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Page Title:
Determination of the heat of reaction and the volume of gaseous products |
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|  MIL-E-70610(AR)
(See 3.8) Nest the specified sieve or
4.5.6 Granulation.
sieves (see Table II) on a bottom pan. Place a weighed portion of
100 gm of the sample on the upper sieve, cover the sieve, and stroke
the assembly for 10 minutes by hand, or for 5 minutes by means of a
mechanical shaker geared to produce 300 15 gyrations and 150 10
taps of the striker per minute. Weigh the amount retained or
passing through the sieves, and calculate to percentages as required.
4.5.7 Determination of the heat of reaction and the volume of
(See 3.9) The determination shall be performed
gaseous products.
in accordance with the following procedure and using "Parr"
Adiabatic Calorimeter, or approved equal.
a. Weigh, approximately, 3.0 grams of a sample of Eimite to
0.0002 grams in a Coors, size 2, porcelain crucible.
b. Coil 9" of 0.01" diameter platinum wire around a piece of
asbestos, 3/16" wide by 3/4" long.
c. Attach ends of wire to the bomb electrodes and place the
coil in contact with the surface of the sample and assemble the bomb.
d. Fill the bomb with purified helium to 20 atmospheres and
(The
exhaust the helium slowly. Repeat this operation three times.
final pressure of the bomb is 1 atmosphere.)
e. Fill the bucket with the same quantity of water and at the
approximate tempe rature as in the standardization procedure using
the prepared tare as the counterbalance.
f. Place the bucket of water in the calorimeter, set the bomb
in the bucket, and attach the electrical connection to the bomb
firing terminal.
g. Close the calorimeter with the therometers in place.
h. Adjust the jacket temperature to equal the temperature of
the water in the bucket by injecting hot or cold water, as required.
1. Maintain the equalization temperature for a period of five
minutes after equilibrium has been reached and record temperature of
bucket .
Ignite sample.
(A 12 volt
k. Measuue the energy required for ignition.
for ignitor and a Weston Watt-Second Integrator, Model
#808, for determining the ignition energy have been found
satisfactory.)
l. Inject hot water into the calorimeter jacket as the
temperature of the calorimeter is rising, maintaining equilibrium
temperature conditions until the maximum temperature is reached.
m. Record the final temperature of the reaction and ambient air
temperature. Check the bomb for leakage, and disassemble the
calorimeter .
n. Exhaust the gases from the bomb slowly into the audiometer
and record the volume of gas, the bath and room temperature, and
`barometric pressure.
15
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