Mr. Roger Blaine, New Castle, DE 19720 USA 302-427-4017 ASTM International 100 Barr Harbor Drive West Conshohocken, PA 19428-2959

This Research Report is issued under the fixed designation RR: E37-1030.
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this document. Copyright ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428. All rights reserved.
25 November 2003
Committee £37 on Thermal Measurements

Subcommittee E37.01 on Thermal Test Methods and Practices
Research Report RR # E37-1030
Inter-Laboratory Study to Establish Precision Statements for ASTM

E2160, Standard Test Method for Heat of Reaction of Thermally
Reactive Materials by Differential Scanning Calorimetry
Technical Contact:
Mr. Roger Blaine,
New Castle, DE 19720
USA
302-427-4017
RBlaine@tainstruments.com
ASTM International
100 Barr Harbor Drive
West Conshohocken, PA 19428-2959
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COMMITTEE E-37 ON THERMAL MEASUREMENTS
RESEARCH REPORT RR: E-37xxxx
INTERLABORATORY TEST STUDY FOR ENTHALPY OF
REACTION: STANDARD METHOD E 2160-01
Introduction
This report describes an Interlaboratory Test Study that was conducted for ASTM
International Standard Test Method E 2160-01 - Standard Test Method for Heat of Reaction of
Thermally Reactive Materials by Differential Scanning Calorimetry.
The potential uses of the test method are manifold. These uses include, but are not
limited to, determining the fraction of reaction of a thermoset material (degree of cure);
providing input information for determining hazard-potential figures-of-merit for Explosion
Potential, Shock Sensitivity, and others (ASTM International Method E 1231); or determining
the extent of decomposition of an aged material.
Test Method
The test method used for the Interlaboratory Study was ASTM International E 2160-01, a
copy of which is attached.
List of Participating Laboratories
A call for laboratories to participate in the interlaboratory study was placed in January of
2003. A sufficiently large number of laboratories volunteered that it was deemed sufficient for
conduct of two independent studies, each using one of two different thermally reactive materials.
The list of participating laboratories follows.
Technical Safety Laboratory
Eastman Kodak Co.
1100 Ridgeway Ave.
Rochester, NY 14652-6270
Glenn Bodman
Eli Lilly
Lilly Corporate Research Center
Indianapolis, IN 46285
R. Dale Cheetham
Canadian Explosives Research Laboratory
Draft document l Draft Document

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CANMET
555 Both Street
Ottawa, Canada
Barbara Acheson
Ciba Specialty Chemicals Corp

540 White Plains Road
Tarrytown, NY 10591
Ron Burke and Ray O'Brien
Air Products and Chemicals

7201 Hamilton Blvd
Allentown, PA 18195-1501
Frank Prozonic and Scott Voth
Reichhold Inc.
2400 Ellis Road
Durham, NC 27703
Christine Provost
Merck & Co. Inc

126 E. Lincoln Ave, PO Box 2000; R55-228
Rahway, NJ 07065
Donna Franklin
Thomas A. Edison Technical Center

Cooper Power
PO Box 100, 11131 Adams Road,
Franksville, WI 53126
Richard Baumann
GrafTech International
12900 Snow Rd.
Parma, OH 44130
Orest L. Adrainowycz and D. M. Riffle
Safety Consulting Engineers

2131 Hammond Drive
Schaumberg, IL 60173
Ashok Ghose Dastidar
Corning Inc.
Sullivan Park FR-4-1
Corning, NY 14831
E. Robert Fretz
Draft document 2 Draft Document

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Solutia Inc.
3000 Old Chemstrand Rd.
Cantonment, FL 32533
John Tria
ILC Dover, Inc.

