1、Designation: D 3278 96 (Reapproved 2004)e1Standard Test Methods forFlash Point of Liquids by Small Scale Closed-CupApparatus1This standard is issued under the fixed designation D 3278; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision
2、, 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.e1NOTEWarning notes were editorial
3、ly moved into the text in November 2004.1. Scope1.1 These test methods cover procedures for determiningwhether a material does or does not flash at a specifiedtemperature or for determining the lowest finite temperature atwhich a material does flash when using a small scale closed-cup apparatus.2The
4、 test methods are applicable to paints,enamels, lacquers, varnishes, and related products having aflash point between 0 and 110C (32 and 230F) and viscositylower than 150 St at 25C (77F).NOTE 1Tests at higher or lower temperatures are possible.NOTE 2More viscous materials may be tested in accordance
5、 withAnnex A4.NOTE 3Organic peroxides may be tested in accordance with AnnexA5, which describes the applicable safety precautions.NOTE 4The U.S. Department of Labor (OSHA, Hazard Communica-tions), the U.S. Department of Transportation (RSPA), and the U.S.Environmental Protection Agency (EPA) have sp
6、ecified Test MethodsD 3278 as one of several acceptable methods for the determination of flashpoint of liquids in their regulations.NOTE 5These test methods are similar to International Standards ISO3679 and ISO 3680.1.2 The values stated in SI units are to be regarded as thestandard. The values giv
7、en in parentheses are for informationonly.1.3 This standard should be used to measure and describethe response of materials, products, or assemblies to heat andflame under controlled conditions and should not be used todescribe or appraise the fire-hazard or fire-risk of materials,products, or assem
8、blies under actual fire conditions. However,results of the test may be used as elements of a fire-hazard ora fire-risk assessment which takes into account all of thefactors which are pertinent to an assessment of the fire hazardor fire risk of a particular end use.1.4 This standard does not purport
9、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. For specific hazardstatements, see 8.1 and 11.2.2
10、. Referenced Documents2.1 ASTM Standards:3D 56 Test Method for Flash Point by Tag Closed TesterD 93 Test Methods for Flash Point by Pensky-MartensClosed TesterD 850 Test Method for Distillation of Industrial AromaticHydrocarbons and Related MaterialsD 1015 Test Method for Freezing Points of High-Pur
11、ityHydrocarbonsD 1078 Test Method for Distillation Range of VolatileOrganic Liquids2.2 ISO Standards:4ISO 3679 Paints, varnishes, petroleum and relatedproductsDetermination of flash pointRapid equilib-rium methodISO 3680 Paints, varnishes, petroleum and relatedproductsFlash/no flash testRapid equili
12、brium method3. Terminology3.1 Definitions:3.1.1 flash point, nthe lowest temperature, corrected to apressure of 760 mm Hg (101.3 kPa, 1013 mbar), at which1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directr
13、esponsibility of Subcommittee D01.22 on Health and Safety.Current edition approved Nov. 1, 2004. Published November 2004. Originallyapproved in 1973. Last previous edition approved in 1996 as D 3278 96e1.2Small scale closed-cup apparatus has been found suitable for this purpose.3For referenced ASTM
14、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.4Available from American National Standards Institute, 13th Floor, 11 W. 42ndSt.,
15、New York, NY 10036.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.application of an ignition source causes the vapor of thespecimen to ignite under specified conditions of test.4. Summary of Test Methods4.1 By means of a syringe, 2
16、mLof the sample is introducedthrough a leakproof entry port into the tightly closed smallscale closed-cup apparatus2or directly into the cup that hasbeen brought to the required test temperature. As a flash/noflash test, the expected flash point temperature may be aspecification or other operating r
17、equirement.After 1 min, a testflame is applied inside the cup and note is taken whether or notthe test specimen flashes. A fresh specimen must be used if arepeat test is necessary.4.2 For a finite flash point measurement, the temperature issequentially increased through the anticipated range, the te
