1、Designation: D93 16aDesignation: 34/99Standard Test Methods forFlash Point by Pensky-Martens Closed Cup Tester1This standard is issued under the fixed designation D93; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of las
2、t revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.INTRODUCTIONThis flash point test method is a d
3、ynamic test method which depends on specified rates of heatingto be able to meet the precision of the test method. The rate of heating may not in all cases give theprecision quoted in the test method because of the low thermal conductivity of some materials. Thereare flash point test methods with sl
4、ower heating rates available, such as Test Method D3941 (forpaints, resins, and related products, and high viscosity products in the range of 0 C to 110 C), wherethe test conditions are closer to equilibrium.Flash point values are a function of the apparatus design, the condition of the apparatus us
5、ed, 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 specified.1. Scope*1.1 These tes
6、t methods cover the determination of the flashpoint of petroleum products in the temperature range from40 C to 370 C by a manual Pensky-Martens closed-cupapparatus or an automated Pensky-Martens closed-cupapparatus, and the determination of the flash point of biodieselin the temperature range of 60
7、C to 190 C by an automatedPensky-Martens closed cup apparatus.NOTE 1Flash point determinations above 250 C can be performed,however, the precision has not been determined above this temperature.For residual fuels, precision has not been determined for flash pointsabove 100 C. The precision of in-use
8、 lubricating oils has not beendetermined. Some specifications state a D93 minimum flash point below40 C, however, the precision has not been determined below thistemperature.1.2 Procedure A is applicable to distillate fuels (diesel,biodiesel blends, kerosine, heating oil, turbine fuels), new andin-u
9、se lubricating oils, and other homogeneous petroleumliquids not included in the scope of Procedure B or ProcedureC.1.3 Procedure B is applicable to residual fuel oils, cutbackresidua, used lubricating oils, mixtures of petroleum liquidswith solids, petroleum liquids that tend to form a surface filmu
10、nder test conditions, or are petroleum liquids of such kine-matic viscosity that they are not uniformly heated under thestirring and heating conditions of Procedure A.1.4 Procedure C is applicable to biodiesel (B100). Since aflash point of residual alcohol in biodiesel is difficult to observeby manu
11、al flash point techniques, automated apparatus withelectronic flash point detection have been found suitable.1.5 These test methods are applicable for the detection ofcontamination of relatively nonvolatile or nonflammable ma-terials with volatile or flammable materials.1.6 The values stated in SI u
12、nits are to be regarded as thestandard.1.6.1 ExceptionThe values given in parentheses are forinformation only.NOTE 2It has been common practice in flash point standards for manydecades to alternately use a C-scale or an F-scale thermometer fortemperature measurement. Although the scales are close in
13、 increments,they are not equivalent. Because the F-scale thermometer used in thisprocedure is graduated in 5 F increments, it is not possible to read it tothe 2 C equivalent increment of 3.6 F. Therefore, for the purposes ofapplication of the procedure of the test method for the separate tempera-tur
14、e scale thermometers, different increments must be used. In this testmethod, the following protocol has been adopted: When a temperature isintended to be a converted equivalent, it will appear in parenthesesfollowing the SI unit, for example 370 C (698 F). When a temperature1These test methods are u
15、nder the joint jurisdiction ofASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and are the direct responsibilityof Subcommittee D02.08 on Volatility. In the IP, these test methods are under thejurisdiction of the Standardization Committee.Current edition approved Oct. 1, 2016. P
16、ublished October 2016. Originallyapproved in 1921. Last previous edition approved in 2016 as D93 16. DOI:10.1520/D0093-16A.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United State
17、s1is intended to be a rationalized unit for the alternate scale, it will appearafter “or,” for example, 2 C or 5 F.1.7 This 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
18、safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see 6.4, 7.1, 9.3, 9.4, 11.1.2, 11.1.4, 11.1.8,11.2.2, and 12.1.2.2. Referenced Documents2.1 ASTM Standards:2D56 Test Method for Flash Point by Tag Closed Cup TesterD3
