ASTM D3828-2012 Standard Test Methods for Flash Point by Small Scale Closed Cup Tester《小刻度闭杯试验器测定液体闪点的标准试验方法》.pdf

1、Designation: D3828 12Standard 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 Department of Defense.INTRODUCTIONThese small scale flash point methods are generally used f

3、or 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 condi

4、tion 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 specifie

5、d.1. Scope*1.1 These test methods cover procedures for flash pointtests, within the range of 30 to 300C, of petroleum productsand biodiesel liquid fuels, using a small scale closed cup tester.The procedures may be used to determine, whether a productwill or will not flash at a specified temperature

6、(flash/no flashMethod A) or the flash point of a sample (Method B). Whenused in conjunction with an electronic thermal flash detector,these test methods are also suitable for flash point tests onbiodiesels such as fatty acid methyl esters (FAME).1.2 The values stated in SI units are to be regarded a

7、s 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 the fi

8、re 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 This s

9、tandard 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 statementsappear

10、 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 Practice for A

11、utomatic Sampling of Petroleum andPetroleum ProductsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceE300 Practice for Sampling Industrial ChemicalsE1137/E1137M Specification for Industrial Platinum Resis-tan

12、ce Thermometers2.2 ISO Standards:31These test methods are under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.08 on Volatility.Current edition approved May 15, 2012. Published October 2012. Originallyapproved in 1979. L

13、ast previous edition approved in 2009 as D382809. DOI:10.1520/D3828-12.2For 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 AST

14、M website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-29

15、59, United States.Guide 34 Quality Systems Guidelines for the Production ofReference MaterialsGuide 35 Certification of Reference MaterialsGeneraland Statistical PrinciplesEN ISO 3679 Determination of Flash PointRapid Equi-librium Closed Cup MethodEN ISO 3680 Determination of Flash/No FlashRapidEqui

16、librium Closed Cup MethodISO 60751 Industrial platinum resistance thermometers andplatinum temperature sensors2.3 Energy Institute Standards:4IP 523 Determination of flash point Rapid equilibriumclosed cup methodIP 524 Determination of flash/no flash Rapid equilibriumclosed cup method3. Terminology3

17、.1 Definitions:3.1.1 equilibrium, nin flash point test methods, the con-dition where the vapor above the test specimen, and 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 temperat

18、ure may not be uniformthroughout the test specimen, and the test cover and shutter onthe apparatus can be cooler or warmer.3.1.2 flash point, nin flash point test methods, the lowesttemperature corrected to a pressure of 101.3 kPa (760 mm Hg)at which application of an ignition source causes the vapo

19、rs ofa specimen of the sample to ignite under specified conditions oftest.4. Summary 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

20、 ignition source is applied and adetermination made as to whether or not a flash 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

21、 specimen is introduced into the test cup of theselected apparatus that is maintained 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 a

22、re cleaned, and the test temperatureadjusted 5C (9F) lower or higher depending on whether ornot a flash occurred previously. A fresh test specimen isintroduced and tested. This procedure is repeated until the flashpoint is established within 5C (9F).4.2.3 The procedure is then repeated at 1C (2F) in

23、tervalsuntil the flash point is determined to the nearest 1C (2F).4.2.4 If improved accuracy is desired the procedure isrepeated at 0.5C (1F) intervals until the flash point isdetermined to the nearest 0.5C (1F).4.3 Test Time and Specimen Volume:4.3.1 For all products, except biodiesel; for test tem

24、pera-tures up to and including 100C (212F), the test time is 1minute and the specimen volume is 2 mL.4.3.2 For all products, except biodiesel; for test tempera-tures over 100C (212F), the test time is 2 minute and thespecimen volume is 4 mL.4.3.3 For biodiesel; for all test temperatures, the test ti

25、me is1 minute and the specimen volume is 2 mL.5. Significance and Use5.1 Flash 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 ha

26、zard of amaterial.5.2 Flash point is used in shipping and safety regulations 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 fl

27、ammable materials in a relatively nonvolatile ornonflammable material.5.4 These test methods use a smaller sample (2 to 4 mL) anda shorter test time (1 to 2 min) than traditional test methods.5.5 MethodA, IP 524 and EN ISO 3680 are similar methodsfor flash no-flash tests. Method B, IP 523 and EN ISO

28、 3679 aresimilar methods for flash point determination.6. Apparatus6.1 Test Cup and Cover AssemblyThe essential dimen-sions and requirements of the apparatus are shown in Fig. A1.1and TableA1.1 ofAnnexA1. The apparatus and accessories aredescribed in detail inAnnexA1. The temperature range is from30

29、 to 300C. Some versions of the apparatus may not coverthe full 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

30、in circumstances whereprotection from drafts does not exist.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

31、 health hazard.Dispose of solvents and waste material in accordance 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 fro

32、m Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.D3828 1228. 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 con

33、tainers atnormal room temperature (20 to 25C) or colder.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 o

34、f valid results.8.4 Erroneously high flash points can be 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 10C below theexpected flash point. Where possible perform the flas

35、h point asthe first test on the sample.8.5 Samples containing 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

36、itscontainer to at least 10C below the expected flash point beforeopening 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

37、 the samplevolume falls below 50 % of the containers 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 i

38、tscontainer to a temperature not warmer than 10C below the testtemperature, 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 ori

39、fice by heating inaccordance with 8.7, transfer the 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 bee

40、n determined for solidsamples.9. Preparation of Apparatus9.1 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 extra

41、cted airand vapors can be withdrawn without causing 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 a

42、ccordance withthe manufacturers instructions for calibrating, 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

43、its accessories with anappropriate solvent (7.1) to 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 th

44、e barometric pressure (6.2) beforecommencing a test.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

45、 apparatus has integral test cup cooling facilities.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 w

46、ith A1.2.2 andAnnex A5.10.2 Verify the performance 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

47、be tested according toMethod B, Section 12 and the 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 unl

48、isted CRM (see AnnexA2).10.3 Once the performance of 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 f

49、lash 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 the ignitionsource, the position of the ignition source (A1.3), the operationof the flash detector (if fitted) and correct reading of thetemperature measuring device.After any adjustment, repeat thetest in 10.2 or 10.3 using a fresh test specimen, wit