1、Designation: D 2883 95 (Reapproved 2005)An American National StandardStandard Test Method forReaction Threshold Temperature of Liquid and SolidMaterials1This standard is issued under the fixed designation D 2883; the number immediately following the designation indicates the year oforiginal adoption
2、 or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers determination of the pre-flame,cool-flame, and hot-
3、flame reaction threshold temperatures andthe incipient reaction temperature of liquids and solids. Datamay be obtained at pressures from low vacuum to 0.8 MPa(115 psia) for temperatures within the range from roomtemperature to 925 K (1200F).1.2 This test method may be applied to any substance that i
4、sa liquid or a solid at room temperature and atmosphericpressure and that, at room temperature, is compatible withglass and stainless steel.Air is the intended oxidizing medium;however, other media may be substituted provided appropriateprecautions are taken for their safe use.1.3 The values stated
5、in SI units are to be regarded as thestandard. In cases where materials, products, or equipment areavailable in inch-pound units only, SI units are omitted.1.4 This standard should be used to measure and describethe properties of materials, products, or assemblies in responseto heat and flame under
6、controlled laboratory conditions andshould not be used to describe or appraise the fire hazard orfire risk of materials, products, or assemblies under actual fireconditions. However, results of this test may be used aselements of a fire risk assessment which takes into account allof the factors whic
7、h are pertinent to an assessment of the firehazard of a particular end use.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determin
8、e the applica-bility of regulatory limitations prior to use. For specific hazardstatements, see 6.8, Sections 7 and 9.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 2021 Specification for Neutral Detergent, 40 PercentAlkylbenzene Sulfonate TypeE 659 Test Method fo
9、r Autoignition Temperature of LiquidChemicals2.2 Military Standards:3MIL-C-81302 TrichlorotrifluoroethaneMIL-T-7003 Trichloroethylene3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 catalytic reaction, na fast, self-sustaining, energetic,sometimes luminous, sometimes audible re
10、action that occurs asa result of catalytic action on the surface of the thermocoupleor other solid surface within the combustion chamber.3.1.2 cool-flame reaction, na relatively slow, self-sustaining, barely luminous reaction of the sample or itsdecomposition products with the atmosphere in the comb
11、ustionchamber.3.1.2.1 DiscussionThis type of flame is visible only in adarkened area. Figs. 1-4 illustrate the type of temperaturerecords obtained for cool-flames.3.1.3 hot-flame reaction, na rapid, self-sustaining, lumi-nous, sometimes audible reaction of the sample or its decom-position products w
12、ith the atmosphere in the combustionchamber.3.1.3.1 DiscussionA yellow or blue flame usually accom-panies the reaction. Figs. 5-7 illustrate the type of temperaturerecords obtained for hot-flames.1This test method is under the jursidiction of ASTM Committee D02 onPetroleum Products and Lubricants an
13、d is the direct responsibility of SubcommitteeD02.11 on Engineering Sciences of High Performance Fluids and Solids.Current edition approved June 1, 2005. Published September 2005. Originallyapproved in 1970. Last previous edition approved in 2000 as D 288395(2000)e1.2For referenced ASTM standards, v
14、isit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from Standardization Documents Order Desk, Bldg 4, Section D, 700Robbins Ave., Phil
15、adelphia, PA 19111-5094. Attn: NPODS.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.4 incipient reaction temperature, nthe temperatureobtained by extrapolation of a plot of the reciprocal of thereaction delay time versus the ini
16、tial reaction temperature tothat value of the reciprocal which represents infinite delay(t1=0)(Fig. 8).3.1.4.1 DiscussionThe detection of sample reactions andthe distinctions between different reactions are based upon therecords produced by the various sensing devices used in theapparatus. The tempe
17、rature record is basic to the method andshall be regarded as the primary source of such data. The useof a pressure record and the records of other sensing devices toobtain additional data is optional.3.1.5 noncombustive reaction, na reaction other thancombustion or thermal degradation undergone by c
18、ertain ma-terials upon exposure to elevated temperatures.3.1.5.1 DiscussionThermal polymerization is an exampleof the type of reaction that may occur when dealing withpotentially reactive substances.FIG. 1 Time-Temperature Profile for Typical Cool-Flame ReactionsFIG. 2 Time-Temperature Profile for T
19、ypical Cool-Flame ReactionsFIG. 3 Time-Temperature Profile for Typical Cool-Flame ReactionsD 2883 95 (2005)23.1.6 pre-flame reaction, na slow, nonluminous reactionof the sample or its decomposition products with the atmo-sphere in the combustion chamber.3.1.6.1 DiscussionFig. 9 and Fig. 10 illustrat
20、e the type oftemperature records obtained for preflame reactions.3.1.7 reaction delay time, nthe time, measured in seconds,that elapses between the introduction of the sample into thereaction chamber and the attainment of maximum responsefrom one of the sensors used to follow the reaction (Fig. 3).3
