1、Designation: D 93 07Designation: 34/99An American National StandardStandard Test Methods forFlash Point by Pensky-Martens Closed Cup Tester1This standard is issued under the fixed designation D 93; the number immediately following the designation indicates the year of originaladoption or, in the cas
2、e of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon (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.INTRODUCTIONThis flas
3、h point test method is a 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.Flash point valu
4、es are a function of the apparatus design, the condition of the 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,
5、 or with test apparatus different from that specified.1. Scope*1.1 These test methods 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.NOTE 1Flash
6、 point determination as above 250C can be performed,however, the precisions have not been determined above this temperature.For residual fuels, precisions have not been determined for flash pointsabove 100C.1.2 Procedure A is applicable to distillate fuels (diesel,kerosine, heating oil, turbine fuel
7、s), new lubricating oils, andother homogeneous petroleum liquids not included in the scopeof Procedure B.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
8、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 These test methods is applicable for the detection ofcontamination of relatively nonvolatile or nonflammable ma-terials with volatile or fl
9、ammable materials.1.5 The values stated in SI units are to be regarded 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. A
10、lthough the scales are close in increments,they are not equivalent. 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 fo
11、r the separate tempera-ture 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 370C (698F). When a temperature
12、isintended to be a rationalized unit for the alternate scale, it will appear after“or,” for example, 2C or 5F.1.6 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 safet
13、y and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardsstatements, see 6.4, 7.1, 9.3, 9.4, 11.1.2, 11.1.4, 11.1.8, and12.1.2.1These test methods are under the joint jurisdiction ofASTM Committee D02 onPetroleum Products and Lubricants and
14、are the direct responsibility of Subcommit-tee D02.08 on Volatility. In the IP, these test methods are under the jurisdiction ofthe Standardization Committee.Current edition approved May 1, 2007. Published May 2007. Originallyapproved in 1921. Last previous edition approved in 2006 as D 9306.1*A Sum
15、mary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.2. Referenced Documents2.1 ASTM Standards:2D56 Test Method for Flash Point by Tag Closed Cup TesterD 4057 Practice for Manual
16、Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsE1 Specification for ASTM Liquid-in-Glass ThermometersE 300 Practice for Sampling Industrial ChemicalsE 502 Test Method for Selection and Use of ASTM Stan-dards for the Determination o
17、f 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 Definitions:3.1.1 dynamic, adjin petroleum productsin petroleump
18、roduct 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.3.1.1.1 DiscussionThis is primarily caused by the heatingof the test specimen at the constant prescribed rate wit
19、h thevapor temperature lagging behind the test specimen tempera-ture.3.1.2 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
20、.1.2.1 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.3.1.3 flash point, nin petroleum products, the lowesttemperature corrected to a barometric pressure
21、 of 101.3 kPa(760 mm Hg), 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 ofs
22、pecified dimensions, is heated and the specimen stirred atspecified rates, by either of two defined procedures (A or B).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 repor
23、ted asdefined in 3.1.3.5. 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 flamma
24、bility 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 classifications.NOTE 3The U.S. Department of Transportation (DOT)4and U.S.Depart
25、ment of Labor (OSHA) 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,
26、 or have a tendency 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
27、 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, orassemblies under actual fire conditions. However, results ofthese test methods may be used as elements of a fire riskassessment whic
28、h 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 provides the only closed cup flashpoint test procedures for temperatures up to 370C (698F).6. Apparatus6.1 Pensky-Martens Closed Cup Apparatus (manual)Thisappa
29、ratus 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. The assembledmanual apparatus, test cup, test cup cover, and test cupassembly are illustrated in Figs. A1.1-A1.4, respectively. Di-m
30、ensions are listed respectively.6.2 Pensky-Martens Closed Cup Apparatus (automated)This apparatus is an automated flash point instrument that iscapable of performing the test in accordance with Section 11(Procedure A) and Section 12 (Procedure B) of these testmethods. The apparatus shall use the tes
31、t cup, test cover andshutter, stirring device, heating source, and ignition sourcedevice described in detail in Annex A1.6.3 Temperature Measuring DeviceThermometer havinga range as shown as follows and conforming to the require-ments prescribed in Specification E1or in Annex A3,oranelectronic tempe
32、rature measuring device, such as resistancethermometers or thermocouples. The device shall exhibit thesame temperature response as the mercury thermometers.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of AST
33、MStandards 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 of Transportation regulations, see Codesof U.S. Regulations 49
34、 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.D93072Thermometer NumberTemperature Range ASTM IP5 to +110C (20 to 230F) 9C (9F) 1
35、5C+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 o
36、f 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 3
37、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 lev
38、el 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, and
39、 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 D 4057, D 4177, or E 300.8.2 At least 75 mL of sample is required for each test. Referto Pract
40、ice D 4057. 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.8.3 Succes
41、sive 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
42、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 loss of volatilematerial or possible introduction of moisture, or both. Avoidstorage of sampl
43、es 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 expected flash point.8.5 Do not store samples in gas-permeable containers, sincevolatile mate
44、rial 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 ade
45、quate 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 horizont
46、ally,before transferring to the specimen cup. No sample shall beheated and transferred unless its temperatures is more than18C or 32F below its expected flash point. When the samplehas been heated above this temperature, allow the sample tocool until its temperature is at least 18C or 32F below thee
47、xpected flash point before transferring.NOTE 5Volatile vapors can escape during heating when the samplecontainer is not properly sealed.NOTE 6Some viscous samples may not completely liquefy even afterprolonged periods of heating. Care should be exercised when increasingthe heating temperature to avo
48、id 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 absorbent cotton.Warming the sample is permitted, b
49、ut it shall not be heated forprolonged periods or greater than a temperature of 18C 32Fbelow its expected flash point.NOTE 7If the sample is suspected of containing volatile contaminants,the treatment described in 8.6 and 8.7 should be omitted.9. Preparation of Apparatus9.1 Support the manual or automated apparatus on a levelsteady surface, such as a table.9.2 Tests are to be performed in a draft-free room orcompartment. Tests made in a laboratory hood or in anylocation where drafts occur are not reliable.NOTE 8A shield,
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