1 Moonwalker Rd.
Frederica, DE 19946
Michael Kinnel
Ciba Specialty Chemicals Corp

Ciba Road
Mclntosh, AL 3653
Michael Oliver
Interlaboratory Test Program.
The test materials were shipped to the laboratories and individual laboratory results were
collected during the summer of 2003. The study group comprised four different models of
differential scanning calorimeters from two different manufacturers and it comprised several
different types of sample containers.
The first of the two materials included in the study was l-phenyl-lH-tetrazole-5-thiol, a
thermally unstable mercaptan (this sample is referred herein as "mercaptan"). The second
material was a commercial sample of 2-butanone peroxide, a free radical initiator used for
initiation of free radical polymerization. The two materials have different reaction
characteristics. The mercaptan sample decomposed in such a way that there was not a significant
statistical difference between values obtained with high-pressure sealed vessels as opposed to
hermetically sealed aluminum pans. The peroxide thermal decomposition, a self-accelerating
reaction, generates gaseous reaction species. The gaseous products react further, and if lost
during the measurement process, cause the measured heat of reaction to be smaller than the true
value. The measurements on the peroxide show that a degree of caution is required when
making decisions about thermal hazards based on measured heats of reaction and initiation
temperatures.
We planned for the mercaptan results to be indicative of the interlaboratory precision of

the Standard Test Method E 2160. We planned the peroxide results to be indicative of

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confounding variable factors that can arise from the nature of the sample/specimen closure
method used for the measurements.
Interlaboratory Test Program Instructions
Contained below are directions sent by Email to the two respective groups. A reporting
form was distributed to the participants, a blank copy of which is attached to this report. The
laboratories submitted these forms completed and copies of their thermograms as their individual
laboratory reports.
Directions for Mercaptan Group
Message 1:
"Dear Colleagues:
You are receiving this message because you volunteered previously to take part in an
Interlaboratory Test for an ASTM International Standard on Heat of Reaction. On behalf of
ASTM International, I thank you for donating your time and facilities to make our standards
better.
I have been informed today that some of you have begun receiving samples of 1-phenyl-lH-
tetrazole-5-thiol. Shipping obviously found a way to obtain expeditious delivery of the material;
I'm pleased. I had been waiting to contact you until they had found a way to ship this material.
The purpose of the Interlaboratory Test is to gather sufficient information to generate a Precision
and Bias statement for ASTM International Standard E2160-01 on heat of reaction. ASTM
Precision and Bias statements are required for every standard method. They allow users of the
method to determine whether differences in results within a laboratory or between laboratories is
significant or not.
Attached you will find a copy of ASTM International standard E2160-01. The ASTM method
must be followed for your results to be included in the Research Report that will be submitted in
conjunction with the generation of a Precision and Bias Section of E2160.
There are two groups working in this ILT. Your group will be receiving the 1-phenyl-lH-
tetrazole-5-thiol sample. A Manufacturer's Safety Data Sheet (MSDS) was included with it. If
your MSDS has been removed (our safety office takes our MSDSs as chemicals arrive; so we have
to go get new ones for the labs) and you want one, let me know and I will get you another, or you
can download one from Aldrich's website.
The other group will receive a stabilized peroxide to measure.
Some of the materials considered for this ILT generate sufficient pressure that hermetically-sealed
aluminum pans would become unsealed. The resultant leak presents as a large sharp endotherm,
sometimes preceded by an endothermic slope. The large endotherms were observed for liquid
materials that vaporized at high temperatures when the pan seal failed. There are two obvious
ways of preventing this problem if you find problems with pan leakage. The first is to reduce the
amount of material in the pan, thereby reducing the pressure arising from the decomposition. The
second is to use cells that seal higher pressures.

