1、Designation: D93 11Designation: 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 Department of Defense.INTRODUCTIONThis flash point test method is a dynamic
3、 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 slower h
4、eating rates available, such as Test Method D3941 (forpaints, resins, and related products, and high viscosity products in the range of 0 to110C), where thetest conditions are closer to equilibrium.Flash point values are a function of the apparatus design, the condition of the apparatus used, andthe
5、 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 methods
6、cover the determination of the flashpoint of petroleum products in the temperature range from 40to 360C by a manual Pensky-Martens closed-cup apparatus oran automated Pensky-Martens closed-cup apparatus, and thedetermination of the flash point of biodiesel in the temperaturerange of 60 to 190C by an
7、 automated Pensky-Martens closedcup apparatus.NOTE 1Flash point determination as above 250C can be performed,however, the precision has not been determined above this temperature.For residual fuels, precision has not been determined for flash pointsabove 100C. The precision of in-use lubricating oil
8、s has not beendetermined. Some specifications state a D93 minimum flash point below40C, 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-use lubricating oi
9、ls, 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 filmunder test conditi
10、ons, 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 manual flash point te
11、chniques, 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 units are to be re
12、garded as thestandard. The values given in parentheses are for informationonly.NOTE 2It has been common practice in flash point standards for manydecades to alternately use a Cscale or an Fscale thermometer fortemperature measurement. Although the scales are close in increments,they are not equivale
13、nt. Because the Fscale thermometer used in thisprocedure is graduated in 5 increments, it is not possible to read it to the2C equivalent increment of 3.6F. Therefore, for the purposes ofapplication of the procedure of the test method for the separate tempera-ture scale thermometers, different increm
14、ents 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 370C (698F). When a temperature isintended to be a rationalized unit for the alternate scale, it
15、 will appear after“or,” for example, 2C or 5F.1These test methods are under the joint jurisdiction ofASTM Committee D02 onPetroleum Products and Lubricants and are the direct responsibility of Subcommit-tee D02.08 on Volatility. In the IP, these test methods are under the jurisdiction ofthe Standard
16、ization Committee.Current edition approved Oct. 1, 2011. Published November 2011. Originallyapproved in 1921. Last previous edition approved in 2010 as D9310a. DOI:10.1520/D0093-11.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive,
17、 PO Box C700, West Conshohocken, PA 19428-2959, United States.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 safety and health practices and determine the applica
18、-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 Test Method for Flash Point by the EquilibriumMet
19、hod 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 Sampling Industrial ChemicalsE502 Test Method for Select
20、ion and Use of ASTM Stan-dards for the Determination of Flash Point of Chemicals byClosed Cup Methods2.2 ISO Standards3Guide 34 Quality Systems Guidelines for the Production ofReference MaterialsGuide 35 Certification of Reference MaterialGeneral andStatistical Principles3. Terminology3.1 Definition
21、s: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 petroleum productsin petroleumproduct flash point test
22、 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 constant prescribed rate with thevapor temperature
23、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 ignition source is applied.3.1.4.1 DiscussionThis c
24、ondition 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 petroleum products, the lowesttemperature corrected to a barometric pressure of 101.3 kPa(760 mm Hg
25、), at which application of an ignition source causesthe vapors of a specimen of the sample to ignite under specifiedconditions of test.4. Summary of Test Method4.1 A brass test cup of specified dimensions, filled to theinside mark with test specimen and fitted with a cover ofspecified dimensions, is
26、 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 stirring, until aflash is detected (see 11.1.8). The flash point is reported asdefined in
27、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 properties which must be considered inassessing the overall flammability hazard of
28、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 classifications.NOTE 3The U.S. Department of Transportation (DOT)4and U.S.Department of Labor (OS
29、HA) have established that liquids with a flashpoint under 37.8C (100F) are flammable, as determined by these testmethods, for those liquids which have a kinematic viscosity of 5.8 mm 2/s(cSt) or more at 37.8C or 9.5 mm 2/s (cSt) or more at 25C (77F), or thatcontain suspended solids, or have a tenden
30、cy to form a surface film whileunder test. Other classification flash points have been established by thesedepartments for liquids using these test methods.5.3 These test methods should be used to measure anddescribe the properties of materials, products, or assemblies inresponse to heat and an igni
31、tion source under controlledlaboratory conditions and should not be used to describe orappraise the fire hazard or fire risk of materials, products, orassemblies under actual fire conditions. However, results ofthese test methods may be used as elements of a fire riskassessment which takes into acco
32、unt 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 flashpoint test procedures for temperatures up to 370C (698F).6. Apparatus6.1 Pensky-Martens Closed Cup Apparatus (manual)Thisapparatus consists of
33、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. The assembledmanual apparatus, test cup, test cup cover, and test cup2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact A
34、STM 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 Floor, New York, NY 10036.4For information on U.S. Department
35、 of Transportation regulations, see Codesof U.S. Regulations 49 CFR Chapter 1 and the U.S. Department of Labor, see 29CFR Chapter XVII. Each of these items is revised annually and may be procuredfrom the Superintendent of Documents, Government Printing Office, Washington,DC 20402.D93112assembly are
36、illustrated in Figs. A1.1-A1.4, respectively. Di-mensions are listed respectively.6.2 Pensky-Martens Closed Cup Apparatus (Automated)5This apparatus is an automated flash point instrument that iscapable of performing the test in accordance with Section 11(ProcedureA), Section 12 (Procedure B), and 1
37、3 (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 as follows and conforming to the require-me
38、nts 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.Thermometer NumberTemperature Range ASTM IP5 to +110C (20 to 230F) 9C (9F)
39、 15C+10 to 200C (50 to 392F) 88C (88F) 101C+90 to 370C (200 to 700F) 10C (10F) 16C6.4 Ignition SourceNatural gas 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
40、 of the pilot flamedescribed in A1.1.2.3. The electric ignitors shall be of thehot-wire type and shall position 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
41、3 kPa (12 in.) ofwater pressure.)6.5 BarometerWith accuracy of 60.5 kPa.NOTE 4The barometric pressure used in this calculation is theambient pressure for the laboratory at the time of the test. Many aneroidbarometers, such as those used at weather stations and airports, areprecorrected to give sea l
42、evel readings and would not give the correctreading for this test.7. Reagents and Materials7.1 Cleaning SolventsUse 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, a
43、nd many solvents areflammable and a health hazard. Dispose of solvents and wastematerial in accordance with local regulations.)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
44、 D4057. When obtaining a sample of residual fueloil, the sample container shall be from 85 to 95 % full. Forother types of 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
45、(B100) samples, a typical one liter container filled to 85%volume is recommended.8.3 Successive 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 % fi
46、lled. The resultsof flash point determinations can be affected if the samplevolume is less than 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 lo
47、ss of volatilematerial or possible introduction of moisture, or both. Avoidstorage of samples at temperatures in excess of 35C or 95F.Samples for storage shall be capped tightly with inner seals. Donot make a transfer unless the sample temperature is at least theequivalent of 18C or 32F below the ex
48、pected flash point.8.5 Do not store samples in gas-permeable containers, sincevolatile material 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
49、/cap slightly loosened to avoid buildupof dangerous pressure, at the lowest temperature adequate toliquefy any solids, not exceeding 28C or 50F 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 to the specimen cup. No sample shall beheated and transferred unless its temperatures is more than18C or 32F belo
