.4 Prepare three (or more) zinc test specimens.
10.4.1 Into a tared specimen container, weigh a single 2.4 to 10.9.3 The temperature of intersection of the baseline (in
2.8 mg of the zinc reference material. Seal the specimen 10.9.1) and the tangent (in 10.9.2) is taken as the extrapolated
container. onset temperature (see Fig. 3).

NOTE 12—The masses for indium, bismuth, and zinc specimens in steps 10.10 Load a bismuth specimen (or material with the
10.2 to 10.4 are selected to provide approximately the same melting mid-range transition temperature) from 10.3 into the instru-
endothermic peak (valley) heights. ment chamber, purge the chamber with dry nitrogen (or other
NOTE 13—The temperatures of the materials selected in steps 10.2 to inert gas) at a flow rate of 10 to 50 mL ⁄min 6 10 % through-
10.4 should be approximately equally distributed over the anticipate out the experiment. An empty specimen container is loaded in
temperature range. Other materials and masses may be used but shall be
reported. the reference position.
10.5 Load an indium (or material with the lowest transition 10.11 Equilibrate at 250°C for one minute.
temperature) specimen into the instrument chamber, purge the 10.12 Heat the test specimen at 10°C/min through the
chamber with dry nitrogen (or other inert gas) at a flow rate of bismuth melting transition to 290°C and record heat flow and
10 to 50 mL ⁄min 6 10 % throughout the experiment. An specimen temperature (see Note 14).
empty sample specimen container is loaded in the reference
position. 10.13 Cool the test specimen to ambient temperature at any
convenient rate. The thermal curve need not be recorded.
10.6 Equilibrate at 120°C for one minute.
10.7 Heat the test specimen at 10°C/min through the indium 10.14 Display the thermal curve for the melting endotherm
melting transition to 180°C and record the thermal curve. with heat flow on the ordinate (Y-axis) and specimen tempera-
ture on the abscissa (X-axis). Determine the extrapolated onset
NOTE 14—Other heating rates may be used but shall be reported. temperature for the bismuth melting endotherm as T(Bi1) to
10.8 Cool the test specimen to ambient temperature at any two places to the right of the decimal point (see 10.9.1 to
convenient rate. The thermal curve need not be recorded. 10.9.3).

FIG. 3 Determination of the Extrapolated Onset Temperature

5
 E2253 − 16
10.15 Load a zinc (or material with the highest transition 11.2 Detection Limit (DL) is given by:
temperature) specimen into the instrument chamber, purge the DL 5 3.3 s o (1)
chamber with dry nitrogen (or other purge gas) at a flow rate of
DL 5 3.3 s (2)
10 to 50 mL ⁄min 6 10 % throughout the experiment, An
empty sample specimen container is loaded in the reference where:
position. DL = detection limit, mJ or °C, and
10.16 Equilibrate at 400ºC for one minute. so = blank enthalpy standard deviation, mJ, and
s = temperature standard deviation, °C.
10.17 Heat the test specimen at 10ºC/min through the zinc NOTE 16—To express the Detection Limit in terms of mass of analyte,
melting temperature to 440ºC and record the heat flow, the value for DL may be divided by the slope value m from 9.20.
specimen temperature and time (Note 14). 11.3 Quantitation Limit (QL) is given by:
10.18 Cooling the test specimen to ambient temperature at QL 5 10 s o (3)
any convenient rate. The thermal curve need not be recorded.
QL 5 10 s (4)
10.19 Display the thermal curve for the melting endotherm
with heat flow on the ordinate (Y-axis) and specimen tempera- where:
ture on the abscissa (X-axis). Determine the extrapolated onset QL = quantitation limit, mJ or °C.
temperature for the zinc melting endotherm as T(Zn1) to two NOTE 17—To express the Quantitation Limit in terms of mass of the
places to the right of the decimal point (see 10.9.1 to 10.9.3). analyte, the value for QL may be divided by the slope value m from 9.20.
11.4 Percent Linearity (L) is given by:
10.20 Repeat steps 10.5 through 10.19 two more times each
for the low, medium, and high temperature materials. Remove
the specimen from the DSC sample chamber and reload with a
L5 F~ ?
100 % 3 Largest δY !
m 3 M max1b
? G (5)