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I have not tried it, but I doubt that running the heat of reaction in open pans will work well, so
please try to use some sort of sealed vessel.
If you have any questions, please feel free to contact me.
Once again thank you for taking part in this Interlaboratory Test."
Message 2:
"Dear ILT Participants:
Please find attached a Data Report form that you may use to report your results. Either Email or
Snail mail are OK. I have responded to those who have asked about a target date for completion,
that about four weeks would be appropriate. That should allow most of you to schedule the
measurements around other more pressing obligations.
Thank you for your efforts."
Directions for Peroxide Group
"Dear Colleagues:
You are receiving this message because you volunteered previously to take part in an
Interlaboratory Test for an ASTM International Standard on Heat of Reaction. On behalf of
ASTM International, I thank you for donating your time and facilities to make our standards
better. You should be receiving a sample of material for the ILT within the next few days.
The purpose of the Interlaboratory Test is to gather sufficient information to generate a Precision
and Bias statement for ASTM International Standard E2160-01 on heat of reaction. ASTM
Precision and Bias statements are required for every standard method. They allow users of the
method to determine whether differences in results within a laboratory or between laboratories is
significant or not.
Attached you will find a copy of ASTM International standard E2160-01. The ASTM method
must be followed for your results to be included in the Research Report that will be submitted in
conjunction with the generation of a Precision and Bias Section of E2160.1 have attached a form
which you can use to report your results for the ILT. There are some further specific directions
given below.
There are two groups working in this ILT. Your group will be receiving a 2-butanone peroxide
sample. A Manufacturer's Safety Data Sheet (MSDS) was included with it. If your MSDS has
been removed (our safety office takes our MSDSs as chemicals arrive; so we have to go get new
ones for the labs) and you want one, let me know and I will get you another, or you can download
one from Aldrich's website.
The other group will receive a mercaptan to measure.
The peroxide sample for this ILT can generate sufficient pressure that hermetically-sealed
aluminum pans can become unsealed. The resultant leak presents as a large sharp endotherm,
sometimes preceded by a fairly steep endothermic slope. Large endotherms result because liquid
materials in the pan vaporize at high temperatures when the pan seal failed. There are at least two
ways of preventing this problem if you find problems with pan leakage. The first is to reduce the
amount of material in the pan, thereby reducing the pressure arising from the decomposition. The
second is to use cells that seal higher pressures.

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There will be an endothermic slope throughout the measurement arising from vaporization of
components from the sample, increasing the pressure within the pan.
There are two exothermic events associated with the 2-butanone thermal reaction. These are seen
in the thermogram included in this message. That thermogram was obtained with 1 mg of material
in a threaded cell that screws closed and is sealed with a gold gasket compressed between the top
and bottom parts of the container. A sigmoid baseline was constructed for calculation of the
enthalpy of reaction and is seen in the figure.
17
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Temperature (°C)
Specific Directions:
My advice is that we need at least five replicates from each laboratory. This should be enough that
baseline effects are randomized and provides more statistical degrees of freedom for the final
analysis.
Calibration requirements are described in Section 8 of the Standard.
Please forward the thermograms that correspond to the reported determinations of the enthalpy of
reaction. They can be sent either as Email attachments (ASCII please) or as photocopies of the
printed thermograms.
I raise the issue of straight-line baseline vs. use of a sigmoidal baseline. The ASTM standard
leaves this decision to those using the standard. My opinion is that you will obtain better results
with a sigmoidal baseline.
As I am always asked by somebody for a deadline, I will choose an arbitrary "target" date of the
end of May for completion of measurements. I understand that many of you have to schedule time
for these measurements in very busy scheduling for your instrumentation and that you might not
be able to get to these measurements by then. If you cannot complete the measurements by then,
please do not drop out of the ILT, just drop me a message with an approximate completion date.
If you have any questions or comments, please don't hesitate to contact me.
Once again, I thank you for donating your time and effort in helping us to make ASTM's standards
as useful as possible to you.
Good luck and best wishes."
Draft document Draft Document