18、stflame being applied at 5C (9F) intervals until a flash isobserved. A true determination is then made using a freshspecimen, starting the test at the temperature of the last intervalbefore the flash point of the material and making tests atincreasing 0.5C (1F) intervals.5. Significance and Use5.1 F
19、lash point is one of the properties used to define theflammability of a liquid. It is used to classify liquids accordingto their flammability by governmental regulatory agencies. Itmay also be used to determine the presence of impurities orcontaminants in a given liquid, such as the presence of resi
20、dualsolvents in solvent-refined drying oils. See Test Methods D 56and D 93 for alternate flash point testing.6. Apparatus6.1 Test Cup and Cover Assembly5The essential dimen-sions and requirements of the apparatus are shown in Fig.A1.1and described in Annex A1.6.2 Thermometers,6low, medium, high temp
21、erature smallscale. Test to determine that the scale error does not exceed0.25C (0.5F). The use of a magnifying lens assists in makingtemperature observations.6.3 Glass Syringe,26 0.1-mL capacity at 25C (77F), toprovide a means of taking a uniform specimen. Check thecapacity by discharging water int
22、o a weighing bottle andweighing. Adjust plunger if necessary. A disposable syringe ofequal precision may be used.6.4 Aluminum Cooling Block7(describing in Annex A2),that fits snugly within the test cup used for rapid cooling of thesample cup.6.5 Barometer.7. Reagents and Materials7.1 p-Xylene,8refer
23、ence standard.7.2 n-Butanol,9reference standard.7.3 Cooling Mixtures of ice and water or solid CO2(dryice) and acetone.7.4 Liquified Petroleum Gas.7.5 Heat Transfer Paste.108. Sampling8.1 The specimen size for each test is 2 mL. Obtain at leasta 25-mLsample from the bulk source and store in a nearly
24、 full,tightly closed, clean glass container or in other containersuitable for the type of liquid being sampled. (WarningErroneously high flash points may be obtained if precautionsare not taken to avoid loss of volatile material. Do not opensample containers unnecessarily and do not transfer the spe
25、ci-men to the cup unless the temperature of the specimen is atleast 10C (20F) below the expected flash point. Discardsamples in leaky containers.) (WarningDo not store samplesin plastic bottles (polyethylene, polypropylene, etc.), as volatilematerial may diffuse through the walls.)9. Preparation of
26、Apparatus9.1 Prior to initial use or after removal of the thermometer,insert the thermometer into its pocket (see Fig. A1.1) with agood heat transfer paste.9.2 To help in making the necessary settings during a test,before the initial use determine the relationship between thetemperature control dial
27、 and thermometer readings at intervalsnot over 5C (9F) throughout the scale range of the heater.9.3 Place the tester in a subdued light and in a position notexposed to disturbing drafts. Provide a black-coated shield, ifnecessary.9.4 Read the manufacturers operating and maintenanceinstructions on th
28、e care and servicing of the tester. Observe thespecific suggestions regarding the operation of the variouscontrols.9.5 Check the accuracy of the tester by duplicate determi-nation of the flash point of the p-xylene reference standard(Annex A3). The mean of the results should be 27.2 6 0.8C(81 6 1.5F
29、). An additional reference standard, n-butanol(Annex A3), may be used to check the accuracy at approxi-mately the temperature specified by U.S. regulatory agencies indefining flammable liquids. The mean of duplicates should be36.7 6 0.8C (98 6 1.5F). If not, remove the thermometerand observe whether
30、 sufficient heat transfer paste surrounds thethermometer to provide good heat transfer from the cup to thethermometer.5Closed-cup flash point testers and their accessories meeting the requirements ofthe unit shown in Fig. A1.1 are available from ERDCO Engineering Corp., 721Custer Ave., Evanston, IL
31、60202 or Stanhope-Seta Ltd., Park Close EnglefieldGreen, Engham, Surrey, TW20 OXD, England.6Thermometers may be obtained from the suppliers of the Small Scale Tester.7Cooling blocks may be obtained from ERDCO Engineering Corp.8p-Xylene is available as “Flash Point Check Fluid” from Special Products
32、Div.,Chemical Dept., Phillips Petroleum Co., Borger, TX 25303.9n-Butanol may be obtained from chemical supply companies.10Heat transfer paste is available from the suppliers of the Small Scale Tester.No. 340 Silicone is available from Dow Corning Corp., 2030 Willard H. DowCenter, Midland, MI 48674.
