1、Designation: D7094 04 (Reapproved 2009)D7094 12Standard Test Method forFlash Point by Modified Continuously Closed Cup(MCCCFP) Tester1This standard is issued under the fixed designation D7094; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope Scope*1.1 This test method covers the determination of the flash point of fuels, lube oils, solvent
3、s and other liquids by a continuouslyclosed cup tester utilizing a specimen size of 2 mL, cup size of 7 mL, with a heating rate of 2.5C per minute.1.1.1 Apparatus requiring a specimen size of 1 mL, cup size of 4 mL, and a heating rate of 5.5C per minute must be runaccording to Test Method D6450.1.2
4、This flash point test method is a dynamic method and depends on definite rates of temperature increase. It is one of the manyflash point test methods available and every flash point test method, including this one, is an empirical method.NOTE 1Flash point values are not a constant physical chemical
5、property of materials tested. They are a function of the apparatus design, the conditionof the apparatus used, and the operational procedure carried out. Flash point can, therefore, only be defined in terms of a standard test method and nogeneral valid correlation can be guaranteed between results o
6、btained by different test methods or where different test apparatus is specified.1.3 This test method utilizes a closed but unsealed cup with air injected into the test chamber.1.4 This test method is suitable for testing samples with a flash point from 35 to 225C.NOTE 2Flash point determinations be
7、low 35C and above 225C may be performed; however, the precision has not been determined below and abovethese temperatures.1.5 If the users specification requires a defined flash point method other than this method, neither this method nor any othertest method should be substituted for the prescribed
8、 test method without obtaining comparative data and an agreement from thespecifier.1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.Temperatures are in degrees Celsius, pressure in kilo-Pascals.1.6.1 Temperatures are in deg
9、rees Celsius, pressure in kilo-Pascals.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 regulatorylim
10、itations prior to use. For specific warning statements, see 7.2, 8.5, and 10.1.2.2. Referenced Documents2.1 ASTM Standards:2D93 Test Methods for Flash Point by Pensky-Martens Closed Cup TesterD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling
11、of Petroleum and Petroleum ProductsD6450 Test Method for Flash Point by Continuously Closed Cup (CCCFP) TesterD6708 Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purportto Measure the Same Property of a MaterialE300 Practice for Sampling Indu
12、strial Chemicals2.2 ISO Standards:3ISO Guide 34 Quality Systems Guidelines for the Production of Reference MaterialsISO Guide 35 Certification of Reference MaterialsGeneral and Statistical Principles1 This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubrican
13、ts and is the direct responsibility of Subcommittee D02.08 onVolatility.Current edition approved Dec. 1, 2009Dec. 1, 2012. Published February 2010March 2013. Originally approved in 2004. Last previous edition approved in 20042009 asD709404.D709404(2009). DOI: 10.1520/D7094-04R09.10.1520/D7094-12.2 F
14、or 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 Institute (ANSI), 2
15、5 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.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
16、 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 appears at the end of this standardCopyright ASTM International, 10
17、0 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13. Terminology3.1 Definitions:3.1.1 flash point, nthe lowest temperature corrected to a pressure of 101.3 kPa at which application of an ignition sourcecauses the vapors of a specimen of the sample to ignite momentaril
18、y under specified conditions of the test.3.1.1.1 DiscussionFor the purpose of this test method, the test specimen is deemed to have flashed when the hot flame of the ignited vapor causesan instantaneous pressure increase of at least 20 kPa inside the closed measuring chamber.3.1.2 dynamic, adjthe co
19、ndition where the vapor above the test specimen and the test specimen are not in temperatureequilibrium at the time at which the ignition source is applied.4. Summary of Test Method4.1 The lid of the test chamber is regulated to a temperature at least 18C below the expected flash point. A 2 6 0.2 mL
