1、Designation: D93 11 D93 12Designation: 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. 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
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 s
4、lower heating 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,
5、 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 m
6、ethods cover the determination of the flash point of petroleum products in the temperature range from 40 to360C 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 temperature range of 60 to
7、190C by an automated Pensky-Martens closed cupapparatus.NOTE 1Flash point determination as above 250C can be performed, however, the precision has not been determined above this temperature. Forresidual fuels, precision has not been determined for flash points above 100C. The precision of in-use lub
8、ricating oils has not been determined. Somespecifications state a D93 minimum flash point below 40C, however, the precision has not been determined below this temperature.1.2 Procedure A is applicable to distillate fuels (diesel, biodiesel blends, kerosine, heating oil, turbine fuels), new and in-us
9、elubricating 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, petroleum liquids that tend to form a surface film
10、 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 alcohol in biodiesel is difficult to observe byma
11、nual 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 or flammable materials.1.6 The values stated in SI
12、 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 Cscale or an Fscale thermometer for temperaturemeasurement. Although the scales are close in increments
13、, they are not equivalent. Because the Fscale thermometer used in this procedure is graduatedin 5 increments, it is not possible to read it to the 2C equivalent increment of 3.6F. Therefore, for the purposes of application of the procedure of the1 These test methods are under the joint jurisdiction
14、of ASTM Committee D02 on Petroleum Products and Lubricants and are the direct responsibility of SubcommitteeD02.08 on Volatility. In the IP, these test methods are under the jurisdiction of the Standardization Committee.Current edition approved Oct. 1, 2011Nov. 1, 2012. Published November 2011Novemb
15、er 2012. Originally approved in 1921. Last previous edition approved in 20102011as D9310a.11. DOI: 10.1520/D0093-11.10.1520/D0093-12.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version
16、. 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 to be considered the official document.*A Summary of Changes section
17、 appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1test method for the separate temperature scale thermometers, different increments must be used. In this test method, the following protocol has beenad
18、opted: When a temperature is intended to be a converted equivalent, it will appear in parentheses following the SI unit, for example 370C (698F).When a temperature is intended to be a rationalized unit for the alternate scale, it will appear after “or,” for example, 2C or 5F.1.7 This standard does n
19、ot 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 health practices and determine the applicability of regulatorylimitations prior to use. For specific warning statements, see 6.4
20、, 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 Equilibrium Method With a Closed-Cup ApparatusD4057 Practice for Manual Sampling of Petroleum and Pe
21、troleum ProductsD4177 Practice for Automatic Sampling of Petroleum and Petroleum ProductsE1 Specification for ASTM Liquid-in-Glass ThermometersE300 Practice for Sampling Industrial ChemicalsE502 Test Method for Selection and Use of ASTM Standards for the Determination of Flash Point of Chemicals by
22、Closed CupMethods2.2 ISO Standards3Guide 34 Quality Systems Guidelines for the Production of Reference MaterialsGuide 35 Certification of Reference MaterialGeneral and Statistical Principles3. Terminology3.1 Definitions:3.1.1 biodiesel, na fuel comprised of mono-alkyl esters of long chain fatty acid
23、s 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 productsin petroleum product flash point test methodsthe condition where the vaporabove the test specimen and the test speci
24、men 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 constant prescribed rate with the vapor temperature laggingbehind the test specimen temperature.3.1.4 equilibrium, n in petrole
25、um 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 ignition source is applied.3.1.4.1 DiscussionThis condition may not be fully achieved in practice, since the temperature may
26、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 corrected to a barometric pressure of 101.3 kPa (760 mmHg), at which application of an ignition source causes the vapors of a s
27、pecimen of the sample to ignite under specified conditionsof test.4. Summary of Test Method4.1 A brass test cup of specified dimensions, filled to the inside mark with test specimen and fitted with a cover of specifieddimensions, is heated and the specimen stirred at specified rates, using one of th
