ASTM D2883-95(2000)e1
(Test Method)Standard Test Method for Reaction Threshold Temperature of Liquid and Solid Materials
Standard Test Method for Reaction Threshold Temperature of Liquid and Solid Materials
SCOPE
1.1 This test method covers determination of the pre-flame, cool-flame, and hot-flame reaction threshold temperatures and the incipient reaction temperature of liquids and solids. Data may be obtained at pressures from low vacuum to 0.8 MPa (115 psia) for temperatures within the range from room temperature to 925 K (1200oF).
1.2 This test method may be applied to any substance that is a liquid or a solid at room temperature and atmospheric pressure and that, at room temperature, is compatible with glass and stainless steel. Air is the intended oxidizing medium; however, other media may be substituted provided appropriate precautions are taken for their safe use.
1.3 The values stated in SI units are to be regarded as the standard. In cases where materials, products, or equipment are available in inch-pound units only, SI units are omitted.
1.4 This standard should be used to measure and describe the properties of materials, products, or assemblies in response to heat and flame under controlled laboratory conditions and should not be used to describe or appraise the fire hazard or fire risk of materials, products, or assemblies under actual fire conditions. However, results of this test may be used as elements of a fire risk assessment which takes into account all of the factors which are pertinent to an assessment of the fire hazard of a particular end use.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see 6.8, Sections 7 and 9.
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An American National Standard
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Designation: D 2883 – 95 (Reapproved 2000)
Standard Test Method for
Reaction Threshold Temperature of Liquid and Solid
Materials
This standard is issued under the fixed designation D2883; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Warning notes were placed in the text editorially in November 2000.
1. Scope 2. Referenced Documents
1.1 This test method covers determination of the pre-flame, 2.1 ASTM Standards:
cool-flame, and hot-flame reaction threshold temperatures and D1193 Specification for Reagent Water
the incipient reaction temperature of liquids and solids. Data D2021 Specification for Neutral Detergent, 40 Percent
may be obtained at pressures from low vacuum to 0.8 MPa Alkylbenzene Sulfonate Type
(115 psia) for temperatures within the range from room E659 Test Method forAutoignition Temperature of Liquid
temperature to 925 K (1200°F). Chemicals
1.2 Thistestmethodmaybeappliedtoanysubstancethatis 2.2 Military Standards:
a liquid or a solid at room temperature and atmospheric MIL-C-81302 Trichlorotrifluoroethane
pressure and that, at room temperature, is compatible with MIL-T-7003 Trichloroethylene
glass and stainless steel.Air is the intended oxidizing medium;
3. Terminology
however, other media may be substituted provided appropriate
3.1 Definitions of Terms Specific to This Standard:
precautions are taken for their safe use.
1.3 The values stated in SI units are to be regarded as the 3.1.1 catalytic reaction, n—afast,self-sustaining,energetic,
sometimesluminous,sometimesaudiblereactionthatoccursas
standard. In cases where materials, products, or equipment are
available in inch-pound units only, SI units are omitted. a result of catalytic action on the surface of the thermocouple
or other solid surface within the combustion chamber.
1.4 This standard should be used to measure and describe
the properties of materials, products, or assemblies in response 3.1.2 cool-flame reaction, n—a relatively slow, self-
to heat and flame under controlled laboratory conditions and sustaining, barely luminous reaction of the sample or its
decompositionproductswiththeatmosphereinthecombustion
should not be used to describe or appraise the fire hazard or
fire risk of materials, products, or assemblies under actual fire chamber.
3.1.2.1 Discussion—This type of flame is visible only in a
conditions. However, results of this test may be used as
elements of a fire risk assessment which takes into account all darkened area. Figs. 1-4 illustrate the type of temperature
records obtained for cool-flames.
of the factors which are pertinent to an assessment of the fire
hazard of a particular end use. 3.1.3 hot-flame reaction, n—a rapid, self-sustaining, lumi-
nous, sometimes audible reaction of the sample or its decom-
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the position products with the atmosphere in the combustion
chamber.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 3.1.3.1 Discussion—Ayellow or blue flame usually accom-
panies the reaction. Figs. 5-7 illustrate the type of temperature
bility of regulatory limitations prior to use. For specific hazard
statements, see 6.8, Sections 7 and 9. records obtained for hot-flames.
