Astm E659 - 033928
Astm E659 - 033928
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
INTRODUCTION
This test method is one of several methods developed by ASTM Committee E27 for determining
the hazards of chemicals. It is designed to be used in conjunction with other tests to characterize the
hazard potential of the chemical under test.
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FIG. 1 Autoignition Temperature Apparatus
needle with a right-angle bend be used so that the operator’s 6.9 Timer—A stop watch or electric timer (preferably foot-
fingers can be kept away from the flask opening. switch operated) calibrated in 0.1 s or 0.2 s units shall be used
6.5 Balance—A laboratory balance capable of weighing to to determine the time lag before ignition (time interval between
the nearest 10 mg shall be used for preparing samples that are the instant of sample insertion and that of ignition as evidenced
solid at room temperature. Sample weights will range from by the appearance of the flame). If visual ignition is difficult to
10 mg to 1000 mg. observe, the temperature-time recorder trace may be used to
estimate the time lag.
6.6 Powder Funnel—A 60 mm filling funnel is used to aid
the insertion of solid samples into the flask. It is suggested that 6.10 Mirror—A 6 in. mirror or other suitable size, mounted
a holder such as a small buret clamp be used so that the above the flask so that the observer may see into the flask
operator’s fingers can be kept away from the flask opening. without having to be directly over it.
6.7 Thermocouple—A fine Chromel-Alumel thermocouple 6.11 Hot-Air Gun—A suitable hot-air gun may be used to
(36 B and S gauge) is used for measuring the gas temperature purge the product gases after a reaction is completed and
(T) inside the flask. Position the tip of the thermocouple at the before the next test. A temperature-controlled, hot-air guncan
center of the flask. Thermocouples should be calibrated against reduce testing time if used to aid in achieving the desired flash
standard temperatures or a standard thermocouple, and should temperature between trials and upon insertion of clean test
be rechecked frequently. Iron-constantan thermocouples are to flasks.
be avoided because they may promote catalytic oxidation on
the iron-oxide surface. External flask temperatures are mea- 7. Safety Considerations
sured with a No. 20 B and S gauge or finer thermocouple 7.1 No explosion hazard is encountered in conducting the
mounted at the top (t1), middle (t2), and bottom (t3) of the flask. determination as outlined in Section 7. However, flames are
6.8 Recording Potentiometer—A fast response (1 s or less occasionally emitted well above the top of the flask. Thus, the
for full scale pen travel) variable range and variable chart speed operator should always use a mirror for observation of the flask
recording potentiometer shall be used for recording the signal interior. The use of a right-angle syringe and, for solids, the use
from the internal gas thermocouple (T). An X–Y recorder has of a holder for the powder funnel will remove the hands from
been found suitable for this purpose. the immediate vicinity of the flask opening.
APPENDIXES
(Nonmandatory Information)
X1. APPARATUS
X1.1 Dimensions of the test vessel. Proper placement of the junction is facilitated
X1.1.1 Fig. 1 is a cut-away diagram of a typical test flask by inserting the leads through properly shaped small diameter
installation in a commercial pot-type crucible furnace. Other glass tubing. The glass tubing should not extend below the
furnaces or laboratory sand baths capable of maintaining the flash shoulder into the spherical portion of the flask to avoid
required temperature uniformity are satisfactory. The following flame quenching effects. This thermocouple is fed to the
dimensions are for a Heavy-Duty Laboratory Crucible Fur- recording potentiometer (see 5.8).
nace:4 X1.3.2 External flask temperatures are measured with ther-
(a) 7 in. (17.8 cm) mocouples t1, t2, and t3 located outside the test vessel and
(b) 5 in. (12.7 cm)
(c) 51⁄2 in. (14.0 cm) beneath the aluminum foil wrap. These thermocouples can be
(d) 1 in. (2.5 cm) monitored by a suitable strip chart recorder or manual poten-
(e) 10 in. (25.4 cm)
(f) 17⁄8 in. (4.8 cm) tiometer. If the temperature uniformity of the test set-up has
(g) 81⁄8 in. (20.6 cm) been adequately established, as in X1.5, the routine use of
(h) 21⁄2 in. (6.4 cm) exterior thermocouples is not necessary. The three exterior
(i) 3⁄4 in. (1.9 cm)
(j) 17 in. (43.2 cm) thermocouples are required if a multiple top, sidewall, and
bottom heater system is employed to obtain flask temperature
X1.2 Insulated Cover
uniformity.