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Data Reports, Statistical Data Summary, and Research Report Summary
Data reports comprise primarily printed pages that contain plotted thermograms, which
are figures that show heat flow against temperature during the course of a measurement. The
printed pages, thermograms, also contain the numerical values reported, as these numerical
values are extracted from the plotted curves. Many of these thermograms contain the identity of
the laboratory participants and are therefore not attached to this report. The numerical values
reported by the laboratories, and the subsequent statistical calculations, are reported in tables and
figures on following pages and are discussed below.
Mercaptan. Eight laboratories reported results for the mercaptan sample. The
determinations of heat of reaction, onset temperature, and peak temperature are given in Tables 1
through 3, respectively. Also given in Table 1 is information on the sample container, the mass
(range) of sample used in the measurements, and the precision to which the mass values were
reported. A significant induction period was not observed for the mercaptan and we have
therefore not tabulated values of the temperature of first deviation.
No outliers were observed (see Figures 1 through 3; per ASTM International Standard
Practice E 691-99). The reported data led to the following statistics. The average heat of
reaction was 1105 J/g, with repeatability and reproducibility standard deviations of 5.3% and
7.4%, respectively. Multiplication by 2.8 (per ASTM International E 691-99) leads to 95%
confidence intervals for repeatability and reproducibility of 14.8% and 20.7%, respectively. The
average peak temperature was 161.33 K, with repeatability and reproducibility standard
deviations of 0.94 K and 1.68 K, respectively. Multiplication by 2.8 leads to 95% confidence
intervals for repeatability and reproducibility of 2.6 K and 4.7 K, respectively. The average
onset temperature was 156.87 K, with repeatability and reproducibility standard deviations of
0.81 K and 1.87 K, respectively. Multiplication by 2.8 leads to 95% confidence intervals for
repeatability and reproducibility of 2.3 K and 5.2 K, respectively. These values will be balloted
for inclusion as the Precision statement for Standard Method E 2160. There are no established
reference values with which to generate a Bias statement.
2-Butanone peroxide. Six laboratories reported results for the 2-butanone peroxide
sample. Several different sample containers were used in this part of the interlaboratory study.
Two laboratories reported results in which each of the two laboratories used two different types

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of sample enclosures; one type was a high-pressure container and the other type was a
hermetically sealed aluminum container. We treated each of the studies with different sample
enclosures as a separate laboratory result. We thus counted eight studies, four with high-pressure
vessels and four with hermetically sealed aluminum vessels. The individual measured values of
heat of reaction, peak temperature, and temperature of first deviation are given in Tables 4
through 6, respectively. Also given in Table 4 is information on the sample containers, the mass
(range) of sample used in the measurements, and the precision to which the mass values were
reported.
The average heat of reaction obtained from the four sets of data from the high-pressure
vessels was 1391 J/g. The differences from the grand mean of the four averaged values, one
from each study, were all smaller than 3%, in agreement with the Precision figure calculated
from the mercaptan data. The thermograms from these studies showed either two distinct
exothermic peaks, or one large exothermic peak with an obvious shoulder corresponding to a
second exothermic event. This average heat of reaction, 1391 J/g, was obtained without
significant mass losses in the individual observations and will serve as a reference with which to
compare the determinations that were made with hermetically sealed aluminum containers.
The average heat of reaction from the four studies using hermetically sealed containers
was 1039 (J/g). The standard deviation of the cell averages was approximately 40%. The cell
averages obtained with hermetically sealed containers were compared individually to the average
value obtained from the measurements made with high-pressure containers. Three of the four
studies that used hermetically sealed pans showed heats of reaction that were much smaller than
the average obtained from the high-pressure containers. These three studies we label group A for
brevity. The thermograms from group A showed only one exothermic peak in each thermogram.
The absence of the second exothermic peak was consistent with loss of a reactive component
through vaporization. The fourth study obtained with hermetically sealed pans, laboratory
designation 16, agreed statistically with the average from the high-pressure vessels. Examination
of the individual thermograms from this last study showed two exothermic events and showed
endothermic events occurring at temperatures greater than 200 °C. Those endothermic events
occurred from rupture of the hermetic seal on the pan followed by volatilization of liquid
contents from the pan. In this one laboratory study, the hermetic pans were sealed with
sufficiently small mass inside that they remained sealed effectively through the complete

