1、Designation: D 3828 07aDesignations: 523/05 and 524/05An American National StandardStandard 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
2、 or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.INTROD
3、UCTIONThe flash point method is generally used for testing a sample at a specific temperature. At a settemperature, the specimen being tested and the airvapor mixture above it are close to thermalequilibrium. Test methods for other flash point equipment operated at a specific temperature aredescribe
4、d in Test Method D 3941.Flash point values are a function of the apparatus design, the 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 re
5、sults obtained by differenttest methods, or with test apparatus different from that specified.1. Scope*1.1 These test methods cover procedures for the determina-tion of the flash point by a small scale closed tester. Theprocedures may be used to determine the actual flash pointtemperature of a sampl
6、e or whether a product will or will notflash at a specified temperature (flash/no flash). When used inconjunction with an electronic thermal flash detector, these testmethods are also suitable for flash point tests on fatty acidmethyl esters (FAME).1.2 The values stated in SI units are to be regarde
7、d 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 the
8、 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 Thi
9、s 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 statementsapp
10、ear throughout. 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 6299 Practice for Applying Statistical Quality AssuranceTechniques to Evaluate Anal
11、ytical Measurement SystemPerformance2.2 ISO Standards:3Guide 34 Quality Systems Guidelines for the Production ofReference MaterialsGuide 35 Certification of Reference MaterialsGeneraland Statistical PrinciplesEN ISO 3679 Determination of flashpoint with closed cupequilibrium methodEN ISO 3680 Determ
12、ination of flashpoint with closed cupequilibrium method1These test methods are under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.08.0B on Flammability.Current edition approved July 15, 2007. Published August 2007. Ori
13、ginallyapproved in 1979. Last previous edition approved in 2007 as D 382807.This is also a standard(s) of the Energy Institute issued under the fixeddesignations IP 523 and IP 524 (originally designated IP 303). The final numberindicates the year of last revision. These test methods were originally
14、adopted as ajoint ASTM-IP standard in 1979.2For 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 Am
15、erican National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.1*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 19428-2959, United States.3. Terminology3.1 Definitions:
16、3.1.1 equilibriumthe vapor above the liquid (specimen)and the liquid in a flash point apparatus specimen cup are at thesame temperature at the time the ignition source is applied.3.1.1.1 DiscussionThis condition may not be fullyachieved in practice. Although the temperature pattern is inequilibrium,
17、 the temperature is not uniform throughout thespecimen cup because of the contrast between the hot liquidtest specimen and the cooler lid and shutter.3.1.2 flash pointthe lowest temperature corrected to apressure of 760 mm Hg (101.3 kPa) at which application of atest flame causes the vapors of a spe
18、cimen of the sample toignite under specified conditions of test.3.1.2.1 DiscussionThe specimen is deemed to haveflashed when a flame appears and instantaneously propagatesitself over the surface of the specimen.3.1.2.2 DiscussionOccasionally, particularly near the ac-tual flash point, application of
19、 the test flame will cause a bluehalo or an enlarged flame; this is not a flash and should beignored.4. Summary of Test Method4.1 Method AFlash/No Flash TestA specimen of asample is introduced by a syringe into the cup of the selectedapparatus that is set and maintained at the specified tempera-ture
20、. After a specific time a test flame is applied and anobservation made as to whether or not a flash occurred.4.2 Method BFinite (or Actual) Flash Point:4.2.1 A specimen of a sample is introduced into the cup ofthe selected apparatus that is maintained at the expected flashpoint. After a specified ti
21、me a test flame is applied and theobservation made whether or not a flash occurred.4.2.2 The specimen is removed from the cup, the cupcleaned, and the cup temperature adjusted 5C (9F) lower orhigher depending on whether or not a flash occurred previ-ously. A fresh specimen is introduced and tested.
22、This proce-dure is repeated until the flash point is established within 5C(9F).4.2.3 The procedure is then repeated at 1C (2F) intervalsuntil 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 poi
23、nt isdetermined to the nearest 0.5C (1F).5. Significance and Use5.1 Flash point measures the response of the specimen ofthe sample to heat and flame under controlled laboratoryconditions. It is only one of a number of properties that must beconsidered in assessing the overall flammability hazard of
24、amaterial.5.2 Flash point is used in shipping and safety regulations todefine flammable and combustible materials and classify them.One should consult the particular regulation involved forprecise definitions of these classes.5.3 Flash point can indicate the possible presence of highlyvolatile and f
25、lammable materials in a relatively nonvolatile ornonflammable material.5.4 Requires smaller sample (2 to 4 mL) and thereforereduced test time (1 to 2 min).6. Apparatus6.1 Test Cup and Cover AssemblyThe essential dimen-sions and requirements of the apparatus are shown in Fig.A1.1andTableA1.1 ofAnnexA
26、1.The apparatus and accessories aredescribed in detail in Annex A1. The temperature range from20 to 300C may require more than one instrument.7. Hazards7.1 The operator must exercise and take appropriate safetyprecautions during the initial application of the test flame to thesample. Samples contain
27、ing low-flash material can give anabnormally strong flash when the test flame is first applied.7.2 When using the instruments at elevated temperatures,take care to keep hands away from the cup area, except for theoperating handles as temperatures can exceed 40C (104F).8. Sample8.1 Erroneously high f