1 2
This test method is under the jursidiction of ASTM Committee D02 on Annual Book of ASTM Standards, Vol 11.01.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Annual Book of ASTM Standards, Vol 15.04.
D02.11 on Engineering Sciences of High Performance Fluids and Solids. Annual Book of ASTM Standards, Vol 14.02.
Current edition approved Jan. 15, 1995. Published March 1995. Originally AvailablefromStandardizationDocumentsOrderDesk,Bldg4,SectionD,700
published as D2883–70T. Last previous edition D2883–93. Robbins Ave., Philadelphia, PA 19111-5094. Attn: NPODS.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D 2883 – 95 (2000)
FIG. 1 Time-Temperature Profile for Typical Cool-Flame Reactions
FIG. 2 Time-Temperature Profile for Typical Cool-Flame Reactions
FIG. 3 Time-Temperature Profile for Typical Cool-Flame Reactions
3.1.4 incipient reaction temperature, n—the temperature shall be regarded as the primary source of such data. The use
obtained by extrapolation of a plot of the reciprocal of the ofapressurerecordandtherecordsofothersensingdevicesto
reaction delay time versus the initial reaction temperature to obtain additional data is optional.
that value of the reciprocal which represents infinite delay 3.1.5 noncombustive reaction, n—a reaction other than
−1
(t =0) (Fig. 8). combustion or thermal degradation undergone by certain ma-
3.1.4.1 Discussion—The detection of sample reactions and terials upon exposure to elevated temperatures.
the distinctions between different reactions are based upon the 3.1.5.1 Discussion—Thermal polymerization is an example
records produced by the various sensing devices used in the of the type of reaction that may occur when dealing with
apparatus. The temperature record is basic to the method and potentially reactive substances.
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D 2883 – 95 (2000)
temperatures obtained by Test Method E659, for hot-flame autoignition,
cool-flame autoignition, and reaction threshold temperature, respectively.
5. Significance and Use
5.1 The reaction thresholds of a material are a measure of
the tendency of the material or its decomposition products to
undergo gas phase reactions of various types. Hot-flame and
cool-flame thresholds relate directly to reactions which are
involved in autoignition phenomena. Pre-flame, catalytic and
thermalpolymerizationthresholdsalsorelatetoautoignitionin
that they represent reactions which can be under some condi-
tions the precursors of ignition reactions.
6. Apparatus
6.1 Oven, fan-assisted air-circulating, with a 300 by 300 by
FIG. 4 Time-Temperature Profile for Typical Cool-Flame Reactions
300 mm minimum volume, centrally located in the oven work
spacewithinwhichtemperatureuniformityshallbe 63Kover
the temperature range from room temperature to 925 K. A
3.1.6 pre-flame reaction, n—a slow, nonluminous reaction
typical oven is detailed in the Appendix.
of the sample or its decomposition products with the atmo-
6.1.1 Temperature uniformity shall be determined by the
sphere in the combustion chamber.
following test: Eight thermocouples shall be arranged within
3.1.6.1 Discussion—Fig. 9 and Fig. 10 illustrate the type of
theoveninsuchamannerthattheyshallbelocatedatpositions
temperature records obtained for preflame reactions.
designated by the corners of a 300 mm cube. Awg No. 30,
3.1.7 reactiondelaytime,n—thetime,measuredinseconds,
calibrated, bare junction iron-constantan or Chromel-Alumel
that elapses between the introduction of the sample into the
thermocouplesaresuitable.Lead-inportsmaybepluggedwith
reaction chamber and the attainment of maximum response
insulating material during the uniformity test.
from one of the sensors used to follow the reaction (Fig. 3).
