1、Designation: D93 15D93 15aDesignation: 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
2、of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscriptepsilon () 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
3、 dynamic 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
4、slower heating rates available, such as Test Method D3941 (forpaints, resins, and related products, and high viscosity products in the range of 0 to110C), 0 C to110 C), where the test conditions are closer to equilibrium.Flash point values are a function of the apparatus design, the condition of the
5、 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 results obtained by differenttest methods, or with test apparatus different from that specified.1. Scope*
6、1.1 These test methods cover the determination of the flash point of petroleum products in the temperature range from 4040 Cto 370C370 C by a manual Pensky-Martens closed-cup apparatus or an automated Pensky-Martens closed-cup apparatus, and thedetermination of the flash point of biodiesel in the te
7、mperature range of 6060 C to 190C190 C by an automated Pensky-Martensclosed cup apparatus.NOTE 1Flash point determinations above 250C250 C can be performed, however, the precision has not been determined above this temperature.For residual fuels, precision has not been determined for flash points ab
8、ove 100C.100 C. The precision of in-use lubricating oils has not beendetermined. Some specifications state a D93D93 minimum flash point below 40C,40 C, however, the precision has not been determined below thistemperature.1.2 Procedure A is applicable to distillate fuels (diesel, biodiesel blends, ke
9、rosine, heating oil, turbine fuels), new and in-uselubricating oils, and other homogeneous petroleum liquids not included in the scope of Procedure B or Procedure C.1.3 Procedure B is applicable to residual fuel oils, cutback residua, used lubricating oils, mixtures of petroleum liquids withsolids,
10、petroleum liquids that tend to form a surface film under test conditions, or are petroleum liquids of such kinematic viscositythat they are not uniformly heated under the stirring and heating conditions of Procedure A.1.4 Procedure C is applicable to biodiesel (B100). Since a flash point of residual
11、 alcohol in biodiesel is difficult to observe bymanual flash point techniques, automated apparatus with electronic flash point detection have been found suitable.1.5 These test methods are applicable for the detection of contamination of relatively nonvolatile or nonflammable materialswith volatile
12、or flammable materials.1.6 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.NOTE 2It has been common practice in flash point standards for many decades to alternately use a CscaleC-scale or an FscaleF-scale thermometerfor temp
13、erature measurement. Although the scales are close in increments, they are not equivalent. Because the FscaleF-scale thermometer used in thisprocedure is graduated in 5 5 F increments, it is not possible to read it to the 2C2 C equivalent increment of 3.6F.3.6 F. Therefore, for the purposes1 These t
14、est methods are under the joint jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and are the direct responsibility ofSubcommittee D02.08 on Volatility. In the IP, these test methods are under the jurisdiction of the Standardization Committee.Current edition appr
15、oved Jan. 1, 2015Oct. 15, 2015. Published February 2015November 2015. Originally approved in 1921. Last previous edition approved in 20132015as D93 13D93 15.1. DOI: 10.1520/D0093-15.10.1520/D0093-15A.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard a
16、n indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is t
17、o be considered the official document.*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 States1of application of the procedure of the test method for the separate temperature sca
18、le thermometers, different increments must be used. In this test method,the following protocol has been adopted: When a temperature is intended to be a converted equivalent, it will appear in parentheses following the SI unit,for example 370C (698F).370 C (698 F). When a temperature is intended to b
19、e a rationalized unit for the alternate scale, it will appear after “or,” forexample, 2C2 C or 5F.5 F.1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and he
20、alth practices and determine the applicability of regulatorylimitations prior to use. For specific warning 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 Meth
21、od for Flash Point by the Equilibrium Method With a Closed-Cup ApparatusD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petroleum and Petroleum ProductsE1 Specification for ASTM Liquid-in-Glass ThermometersE300 Practice for Sampling Indu
22、strial ChemicalsE502 Test Method for Selection and Use ofASTM Standards for the Determination of Flash Point of Chemicals by Closed CupMethods2.2 ISO Standards3Guide 34 Quality Systems Guidelines for the Production of Reference MaterialsGuide 35 Certification of Reference MaterialGeneral and Statist
23、ical Principles3. Terminology3.1 Definitions:3.1.1 biodiesel, na fuel comprised of mono-alkyl esters of long chain fatty acids derived from vegetable oils or animal fats,designated B100.3.1.2 biodiesel blends, na blend of biodiesel fuel with petroleum-based diesel fuel.3.1.3 dynamic, adjin petroleum
24、 productsin petroleum product flash point test methodsthe condition where the vaporabove the test specimen and the test specimen are not in temperature equilibrium at the time that the ignition source is applied.3.1.3.1 DiscussionThis is primarily caused by the heating of the test specimen at the co
25、nstant prescribed rate with the vapor temperature laggingbehind the test specimen temperature.3.1.4 equilibrium, n in petroleum productsin petroleum product flash point test methodsthe condition where the vaporabove the test specimen and the test specimen are at the same temperature at the time the
26、ignition source is applied.3.1.4.1 DiscussionThis condition may not be fully achieved in practice, since the temperature may not be uniform throughout the test specimen, andthe test cover and shutter on the apparatus can be cooler.3.1.5 flash point, n in petroleum products, the lowest temperature co
27、rrected to a barometric pressure of 101.3 kPa (760 mm101.3 kPa (760 mm Hg), at which application of an ignition source causes the vapors of a specimen of the sample to ignite underspecified conditions of test.4. Summary of Test Method4.1 A brass test cup of specified dimensions, filled to the inside