fresh specimen for each determination. Record the melting

temperature values as T(In2), T(Bi2), T(Zn2), T(In3), T(Bi3) L5 F ~~ ?
100 % 3 Largest δY
m 3 ~ T ~ Zn! 2 T ~ In 1b!! ! G
?! (6)
and T(Zn3) in ºC.
where:
10.21 Calculate (see Practice E1970) the mean (T) and
L = linearity, %,
standard deviation (σ) for the melting temperatures for indium, m = slope, mJ mg-1, (from 9.20), or
bismuth, and zinc as T(In), T(Bi), T(Zn), σ(In), σ(Bi), and dimensionless, (from 10.23),
σ(Zn), respectively. b = intercept, mJ, (from 9.20), or dimensionless,
10.22 Pool (see Practice E1970) the three standard deviation from 10.23),
values from 10.21 and record as s. Mmax = mass of largest test specimen, mg, or highest
temperature, °C, (from 10.21),
10.23 Using the pooled standard deviation s from 10.22, |Largest δY | = absolute value of the largest deviation from
determine the detection limit (DL) and quantitation limit (QL) best fit straight line,
as calculated in Eq 2 and Eq 4. Report Temperature DL and T(Zn) = melting temperature of zinc, and
QL. T(In) = Melting temperature of indium.
10.24 Using the three literature values for the melting 11.5 Calorimetric and temperature Bias (Bias) is given by:
temperature of indium, bismuth and zinc (for example, from
Table 1) as the independent (X) value and the three (or more) ~ ∆H ref 2 m ! 3 100 %
Bias 5 (7)
∆H ref
mean values for the observed melting temperatures values from
10.9, 10.10, 10.14, and 10.19 as the dependent (Y) values, Bias 5 @ ~ m 2 1.00000! 3 100 % # (8)
determine the least-squares (linear regression) best-fit value for where:
the slope (m), and intercept (b) (see Practice E1970).
∆Href = accepted reference value for indium heat of fusion,
NOTE 15—The value for m will be dimensionless, and the value for b 28.58 mJ mg-1.4
will be in °C.
10.25 Calculate the Percent Linearity (L) of the temperature 12. Example Calculations
determination from the values in 10.24 and the calculation of 12.1 For the example calculations described below, the
Eq 5. following experimental data is used:
10.26 Compare the slope (m) from 10.24 to the anticipated Mmax = 15.680 mg Qmax = 444.33 mJ
Mmid = 8.000 mg Qmid = 233.33 mJ
value of 1.00000). Report this value as the Temperature Bias Mmin = 0.376 mg Qmin = 11.133 mJ
(TBias) as a percentage according to Eq 7. Mo = 0.000 mg Qo = 0.0019093 mJ
nmax = 3 smax = 6.4470 mJ
nmid = 3 smid = 0.14012 mJ
11. Calculations nmin = 3 smin = 0.089629 mJ
no = 3 so = 0.0041285 mJ
11.1 When performing these calculations, retain all avail-
able decimal places in the measured values and in intermediate
calculated values. The final result should be rounded to three
significant figures. 4
Stølen, S., Grønvold, F., Thermochimica Acta, Vol 327, 1999, p. 1.

6
 E2253 − 16
where: 12.6 Example calculation for Calorimetric Bias:
n = number of replicate determinations. ~ 28.58 mJ mg21 2 28.305 mJ mg21 ! 3 100 %
Bias 5 (15)
12.2 Example calculation for Detection Limit: 28.58 mJ mg21

DL 5 3.3 3 0.0041285 mJ 5 0.0136 mJ (9) 50.962 %

12.3 Example calculation for Quantitation Limit:
QL 5 10 3 0.0041285 mJ 5 0.0413 mJ (10) 13. Report
12.4 Example calculation for Calorimetric Repeatability: 13.1 Manufacturer and model of the DSC apparatus.
RSDmax 5 6.4470 mJ 3 100 %/444.33 mJ 5 1.4509 % (11) 13.2 Time conformity from Test Method E1860.
RSDmid 5 0.14012 mJ 3 100 %/233.33 mJ 5 0.060052 % 13.3 Temperature calibration from Test Method E967.
RSDmin 5 0.089629 mJ 3 100 %/11.133 mJ 5 0.80508 % 13.4 Heat flow calibration from Practice E968.
13.5 Some or all of the performance parameters described
r5 F 2 3 1.4509 % 2 12 3 0.060052 % 2 12 3 0.80508 % 2
21212 G 1/2

by this test method useful for the application at hand, includ-

ing:
r5 F 4.210210.007211.2963
6 G F
1/2
5
5.5137
6 G 1/2
13.5.1 Range (Qmin to Qmax, or Mmin to Mmax),
13.5.2 Temperature and Calorimetric Detection Limit (DL),
50.918951/2 5 0.959 % 13.5.3 Temperature and Calorimetric Quantitation Limit
12.5 Example calculation of Percent Linearity: (QL),
12.5.1 From the best fit to the max, mid, and min data of 13.5.4 Temperature and Calorimetric Percent Linearity (L),
12.1: 13.5.5 Temperature and Calorimetric Bias (Bias), and
m 5 28.305 mJ mg21 5 28.305 J g 21 (12) 13.5.6 Calorimetric Repeatability (r).
b 5 2.6284 mJ 13.6 The specific dated version of this test method used.
12.5.2 From the best fit straight line:
14. Precision and Bias
δY max 5 2.123 mJ (13)
14.1 Precision and bias are determined by the procedures in
δY mid 5 24.261 mJ ← Largest deviation from the best fit line this document. No separate precision and bias information is
required.
δY min 5 2.138 mJ

12.5.3 Example calculation: 15. Keywords

L5 F 100 % 3 4.261 mJ
28.305 mJ·mg21 3 15.68 mg12.6284 mJ G (14)
15.1 detection limit; differential scanning calorimetry; en-
thalpy; linearity; precision; quantitation limit; range; repeat-
ability; thermal analysis; validation
5 F 426.2 mJ
446.451 mJG5 0.954 %

SUMMARY OF CHANGES

Committee E37 has identified the location of selected changes to this standard since the last issue (E2253 – 11)
that may impact the use of this standard. (Approved April 1, 2016.)

(1) Minor editorial changes to 3.1, 4.4.1, 4.5.2, 9.20, 9.21,

Section 10 heading, and 10.24.

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 E2253 − 16
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