1、Designation: D7094 04 (Reapproved 2009)Standard 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 revision
2、, 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. Scope1.1 This test method covers the determination of the flashpoint of fuels, lube oils, solvents and other liqu
3、ids by acontinuously closed cup tester utilizing a specimen size of 2mL, 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 sizeof 4 mL, and a heating rate of 5.5C per minute must be runaccording to Test Method D6450.1.2 This flash point t
4、est method is a dynamic method anddepends on definite rates of temperature increase. It is one ofthe many flash point test methods available and every flashpoint test method, including this one, is an empirical method.NOTE 1Flash point values are not a constant physical chemicalproperty of materials
5、 tested. They are a function of the apparatus design,the condition of the apparatus used, and the operational procedure carriedout. Flash point can, therefore, only be defined in terms of a standard testmethod and no general valid correlation can be guaranteed between resultsobtained by different te
6、st methods or where different test apparatus isspecified.1.3 This test method utilizes a closed but unsealed cup withair injected into the test chamber.1.4 This test method is suitable for testing samples with aflash point from 35 to 225C.NOTE 2Flash point determinations below 35C and above 225C may
7、be performed; however, the precision has not been determined below andabove these temperatures.1.5 If the users specification requires a defined flash pointmethod other than this method, neither this method nor anyother test method should be substituted for the prescribed testmethod without obtainin
8、g comparative data and an agreementfrom the specifier.1.6 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6.1 Temperatures are in degrees Celsius, pressure inkilo-Pascals.1.7 This standard does not purport to address all of th
9、esafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see 7.2, 8.5, and 10.1.2.2. Reference
10、d Documents2.1 ASTM Standards:2D93 Test Methods for Flash Point by Pensky-MartensClosed Cup TesterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6450 Test Method for Flash Point by Continuously ClosedCup (
11、CCCFP) TesterD6708 Practice for StatisticalAssessment and Improvementof Expected Agreement Between Two Test Methods thatPurport to Measure the Same Property of a MaterialE300 Practice for Sampling Industrial Chemicals2.2 ISO Standards:3ISO Guide 34 Quality Systems Guidelines for the Produc-tion of R
12、eference MaterialsISO Guide 35 Certification of Reference MaterialsGeneral and Statistical Principles3. Terminology3.1 Definitions:3.1.1 flash point, nthe lowest temperature corrected to apressure of 101.3 kPa at which application of an ignitionsource causes the vapors of a specimen of the sample to
13、 ignitemomentarily under specified conditions of the test.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.08 on Volatility.Current edition approved Dec. 1, 2009. Published February 2010. Origina
14、llyapproved in 2004. Last previous edition approved in 2004 as D709404. DOI:10.1520/D7094-04R09.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Docume
15、nt Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.1.1 DiscussionFor t
16、he purpose of this test method, thetest specimen is deemed to have flashed when the hot flame ofthe ignited vapor causes an instantaneous pressure increase ofat least 20 kPa inside the closed measuring chamber.43.1.2 dynamic, adjthe condition where the vapor abovethe test specimen and the test speci
17、men 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 temperatureat least 18C below the expected flash point.A2 6 0.2 mL testspecimen of a sample is introduced into the sample cup. Bothspec
18、imen and cup are at a temperature at least 18C below theexpected flash point; cooled if necessary. The cup is then raisedand pressed onto the lid of specified dimensions to form thecontinuously closed but unsealed test chamber with an overallvolume of 7.0 6 0.3 mL.4.2 After closing the test chamber,
19、 the temperatures of thetest specimen and the regulated lid are allowed to equilibrate towithin 1C. Then the lid is heated at a prescribed, constant rate.For the flash tests, a high voltage arc of defined energy isdischarged inside the test chamber at regular intervals. Aftereach ignition, a variabl
20、e amount of air (see Table 1)isintroduced into the test chamber to provide the necessaryoxygen for the next flash test. The pressure inside the continu-ously closed but unsealed test chamber remains at ambientbarometric pressure except for the short time during the airintroduction and at a flash poi
21、nt.4.3 After each arc application, the instantaneous pressureincrease above the ambient barometric pressure inside the testchamber is monitored. When the pressure increase exceeds 20kPa, the temperature at that point is recorded as the uncorrectedflash point, which is then corrected to barometric pr
22、essure.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 flammability hazard of
23、 a material.5.2 Flash point is used in shipping and safety regulations todefine flammable and combustible materials and for classifica-tion purposes. This definition may vary from regulation toregulation. Consult the particular regulation involved for pre-cise definitions of these classifications.5.
