ASTM D3828-2016 Standard Test Methods for Flash Point by Small Scale Closed Cup Tester《用小型闭杯试验机测定闪点的标准试验方法》.pdf

1、Designation: D3828 16Standard Test Methods forFlash Point by Small Scale Closed Cup Tester1This standard is issued under the fixed designation D3828; 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 () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.INTRODUCTIONThese small scale flash point methods are generally u

3、sed for testing a sample at a specifictemperature where the specimen being tested and the airvapor mixture above it are close to thermalequilibrium. Test Method D3941 covers other flash point equipment operated at a specific temperature.Flash point values are a function of the apparatus design, the

4、condition of the apparatus used, andthe operational procedure carried out. Flash point can therefore only be defined in terms of a standardtest method, and no general valid correlation can be guaranteed between results obtained by differenttest methods, or with test apparatus different from that spe

5、cified.1. Scope*1.1 These test methods cover procedures for flash pointtests, within the range of 30 C to 300 C, of petroleumproducts and biodiesel liquid fuels, using a small scale closedcup tester. The procedures may be used to determine, whethera product will or will not flash at a specified temp

6、erature(flash/no flash Method A) or the flash point of a sample(Method B). When used in conjunction with an electronicthermal flash detector, these test methods are also suitable forflash point tests on biodiesels such as fatty acid methyl esters(FAME).1.2 The values stated in SI units are to be reg

7、arded as thestandard. The values given in parentheses are for informationonly.1.3 This standard should be used to measure and describethe properties of materials, products, or assemblies in responseto heat and flame under controlled laboratory conditions andshould not be used to describe or appraise

8、 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 which are pertinent to an assessment of the firehazard of a particular end use.1.4

9、 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 determine the applica-bility of regulatory limitations prior to use. Warning statement

10、sappear throughout. See also the Material Safety Data Sheets forthe product being tested.2. Referenced Documents2.1 ASTM Standards:2D3941 Test Method for Flash Point by the EquilibriumMethod With a Closed-Cup ApparatusD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practic

11、e for Automatic Sampling of Petroleum andPetroleum ProductsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD6708 Practice for Statistical Assessment and Improvementof Expected Agreement Between Two Test Meth

12、ods thatPurport to Measure the Same Property of a MaterialE300 Practice for Sampling Industrial ChemicalsE1137/E1137M Specification for Industrial Platinum Resis-tance Thermometers2.2 ISO Standards:3Guide 34 Quality Systems Guidelines for the Production ofReference Materials1These test methods are u

13、nder the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.08 on Volatility.Current edition approved June 1, 2016. Published July 2016. Originally approvedin 1979. Last previous edition approved in 2012 as D3828

14、12a. DOI: 10.1520/D3828-16.2For referenced ASTM standards, visit 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 American National

15、Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1Guide 35 Certification of Re

16、ference MaterialsGeneral andStatistical PrinciplesEN ISO 3679 Determination of Flash PointRapid Equilib-rium Closed Cup MethodEN ISO 3680 Determination of Flash/No FlashRapidEquilibrium Closed Cup MethodISO 60751 Industrial Platinum Resistance Thermometersand Platinum Temperature Sensors2.3 Energy I

17、nstitute Standards:4IP 523 Determination of Flash PointRapid EquilibriumClosed Cup MethodIP 524 Determination of Flash/No FlashRapid Equilib-rium Closed Cup Method3. Terminology3.1 Definitions:3.1.1 equilibrium, nin flash point test methods, the condi-tion where the vapor above the test specimen, an

18、d the testspecimen are at the same temperature at the time the ignitionsource is applied.3.1.1.1 DiscussionThis condition may not be fullyachieved in practice, since the temperature may not be uniformthroughout the test specimen, and the test cover and shutter onthe apparatus can be cooler or warmer

19、.3.1.2 flash point, nin flash point test methods, the lowesttemperature of the test specimen, adjusted to account forvariations in atmospheric pressure from 101.3 kPa, at whichapplication of an ignition source causes the vapors of the testspecimen to ignite under specified conditions of test.4. Summ