21、.1.8 reaction threshold temperature, nthe lowest tem-perature at which any reaction of the sample or its decompo-sition products may be detected by a thermocouple or othersensing devices.3.2 Symbols:T = temperature, CT8 = incipient reaction temperature, Ct = delay time, sP = pressure, Pa or torrh =
22、hot-flame reactionc = cool-flame reactionp = pre-flame reactionc = catalytic reactionn = noncombustion reaction4. Summary of Test Method4.1 A small measured amount of the sample contained in aglass ampoule is introduced into a stainless steel reactionchamber maintained at preselected temperature and
23、 pressure.The reactions of the sample subsequent to its introduction intothe reaction chamber are followed by monitoring the tempera-ture or the temperature and pressure (optional) of the reactionchamber as a function of time.4.2 At any selected system pressure, the minimum tempera-ture (reaction th
24、reshold temperature) required to produce agiven reaction is determined as a function of the size of thesample employed. The delay times for cool-flame and hot-flame reactions are also measured. A plot of the reciprocal ofthe reaction delay time versus the initial reaction chambertemperature for a co
25、ol-flame or hot-flame reaction may be usedto determine the incipient reaction temperature by extrapola-tion to infinite delay time (t1= 0).NOTE 1The hot-flame reaction, cool-flame reaction, and reactionthreshold temperature obtained by this test method may approximate thosetemperatures obtained by T
26、est Method E 659, for hot-flame autoignition,cool-flame autoignition, and reaction threshold temperature, respectively.5. Significance and Use5.1 The reaction thresholds of a material are a measure ofthe tendency of the material or its decomposition products toundergo gas phase reactions of various
27、types. Hot-flame andcool-flame thresholds relate directly to reactions which areinvolved in autoignition phenomena. Pre-flame, catalytic andthermal polymerization thresholds also relate to autoignition inthat they represent reactions which can be under some condi-tions the precursors of ignition rea
28、ctions.6. Apparatus4,56.1 Oven, fan-assisted air-circulating, with a 300 by 300 by300 mm minimum volume, centrally located in the oven workspace within which temperature uniformity shall be 63 K overthe temperature range from room temperature to 925 K. Atypical oven is detailed in the Appendix.6.1.1
29、 Temperature uniformity shall be determined by thefollowing test: Eight thermocouples shall be arranged withinthe oven in such a manner that they shall be located at positionsdesignated by the corners of a 300 mm cube. Awg No. 30,calibrated, bare junction iron-constantan or Chromel-Alumelthermocoupl
30、es are suitable. Lead-in ports may be plugged withinsulating material during the uniformity test.6.2 Reaction Temperature Apparatus, assembly as shown inFig. 11, comprising the following:6.2.1 Combustion Chamber, 1000 mL round-bottom, long-neck, AISI Type 316 stainless steel flask with 25.4 mm (1-in
31、.)Corning ferrule, as shown in Fig. 12.6.2.2 Pressure Control Manifold, as shown in Fig. 13,consisting of:6.2.2.1 Thermocouple Gland.5,66.2.2.2 Insertion Rod Guide, AISI Type 316 tube, 6.4 mm(14 in.) in outside diameter by 1.245 mm (0.049 in.) wall.6.2.2.3 Chamber Head with 25.4 mm (1-in.) Corning f
32、er-rule.6.2.2.4 Pressure Transducer (optional).6.2.2.5 Pressure Relief Valve, capable of relieving pressureat 40 % above test equilibrium pressure.6.2.2.6 Air Inlet Valve, AISI Type 316 stainless steel.6.2.3 Electromagnet, capable of propelling insertion rodagainst anvil with sufficient force to bre
33、ak sample ampoule.6.2.4 Insertion Rod, AISI Type 316 tubing, 3.2 mm (18 in.)in outside diameter by 673 mm (26.5 in.) in length withattached armature.6.2.5 Flange Assembly, Corning Style 1 for 25.4 mm (1-in.)pipe.6.2.6 Thermocouples, calibrated precision grade iron-constantan (ISA-Type and Chromel-Al
34、umel (ISA-Type K),4The sole source of supply of the apparatus known to the committee at this timeis W.A. Sales Ltd., 419 Harvester Ct., Wheeling, IL 60090.5If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful
35、 consider-ation at a meeting of the responsible technical committee,1which you may attend.6Reducer, Swagelok 200-R-4-316BT with silicone rubber disk insert to formseal around wire has been found satisfactory.FIG. 4 Time-Temperature Profile for Typical Cool-Flame ReactionsD 2883 95 (2005)3Awg No. 30
36、glass-fiber insulated, bare-junction (welded) in5-mm borosilicate glass tube.6.3 Sample Ampoule, illustrated for solids and liquids inFig. 14.FIG. 5 Time-Temperature Profile and Delay Time for Typical Hot-Flame ReactionsFIG. 6 Time-Temperature Profile and Delay Time for Typical Hot-Flame ReactionsFI
37、G. 7 Time-Temperature Profile and Delay Time for Typical Hot-Flame ReactionsD 2883 95 (2005)46.4 Temperature Recorder,5,7475 to 1025 K, (400 to1400F) range,14 s full-scale deflection, thermocouple actua-tion with range changes for iron-constantan and Chromel-Alumel elements.6.5 Hypodermic Syringe,5,
38、8fluorocarbon-tipped 0.5 mLand2.5 mL with hypodermic needles suitable for introduction intosample ampoules.6.6 Pressure Gages, capable of determining the appropriatepressure with an accuracy of 61%.6.7 Vacuum System, capable of attaining and maintainingthe required pressure with mechanical vacuum pu
39、mp5,9andcold trap inserted in the line between the reaction temperatureapparatus and the pump.6.8 Gas Supply System,5,10capable of supplying the ap-propriate gas, dewpoint 215 K (70F) maximum and essen-tially free of contaminants at pressures up to 0.8 MPa.(WarningCompressed gas under high pressure.
