ASTM D3828-2012a 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

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1、Designation: D3828 12D3828 12aStandard 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 revisio

2、n. A number 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 general

3、ly used 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, t

4、he 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

5、specified.1. Scope*1.1 These test methods cover procedures for flash point tests, within the range of 30 to 300C, of petroleum products andbiodiesel liquid fuels, using a small scale closed cup tester. The procedures may be used to determine, whether a product will orwill not flash at a specified te

6、mperature (flash/no flash Method A) or the flash point of a sample (Method B). When used inconjunction with an electronic thermal flash detector, these test methods are also suitable for flash point tests on biodiesels suchas fatty acid methyl esters (FAME).1.2 The values stated in SI units are to b

7、e regarded as the standard. The values given in parentheses are for information only.1.3 This standard should be used to measure and describe the properties of materials, products, or assemblies in response toheat and flame under controlled laboratory conditions and should not be used to describe or

8、 appraise the fire hazard or fire riskof materials, products, or assemblies under actual fire conditions. However, results of this test may be used as elements of a firerisk assessment which takes into account all of the factors which are pertinent to an assessment of the fire hazard of a particular

9、end use.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. Warning

10、statements appear throughout. See also the Material Safety Data Sheets for the product beingtested.2. Referenced Documents2.1 ASTM Standards:2D3941 Test Method for Flash Point by the Equilibrium Method With a Closed-Cup ApparatusD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD

11、4177 Practice for Automatic Sampling of Petroleum and Petroleum ProductsD6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-ment System PerformanceD6708 Practice for Statistical Assessment and Improvement of Expected Agreement Betw

12、een Two Test Methods that Purportto Measure the Same Property of a Material1 These test methods are under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.08on Volatility.Current edition approved May 15, 2012Nov. 1, 2012

13、. Published October 2012February 2013. Originally approved in 1979. Last previous edition approved in 20092012as D382809.12. DOI: 10.1520/D3828-12.10.1520/D3828-12A.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Boo

14、k of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be techni

15、cally possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this s

16、tandardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E300 Practice for Sampling Industrial ChemicalsE1137/E1137M Specification for Industrial Platinum Resistance Thermometers2.2 ISO Standards:3Guide 34 Quality Systems Guidelines for

17、 the Production of Reference MaterialsGuide 35 Certification of Reference MaterialsGeneral and Statistical PrinciplesEN ISO 3679 Determination of Flash PointRapid Equilibrium Closed Cup MethodEN ISO 3680 Determination of Flash/No FlashRapid Equilibrium Closed Cup MethodISO 60751 Industrial platinum

18、resistance thermometers and platinum temperature sensors2.3 Energy Institute Standards:4IP 523 Determination of flash point Rapid equilibrium closed cup methodIP 524 Determination of flash/no flash Rapid equilibrium closed cup method3. Terminology3.1 Definitions:3.1.1 equilibrium, nin flash point te

19、st methods, the condition where the vapor above the test specimen, and the test specimenare at the same temperature at the time the ignition source is applied.3.1.1.1 DiscussionThis condition may not be fully achieved in practice, since the temperature may not be uniform throughout the test specimen

20、, andthe test cover and shutter on the apparatus can be cooler or warmer.3.1.2 flash point, nin flash point test methods, the lowest temperature corrected to a pressure of 101.3 kPa (760 mm Hg) atwhich application of an ignition source causes the vapors of a specimen of the sample to ignite under sp

21、ecified conditions of test.4. Summary of Test Methods4.1 Method AFlash/No Flash TestAtest specimen is introduced, by a syringe, into the test cup of the selected apparatus thatis set and maintained at the specified temperature. After a specific time an ignition source is applied and a determination

22、made asto whether or not a flash occurred.4.2 Method BFinite (or Actual) Flash PointThis method essentially repeats Method A a number of times, and by changingthe test temperature and test specimen a number of times, determines the flash point.4.2.1 Atest specimen is introduced into the test cup of

23、the selected apparatus that is maintained at the expected flash point.Aftera specified time an ignition source is applied and a determination made whether or not a flash occurred.4.2.2 The test specimen is removed from the test cup; the test cup and cover are cleaned, and the test temperature adjust

24、ed 5C(9F) lower or higher depending on whether or not a flash occurred previously.Afresh test specimen is introduced and tested. Thisprocedure is repeated until the flash point is established within 5C (9F).4.2.3 The procedure is then repeated at 1C (2F) intervals until the flash point is determined

25、 to the nearest 1C (2F).4.2.4 If improved accuracy is desired the procedure is repeated at 0.5C (1F) intervals until the flash point is determined tothe nearest 0.5C (1F).4.3 Test Time and Specimen Volume:4.3.1 For all products, except biodiesel; for test temperatures up to and including 100C (212F)

26、, the test time is 1 minute andthe specimen volume is 2 mL.4.3.2 For all products, except biodiesel; for test temperatures over 100C (212F), the test time is 2 minute and the specimenvolume is 4 mL.4.3.3 For biodiesel; for all test temperatures, the test time is 1 minute and the specimen volume is 2

27、 mL.5. Significance and Use5.1 Flash point measures the response of the test specimen to heat and ignition source under controlled laboratory conditions.It is only one of a number of properties that must be considered in assessing the overall flammability hazard of a material.5.2 Flash point is used

28、 in shipping and safety regulations to define flammable and combustible materials and classify them.Consult the particular regulation involved for precise definitions of these classes.5.3 Flash point can indicate the possible presence of highly volatile and flammable materials in a relatively nonvol

29、atile ornonflammable material.5.4 These test methods use a smaller sample (2 to 4 mL) and a shorter test time (1 to 2 min) than traditional test methods.3 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.4 Available from E