19、941 Test Method for Flash Point by the EquilibriumMethod With a Closed-Cup ApparatusD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsE1 Specification for ASTM Liquid-in-Glass ThermometersE300 Practice for Sam
20、pling Industrial ChemicalsE502 Test Method for Selection and Use of ASTM Stan-dards for the Determination of Flash Point of Chemicalsby Closed Cup Methods2.2 ISO Standards3Guide 34 General requirements for the competence of refer-ence material producersGuide 35 Reference materialGeneral and statisti
21、cal prin-ciples for certification3. Terminology3.1 Definitions:3.1.1 biodiesel, na fuel comprised of mono-alkyl esters oflong chain fatty acids derived from vegetable oils or animalfats, designated B100.3.1.2 biodiesel blends, na blend of biodiesel fuel withpetroleum-based diesel fuel.3.1.3 dynamic,
22、 adjin petroleum productsin petroleumproduct flash point test methodsthe condition where thevapor above the test specimen and the test specimen are not intemperature equilibrium at the time that the ignition source isapplied.3.1.3.1 DiscussionThis is primarily caused by the heatingof the test specim
23、en at the constant prescribed rate with thevapor temperature lagging behind the test specimen tempera-ture.3.1.4 equilibrium, nin petroleum productsin petroleumproduct flash point test methodsthe condition where thevapor above the test specimen and the test specimen are at thesame temperature at the
24、 time the ignition source is applied.3.1.4.1 DiscussionThis condition may not be fullyachieved in practice, since the temperature may not be uniformthroughout the test specimen, and the test cover and shutter onthe apparatus can be cooler.3.1.5 flash point, nin flash point test methods, the lowestte
25、mperature of the test specimen, adjusted to account forvariations in atmospheric pressure from 101.3 kPa, at whichapplication of an ignition source causes the vapors of the testsample to ignite under specified conditions of test.4. Summary of Test Method4.1 A brass test cup of specified dimensions,
26、filled to theinside mark with test specimen and fitted with a cover ofspecified dimensions, is heated and the specimen stirred atspecified rates, using one of three defined procedures (A, B, orC). An ignition source is directed into the test cup at regularintervals with simultaneous interruption of
27、the stirring, until aflash is detected (see 11.1.8). The flash point is reported asdefined in 3.1.5.5. Significance and Use5.1 The flash point temperature is one measure of thetendency of the test specimen to form a flammable mixturewith air under controlled laboratory conditions. It is only oneof a
28、 number of properties which must be considered inassessing the overall flammability hazard of a material.5.2 Flash point is used in shipping and safety regulations todefine flammable and combustible materials. One should con-sult the particular regulation involved for precise definitions ofthese cla
29、ssifications.5.3 These test methods should be used to measure anddescribe the properties of materials, products, or assemblies inresponse to heat and an ignition source under controlledlaboratory conditions and should not be used to describe orappraise the fire hazard or fire risk of materials, prod
30、ucts, orassemblies under actual fire conditions. However, results ofthese test methods may be used as elements of a fire riskassessment which takes into account all of the factors whichare pertinent to an assessment of the fire hazard of a particularend use.5.4 These test methods provide the only cl
31、osed cup flashpoint test procedures for temperatures up to 370 C (698 F).6. Apparatus6.1 Pensky-Martens Closed Cup Apparatus (manual)This apparatus consists of the test cup, test cover and shutter,stirring device, heating source, ignition source device, air bath,and top plate described in detail in
32、Annex A1. The assembledmanual apparatus, test cup, test cup cover, and test cupassembly are illustrated in Figs. A1.1-A1.4, respectively. Di-mensions are listed respectively.6.2 Pensky-Martens Closed Cup Apparatus (Automated)4This apparatus is an automated flash point instrument that is2For referenc
33、ed 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 American National Standards Institute (ANSI), 25 W. 43rd S
34、t.,4th Floor, New York, NY 10036, http:/www.ansi.org.4Supporting data regarding a variant of the cover locking mechanism have beenfiled at ASTM International Headquarters and may be obtained by requestingResearch Report RR:D02-1706.D93 16a2capable of performing the test in accordance with Section 11