20、ary of Test Methods4.1 Method AFlash/No Flash TestA test specimen isintroduced, by a syringe, into the test cup of the selectedapparatus that is set and maintained at the specified tempera-ture. After a specific time an ignition source is applied and adetermination made as to whether or not a flash

21、occurred.4.2 Method BFinite (or Actual) Flash PointThismethod essentially repeats MethodAa number of times, and bychanging the test temperature and test specimen a number oftimes, determines the flash point.4.2.1 A test specimen is introduced into the test cup of theselected apparatus that is mainta

22、ined at the expected flashpoint. After a specified time an ignition source is applied and adetermination made whether or not a flash occurred.4.2.2 The test specimen is removed from the test cup; thetest cup and cover are cleaned, and the test temperatureadjusted 5 C (9 F) lower or higher depending

23、on whether ornot a flash occurred previously. A fresh test specimen isintroduced and tested. This procedure is repeated until the flashpoint is established within 5 C (9 F).4.2.3 The procedure is then repeated at 1 C (2 F) intervalsuntil the flash point is determined to the nearest 1 C (2 F).4.2.4 I

24、f improved accuracy is desired the procedure isrepeated at 0.5 C (1 F) intervals until the flash point isdetermined to the nearest 0.5 C (1 F).4.3 Test Time and Specimen Volume:4.3.1 For all products, except biodiesel; for test tempera-tures up to and including 100 C (212 F), the test time is1 min a

25、nd the specimen volume is 2 mL.4.3.2 For all products, except biodiesel; for test tempera-tures over 100 C (212 F), the test time is 2 min and thespecimen volume is 4 mL.4.3.3 For biodiesel; for all test temperatures, the test time is1 min and the specimen volume is 2 mL.5. Significance and Use5.1 F

26、lash point measures the response of the test specimento heat and ignition source under controlled laboratory condi-tions. It is only one of a number of properties that must beconsidered in assessing the overall flammability hazard of amaterial.5.2 Flash point is used in shipping and safety regulatio

27、ns todefine flammable and combustible materials and classify them.Consult the particular regulation involved for precise defini-tions of these classes.5.3 Flash point can indicate the possible presence of highlyvolatile and flammable materials in a relatively nonvolatile ornonflammable material.5.4

28、These test methods use a smaller sample (2 mL to 4 mL)and a shorter test time (1 min to 2 min) than traditional testmethods.5.5 MethodA, IP 524 and EN ISO 3680 are similar methodsfor flash no-flash tests. Method B, IP 523 and EN ISO 3679 aresimilar methods for flash point determination.6. Apparatus6

29、.1 Test Cup and Cover AssemblyThe essential dimen-sions and requirements of the apparatus are shown in Fig. A1.1and Table A1.1 of Annex A1. The apparatus and accessoriesare described in detail in Annex A1. The temperature range isfrom 30 C to 300 C. Some versions of the apparatus maynot cover the fu

30、ll temperature range.6.2 Barometer, accurate to 0.5 kPa. Barometers that havebeen pre-corrected for use at weather stations or airports arenot suitable.6.3 Draft ShieldA shield located at the back and on twosides of the instrument, for use in circumstances whereprotection from drafts does not exist.

31、7. Reagents and Materials7.1 Cleaning SolventUse only non-corrosive solvents ca-pable of cleaning the test cup and cover. Two commonly usedsolvents are toluene and acetone. (WarningToluene, acetoneand many other solvents are flammable and a health hazard.Dispose of solvents and waste material in acc

32、ordance withlocal regulations. )7.2 Butane, Propane and Natural GasFor use as a pilotand ignition source (not required if an electric ignitor is used).(WarningButane, propane and natural gases are flammableand a health hazard.)4Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,U

33、.K., http:/www.energyinst.org.uk.D3828 1628. Sampling8.1 Obtain at least a 50 mL sample from a bulk test site inaccordance with Practices D4057, D4177, E300 or othercomparable sampling practices.8.2 Store samples in clean, tightly sealed containers atnormal room temperature (20 C to 25 C) or colder.