28、ree defined procedures (A, B, or C). An ignitionsource is directed into the test cup at regular intervals with simultaneous interruption of the stirring, until a flash is detected (see11.1.8). The flash point is reported as defined in 3.1.5.2 For referenced ASTM standards, visit the ASTM website, ww
29、w.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036.D93 1225
30、. Significance and Use5.1 The flash point temperature is one measure of the tendency of the test specimen to form a flammable mixture 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 mat
31、erial.5.2 Flash point is used in shipping and safety regulations to define flammable and combustible materials. One should consultthe particular regulation involved for precise definitions of these classifications.NOTE 3The U.S. Department of Transportation (DOT)4 and U.S. Department of Labor (OSHA)
32、 have established that liquids with a flash point under37.8C (100F) are flammable, as determined by these test methods, for those liquids which have a kinematic viscosity of 5.8 mm 2/s (cSt) or more at37.8C or 9.5 mm 2/s (cSt) or more at 25C (77F), or that contain suspended solids, or have a tendenc
33、y to form a surface film while under test. Otherclassification flash points have been established by these departments for liquids using these test methods.5.3 These test methods should be used to measure and describe the properties of materials, products, or assemblies in responseto heat and an ign
34、ition source under controlled laboratory conditions and should not be used 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
35、account all of the factors which are pertinent to an assessment of the firehazard 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).6. Apparatus6.1 Pensky-Martens Closed Cup Apparatus (manual) This apparatus cons
36、ists of the test cup, test cover and shutter, stirringdevice, 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 a
37、re listedrespectively.6.2 Pensky-Martens Closed Cup Apparatus (Automated)5This 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
38、use the test cup, test cover and shutter, stirring device, heating source, and ignition source devicedescribed in detail in Annex A1.6.3 Temperature Measuring DeviceThermometer having a range as shown as follows and conforming to the requirementsprescribed in Specification E1 or in Annex A3, or an e
39、lectronic temperature measuring device, such as resistance thermometersor thermocouples. The device shall exhibit the same temperature response as the mercury thermometers.Thermometer NumberTemperature Range ASTM IP5 to +110C (20 to 230F) 9C (9F) 15C+10 to 200C (50 to 392F) 88C (88F) 101C+90 to 370C
40、 (200 to 700F) 10C (10F) 16C6.4 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 in Fig. A1.4 requires the use of the pilot flame described inA1.1.2.3. The electr
41、ic 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 should not beallowed to exceed 3 kPa (12 in.) of water pressure.)6.5 BarometerWit
42、h accuracy of 60.5 kPa.NOTE 4The 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 weather stations and airports, are precorrected to give sea level readings and would not give the correct re
43、ading 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 solvents are toluene and acetone. (WarningToluene, acetone, and many solvents are flammableand a health h
44、azard. Dispose of solvents and waste material in accordance with local regulations.)8. Sampling8.1 Obtain a sample in accordance with instructions given in Practices D4057, D4177, or E300.8.2 At least 75 mL of sample is required for each test. Refer to Practice D4057. When obtaining a sample of resi
45、dual fuel oil,the sample container shall be from 85 to 95 % full. For other types of samples, the size of the container shall be chosen such that4 For information on U.S. Department of Transportation regulations, see Codes of U.S. Regulations 49 CFR Chapter 1 and the U.S. Department of Labor, see 29
46、 CFRChapter XVII. Each of these items is revised annually and may be procured from the Superintendent of Documents, Government Printing Office, Washington, DC 20402.5 Supporting data regarding a variant of the cover locking mechanism have been filed at ASTM International Headquarters and may be obta
47、ined by requesting ResearchReport RR:D02-1706.D93 123the container is not more than 85 % full or less than 50 % 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 taken from
48、 the same sample container. Repeat tests have been shown to be within theprecisions of the 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 capa
49、city.8.4 Erroneously high flash points may be obtained if precautions are not taken to avoid 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 35C or 95F. Samples for storage shall be capped tightly with inner seals. Do not make a transferunless the sample temperature is at least the equivalent of 18C or 32F below the expected flash point.8.5 Do not store samples in gas
