ASTM E2046-2003 Standard Test Method for Reaction Induction Time by Thermal Analysis《用热分析法测定反应感应时间的标准试验方法》.pdf

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1、Designation: E 2046 03Standard Test Method forReaction Induction Time by Thermal Analysis1This standard is issued under the fixed designation E 2046; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A numb

2、er 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 describes the measurement of ReactionInduction Time (RIT) of chemical materials that undergoexothermic reactions with an

3、induction period. The techniquesand apparatus described may be used for solids, liquids, orslurries of chemical substances. The temperature range coveredby this test method is typically from ambient to 400C. Thisrange may be extended depending upon the apparatus used.1.2 The RIT is a relative index

4、value, not an absolutethermodynamic property.As an index value, the RIT value maychange depending upon experimental conditions. A compari-son of RIT values may be made only for materials tested undersimilar conditions of apparatus, specimen size, and so forth.Furthermore, the RIT value may not predi

5、ct behavior of largequantities of material.1.3 The RIT shall not be used by itself to establish a safeoperating temperature. It may be used in conjunction withother test methods (for example, E 487, E 537, and E 1981 aspart of a hazard analysis of a particular operation.1.4 This test method may be u

6、sed for RIT values greaterthan 15 min (as relative imprecision increases at shorterperiods).1.5 This test method is used to study catalytic and autocata-lytic reactions. These reactions depend upon time as well astemperature. Such reactions are often studied by fixing oneexperimental parameter (that

7、 is, time or temperature) and thenmeasuring the other parameter (that is, temperature or time).This test method measures time to reaction onset detectionunder isothermal conditions. It is related to Test Method E 487that measures detected reaction onset temperature under con-stant time conditions1.6

8、 SI units are the standard.1.7 There is no ISO standard equivalent to this test method.1.8 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 consult andestablish appropriate safety and health

9、practices and deter-mine the applicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:D 3350 Specification for Polyethylene Plastics Pipe andFittings Materials2D 3895 Test Method for Oxidative-Induction Time of Poly-olefins by Differential Scanning Calorimetry2D

10、 4565 Test Methods for Physical and Environmental Per-formance Properties of Insulations and Jackets for Tele-communications Wire and Cable3D 5483 Test Method for Oxidation Induction Time of Lu-bricating Greases by Pressure Differential Scanning Calo-rimetry4D 6186 Test Method for Oxidation Inductio

11、n Time of Lu-bricating Oils by Pressure Differential Scanning Calorim-etryE 473 Terminology Relating to Thermal Analysis5E 487 Test Method for Constant-Temperature Stability ofChemical Materials5E 537 Test Method for Assessing the Thermal Stability ofChemicals by Methods of Differential Thermal Anal

12、ysis5E 967 Practice for Temperature Calibration of DifferentialScanning Calorimeters and Differential Thermal Analyz-ers5E 968 Practice for Heat Flow Calibration of DifferentialScanning Calorimeters5E 1445 Terminology Relating to Hazardous Potential ofChemicals5E 1858 Test Method for Determining Oxi

13、dative InductionTime of Hydrocarbons by Differential Scanning Calorim-etry5E 1860 Test Method for Elapsed Time Calibration of Ther-mal Analyzers5E 1981 Guide for Assessing the Thermal Stability of Mate-rials by Method of Accelerating Rate Calorimetry5E 2070 Test Method for Kinetic Parameters by Diff

14、erentialScanning Calorimetry Using Isothermal Methods53. Terminology3.1 The specialized terms used in this test method aredescribed in Terminologies E 473 and E 1445.1This test method is under the jurisdiction of ASTM Committee E27 on HazardPotential of Chemicals and is the direct responsibility of

15、Subcommittee E27.02 onThermal Stability and Condensed Phases.Current edition approved July 10, 2003. Published September 2003. Originallyapproved in 1999. Last previous edition approved in 1999 as E 2046 99.2Annual Book of ASTM Standards, Vol 08.02.3Annual Book of ASTM Standards, Vol 10.02.4Annual B

16、ook of ASTM Standards, Vol 05.03.5Annual Book of ASTM Standards, Vol 14.02.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2 Definitions of Terms Specific to This Standard:3.2.1 constant temperature stability (CTS) value, nthemaxim

17、um temperature at which a chemical compound ormixture may be held for a minimum of two hours withoutexhibiting a measurable exothermic reaction. (See Test MethodE 487.)3.2.2 reaction induction time (RIT) value, nthe time achemical compound or mixture may be held under isothermalconditions until it e