6.2 Reaction Temperature Apparatus, assembly as shown in
3.1.8 reaction threshold temperature, n—the lowest tem-
Fig. 11, comprising the following:
perature at which any reaction of the sample or its decompo-
6.2.1 Combustion Chamber, 1000 mL round-bottom, long-
sition products may be detected by a thermocouple or other
neck,AISI Type 316 stainless steel flask with 25.4 mm (1-in.)
sensing devices.
Corning ferrule, as shown in Fig. 12.
3.2 Symbols:
6.2.2 Pressure Control Manifold, as shown in Fig. 13,
T = temperature,° C
consisting of:
T8 = incipient reaction temperature,° C
6.2.2.1 Thermocouple Gland.
t = delay time, s
P = pressure, Pa or torr
6.2.2.2 Insertion Rod Guide, AISI Type 316 tube, 6.4 mm
h = hot-flame reaction
( ⁄4 in.) in outside diameter by 1.245 mm (0.049 in.) wall.
c = cool-flame reaction
6.2.2.3 Chamber Head with 25.4 mm (1-in.) Corning fer-
p = pre-flame reaction
c = catalytic reaction
rule.
n = noncombustion reaction
6.2.2.4 Pressure Transducer (optional).
6.2.2.5 Pressure Relief Valve, capable of relieving pressure
4. Summary of Test Method
at 40% above test equilibrium pressure.
4.1 A small measured amount of the sample contained in a
6.2.2.6 Air Inlet Valve, AISI Type 316 stainless steel.
glass ampoule is introduced into a stainless steel reaction
6.2.3 Electromagnet, capable of propelling insertion rod
chamber maintained at preselected temperature and pressure.
against anvil with sufficient force to break sample ampoule.
The reactions of the sample subsequent to its introduction into
6.2.4 Insertion Rod,AISI Type 316 tubing, 3.2 mm ( ⁄8 in.)
the reaction chamber are followed by monitoring the tempera-
in outside diameter by 673 mm (26.5 in.) in length with
ture or the temperature and pressure (optional) of the reaction
attached armature.
chamber as a function of time.
6.2.5 Flange Assembly, Corning Style 1 for 25.4 mm (1-in.)
4.2 Atanyselectedsystempressure,theminimumtempera-
pipe.
ture (reaction threshold temperature) required to produce a
6.2.6 Thermocouples, calibrated precision grade iron-
given reaction is determined as a function of the size of the
constantan (ISA-Type and Chromel-Alumel (ISA-Type K),
sample employed. The delay times for cool-flame and hot-
Awg No. 30 glass-fiber insulated, bare-junction (welded) in
flame reactions are also measured. A plot of the reciprocal of
5-mm borosilicate glass tube.
the reaction delay time versus the initial reaction chamber
temperatureforacool-flameorhot-flamereactionmaybeused
to determine the incipient reaction temperature by extrapola-
−1
Apparatus obtained from W.A. Sales Ltd., 419 Harvester Ct., Wheeling, IL
tion to infinite delay time (t =0).
60090 has been found satisfactory.
NOTE 1—The hot-flame reaction, cool-flame reaction, and reaction
Reducer, Swagelok 200-R-4-316BT with silicone rubber disk insert to form
thresholdtemperatureobtainedbythistestmethodmayapproximatethose seal around wire has been found satisfactory.
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D 2883 – 95 (2000)
FIG. 5 Time-Temperature Profile and Delay Time for Typical Hot-Flame Reactions
FIG. 6 Time-Temperature Profile and Delay Time for Typical Hot-Flame Reactions
FIG. 7 Time-Temperature Profile and Delay Time for Typical Hot-Flame Reactions
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D 2883 – 95 (2000)
7.3 Chloroform,technicalgrade.(Warning—Canbefatalif
swallowed. Harmful if inhaled. Can produce toxic vapors if
burned. See A2.5.)
7.4 Detergent, free-rinsing, conforming to Specification
D2021.
7.5 Reagent Water, conforming to Specification D1193,
either grade.