28、lash points can be obtained whenprecautions are not taken to avoid the loss of volatile material.Do not open containers unnecessarily and make a transferunless the sample temperature is at least 10C (18F) below theexpected flash point. Do not use specimens from leaky con-tainers for this test.8.2 Do
29、 not store samples in gaspermeable containers sincevolatile material can diffuse through the walls of the enclosure.Samples in leaky containers are suspect and not a source ofvalid results.8.3 A 2 or 4-mL specimen is required for each test. Obtainat least a 50-mL sample from the bulk test site and s
30、tore in aclean, tightly closed container.9. Preparation of Apparatus9.1 Place the tester on a level, stable surface. Unless testsare made in a draft-free area, surround the tester on three sideswith a shield for protection. Do not rely on tests made in alaboratory draft hood or near ventilators.TABL
31、E 1 Calibration of TesterMaterial p-xyleneA,B(1.4Dimethylbenzene) (Warning)Cn-butanolA(Butan-1-ol) (Warning)CSpecific gravity, 15.6/15.6C (60/60F) 0.860 to 0.866 0.810 to 0.812Boiling range, C (F) 2 (4) maximum including 138.35 (281.03) 2 (4) maximum including 117.5 (243.5)Freezing point, C (F) 52.2
32、 (11.23) minimum 90 (130) minimumFlash point, C (F) (acceptable range) 25.6 6 0.5 (78 6 1) 36.6 6 0.8 (97.9 6 1.7)AAvailable as Flash Point Check Fluid from Special Products Div., Phillips Petroleum Co., Drawer O, Bergen, TX 79007.BContains less than 500 v ppm of C6and lighter hydrocarbons by gas ch
33、romatography.C(WarningHandle xylene and n-butanol with care. Avoid inhalation.)D 3828 07a29.2 Read the manufacturers instructions on the care andservicing of the instrument and for correct operation ofcontrols. Low temperature testing is ambient to 110C (230F).High temperature is 100 to 300C (212 to
34、 572F).10. Calibration and Standardization10.1 Before initial use determine and plot the relationshipbetween the temperature control dial and the thermometerreadings:10.1.1 Turn the temperature control knob (see Note 1) fullycounterclockwise (“0” reading). Advance the temperature con-trol knob clock
35、wise until the indicator light is illuminated seeNote 2). Advance the knob clockwise to the next numberedline.After the thermometer mercury column ceases to advance,record the dial reading and the temperature. Advance the knobclockwise to the next numbered line. After the thermometermercury column c
36、eases to advance, record the dial reading andthe temperature. Repeat this procedure through the full rangeof the instrument. Plot the dial readings versus the respectivetemperatures.NOTE 1When the instrument has two temperature control knobs, setthe fine control (center, small knob) at its mid-posit
37、ion and allow it toremain there throughout the calibration. The calibration is determined byadjusting the coarse control (larger, out knob) only.NOTE 2When testing at low temperatures, it will be found that theindicator light need not illuminate and the temperature need not rise untilan upscale temp
38、erature control setting is reached.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 mat
39、erial shall be tested according toMethod B, Section 12. Procedure of this test method and theobserved flash point obtained in 12.6 shall be corrected forbarometric pressure (see Section 13). The flash point obtainedshall be within the limits stated in Table A2.1 for the identifiedCRM or within the l
40、imits calculated for an unlisted CRM (seeAnnex A2).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 (se
41、e 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 inAnnexA1, especially with regard to tightness of the lid (A1.1.1), theaction of the shutter, the position of
42、the ignition source (A1.2),and the angle and position of the temperature measuringdevice. After any adjustment, repeat the test in 10.2 or 10.3using a fresh test specimen, with special attention to theprocedural details prescribed in the test method.METHOD AFLASH/NO FLASH TEST11. Procedure11.1 Deter
43、mine the target flash point as follows:I! Target flash point, C 5 Sc2 0.25101.3 2 A! (1)II! Target flash point, C 5 Sc2 0.03760 2 B! (2)III! Target flash point, F 5 Sf2 0.06760 2 B! (3)where:Sc= specification, or uncorrected target, flash point, C,Sf= specification, or uncorrected target, flash poin
44、t, F,andB = ambient barometric pressure, mm Hg, andA = ambient barometric pressure, kPa.11.2 The barometric pressure used in this calculation shallbe the ambient pressure for the laboratory at the time of test.Many aneroid barometers, such as those used at weatherstations and airports, are precorrec
45、ted to give sea level read-ings; these shall not be used.11.3 Select the proper instrument, as recommended by themanufacturer, for the target flash point (see 8.2).11.3.1 Inspect the inside of the sample cup, lid, and shuttermechanism for cleanliness. Use an absorbent paper tissue towipe clean, when
46、 necessary. Put cover in place and locksecurely. The filling orifice can be conveniently cleaned with apipe cleaner.11.4 For Target Temperature Above AmbientSwitch theinstrument on and turn the coarse temperature control knobfully clockwise (full on) causing the indicator light to illumi-nate (see N
47、ote 3). When the thermometer indicates a tempera-ture about 3C (5F) below the target (or specification)temperature, reduce the heat input to the sample cup by turningthe coarse temperature control knob counterclockwise to thedesired control point (see 11.1). When the indicator lightslowly cycles on
48、and off read the temperature on the thermom-eter. When necessary, adjust the fine (center) temperaturecontrol knob to obtain the desired test (target) temperature.When the test temperature is reached and the indicator lampslowly cycles on and off, prepare to introduce the specimen ofthe sample.NOTE
49、3The target temperature can be attained by originally turningthe coarse temperature control knob to the proper setting (see 9.1) for thetemperature desired rather than to the maximum setting (full on). Theelapsed time to reach the temperature will be greater, except for maximumtemperature; however, less attention will be required during the interven-ing period.11.5 Charge the syringe with a 2-mL portion of the sampleto be tested; transfer the syringe to the filling orifice, takingcare not to lose any sample; discharge th