40、 Gas reducesoxygen available for breathing. See A2.1.)6.9 Exhaust Hood, capable of disposing of fumes ventedfrom the reaction temperature apparatus.7. Reagents and Materials7.1 Trichloroethylene, conforming to MIL-T-7003. Trichlo-rotrifluoroethane conforming to MIL-C-81302 or high flashpoint naphtha
41、 may be used as alternatives. (WarningHarmful if inhaled. High concentrations may cause uncon-sciousness or death. Contact can cause skin irritation anddermatitis. See A2.2.)7.2 Cleaning Compounds.5,117.3 Chloroform, technical grade. (WarningCan be fatal ifswallowed. Harmful if inhaled. Can produce
42、toxic vapors ifburned. See A2.5.)7.4 Detergent, free-rinsing, conforming to SpecificationD 2021.7.5 Reagent Water, conforming to Specification D 1193,either grade.7.6 Acetic Acid, ACS reagent grade.7.7 Hydroiodic Acid, 57 % reagent grade.8. Test Specimen8.1 Liquid Sample200 mL is sufficient for the
43、determina-tion of the various reaction threshold temperatures at a singlepressure.8.2 Solid Sample150 g is sufficient for the determinationof the various reaction threshold temperatures at a singlepressure.9. Procedure9.1 Method A for Liquids:9.1.1 Clean a combustion chamber as follows: rinse withtr
44、ichloroethylene (WarningHarmful if inhaled. High con-centrations may cause unconsciousness or death. Contact cancause skin irritation and dermatitis. See A2.2.), immerse incleaning compound for a minimum of 15 min at 293 to 308 K,wash with detergent, and rinse thoroughly with reagent water.Dry in an
45、 oven at 393 to 423 K. Discard the chamber if not freeof deposits. Clean the thermocouple internal supports, anvil,and insertion rod in the same manner.NOTE 2Achloroform (see 7.3) rinse prior to washing can prove usefulin some cases. Difficult deposits may be removed by walnut shellabrasion. Discard
46、 the chamber if deposits can not be removed or ifinspection reveals that the interior of the chamber has been damaged orcorroded.NOTE 3Stainless steel, Type 316 combustion chambers and an airatmosphere have been specified with this test method. However, chambersof other materials and of different si
47、zes, and atmospheres of other gasesmay be used when required.NOTE 4Chambers may be tested for the presence of peroxide or freeradical residues by purging them with nitrogen and rinsing with a freshlyprepared mixture of 3 mL each of chloroform, glacial acetic acid,(WarningPoison. Corrosive. Combustib
48、le. Can be fatal if swallowed.Causes severe burns. Harmful if inhaled. See A2.6) and hydroiodic acid(57 % analytical grade, not stabilized) (WarningPoison. Corrosive. Canbe fatal if swallowed. Liquid and vapor cause severe burns. Harmful ifinhaled. See A2.7). When this mixture is poured into a clean
49、 glass vesseland 10 drops of stabilized starch solution added, a trace of the starch-iodine color reaction indicates no peroxides or free radicals are present.9.1.2 Assemble the reaction temperature apparatus in accor-dance with Fig. 11, using a clean combustion chamber. Insertthe assembly horizontally in the oven to the middle of thetemperature-controlled zone to a minimum inside depth of 21cm.9.1.3 Connect the vacuum system, gas supply system(WarningCompressed gas under high pressure. Gas reducesoxygen available for breathing. SeeA2.1.), pres