28、 mark with test specimen and fitted with a cover of specifieddimensions, is heated and the specimen stirred at specified rates, using one of three defined procedures (A, B, or C). An ignitionsource is directed into the test cup at regular intervals with simultaneous interruption of the stirring, unt
29、il a flash is detected (see11.1.8). The flash point is reported as defined in 3.1.5.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary pa
30、ge on the ASTM website.3 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036.10036, http:/www.ansi.org.D93 15a25. Significance and Use5.1 The flash point temperature is one measure of the tendency of the test specimen to form a flammable mixture
31、 with air undercontrolled laboratory conditions. It is only one of a number of properties which must be considered in assessing the overallflammability hazard of a material.5.2 Flash point is used in shipping and safety regulations to define flammable and combustible materials. One should consultthe
32、 particular regulation involved for precise definitions of these classifications.5.3 These test methods should be used to measure and describe the properties of materials, products, or assemblies in responseto heat and an ignition source under controlled laboratory conditions and should not be used
33、to describe or appraise the fire hazardor fire risk of materials, products, or assemblies under actual fire conditions. However, results of these test methods may be usedas elements of a fire risk assessment which takes into account all of the factors which are pertinent to an assessment of the fire
34、hazard of a particular end use.5.4 These test methods provide the only closed cup flash point test procedures for temperatures up to 370C (698F).370 C(698 F).6. Apparatus6.1 Pensky-Martens Closed Cup Apparatus (manual) This apparatus consists of the test cup, test cover and shutter, stirringdevice,
35、heating source, ignition source device, air bath, and top plate described in detail in Annex A1. The assembled manualapparatus, test cup, test cup cover, and test cup assembly are illustrated in Figs. A1.1-A1.4, respectively. Dimensions are listedrespectively.6.2 Pensky-Martens Closed Cup Apparatus
36、(Automated)4This apparatus is an automated flash point instrument that is capableof performing the test in accordance with Section 11 (Procedure A), Section 12 (Procedure B), and 13 (Procedure C) of these testmethods. The apparatus shall use the test cup, test cover and shutter, stirring device, hea
37、ting source, and ignition source devicedescribed in detail in Annex A1.6.3 Temperature Measuring DeviceThermometer having a range as shown in Table 1 and conforming to the requirementsprescribed in Specification E1 or in Annex A3, or an electronic temperature measuring device, such as resistance the
38、rmometersor thermocouples. The device shall exhibit the same temperature response as the mercury thermometers.6.4 Ignition SourceNatural gas flame, bottled gas flame, and electric ignitors (hot wire) have been found acceptable for useas the ignition source. The gas flame device described in detailed
39、 in Fig. A1.4 requires the use of the pilot flame described inA1.1.2.3. The electric ignitors shall be of the hot-wire type and shall position the heated section of the ignitor in the aperture ofthe test cover in the same manner as the gas flame device. (WarningGas pressure supplied to the apparatus
40、 should not beallowed to exceed 3 kPa (12 in.) 3 kPa (12 in.) of water pressure.)6.5 BarometerWith accuracy of 60.5 kPa.60.5 kPa.NOTE 3The barometric pressure used in this calculation is the ambient pressure for the laboratory at the time of the test. Many aneroid barometers,such as those used at we
41、ather stations and airports, are precorrected to give sea level readings and would not give the correct reading for this test.7. Reagents and Materials7.1 Cleaning SolventsUse suitable solvent capable of cleaning out the specimen from the test cup and drying the test cup andcover. Some commonly used
42、 solvents are toluene and acetone. (WarningToluene, acetone, and many solvents are flammableand a health hazard. Dispose of solvents and waste material in accordance with local regulations.)4 Supporting data regarding a variant of the cover locking mechanism have been filed at ASTM International Hea
43、dquarters and may be obtained by requesting ResearchReport RR:D02-1706.TABLE 1 Temperature Measuring DeviceTemperature Range Thermometer Number TemperatureRangeThermometer NumberASTM IP5 to 110C(20 to 230F)9C (9F) 5 to110C15C5 C to 110 C(20 F to 230 F)9C (9F) 5 C to110 C15C+10 to 200C(50 to 392F)88C
44、 (88F) +20 to150C101C+10 C to 200 C(50 F to 392 F)88C (88F) +20 C to150 C101C+90 to 370C(200 to 700F)10C (10F) +90 to370C16C+90 C to 370 C(200 F to 700 F)10C (10F) +90 C to370 C16CD93 15a38. Sampling8.1 Obtain a sample in accordance with instructions given in Practices D4057, D4177, or E300.8.2 At l
45、east 75 mL 75 mL of sample is required for each test. Refer to Practice D4057. When obtaining a sample of residualfuel oil, the sample container shall be from 8585 % to 95 % full. For other types of samples, the size of the container shall bechosen such that the container is not more than 85 % full
46、or less than 50 % full prior to any sample aliquot being taken. Forbiodiesel (B100) samples, a typical one liter container filled to 85%85 % volume is recommended.8.3 Successive test specimens can be taken from the same sample container. Repeat tests have been shown to be within theprecisions of the
47、 method when the second specimen is taken with the sample container at least 50 % filled. The results of flashpoint determinations can be affected if the sample volume is less than 50 % of sample container capacity.8.4 Erroneously high flash points may be obtained if precautions are not taken to avo
48、id the loss of volatile material. Do not opencontainers unnecessarily, to prevent loss of volatile material or possible introduction of moisture, or both.Avoid storage of samplesat temperatures in excess of 35C35 C or 95F.95 F. Samples for storage shall be capped tightly with inner seals. Do not mak
49、ea transfer unless the sample temperature is at least the equivalent of 18C18 C or 32F32 F below the expected flash point.8.5 Do not store samples in gas-permeable containers, since volatile material may diffuse through the walls of the enclosure.Samples in leaky containers are suspect and not a source of valid results.8.6 Samples of very viscous materials shall be heated in their containers, with lid/cap slightly loosened to avoid buildup ofdangerous pressure, at the lowest tem
