240 - 14. PCS PDF
240 - 14. PCS PDF
240 - 14. PCS PDF
where: 9.1.2.1 Add the sample to the cup by inserting the tip of the
needle through the tape disk at a point so that the flap of tape
Qpst = heat of combustion of the pressure-sensitive tape or
will cover the puncture upon removal of the needle. Seal down
mineral oil, MJ/kg,
∆t = corrected temperature rise, as calculated in accor- the flap by pressing lightly with a metal spatula. Reweigh the
dance with 10.1 or 10.2,°C, cup with the tape and sample. Take care throughout the
W = energy equivalent of the calorimeter, MJ/°C, weighing and filling operation to avoid contacting the tape or
e1 = correction for the heat of formation of HNO3, MJ, and cup with bare fingers. Place the cup in the curved electrode and
arrange the fuse wire so that the central portion of the loop
a = mass of the pressure-sensitive tape or gelatin capsule/ presses down on the center of the tape disk.
mineral oil, g. 9.1.3 Gelatin/Mineral Oil—Weigh the cup and gelatin cap-
sule. The capsule should only be handled with forceps. Add the
sample to the capsule. Reweigh the cup with capsule and
6
Jessup, R. S., “Precise Measurement of Heat of Combustion with a Bomb sample. If poor combustion is expected with the capsule, add
Calorimeter,” NBS Monograph 7, U. S. Government Printing Office. several drops of mineral oil on the capsule and reweigh the cup
ANNEXES
(Mandatory Information)
A1.1 Test Room—The room in which the calorimeter is than 0.01 °C starting with identical temperatures in the
operated must be free from drafts and not subject to sudden calorimeter, room, and jacket. The immersed portion of the
temperature changes. The direct rays of the sun shall not strike stirrer shall be coupled to the outside through a material of low
the jacket or thermometers. Adequate facilities for lighting, heat conductivity.
heating, and ventilating shall be provided. Thermostatic control NOTE A1.1—As used in this test method, the term calorimeter desig-
nates the bomb, the vessel with stirrer, and the water in which the bomb
of room temperature and controlled relative humidity are is immersed.
desirable.
A1.4 Jacket—The calorimeter shall be completely enclosed
A1.2 Oxygen Bomb—The oxygen bomb is to have an within a stirred water jacket and supported so that its sides, top,
internal volume of 350 mL 6 50 mL. All parts are to be and bottom are approximately 10 mm from the jacket wall. The
constructed of materials which are not affected by the combus- jacket can be arranged so as to remain at substantially constant
tion process or products sufficiently to introduce measurable temperature, or with provision for rapidly adjusting the jacket
heat input or alteration of end products. If the bomb is lined temperature to equal that of the calorimeter for adiabatic
with platinum or gold, all openings shall be sealed to prevent operation. It must be constructed so that any water evaporating
combustion products from reaching the base metal. The bomb from the jacket will not condense on the calorimeter.9
must be designed so that all liquid combustion products can be A1.4.1 A double-walled jacket with a dead-air insulation
completely recovered by washing the inner surfaces. There space may be substituted for the constant-temperature water
must be no gas leakage during a test. The bomb must be jacket if the calorimeter is operated in a constant-temperature
capable of withstanding a hydrostatic pressure test to a gauge (62 °F) (61 °C) room. The same ambient conditions must be
pressure of 3000 psi (20 MPa) at room temperature, without maintained for all experiments, including standardization.
stressing any part beyond its elastic limit. (See Note 3.)
A1.5 Thermometers—Temperatures in the calorimeter and
A1.3 Calorimeter—The calorimeter (Note A1.1) vessel jacket shall be measured with the following thermometers or
shall be made of metal (preferably copper or brass) with a combinations thereof:
tarnish-resistant coating, and with all outer surfaces highly
polished. Its size shall be such that the bomb will be com-
pletely immersed in water when the calorimeter is assembled. 9
The sole source of supply of the apparatus known to the committee at this time
It shall have a device for stirring the water thoroughly and at a is Parr Instrument Co., 211 Fifty-Third St., Moline, IL 61265. If you are aware of
alternative suppliers, please provide this information to ASTM Headquarters. Your
uniform rate, but with minimum heat input. Continuous stirring comments will receive careful consideration at a meeting of the responsible
for 10 min shall not raise the calorimeter temperature more technical committee,1 which you may attend.
A2. CORRECTIONS
A3.1 Sodium Hydroxide Keep surfaces clean to prevent ignition or explosion, or both,
A3.1 Warning—Corrosive. Can cause severe burns or on contact with oxygen.
blindness. Evolution of heat produces a violent reaction or Always use a pressure regulator. Release regulator tension
eruption upon too rapid mixture with water. before opening cylinder valve.
