1、Designation: D 3828 09Standard Test Methods forFlash Point by Small Scale Closed Cup Tester1This standard is issued under the fixed designation D 3828; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A nu
2、mber 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
3、 for testing a sample at a specifictemperature where the specimen being tested and the airvapor mixture above it are close to thermalequilibrium. Test Method D 3941 covers other flash point equipment operated at a specifictemperature.Flash point values are a function of the apparatus design, the con
4、dition 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 specif
5、ied.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 temperatur
6、e (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
7、 as thestandard. The values given in parentheses are for informationonly.1.3 WarningMercury has been designated by EPA andmany state agencies as a hazardous material that can causecentral nervous system, kidney, and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomater
8、ials. Caution should be taken when handling mercury andmercury-containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAs website(http:/www.epa.gov/mercury/faq.htm) for additional informa-tion. Users should be aware that selling mercury or mercury-contain
9、ing products, or both, in your state may be prohibited bystate law.1.4 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 fire h
10、azard 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.1.5 This stand
11、ard 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 thr
12、oughout. See also the Material Safety Data Sheets forthe product being tested.2. Referenced Documents2.1 ASTM Standards:2D 3941 Test Method for Flash Point by the EquilibriumMethod With a Closed-Cup ApparatusD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Au
13、tomatic Sampling of Petroleum andPetroleum ProductsD 6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceE 300 Practice for Sampling Industrial Chemicals1These test methods are under the jurisdiction of ASTM Comm
14、ittee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.08 on Volatility.Current edition approved Sept. 1, 2009. Published September 2009. Originallyapproved in 1979. Last previous edition approved in 2007 as D 382807a.2For referenced ASTM standards, visit t
15、he 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.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100
16、 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.2.2 ISO Standards:3Guide 34 Quality Systems Guidelines for the Production ofReference MaterialsGuide 35 Certification of Reference MaterialsGeneraland Statistical PrinciplesEN ISO 3679 Determination of Flash PointRapid
17、Equi-librium Closed Cup MethodEN ISO 3680 Determination of Flash/No FlashRapidEquilibrium Closed Cup Method2.3 Energy Institute Standards:4IP 523 Determination of flash point Rapid equilibriumclosed cup methodIP 524 Determination of flash/no flash Rapid equilibriumclosed cup method3. Terminology3.1
18、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 temperature
19、 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 vapors
20、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 ig
21、nition 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 sp
22、ecimen 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 are
23、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) inter
24、valsuntil 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 temper
25、a-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 time
26、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 hazar
27、d 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 flamm
28、able 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 36
29、79 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 to
30、 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 in
31、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 he
32、alth 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.)3Available from A
33、merican National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.4Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.D38280928. Sampling8.1 Obtain at least a 50 mL sample from a bulk test site inaccord
34、ance with Practices D 4057, D 4177, E 300 or othercomparable sampling practices.8.2 Store samples in clean, tightly sealed containers 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,beca
35、use 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 obtained whenprecautions are not taken to avoid loss of volatile materials. Donot open containers unnecessarily. Do n
36、ot make a transferunless the sample temperature is at least 10C below theexpected flash point. Where possible perform the flash 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 v
37、olatile 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 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, e
38、nsure 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 capacity.8.7 If sufficiently fluid, mix samples by gently shaking byhand prior to removal of the test specimen, taking ca
39、re 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 10C below the testtemperature, such that the sample can be mixed by gentleshaking.8.8 If the sample cannot be made sufficiently f
40、luid to beintroduced into the test cup through the orifice 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 th
41、e test cup asevenly as possible. Precision has not been 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 on
42、tests made in a laboratory draft hood unless the extracted 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 an
43、ycontrols.9.3 Prepare the apparatus for operation in accordance 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 aff
44、ect the testresult.)9.4 Clean the test cup, cover and 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 use
45、d to clean the fillerorifice.9.5 Measure and record the 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).9.7 For sub-ambient test temperatures see Annex A4, unlessthe ap
46、paratus has integral test cup cooling facilities.10. Verification of Apparatus10.1 Verify that the temperature measuring device is inaccordance with A1.2.2.10.2 Verify the performance of the apparatus at least onceper year by determining the flash point of a certified referencematerial (CRM) such as
47、 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 observed flash point obtained in12.1.6 and 12.1.6.1 shall be corrected for barometric pressure(see Section 13). The
48、flash point obtained shall be within thelimits stated in TableA2.1 for the identified CRM or within thelimits calculated for an unlisted CRM (see Annex A2).10.3 Once the performance of the apparatus has beenverified, the flash point of secondary working standards (SWS)can be determined along with th
49、eir 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 the ignitionsource, the position of the ignition source (A1.3), the operationof the flash detector (if fitted) and cor
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