X1.2.1 The insulated cover is fabricated from mineral
insulating block as a split unit to facilitate test flask removal X1.3.3 A furnace control thermocouple may be contained in
and installation. The cover bottom is lined with aluminum foil. the flask cavity. In the furnace illustrated in Fig. 1, the
thermocouple is inset in the face of the furnace refractory, as
X1.3 Thermocouples are the heating elements.
X1.3.1 Test temperature thermocouple (T) is a bare 36
gauge chromel-alumel (Type K) junction located at the center X1.4 Flask Location
X1.4.1 If furnace depth permits, the top of the flask neck
4
The Lindberg Model 56621, available from laboratory equipment suppliers, has should be recessed beneath the top of the insulated cover,
been found satisfactory for this purpose. If you are aware of alternative suppliers,
please provide this information to ASTM International Headquarters. Your com- positioning the flask near the furnace heater center line, as in
ments will receive careful consideration at a meeting of the responsible technical Fig. 1. The resulting optimum flask location and minimal heat
committee,1 which you may attend. loss, and the use of the aluminum foil flask overwrap result in
excellent flask temperature uniformity.
TABLE X1.1 Temperature Uniformity
Test Temperature External Flask Temperature, °C
X1.5 Temperature Uniformity
(T), °C t1 t2 t3
81 81 82 82 X1.5.1 The temperatures in Table X1.1 were obtained with
232 232 236 235 the furnace configuration shown in Fig. 1; this furnace contains
343 342.3 349 347
505 504.5 512 509.5 vertical heaters set in the furnace sidewall around the entire
circumference.
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X2.1 Numerous investigators5 have noted that the larger the X2.2 The determination of the vessel volume effect involves
test vessel the lower is the autoignition temperature. Thus, repeating these procedures in three or more test volumes, such
caution is indicated in applying the temperatures derived by as 250 mL, 500 mL, 1000 mL, and 5000 mL, of the same
this test method to practical situations.6,7 geometry. A plot of autoignition temperature versus logarithm
of the vessel volume can be helpful in estimating the AITs at
5
other volumes.
Setchkin, N. P., “Self-Ignition Temperatures of Combustible Liquids,” Re-
search Paper 2516, Journal of Research, National Bureau of Standards, Vol 53, No.
7
49, 1954. Kuchta, J. M., “Summary of Ignition Properties of Jet Fuels and Other Aircraft
6
Zabetakis, M. G., Scott, G. S., and Kennedy, R. E., Autoignition of Lubricants Combustible Fluids,” Technical Report AFAPL-TR-70, Air Force Aero Propulsion
at Elevated Pressures, U.S. Bureau of Mines RI 6112, 1962. Laboratory, September 1975.
X4.1 An apparatus that has been used for gas/vapor addition X4.2.1 Sample Vessel—A vessel of sufficient size shall be
is shown in Fig. X4.1. used to prepare the gas/vapor mixtures to be tested.
NOTE X4.1—Rapid, reproducible, and accurate delivery of the test gas
is essential for the accuracy of the test results, because the test method X4.2.2 Heater and Temperature Controller—A heating sys-
seeks to find the lowest AIT corresponding to the optimal (worst case) tem with a temperature controller shall be used to heat the
concentration of the test sample. sample vessel to the desired temperature for preparation of the
X4.2 The setup seen in Fig. X4.1 is comprised of the gas/vapor mixtures. The piping leading from the sample vessel
following items: to the test flask shall also be heated to at least the temperature
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