7.6 Acetic Acid, ACS reagent grade.
7.7 Hydroiodic Acid, 57% reagent grade.
8. Test Specimen
8.1 Liquid Sample—200 mLis sufficient for the determina-
tion of the various reaction threshold temperatures at a single
pressure.
8.2 Solid Sample—150 g is sufficient for the determination
FIG. 8 Effect of the Reaction Temperature on the Delay Time to
of the various reaction threshold temperatures at a single
Determine Incipient Reaction Temperature
pressure.
6.3 Sample Ampoule, illustrated for solids and liquids in
9. Procedure
Fig. 14.
9.1 Method A for Liquids:
6.4 Temperature Recorder, 475to1025K,(400to1400°F)
9.1.1 Clean a combustion chamber as follows: rinse with
range, ⁄4 s full-scale deflection, thermocouple actuation with
trichloroethylene (Warning—Harmful if inhaled. High con-
range changes for iron-constantan and Chromel-Alumel ele-
centrations may cause unconsciousness or death. Contact can
ments.
9 cause skin irritation and dermatitis. See A2.2.), immerse in
6.5 Hypodermic Syringe, fluorocarbon-tipped 0.5 mL and
cleaning compound for a minimum of 15 min at 293 to 308 K,
2.5 mLwith hypodermic needles suitable for introduction into
wash with detergent, and rinse thoroughly with reagent water.
sample ampoules.
Dryinanovenat393to423K.Discardthechamberifnotfree
6.6 Pressure Gages, capable of determining the appropriate
of deposits. Clean the thermocouple internal supports, anvil,
pressure with an accuracy of 61%.
and insertion rod in the same manner.
6.7 Vacuum System, capable of attaining and maintaining
the required pressure with mechanical vacuum pump and
NOTE 2—Achloroform(see7.3)rinsepriortowashingcanproveuseful
cold trap inserted in the line between the reaction temperature in some cases. Difficult deposits may be removed by walnut shell
abrasion. Discard the chamber if deposits can not be removed or if
apparatus and the pump.
inspection reveals that the interior of the chamber has been damaged or
6.8 Gas Supply System, capable of supplying the appro-
corroded.
priate gas, dewpoint 215 K (−70°F) maximum and essentially
NOTE 3—Stainless steel, Type 316 combustion chambers and an air
free of contaminants at pressures up to 0.8 MPa. (Warning—
atmospherehavebeenspecifiedwiththistestmethod.However,chambers
Compressed gas under high pressure. Gas reduces oxygen
of other materials and of different sizes, and atmospheres of other gases
available for breathing. See A2.1.)
may be used when required.
6.9 Exhaust Hood, capable of disposing of fumes vented NOTE 4—Chambers may be tested for the presence of peroxide or free
radical residues by purging them with nitrogen and rinsing with a freshly
from the reaction temperature apparatus.
prepared mixture of 3 mL each of chloroform, glacial acetic acid,
(Warning—Poison. Corrosive. Combustible. Can be fatal if swallowed.
7. Reagents and Materials
Causes severe burns. Harmful if inhaled. See A2.6) and hydroiodic acid
7.1 Trichloroethylene, conforming to MIL-T-7003. Trichlo-
(57%analyticalgrade,notstabilized)(Warning—Poison.Corrosive.Can
rotrifluoroethane conforming to MIL-C-81302 or high flash
be fatal if swallowed. Liquid and vapor cause severe burns. Harmful if
point naphtha may be used as alternatives. (Warning— inhaled. SeeA2.7). When this mixture is poured into a clean glass vessel
and 10 drops of stabilized starch solution added, a trace of the starch-
Harmful if inhaled. High concentrations may cause uncon-
iodine color reaction indicates no peroxides or free radicals are present.
sciousness or death. Contact can cause skin irritation and
dermatitis. See A2.2.)
9.1.2 Assemblethereactiontemperatureapparatusinaccor-
7.2 Cleaning Compounds. dance with Fig. 11, using a clean combustion chamber. Insert
the assemb
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