33、G641 Heat Transfer Compound is available fromGeneral Electric Co., Products Div., 12 Corporate Woods Blvd.,Albany, NY 12211.D 3278 96 (2004)e12TEST METHOD AFLASH/NO FLASH10. ProcedureAmbient to 110C (230F)10.1 Inspect the inside of the test cup, lid, and shuttermechanism for cleanliness and freedom
34、from contamination.Use an absorbent tissue to wipe clean, if necessary. Lock thecover lid tightly in place.10.2 Switch the heater on, if not already at stand-by. Torapidly approach the specification flash temperature of thematerial under test, turn the heater dial fully clockwise (Note 6)causing the
35、 heater signal (red) light to glow. When thethermometer indicates a temperature of about 3C (5F) belowthe specification or target flash-point temperature, reduce theheat input to the test cup by slowly turning the heater controldial counter clockwise until the signal light goes out (Note 7).NOTE 6Wh
36、en a desired temperature is dialed on the controller, theelapsed time to reach this temperature may be greater than if the controlleris turned“ full on,” but less attention is required.NOTE 7The test cup temperature is stable when the signal light slowlycycles on and off.10.3 Determine the barometri
37、c pressure to determine thecorrected specification temperature at that barometric pressure(see 15.1).10.4 After the test-cup temperature has stabilized at thespecification or target flash point, charge the syringe with thesample being tested and insert the tip of the syringe into thefilling orifice
38、(Fig. A1.1), taking care not to lose any material.Discharge the specimen into the test cup by completelydepressing the syringe plunger, then remove the syringe. If thematerial has a viscosity greater than 45 SUS at 38C (100F) orequivalent of 9.5 cSt at 25C (77F), raise the lid and dischargethe conte
39、nts of the syringe directly into the cup. Immediatelyclose the lid tightly.10.5 Set the 1-min timing device. In the meantime, open thegas control valve and light the pilot and test flames. Adjust thetest flame size with the pinch valve to match the size of the532-in. (4-mm) diameter flame gage.10.6
40、After 1 min has elapsed, observe the temperature. If atthe specification temperature (accounting for the differences ofthe barometer reading from 760 mm), apply the test flame byslowly and uniformly opening the slide fully and closingcompletely over a period of approximately 212 s (Note 8),watching
41、for a flash (Note 9) while the flame is inserted.NOTE 8When inserted, the nozzle of the ignition device shouldintersect the plane of the underside of the cover (see A1.1).NOTE 9The material is considered to have flashed only if a compara-tively large blue flame appears and propagates itself over the
42、 surface of theliquid. Occasionally, particularly near the actual flash-point temperature,application of the test flame may give rise to a halo; this effect should beignored.10.7 Turn off the test and pilot flame. Clean the apparatus inpreparation for the next test.11. Procedure0C (32F) to Ambient11
43、.1 If the specification or target flash point is at or belowambient temperature, cool the sample to 5 to 10C (10 to 20F)below that point by some convenient means.11.2 Cool the tester to approximately the temperature of thesample by inserting the cooling block (Fig. A2.1) filled with acooling mixture
44、 into the sample well. Dry the cup with a papertissue to remove any collected moisture prior to adding thespecimen using a precooled syringe. (WarningBe careful inhandling the cooling mixture and cooling block; wear glovesand goggles. Mixtures such as dry ice and acetone can producesevere frost bite
45、.) (WarningBe careful when inserting thecooling block into the tester cup to prevent damage to the cup.)11.3 Introduce the specimen as in 10.4. Allow the tempera-ture to rise under ambient conditions or increase the tempera-ture of the cup by rotating the heater controller clockwiseslowly until the
46、specification temperature adjusted for baro-metric pressure is reached. Determine whether the materialflashes as in 10.5 and 10.6.11.4 Turn off the test and pilot flames. Clean the apparatus.TEST METHOD BFINITE FLASH POINT12. ProcedureAmbient to 110C (230F)12.1 Preliminary or Trial Test:12.1.1 Follo
47、w steps 10.1-10.5, omitting the barometric read-ing and using an estimated finite flash point instead ofspecification flash-point temperature.12.1.2 After 1 min has elapsed, observe the temperature.Apply the test flame by slowly and uniformly opening the slidefully and closing completely over a peri
48、od of 212 s (Note 8),watching for a flash (Note 9) while the flame is inserted.12.2 If a flash is observed, proceed as in 12.3. If no flash isobserved, proceed as in 12.4.12.3 Using a temperature 5C (9F) lower than the tempera-ture observed in 12.1.2, repeat 12.1 (Note 4). If a flash is stillobserve
49、d, repeat at 5C lower intervals until no flash isobserved.NOTE 10Never make a repeat test on the same specimen.Always takea fresh portion for each test.12.3.1 After establishing the approximate flash point, repeat12.1 with a new specimen, but stabilizing the test temperatureat which no flash occurred previously. Observe if a flash occursat this temperature. If not, increase the temperature by makinga small adjustment to the temperature controller so that anincrease of 0.5C (1F) occurs within 1 min. Test for a flash
