1、Designation: D93 131D93 15Designation: 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.1 NOTEEditorially revised 15.1 in February 20
3、14.INTRODUCTIONThis flash 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 ma
4、terials. Thereare flash point test methods with slower 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 appar
5、atus 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, or with test apparatus differ
6、ent from that specified.1. Scope*1.1 These test methods cover the determination of the flash point of petroleum products in the temperature range from 40 to370C by a manual Pensky-Martens closed-cup apparatus or an automated Pensky-Martens closed-cup apparatus, and thedetermination of the flash poin
7、t of biodiesel in the temperature range of 60 to 190C by an automated Pensky-Martens closed cupapparatus.NOTE 1Flash point determinations above 250C can be performed, however, the precision has not been determined above this temperature. Forresidual fuels, precision has not been determined for flash
8、 points above 100C. The precision of in-use lubricating 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, keros
9、ine, 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, pet
10、roleum 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 al
11、cohol 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 or
12、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 Cscale or an Fscale thermometer for temperaturemeasureme
13、nt. Although the scales are close in increments, they are not equivalent. Because the Fscale thermometer used in this procedure is graduated1 These test methods are under the joint jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and are the direct responsibilit
14、y ofSubcommittee D02.08 on Volatility. In the IP, these test methods are under the jurisdiction of the Standardization Committee.Current edition approved July 15, 2013Jan. 1, 2015. Published August 2013February 2015. Originally approved in 1921. Last previous edition approved in 20122013 asD93 12.D9
15、3 131. DOI: 10.1520/D0093-13E01.10.1520/D0093-15.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. Becauseit may not be technically possible to adequately depict all changes accurat
16、ely, 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 appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Dr
17、ive, PO Box C700, West Conshohocken, PA 19428-2959. United States1in 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 thetest method for the separate temperature scale thermometers, different increments
18、 must be used. In this test method, the following protocol has beenadopted: 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 w
19、ill appear after “or,” for example, 2C or 5F.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 health practices and determine the applicability of regulat
20、orylimitations 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 Method for Flash Point by the Equilibrium Method With a Close
21、d-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 Industrial ChemicalsE502 Test Method for Selection and Use of
22、ASTM 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 Statistical Principles3. Terminology3.1 Definitions:3.1.1 biodie
23、sel, 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 productsin petroleum product flash point test methodsthe
24、 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 constant prescribed rate with the vapor temperature lagging
25、behind 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 ignition source is applied.3.1.4.1 DiscussionThis conditi
26、on 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 corrected to a barometric pressure of 101.3 kPa (760 mmHg),
27、 at which application of an ignition source causes the vapors of a specimen 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
28、 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, until a flash is detected (see11.1.8). The flash point is reported as defined
29、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 page on the ASTM website.3 Available from American National Standards Institu
30、te (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036.D93 1525. 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 b
31、e 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 particular regulation involved for precise definitions of these classifications.NOTE 3The U.S. Depart
32、ment of Transportation (DOT)4 and U.S. Department of Labor (OSHA) have established that liquids with a flash point under37.8C (100F) (see Note 1) 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 at 37.8C or 9.5 mm 2/s (
33、cSt) or more at 25C (77F), or that contain suspended solids, or have a tendency to form a surface film while undertest. Other classification 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
34、properties of materials, products, or assemblies in responseto heat and an ignition 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 t
35、est 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 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.
36、 Apparatus6.1 Pensky-Martens Closed Cup Apparatus (manual) This apparatus consists 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 te
37、st cup assembly are illustrated in Figs. A1.1-A1.4, respectively. Dimensions are listedrespectively.6.2 Pensky-Martens Closed Cup Apparatus (Automated)4This apparatus is an automated flash point instrument that is capableof performing the test in accordance with Section 11 (Procedure A), Section 12
38、(Procedure B), and 13 (Procedure C) of these testmethods. The apparatus shall 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 followsin Table 1
39、and conforming to therequirements prescribed in Specification E1 or in Annex A3, or an electronic temperature measuring device, such as resistancethermometers or thermocouples. The device shall exhibit the same temperature response as the mercury thermometers.Thermometer NumberTemperature Range ASTM
40、 IP5 to +110C (20 to 230F) 9C (9F) 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 for useas the ignition source. The gas flame device described in de
41、tailed 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 app
42、aratus should not beallowed to exceed 3 kPa (12 in.) of water pressure.)6.5 BarometerWith accuracy of 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 weather stations and
43、 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 solvents are tolu
44、ene 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 Headquarters and may
45、be obtained by requesting ResearchReport RR:D02-1706.TABLE 1 Temperature Measuring DeviceTemperature Range Thermometer Number Temperature Range Thermometer NumberASTM IP5 to 110C (20 to 230F) 9C (9F) 5 to 110C 15C+10 to 200C (50 to 392F) 88C (88F) +20 to 150C 101C+90 to 370C (200 to 700F) 10C (10F)
46、+90 to 370C 16CD93 1538. 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 residual fuel oil,the sample container shall be from 85 to 95 % fu
47、ll. For other types of samples, the size of the container shall be chosen such thatthe 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 te
48、st specimens can be taken from 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
49、 50 % of sample container capacity.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 expect