18、xhibits a specified exothermic reaction.4. Summary of Test Method4.1 A specimen of the chemical compound or mixture isplaced in an inert container that is then heated to an operator-selected test temperature of interest. The specimen temperatureand the difference in heat flow or temperature between

19、the testspecimen and an inert reference are monitored until an exo-thermic reaction is recorded. The time from the attainment ofthe isothermal test temperature until the extrapolated onset tothe exothermic reaction is taken as the Reaction InductionTime.4.2 Using fresh specimens measurements at more

20、 than oneisothermal test temperature may be made.4.3 The RIT is expressed as time at a specific test tempera-ture. For example:RIT = 120 min at 100C5. Significance and Use5.1 This test method measures the time to extrapolated onsetof an exothermic reaction under constant temperature (isother-mal) co

21、nditions for reactions which have an induction period,for example, those which are catalytic or autocatalytic in natureor which contain reaction inhibitors.5.2 The RIT determined by this test method is to beconsidered an index measurement that is useful for comparingone material to another at the te

22、st temperature of interest and inthe same apparatus type only.5.3 This test method is a useful adjunct to dynamic thermaltests, such as Test Method E 537, which are performed underconditions in which the sample temperature is increasedcontinuously at constant rate. Results obtained under dynamictest

23、 conditions may result in higher estimates of temperature atwhich an exothermic reaction initiates because the detectedonset temperature is dependent upon the heating rate andbecause dynamic methods allow insufficient time for autocata-lytic reactions to measurably affect the onset temperature.5.4 R

24、IT values determined under a series of isothermal testconditions may be plotted as their logarithm versus thereciprocal of the absolute temperature to produce a plot, theslope of which is proportional to the activation energy of thereaction as described in Test Method E 2070.5.5 This test method may

25、 be used in research and develop-ment, manufacturing, process and quality control, and regula-tory compliance.5.6 This test method is similar to that for Oxidation Induc-tion Time (OIT) (for example, Specification D 3350 and TestMethods D 3895, D 4565, D 5483, D 6186, and E 1858) wherethe time to th

26、e oxidation reaction under isothermal testconditions is measured. The OIT test method measures thepresence of antioxidant packages and is a relative measurementof a materials resistance to oxidation.6. Apparatus6.1 The design and complexity of the apparatus required forthis test method depends upon

27、the size of the specimen to beused. In general, observation of an exothermic reaction in smallspecimens (less than 50 mg) is performed using differentialscanning calorimetry or differential thermal analysis equipmentand techniques. Large samples (up to 2 g) may be tested usingdevices such as the Kuh

28、ner Micro CTS apparatus.6.2 The following items are required to obtain the appro-priate experimental data.NOTE 1Commercially available differential scanning calorimetry ap-paratus may be used. Alternatively, the apparatus may be assembled orfabricated from commercially available components.6.2.1 Tes

29、t Chamber, composed of the following:6.2.1.1 Furnace(s), to provide uniform controlled heating ofa specimen and reference to a constant temperature.6.2.1.2 Temperature Sensor, to provide an indication ofspecimen/furnace temperature to 60.1 K.6.2.1.3 Differential Sensor, to detect a difference in hea

30、tflow (or temperature) between the specimen and the referencespecimen equivalent to 10 W or 0.01 mK.NOTE 2A reference material is used when differential heat flow ordifferential temperature measurements are made. The reference materialshould match the physical state and heat capacity of the specimen

31、 asclosely as practical. Typical reference materials include calcined alumi-num oxide, glass beads, silicone oil, or combinations thereof.6.2.1.4 Means of Sustaining a Test Chamber Environment,through the use of an air purge gas at a rate of 10 to 100 6 5mL/min.NOTE 3Typically, air or inert 99.9+ %

32、pure nitrogen, argon, or heliumis employed (when oxidation in air is a concern). Unless effects ofmoisture are to be studied, use of dry purge gas is recommended.NOTE 4For the Kuhner Micro CTS apparatus, the purge gas isprovided by operation in a laboratory hood with the door(s) approximately50 % cl

33、osed.6.2.2 Temperature Controller, capable of heating from am-bient to 400C at a rate of up to 20C/min and maintaining anisothermal temperature constant within that range of 60.4Cfor the duration of the test, or both.6.2.3 Recording Device, either digital or analog, to recordand display any fraction

34、 of the differential heat flow ordifferential temperatures, test specimen temperature, and time,including signal noise, to the sensitivities previously described.Typical temperature ranges are from ambient to 400C. Typicaltime ranges are from 0 to 200 min.6.2.4 Containers (pans, crucibles, vials, te

35、st tubes, and soforth, and lids), which are inert to the specimen and referencematerials at the maximum temperature used and which are ofsuitable structure, shape, and integrity to contain the specimenand reference in accordance with the temperature and massrequirements as described in this section.