35、(ProcedureA), Section 12 (Procedure B), and 13 (Procedure C)of these test methods. The apparatus shall use the test cup, testcover and shutter, stirring device, heating source, and ignitionsource device described in detail in Annex A1.6.3 Temperature Measuring DeviceThermometer havinga range as show
36、n in Table 1 and conforming to the require-ments prescribed in Specification E1 or in Annex A3,oranelectronic temperature measuring device, such as resistancethermometers or thermocouples. The device shall exhibit thesame temperature response as the mercury thermometers.6.4 Ignition SourceNatural ga
37、s flame, bottled gas flame,and electric ignitors (hot wire) have been found acceptable foruse as the ignition source. The gas flame device described indetailed in Fig. A1.4 requires the use of the pilot flamedescribed in A1.1.2.3. The electric ignitors shall be of thehot-wire type and shall position
38、 the heated section of theignitor in the aperture of the test cover in the same manner asthe gas flame device. (WarningGas pressure supplied to theapparatus should not be allowed to exceed 3 kPa (12 in.) ofwater pressure.)6.5 BarometerWith accuracy of 60.5 kPa.NOTE 3The barometric pressure used in t
39、his calculation is the ambientpressure for the laboratory at the time of the test. Many aneroidbarometers, such as those used at weather stations and airports, areprecorrected to give sea level readings and would not give the correctreading for this test.7. Reagents and Materials7.1 Cleaning Solvent
40、sUse suitable solvent capable ofcleaning out the specimen from the test cup and drying the testcup and cover. Some commonly used solvents are toluene andacetone. (WarningToluene, acetone, and many solvents areflammable and a health hazard. Dispose of solvents and wastematerial in accordance with loc
41、al regulations.)8. Sampling8.1 Obtain a sample in accordance with instructions given inPractices D4057, D4177,orE300.8.2 Ensure at least 75 mL of sample is available so there issufficient material for the test. When obtaining a sample ofresidual fuel oil, the sample container shall be from 85 % to95
42、 % full. For other types of samples, the size of the containershall be chosen such that the container is not more than 85 %full or less than 50 % full prior to any sample aliquot beingtaken. For biodiesel (B100) samples, a typical one litercontainer filled to 85 % volume is recommended.8.3 Successiv
43、e test specimens can be taken from the samesample container. Repeat tests have been shown to be withinthe precisions of the method when the second specimen istaken with the sample container at least 50 % filled. The resultsof flash point determinations can be affected if the samplevolume is less tha
44、n 50 % of sample container capacity.8.4 Erroneously high flash points may be obtained if pre-cautions are not taken to avoid the loss of volatile material. Donot open containers unnecessarily, to prevent loss of volatilematerial or possible introduction of moisture, or both. Avoidstorage of samples
45、at temperatures in excess of 35 C or 95 F.Samples for storage shall be capped tightly with inner seals. Donot make a transfer unless the sample temperature is at least theequivalent of 18 C or 32 F below the expected flash point.8.5 Do not store samples in gas-permeable containers, sincevolatile mat
46、erial may diffuse through the walls of the enclo-sure. Samples in leaky containers are suspect and not a sourceof valid results.8.6 Samples of very viscous materials shall be heated intheir containers, with lid/cap slightly loosened to avoid buildupof dangerous pressure, at the lowest temperature ad
47、equate toliquefy any solids, not exceeding 28 C or 50 F below theexpected flash point, for 30 min. If the sample is then notcompletely liquefied, extend the heating period for additional30 min periods as necessary. Then gently agitate the sample toprovide mixing, such as orbiting the container horiz
48、ontally,before transferring to the specimen cup. No sample shall beheated and transferred unless its temperatures is more than18 C or 32 F below its expected flash point. When the samplehas been heated above this temperature, allow the sample tocool until its temperature is at least 18 C or 32 F bel
49、ow theexpected flash point before transferring.NOTE 4Volatile vapors can escape during heating when the samplecontainer is not properly sealed.NOTE 5Some viscous samples may not completely liquefy even afterprolonged periods of heating. Care should be exercised when increasingthe heating temperature to avoid unnecessary loss of volatile vapors, orheating the sample too close to the flash point.8.7 Samples containing dissolved or free water may bedehydrated with calcium chloride or by filtering through aqualitative filter paper o
