1、Designation: D93 16Designation: 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 last
2、 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 dy
3、namic 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 slo
4、wer 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 use
5、d, 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 test
6、 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 C
7、 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-us
9、e 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 filmun
10、der 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 manua
11、l 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 un
12、its 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-ture
14、 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 un
15、der 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 June 1, 2016. Pu
16、blished July 2016. Originally approvedin 1921. Last previous edition approved in 2015 as D93 15a. DOI: 10.1520/D0093-16.*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 States1i
17、s 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 saf
18、ety 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 TesterD3941
19、 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 Sampli
20、ng 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 Quality Systems Guidelines for the Production ofReference MaterialsGuide 35 Certification of Reference MaterialGeneral and
21、Statistical Principles3. 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, adjin petr
22、oleum 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 specimen at the c
23、onstant 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 time the i
24、gnition 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 lowesttemperature o
25、f 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, filled to t
26、heinside 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 the stirrin
27、g, 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 number of
28、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 classification
29、s.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, products, orass
30、emblies 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 closed cup fl
31、ashpoint 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 Annex A1. T
32、he 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 referenced ASTM sta
33、ndards, 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 St.,4th Floo
34、r, 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.D93162capable of performing the test in accordance with Section 11(ProcedureA),
35、 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 shown in Table 1
36、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 gas flame, bott
37、led 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 the heated s
38、ection 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 this calculati
39、on 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 SolventsUse suitable
40、 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 local regulation
41、s.)8. Sampling8.1 Obtain a sample in accordance with instructions given inPractices D4057, D4177,orE300.8.2 At least 75 mL of sample is required for each test. Referto Practice D4057. When obtaining a sample of residual fueloil, the sample container shall be from 85 % to 95 % full. Forother types of
42、 samples, the size of the container shall be chosensuch that the container is not more than 85 % full or less than50 % full prior to any sample aliquot being taken. For biodiesel(B100) samples, a typical one liter container filled to 85 %volume is recommended.8.3 Successive test specimens can be tak
43、en 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 than 50 % of sample container
44、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 at temperatures in excess o
45、f 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 material may diffuse through t
46、he 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 adequate toliquefy any solids
47、, 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 horizontally,before transferring
48、 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 below theexpected flash point
49、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 or a loose plug of dry absorb