30、nergy Institute, 61 New Cavendish St., London, WIG 7AR, U.K., http:/www.energyinst.org.uk.D3828 12a25.5 Method A, IP 524 and EN ISO 3680 are similar methods for flash no-flash tests. Method B, IP 523 and EN ISO 3679 aresimilar methods for flash point determination.6. Apparatus6.1 Test Cup and Cover

31、AssemblyThe essential dimensions and requirements of the apparatus are shown in Fig. A1.1 andTable A1.1 of Annex A1. The apparatus and accessories are described in detail in Annex A1. The temperature range is from 30to 300C. Some versions of the apparatus may not cover the full temperature range.6.2

32、 Barometer, accurate to 0.5 kPa. Barometers that have been pre-corrected for use at weather stations or airports are notsuitable.6.3 Draft ShieldA shield located at the back and on two sides of the instrument, for use in circumstances where protectionfrom drafts does not exist.7. Reagents and Materi

33、als7.1 Cleaning SolventUse only non-corrosive solvents capable of cleaning the test cup and cover.Two commonly used solventsare toluene and acetone. (WarningToluene, acetone and many other solvents are flammable and a health hazard. Dispose ofsolvents and waste material in accordance with local regu

34、lations. )7.2 Butane, Propane and Natural GasFor use as a pilot and ignition source (not required if an electric ignitor is used).(WarningButane, propane and natural gases are flammable and a health hazard.)8. Sampling8.1 Obtain at least a 50 mL sample from a bulk test site in accordance with Practi

35、ces D4057, D4177, E300 or other comparablesampling practices.8.2 Store samples in clean, tightly sealed containers at normal room temperature (20 to 25C) or colder.8.3 Do not store samples for an extended period of time in gas permeable containers, such as those made of plastic, becausevolatile mate

36、rial can diffuse through the walls of the container. Samples in leaky containers are suspect and not a source of validresults.8.4 Erroneously high flash points can be obtained when precautions are not taken to avoid loss of volatile materials. Do not opencontainers unnecessarily. Do not make a trans

37、fer unless the sample temperature is at least 10C below the expected flash point.Where possible perform the flash point as the first test on the sample.8.5 Samples containing dissolved or free water may be dehydrated with calcium chloride. (WarningIf the sample is expectedof containing volatile comp

38、onents, the treatment as described in 8.5 should be omitted.)8.6 Cool, or adjust the temperature of the sample and its container to at least 10C below the expected flash point before openingto remove the test specimen. If an aliquot of the original sample is to be stored prior to testing, ensure tha

39、t the container is filledto between 85 and 95 % of its capacity.NOTE 1Results of flash point tests can be affected if the sample volume falls below 50 % of the containers capacity.8.7 If sufficiently fluid, mix samples by gently shaking by hand prior to removal of the test specimen, taking care to m

40、inimizethe loss of volatile components. If the sample is too viscous at ambient temperature, gently warm the sample in its container toa temperature not warmer than 10C below the test temperature, such that the sample can be mixed by gentle shaking. Ensure thathigh pressures do not develop in the co

41、ntainer when warming.8.8 If the sample cannot be made sufficiently fluid to be introduced into the test cup through the orifice by heating in accordancewith 8.7, transfer the test specimen with a solids dispenser or spatula while the cover is open. The specimen size can be the massequivalent of the

42、required volume and the specimen should be spread over the bottom of the test cup as evenly as possible.Precision has not been determined for solid samples.9. Preparation of Apparatus9.1 Place the apparatus on a level, stable surface. Unless tests are made in a draft-free area, surround the tester o

43、n three sideswith a draft shield (see 6.3) for protection. Do not rely on tests made in a laboratory draft hood unless the extracted air and vaporscan be withdrawn without causing air currents over the test cup during the ignition source application period.9.2 Read the manufacturers instructions on

44、the care and servicing of the instrument and for the correct operation of anycontrols.9.3 Prepare the apparatus for operation in accordance with the manufacturers instructions for calibrating, checking andoperating the equipment, especially the operation of the ignition source. (WarningAn incorrectl

45、y set test flame size or settingof an electric ignitor can significantly affect the test result.)D3828 12a39.4 Clean the test cup, cover and its accessories with an appropriate solvent (7.1) to remove any traces of gum or residue fromthe previous test. Wipe dry with absorbent paper. A stream of dry

46、clean air may be used to remove the last traces of solvent used.A pipe cleaner may be used to clean the filler orifice.9.5 Measure and record the barometric pressure (6.2) before commencing a test.9.6 Use an electronic thermal flash detector for flash point tests on biodiesels such as fatty acid met

47、hyl esters (FAME) (seeA1.7). The flash detector may be used for other test materials.9.7 For sub-ambient test temperatures see Annex A4, unless the apparatus has integral test cup cooling facilities.10. Verification of Apparatus10.1 Verify and correct, if necessary, the readings on the temperature m

48、easuring device at least every 12 months, according tothe manufacturers instructions and that the temperature measuring device is in accordance with A1.2.2 and Annex A5.10.2 Verify the performance of the apparatus at least once per year by determining the flash point of a certified referencematerial

49、 (CRM) such as those listed in Annex A2, which is reasonably close to the expected temperature range of the samples tobe tested. The material shall be tested according to Method B, Section 12 and the detected flash point determined in 12.1.6 and12.1.6.1 shall be corrected for barometric pressure (see Section 13). The flash point obtained shall be within the limits stated inTable A2.1 for the identified CRM or within the limits calculated for an unlisted CRM (see Annex A2).10.3 Once the performance of the apparatus has been ve