36、6.3 Balance, with a capacity of 100 mg or more to weighspecimens or containers to 60.1 mg.NOTE 5A balance capacity of 10 g or more with a readability to 60.1E2046032g is required for use with the Kuhner Micro CTS device.7. Hazards7.1 Dynamic thermal tests, utilizing milligram quantities ofmaterials,

37、 such as Test Method E 537, are normally conductedon specimens before the present test is undertaken. Theexperimenter shall have sufficient knowledge of the magnitudeof hazard associated with the material. Larger specimens shallbe used only after due consideration is given to the potential forhazard

38、ous reaction. Thermodynamic calculations also may beused to determine the potential hazard.7.2 Special precautions shall be taken to protect personneland equipment when the apparatus in use requires the insertionof specimens into a heated block or furnace. These shallinclude adequate shielding and v

39、entilation of equipment, andface and hand protection (see Note 8).8. Sampling8.1 Specimens shall be representative of the material beingstudied and shall be prepared to achieve good thermal contactbetween the specimen and the container.8.2 Specimen size depends upon the sensitivity of theavailable a

40、pparatus.NOTE 6Specimen size of1-7mgistypically used in thermal analysisapparatus. Specimen size of 1 - 2 g is typically used with the KuhnerMicro CTS apparatus.8.3 Specimens may be run in an unconfined or in a sealedcontainer, depending upon which condition has the morerelevance for the end use of

41、the data.9. Calibration9.1 Apparatus temperature calibration shall be performed inaccordance with Practice E 967 at a heating rate of 1C/min.9.2 Apparatus heat flow calibration may be performed inaccordance with Practice E 968.9.3 Apparatus elapsed time shall be verified to be better than61 % by Tes

42、t Method E 1860.10. Procedure10.1 Weigh 1 to 7 with a precision of 6 1 mg of the testspecimen into a clean specimen container. Seal the container, ifdesired.NOTE 7The Kuhner Micro CTS device uses up to 2-g specimens. Forspecimens of a size greater than 1 g, record mass to 60.1 g.10.2 Place the test

43、specimen into the apparatus onto thesample position, at ambient temperature conditions. Place aspecimen container containing 1 to 7 mg of inert referencematerial (1 to 2 g for the Kuhner Micro CTS) in the referenceposition.10.3 Heat the test specimen and reference material fromambient to the isother

44、mal temperature of test at 20C/min withno more than 1C overshoot. Zero time is recorded when thespecimen test temperature reaches the isothermal test tempera-ture 6 1C. Record the thermal curve.NOTE 8In some apparatus, it may be possible to load the specimenand reference into the furnace preheated t

45、o the isothermal test tempera-ture. Appropriate provisions shall be made to ensure the safety of theoperator.NOTE 9A dynamic test method, such as Test Method E 537 may beused to estimate potential isothermal test temperatures.10.4 Record the sample temperature 5 min into the experi-ment.10.5 Termina

46、te the experiment when the peak of the reac-tion exotherm is observed or when no exotherm is observed orafter an operator-selected time. (In the absence of otherinformation, after 200 min). The reaction is exothermic if itresults in a measurable increase in specimen temperature orheat flow above bas

47、eline.10.6 Display the thermal curve with differential heat flow ordifferential temperature on the Y-axis and time on the X-axis.Extend the recorded baseline beyond the reaction exotherm.Construct a tangent at the point of the most rapid rate ofincrease in heat flow and extrapolate it to intersect w

48、ith theconstructed baseline. The time at the intersection of these twolines is the reaction induction time. (See Fig. 1.)NOTE 10The precision of this test method is a constant value (seeSection 12) and does not depend upon the measured value. For this reason,this test method is applicable to RIT val

49、ues greater than 15 min. If RITvalues of less than 15 min are observed, the test temperature may belowered to obtain longer RIT values.NOTE 11In some cases, where agreed upon by the parties involved,the time at the first deviation from baseline may be taken as the RITvalues. This alternative shall be included in the report.10.7 Report the RIT (from 10.6) and the isothermal testtemperature (from 10.4) as follows:RIT = 120 min at 200CNOTE 12If no reaction is observed, then the RIT may be reported asgreater than the condition tested. For example: RIT 200 min at 2