ASTM D2883-95(2009)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D2883 −95(Reapproved 2009)
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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope D2021SpecificationforNeutralDetergent,40PercentAlky-
lbenzene Sulfonate Type (Withdrawn 2000)
1.1 This test method covers determination of the pre-flame,
E659Test Method for Autoignition Temperature of Liquid
cool-flame, and hot-flame reaction threshold temperatures and
Chemicals
the incipient reaction temperature of liquids and solids. Data
2.2 Military Standards:
may be obtained at pressures from low vacuum to 0.8 MPa
MIL-C-81302Trichlorotrifluoroethane
(115 psia) for temperatures within the range from room
MIL-T-7003Trichloroethylene
temperature to 925 K (1200°F).
1.2 Thistestmethodmaybeappliedtoanysubstancethatis
3. Terminology
a liquid or a solid at room temperature and atmospheric
3.1 Definitions of Terms Specific to This Standard:
pressure and that, at room temperature, is compatible with
3.1.1 catalytic reaction, n—afast,self-sustaining,energetic,
glass and stainless steel.Air is the intended oxidizing medium;
sometimesluminous,sometimesaudiblereactionthatoccursas
however, other media may be substituted provided appropriate
a result of catalytic action on the surface of the thermocouple
precautions are taken for their safe use.
or other solid surface within the combustion chamber.
1.3 The values stated in SI units are to be regarded as the
3.1.2 cool-flame reaction, n—a relatively slow, self-
standard. In cases where materials, products, or equipment are
sustaining, barely luminous reaction of the sample or its
available in inch-pound units only, SI units are omitted.
decompositionproductswiththeatmosphereinthecombustion
1.4 This standard is used to measure and describe the
chamber.
response of materials, products, or assemblies to heat and
3.1.2.1 Discussion—This type of flame is visible only in a
flame under controlled conditions, but does not by itself
darkened area. Figs. 1-4 illustrate the type of temperature
incorporate all factors required for fire hazard or fire risk
records obtained for cool-flames.
assessment of the materials, products, or assemblies under
3.1.3 hot-flame reaction, n—a rapid, self-sustaining,
actual fire conditions.
luminous, sometimes audible reaction of the sample or its
1.5 This standard does not purport to address all of the
decompositionproductswiththeatmosphereinthecombustion
safety concerns, if any, associated with its use. It is the
chamber.
responsibility of the user of this standard to establish appro-
3.1.3.1 Discussion—Ayellow or blue flame usually accom-
priate safety and health practices and determine the applica-
panies the reaction. Figs. 5-7 illustrate the type of temperature
bility of regulatory limitations prior to use. For specific
records obtained for hot-flames.
warning statements, see 6.8, Sections 7 and 9.
3.1.4 incipient reaction temperature, n—the temperature
2. Referenced Documents
obtained by extrapolation of a plot of the reciprocal of the
reaction delay time versus the initial reaction temperature to
2.1 ASTM Standards:
that value of the reciprocal which represents infinite delay
D1193Specification for Reagent Water
−1
(t =0)(Fig. 8).
3.1.4.1 Discussion—The detection of sample reactions and
This test method is under the jursidiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
the distinctions between different reactions are based upon the
SubcommitteeD02.L0.07onEngineeringSciencesofHighPerformanceFluidsand
records produced by the various sensing devices used in the
Solids (Formally D02.1100).
apparatus. The temperature record is basic to the method and
Current edition approved Oct. 1, 2009. Published November 2009. Originally
approved in 1970. Last previous edition approved in 2005 as D2883–95(2005).
DOI: 10.1520/D2883-95R09.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or The last approved version of this historical standard is referenced on
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM www.astm.org.
Standards volume information, refer to the standard’s Document Summary page on AvailablefromStandardizationDocumentsOrderDesk,Bldg4,SectionD,700
the ASTM website. 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
D2883−95 (2009)
FIG. 1Time-Temperature Profile for Typical Cool-Flame Reactions
FIG. 2Time-Temperature Profile for Typical Cool-Flame Reactions
FIG. 3Time-Temperature Profile for Typical Cool-Flame Reactions
shall be regarded as the primary source of such data. The use of the type of reaction that may occur when dealing with
ofapressurerecordandtherecordsofothersensingdevicesto potentially reactive substances.
obtain additional data is optional.
3.1.6 pre-flame reaction, n—a slow, nonluminous reaction
3.1.5 noncombustivereaction,n—areactionotherthancom- of the sample or its decomposition products with the atmo-
bustion or thermal degradation undergone by certain materials sphere in the combustion chamber.
upon exposure to elevated temperatures. 3.1.6.1 Discussion—Fig. 9 and Fig. 10 illustrate the type of
3.1.5.1 Discussion—Thermal polymerization is an example temperature records obtained for preflame reactions.
D2883−95 (2009)
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.
5,6
6. Apparatus
6.1 Oven, fan-assisted air-circulating, with a 300 by 300 by
300 mm minimum volume, centrally located in the oven work
spacewithinwhichtemperatureuniformityshallbe 63Kover
the temperature range from room temperature to 925 K. A
FIG. 4 Time-Temperature Profile for Typical Cool-Flame Reac-
tions typical oven is detailed in the Appendix.
6.1.1 Temperature uniformity shall be determined by the
following test: Eight thermocouples shall be arranged within
theoveninsuchamannerthattheyshallbelocatedatpositions
3.1.7 reaction delay time, n—thetime,measuredinseconds, designated by the corners of a 300 mm cube. Awg No. 30,
that elapses between the introduction of the sample into the calibrated, bare junction iron-constantan or Chromel-Alumel
reaction chamber and the attainment of maximum response thermocouplesaresuitable.Lead-inportsmaybepluggedwith
from one of the sensors used to follow the reaction (Fig. 3). insulating material during the uniformity test.