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peroxide reaction process. Results similar to those of laboratory 16 were obtained in the
laboratory of the coordinator of this interlaboratory study with hermetically sealed pans
combined with small sample masses (those results were not included in this interlaboratory
study). Comparisons of thermograms obtained with hermetically sealed sample containers with
thermograms obtained with high-pressure cells in the coordinator's laboratory confirmed the
relation of thermogram peak appearances to the integrity of the sample container prior to
distribution of the peroxide sample to the participating laboratories.
The present interlaboratory test shows that use of hermetically sealed sample pans, or of
vented sample pans, may cause the observed heat of reaction to be much smaller than the true
heat of reaction. In one laboratory's determination, more than half of the heat of reaction was
not observed. We note that open or sealed sample vessels may correspond to actual storage or
process conditions and thus the sample vessel should be chosen with care if volatilization of
reactive material, or if a large heat of vaporization, is anticipated or encountered.
An additional factor that could affect validity of thermal hazard assessments was also
observed with the 2-butanone peroxide samples. Table 6 contains observed values for the
temperature of first deviation and the h factor (see ASTM International Standard Practice E 691-
99) for this set of determinations. The temperature of first deviation is the temperature at which
initiation of the thermal reaction is observed during the measurement. Three types of enclosure
material were used within the set of eight studies; these were gold, glass, and aluminum. Two
laboratories, using gold-plated vessels, observed average temperatures of first deviation of 65 °C
and 57 °C. These temperatures are significantly lower (50 °C lower) than the values that two
laboratories reported using glass vessels, namely, 110.4 °C and 114.7 °C. The aluminum sample
containers gave temperatures of first deviation intermediate between those that were observed
using glass and gold containers. This ordering is in accord with the known behavior of
decomposition of a peroxide to a free radical in the presence of a metal. As was the case for the
heat of reaction, the choice of the sample enclosures, in this case the material of the sample
enclosure, must be considered carefully for proper applicability of the determined temperatures
of first deviation or the onset temperatures.

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Interlaboratory Study of ASTM International Standard Test Method
E2160-01: Heat of Reaction of Thermally Reactive Materials by
Differential Scanning Calorimetry
Name:
Affiliation:
DSC Make and Model:
Software used for calculations:
Sample container type and material:
Heating rate (should be 10°C) and temperature range:
Purge gas type and rate:
Baseline type (sigmoid or straight line):
Values of replicates:
Specimen weight loss, if appropriate:

&RS\ULJKWE\$670,QW
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ASTM International takes no position respecting the validity of any patent rights
asserted in connection with any item mentioned in this research report. Users of this
research report 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 research report 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 research report may be obtained by
contacting ASTM at the above address or at 610-832-9585 (phone), 610-832-9555
(fax), or serviceastm.org (e-mail); or through the ASTM website (www.astm.org).
&RS\ULJKWE\$670,QW
'RZQORDGHGSULQWHGE\

Mr. Roger Blaine, New Castle, DE 19720 USA 302-427-4017 ASTM International 100 Barr Harbor Drive West Conshohocken, PA 19428-2959

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Mr. Roger Blaine, New Castle, DE 19720 USA 302-427-4017 ASTM International 100 Barr Harbor Drive West Conshohocken, PA 19428-2959

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This Research Report is issued under the fixed designation RR: E37-1030.

You agree not to reproduce or circulate or quote, in whole or

Committee £37 on Thermal Measurements

Research Report RR # E37-1030

Inter-Laboratory Study to Establish Precision Statements for ASTM

List of Participating Laboratories

Canadian Explosives Research Laboratory

Draft document l Draft Document

Ciba Specialty Chemicals Corp

Air Products and Chemicals

Merck & Co. Inc

Thomas A. Edison Technical Center

Safety Consulting Engineers

Draft document 2 Draft Document

ILC Dover, Inc.

Ciba Specialty Chemicals Corp

Interlaboratory Test Program.

We planned for the mercaptan results to be indicative of the interlaboratory precision of

Draft document 3 Draft Document

Interlaboratory Test Program Instructions

Directions for Mercaptan Group

The other group will receive a stabilized peroxide to measure.

Draft document 4 Draft Document

If you have any questions, please feel free to contact me.

Thank you for your efforts."

Directions for Peroxide Group

The other group will receive a mercaptan to measure.

Draft document 5 Draft Document

Calibration requirements are described in Section 8 of the Standard.

Good luck and best wishes."

Draft document Draft Document

Draft document 7 Draft Document

Draft document 8 Draft Document

Draft document 9 Draft Document

O "* 1- <° t*~ CO

DSC Make and Model:

Software used for calculations:

Sample container type and material:

Heating rate (should be 10°C) and temperature range:

Purge gas type and rate:

Baseline type (sigmoid or straight line):

Specimen weight loss, if appropriate:

Draft document 18 Draft Document

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