Before using, secure information on procedures and protec- All equipment and containers used must be suitable and
tive measures for safe handling. recommended for oxygen service.
Do not get in eyes, on skin, on clothing. Never attempt to transfer oxygen from cylinder in which it
Avoid breathing dusts or mists. is received to any other cylinder.
Do not take internally. Do not mix gases in cylinders.
When handling, use chemical safety goggles or face shield, Do not drop cylinder. Make sure cylinder is secured at all
protective gloves, boots, and clothing. times.
When mixing with water, add slowly to surface of solution Keep cylinder valve closed when not in use.
to avoid violent spattering. In the preparation of solutions do Stand away from outlet when opening cylinder valve.
not use hot water, limit temperature rise, with agitation, to Keep cylinder out of sun and away from heat.
10 °C ⁄min or limit solution temperature to a maximum of
Keep cylinder from corrosive environment.
90 °C. No single addition should cause a concentration in-
Do not use cylinder without label.
crease greater than 5 %.
Do not use dented or damaged cylinders.
A3.2 Oxygen For technical use only. Do not use for inhalation purposes.
A3.2 Warning—Oxygen vigorously accelerates combus- Use only in well-ventilated area.
tion. See compressed gas association booklets G-4 and G-4.1 for
Do not exceed the sample size limits. details of safe practice in the use of oxygen.
Do not use oil or grease on regulators, gauges, or control
equipment. A3.3 2,2,4-Trimethylpentane
Use only with equipment conditioned for oxygen service by A3.3 Warning—Extremely flammable. Harmful if inhaled.
carefully cleaning to remove oil, grease, and other combus- Vapors may cause flash fire.
tibles. Keep away from heat, sparks, and open flame.
Keep combustibles away from oxygen and eliminate ignition Keep container closed.
sources. Use with adequate ventilation.
REFERENCES
(1) Gross, M. E., Gutherie, G. B., Hubbard, W. N., Katz, C., McCullough, (6) Hubbard, W. N., Huffman, H. M., Knowlton, J. W., Oliver, G. D.,
J. P., Waddington, G., and Williamson, K. D.,“ Thermodynamic Scott, D. W., Smith, J. C., Todd, S. S., and Waddington G.,
Properties of Furan,” Journal, Am. Chemical Soc., Vol 74, No. 18, “Thermodynamic Properties of Thiophene,” Journal, Am. Chemical
Sept. 23, 1952, pp. 4662–4669. Soc., Vol 71, No. 3, March 1949, pp. 797–808.
(2) Jessup, R. S., “Heats of Combustion of the Liquid Normal Paraffin (7) LeTourneau, R. L., and Matteson, R.,“ Measurement of Heat of
Hydrocarbons from Hexane to Dodecane,” Journal of Research, Nat. Combustion of Volatile Hydrocarbons,” Analytical Chemistry, Vol 20,
Bureau Standards, Vol 18, No. 12, February 1937, pp. 115–128. No. 7, July 1948, pp. 663–664.
(3) Prosen, E. J. R., and Rossini, F. D., “Heats of Isomerization of the (8) Dean, E. W., Fisher, N. E., and Williams, A. A., “Operating Procedure
Five Hexanes,” Journal of Research, Nat. Bureau Standards, Vol 27, for Determining the Heat of Combustion of Gasoline,” Industrial and
No. 3, September 1941, pp. 289–310.(Research Paper RP 1420).
Engineering Chemistry, Analytical Edition, Vol 16, No. 3, March
(4) Barry, F., and Richards, T. W., “Heat of Combustion of Aromatic
1944, pp. 182–184.
Hydrocarbons and Hexamethylene,” Journal, Am. Chemical Soc., Vol
(9) Prosen, E. J., and Rossini, F. D., “Heats of Combustion of Eight
37, No. 5, May 1915, pp. 993–1020.
(5) Coops, J., and Verkade, P. E., “A New Method for the Determination Normal Paraffin Hydrocarbons in the Liquid State,” Journal of
of the Heats of Combustion of Volatile Substances in the Calorimetric Research, Nat. Bureau of Standards, Vol 33, No. 4, October 1944, pp.
Bomb,” Recueil traveus chimique, Vol 45, 1926, pp. 545–551. 255–272. (Research Paper RP 1607).
SUMMARY OF CHANGES
Subcommittee D02.05 has identified the location of selected changes to this standard since the last issue
(D240 – 09) that may impact the use of this standard. (Approved Oct. 1, 2014.)
(1) Added D7171 to Referenced Documents. (3) Revised Note 8 and footnote 7.
(2) Revised Sections 3, 9, and 10.
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