34、8.3 Do not store samples for an extended period of time ingas permeable containers, such as those made of plastic,because volatile material can diffuse through the walls of thecontainer. Samples in leaky containers are suspect and not asource of valid results.8.4 Erroneously high flash points can be

35、 obtained whenprecautions are not taken to avoid loss of volatile materials. Donot open containers unnecessarily. Do not make a transferunless the sample temperature is at least 10 C below theexpected flash point. Where possible perform the flash point asthe first test on the sample.8.5 Samples cont

36、aining dissolved or free water may bedehydrated with calcium chloride. (WarningIf the sample isexpected of containing volatile components, the treatment asdescribed in 8.5 should be omitted.)8.6 Cool, or adjust the temperature of the sample and itscontainer to at least 10 C below the expected flash

37、pointbefore opening to remove the test specimen. If an aliquot of theoriginal sample is to be stored prior to testing, ensure that thecontainer is filled to between 85 % and 95 % of its capacity.NOTE 1Results of flash point tests can be affected if the samplevolume falls below 50 % of the containers

38、 capacity.8.7 If sufficiently fluid, mix samples by gently shaking byhand prior to removal of the test specimen, taking care tominimize the loss of volatile components. If the sample is tooviscous at ambient temperature, gently warm the sample in itscontainer to a temperature not warmer than 10 C be

39、low thetest temperature, such that the sample can be mixed by gentleshaking. Ensure that high pressures do not develop in thecontainer when warming.8.8 If the sample cannot be made sufficiently fluid to beintroduced into the test cup through the orifice by heating inaccordance with 8.7, transfer the

40、 test specimen with a solidsdispenser or spatula while the cover is open. The specimen sizecan be the mass equivalent of the required volume and thespecimen should be spread over the bottom of the test cup asevenly as possible. Precision has not been determined for solidsamples.9. Preparation of App

41、aratus9.1 Place the apparatus on a level, stable surface. Unlesstests are made in a draft-free area, surround the tester on threesides with a draft shield (see 6.3) for protection. Do not rely ontests made in a laboratory draft hood unless the extracted airand vapors can be withdrawn without causing

42、 air currents overthe test cup during the ignition source application period.9.2 Read the manufacturers instructions on the care andservicing of the instrument and for the correct operation of anycontrols.9.3 Prepare the apparatus for operation in accordance withthe manufacturers instructions for ca

43、librating, checking andoperating the equipment, especially the operation of the igni-tion source. (WarningAn incorrectly set test flame size orsetting of an electric ignitor can significantly affect the testresult.)9.4 Clean the test cup, cover and its accessories with anappropriate solvent (7.1) to

44、 remove any traces of gum orresidue from the previous test. Wipe dry with absorbent paper.A stream of dry clean air may be used to remove the last tracesof solvent used. A pipe cleaner may be used to clean the fillerorifice.9.5 Measure and record the barometric pressure (6.2) beforecommencing a test

45、.9.6 Use an electronic thermal flash detector for flash pointtests on biodiesels such as fatty acid methyl esters (FAME) (seeA1.7). The flash detector may be used for other test materials.9.7 For sub-ambient test temperatures see Annex A4, unlessthe apparatus has integral test cup cooling facilities

46、.10. Verification of Apparatus10.1 Verify and correct, if necessary, the readings on thetemperature measuring device at least every 12 months, ac-cording to the manufacturers instructions and that the tem-perature measuring device is in accordance with A1.2.2 andAnnex A5.10.2 Verify the performance

47、of the apparatus at least onceper year by determining the flash point of a certified referencematerial (CRM) such as those listed in Annex A2, which isreasonably close to the expected temperature range of thesamples to be tested. The material shall be tested according toMethod B, Section 12 and the

48、detected flash point determinedin 12.1.6 and 12.1.6.1 shall be corrected for barometricpressure (see Section 13). The flash point obtained shall bewithin the limits stated in TableA2.1 for the identified CRM orwithin the limits calculated for an unlisted CRM (see AnnexA2).10.3 Once the performance o

49、f the apparatus has beenverified, the flash point of secondary working standards (SWS)can be determined along with their control limits. Thesesecondary materials can then be utilized for more frequentperformance checks (see Annex A2).10.4 When the flash point obtained is not within the limitsstated in 10.2 or 10.3, check the condition and operation of theapparatus to ensure conformity with the details listed in AnnexA1, especially with regard to tightness of the cover (A1.2.1),the action of the shutter, the size or intensity of