20、 testspecimen of a sample is introduced into the sample cup. Both specimen and cup are at a temperature at least 18C below theexpected flash point; cooled if necessary. The cup is then raised and pressed onto the lid of specified dimensions to form thecontinuously closed but unsealed test chamber wi
21、th an overall volume of 7.0 6 0.3 mL.4.2 After closing the test chamber, the temperatures of the test specimen and the regulated lid are allowed to equilibrate to within1C.Then the lid is heated at a prescribed, constant rate. For the flash tests, a high voltage arc of defined energy is discharged i
22、nsidethe test chamber at regular intervals.After each ignition, a variable amount of air (see Table 1) is introduced into the test chamberto provide the necessary oxygen for the next flash test. The pressure inside the continuously closed but unsealed test chamberremains at ambient barometric pressu
23、re except for the short time during the air introduction and at a flash point.4.3 After each arc application, the instantaneous pressure increase above the ambient barometric pressure inside the testchamber is monitored.When the pressure increase exceeds 20 kPa, the temperature at that point is reco
24、rded as the uncorrected flashpoint, which is then corrected to barometric pressure.5. 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 prop
25、erties 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 and for classificationpurposes. This definition may vary from regulation to regulation. Consult the parti
26、cular regulation involved for precise definitionsof these classifications.5.3 This test method can be used to measure and describe the properties of materials in response to heat and an ignition sourceunder controlled laboratory conditions and shall not be used to describe or appraise the fire hazar
27、d or fire risk of materials underactual fire conditions. However, results of this test method may be used as elements of a fire risk assessment, which takes intoaccount all of the factors which are pertinent to an assessment of the fire hazard of a particular end use.5.4 Flash point can also indicat
28、e the possible presence of highly volatile and flammable materials in a relatively nonvolatile ornonflammable material, such as the contamination of lubricating oils by small amounts of diesel fuel or gasoline. This test methodwas designed to be more sensitive to potential contamination than Test Me
29、thod D6450.6. Apparatus6.1 Flash Point Apparatus, Continuously Closed Cup OperationThe type of apparatus suitable for use in this test methodemploys a lid of solid brass, the temperature of which is controlled electrically. Two temperature sensors for the specimen and thelid temperatures, respective
30、ly, two arc pins for a high voltage arc, and a connecting tube for the pressure monitoring and the airTABLE 1 Volume of Introduced Air as a Function ofSample TemperatureSample TemperatureRange (C)Introduced Volumeof Air (mL)below 80 080 to below 150 0.5 0.15150 to below 200 1 0.2200 to below 300 1.5
31、 0.3300 and above 2 0.4D7094 122introduction are incorporated in the lid. Associated equipment for electrically controlling the chamber temperature is used, and adigital readout of the specimen temperature is provided. The apparatus and its critical elements are shown in Figs.A1.1 and A1.2.46.1.1 Te
32、st ChamberThe test chamber is formed by the sample cup and the temperature controlled lid and shall have an overallvolume of 7 6 0.3 mL. A metal to metal contact between the lid and the sample cup shall provide good heat contact but allowambient barometric pressure to be maintained inside the test c
33、hamber during the test. Critical dimensions are shown in Fig. A1.2.The pressure inside the measuring chamber during the temperature increase is monitored. A seal that is too tight results in apressure increase above ambient due to the temperature and the vapor pressure of the sample.Apoor heat conta
34、ct results in a biggertemperature difference between the sample and the heated lid.6.1.2 Sample CupThe sample cup shall be made of nickel-plated aluminum or other material with similar heat conductivity.It shall have an overall volume of 7 6 0.3 mL and shall be capable of containing 2 6 0.2 mL of sa
35、mple. The critical dimensionsand requirements are shown in Fig. A1.2.6.1.3 Specimen Temperature SensorThe specimen temperature sensor (Fig.A1.1) shall be a thermocouple (NiCr-Ni or similar)in stainless steel of 1 mm diameter with a response time of t(90) = 3 s. It shall be immersed to a depth of at