3.1.8 reaction threshold temperature, n—the lowest tem-
6.2 Reaction Temperature Apparatus, assembly as shown in
perature at which any reaction of the sample or its decompo-
Fig. 11, comprising the following:
sition products may be detected by a thermocouple or other
6.2.1 Combustion Chamber, 1000 mL round-bottom, long-
sensing devices.
neck,AISI Type 316 stainless steel flask with 25.4 mm (1-in.)
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:
T' = incipient reaction temperature,° C
6,7
t = delay time, s
6.2.2.1 Thermocouple Gland.
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
p = pre-flame reaction
6.2.2.3 Chamber Head with 25.4 mm (1-in.) Corning fer-
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 At any selected system pressure, the minimum tempera-
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-
The sole source of supply of the apparatus known to the committee at this time
−1
tion to infinite delay time (t =0). is W.A. Sales Ltd., 419 Harvester Ct., Wheeling, IL 60090.
If you are aware of alternative suppliers, please provide this information to
NOTE 1—The hot-flame reaction, cool-flame reaction, and reaction
ASTM International Headquarters. Your comments will receive careful consider-
thresholdtemperatureobtainedbythistestmethodmayapproximatethose
ation at a meeting of the responsible technical committee, which you may attend.
temperatures obtained by Test Method E659, for hot-flame autoignition, Reducer, Swagelok 200-R-4-316BT with silicone rubber disk insert to form
cool-flame autoignition, and reaction threshold temperature, respectively. seal around wire has been found satisfactory.
D2883−95 (2009)
FIG. 5Time-Temperature Profile and Delay Time for Typical Hot-Flame Reactions
FIG. 6Time-Temperature Profile and Delay Time for Typical Hot-Flame Reactions
FIG. 7Time-Temperature Profile and Delay Time for Typical Hot-Flame Reactions
6.3 Sample Ampoule, illustrated for solids and liquids in
Fig. 14.
D2883−95 (2009)
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 mL is sufficient for the determina-
tion of the various reaction threshold temperatures at a single
FIG. 8 Effect of the Reaction Temperature on the Delay Time to
pressure.
Determine Incipient Reaction Temperature
8.2 Solid Sample—150 g is sufficient for the determination
of the various reaction threshold temperatures at a single
6,8
6.4 Temperature Recorder, 475 to 1025 K, (400 to
pressure.
1400°F) range, ⁄4 s full-scale deflection, thermocouple actua-
tion with range changes for iron-constantan and Chromel-
9. Procedure
Alumel elements.
9.1 Method A for Liquids:
6,9
6.5 HypodermicSyringe, fluorocarbon-tipped0.5mLand
9.1.1 Clean a combustion chamber as follows: rinse with
2.5 mLwith hypodermic needles suitable for introduction into
trichloroethylene (Warning—Harmful if inhaled. High con-
sample ampoules.
centrations may cause unconsciousness or death. Contact can
6.6 Pressure Gauges, capable of determining the appropri-
cause skin irritation and dermatitis. See A2.2.), immerse in
ate pressure with an accuracy of 61%.
cleaning compound for a minimum of 15 min at 293 to 308 K,
wash with detergent, and rinse thoroughly with reagent water.
6.7 Vacuum System, capable of attaining and maintaining
6,10
Dryinanovenat393to423K.Discardthechamberifnotfree
the required pressure with mechanical vacuum pump and
of deposits. Clean the thermocouple internal supports, anvil,
cold trap inserted in the line between the reaction temperature
and insertion rod in the same manner.
apparatus and the pump.
6,11
6.8 Gas Supply System, capable of supplying the appro- NOTE2—Achloroform(see7.3)rinsepriortowashingcanproveuseful
in some cases. Difficult deposits may be removed by walnut shell
priate gas, dewpoint 215 K (−70°F) maximum and essentially
abrasion. Discard the chamber if deposits can not be removed or if
free of contaminants at pressures up to 0.8 MPa. (Warning—
inspection reveals that the interior of the chamber has been damaged or
Compressed gas under high pressure. Gas reduces oxygen
corroded.
available for breathing. See A2.1.)
NOTE 3—Stainless steel, Type 316 combustion chambers and an air
atmospherehavebeenspecifiedwiththistestmethod.However,chambers
6.9 Exhaust Hood, capable of disposing of fumes vented
of other materials and of different sizes, and atmospheres of other gases
from the reaction temperature apparatus.
may be used when required.
NOTE 4—Chambers may be tested for the presence of peroxide or free
7. Reagents and Materials
radical residues by purging them with nitrogen and rinsing with a freshly
prepared mixture of 3 mL each of chloroform, glacial acetic acid,
7.1 Trichloroethylene, conforming to MIL-T-7003. Trichlo-
(Warning—Poison. Corrosive. Combustible. Can be fatal if swallowed.
rotrifluoroethane conforming to MIL-C-81302 or high flash
Causes severe burns. Harmful if inhaled. See A2.6) and hydroiodic acid
point naphtha may be used as alternatives. (Warning—
(57%analyticalgrade,notstabilized)(Warning—Poison.Corrosive.Can
Harmful if inhaled. High concentrations may cause uncon-
be fatal if swallowed. Liquid and vapor cause severe burns. Harmful if
inhaled. SeeA2.7). When this mixture is poured into a clean glass vessel
sciousness or death. Contact can cause skin irritation and
and 10 drops of stabilized starch solution added, a trace of the starch-
dermatitis. See A2.2.)
iodine color
...