36、least 2 mm into thespecimen. It shall have a resolution of 0.1C and a minimum accuracy of 6 0.2C, preferably with a digital readout.6.1.4 Magnetic StirringThe apparatus shall have provisions for stirring of the sample. A rotating magnet outside the samplecup shall drive a small stirring magnet which
37、 is inserted into the sample cup after sample introduction. The stirring magnet shallhave a diameter of 3 6 0.2 mm and a length of 12 6 1 mm. The rotation speed of the driving magnet shall be between 250 and270 rev/min.6.1.5 Air IntroductionThe apparatus shall have provisions for introduction of air
38、 immediately after each flash test. The airshall be introduced by a short air pulse from a small membrane compressor by means of a T-inlet in the connecting tube to thepressure transducer. The volume of the introduced air, from 0.5 to 2 mL, is dependent on the sample temperature (see Table 1).6.1.6
39、Electrical heating and thermoelectric cooling of the lid (see the Peltier element shown in Fig. A1.1) shall be used toregulate the temperature of the test chamber for the duration of the test. The temperature regulation shall have a minimum accuracyof 6 0.2C.6.1.7 A high voltage electric arc shall b
40、e used for the ignition of the flammable vapor. The energy of the arc shall be 1.3 6 0.3J (1.3 6 0.3 Ws) per arc and the energy shall be applied within 19 6 2 m/s. (Warning Because samples containing low flashmaterial or having a flash point below the preset initial temperature can oversaturate the
41、vapor inside the chamber and henceprohibit the detection of a flash point in the chosen range, a precautionary arc set at 5C intervals is required while the lid andsample cup temperatures are equalizing.)6.1.8 The pressure transducer for the flash point detection shall be connected to the connecting
42、 tube in the lid and shall havea minimum operational range from 80 to 177 kPa with a minimum resolution of 0.1 kPa and a minimum accuracy of 6 0.5 kPa.It shall be capable of detecting an instantaneous pressure increase above barometric pressure of a minimum of 20 kPa within 100m/s.NOTE 3The monitori
43、ng of the instantaneous pressure increase above barometric pressure is one of several methods to determine a flash inside thetest chamber. A pressure increase of 20 kPa corresponds to a flame volume of approximately 2.5 mL.NOTE 4An automatic barometric correction, which is performed according to the
44、 procedure described in 12.1, can be installed in the tester. Theabsolute pressure reading of the pressure transducer described in 6.1.8 may be used for the correction.6.1.9 The introduction of a test specimen of 2.060.2 mLshall be accomplished by the use of a pipette or syringe of the requiredaccur
45、acy.7. Reagents and Materials7.1 Purity of ReagentsUse only chemicals of purity specified in Table X1.1. Unless otherwise indicated, it is intended that allreagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where suchspecifications are ava
46、ilable.5 Other grades may be used, provided it is first ascertained that the reagent is of sufficient purity topermit its use without lessening the accuracy of the determination.7.1.1 Anisole(WarningSee 7.2.)7.1.2 Dodecane(WarningSee 7.2.)7.2 Cleaning SolventsUse only noncorrosive solvents capable o
47、f cleaning the sample cup and the lid. Two commonly usedsolvents are toluene and acetone. (WarningAnisole, dodecane, toluene, acetone, and many solvents are flammable and are healthhazards. Dispose of solvents and waste material in accordance with local regulations.)4 The method of detecting the fla
48、sh point by monitoring the instantaneous pressure increase is covered by a patent. Interested parties are invited to submit informationregarding the identification of an alternative(s) to this patented item to the ASTM International Headquarters. Your comments will receive careful consideration at a
49、 meetingof the responsible technical committee, which you may attend.4 The sole source of supply of the continuously closed cup testers meeting these requirements known to the committee at this time are available from Grabner Instruments,A-1220 Vienna/Austria, Dr. Otto-Neurath-Gasse 1. If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Yourcomments will receive careful consideration at a meeting of the responsible technical committee,1 which you may attend.5 Reagent Chemicals,