24、3 This test method can be used to measure and describethe properties of materials in response to heat and an ignitionsource under controlled laboratory conditions and shall not beused to describe or appraise the fire hazard or fire risk ofmaterials under actual fire conditions. However, results of t
25、histest method may be used as elements of a fire risk assessment,which takes into account all of the factors which are pertinentto an assessment of the fire hazard of a particular end use.5.4 Flash point can also indicate the possible presence ofhighly volatile and flammable materials in a relativel
26、y non-volatile or nonflammable material, such as the contaminationof lubricating oils by small amounts of diesel fuel or gasoline.This test method was designed to be more sensitive to potentialcontamination than Test Method D6450.6. Apparatus6.1 Flash Point Apparatus, Continuously Closed CupOperatio
27、nThe type of apparatus suitable for use in this testmethod employs a lid of solid brass, the temperature of whichis controlled electrically. Two temperature sensors for thespecimen and the lid temperatures, respectively, two arc pinsfor a high voltage arc, and a connecting tube for the pressuremonit
28、oring and the air introduction are incorporated in the lid.Associated equipment for electrically controlling the chambertemperature is used, and a digital readout of the specimentemperature is provided. The apparatus and its critical elementsare shown in Figs. A1.1 and A1.2.56.1.1 Test ChamberThe te
29、st chamber is formed by thesample cup and the temperature controlled lid and shall have anoverall volume of 7 6 0.3 mL. A metal to metal contactbetween the lid and the sample cup shall provide good heatcontact but allow ambient barometric pressure to be maintainedinside the test chamber during the t
30、est. Critical dimensions areshown in Fig. A1.2. The pressure inside the measuring cham-ber during the temperature increase is monitored. A seal that istoo tight results in a pressure increase above ambient due to thetemperature and the vapor pressure of the sample. A poor heatcontact results in a bi
31、gger temperature difference between thesample and the heated lid.6.1.2 Sample CupThe sample cup shall be made ofnickel-plated aluminum or other material with similar heatconductivity. It shall have an overall volume of 7 6 0.3 mLandshall be capable of containing 2 6 0.2 mL of sample. Thecritical dim
32、ensions and requirements are shown in Fig. A1.2.6.1.3 Specimen Temperature SensorThe specimen tem-perature sensor (Fig. A1.1) shall be a thermocouple (NiCr-Nior similar) in stainless steel of 1 mm diameter with a responsetime of t (90) = 3 s. It shall be immersed to a depth of at least2 mm into the
33、specimen. It shall have a resolution of 0.1C anda minimum accuracy of 6 0.2C, preferably with a digitalreadout.4The method of detecting the flash point by monitoring the instantaneouspressure increase is covered by a patent. Interested parties are invited to submitinformation regarding the identific
34、ation of an alternative(s) to this patented item tothe ASTM International Headquarters. Your comments will receive careful consid-eration at a meeting of the responsible technical committee, which you may attend.5The sole source of supply of the continuously closed cup testers meeting theserequireme
35、nts known to the committee at this time are available from GrabnerInstruments, A-1220 Vienna/Austria, Dr. Otto-Neurath-Gasse 1. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting o
36、f theresponsible technical committee,1which you may attend.TABLE 1 Volume of Introduced Air as a Function ofSample TemperatureSample TemperatureRange (C)Introduced Volumeof Air (mL)below 80 080 to below 150 0.5 6 0.15150 to below 200 1 6 0.2200 to below 300 1.5 6 0.3300 and above 2 6 0.4D7094 04 (20
37、09)26.1.4 Magnetic StirringThe apparatus shall have provi-sions for stirring of the sample. A rotating magnet outside thesample cup shall drive a small stirring magnet which is insertedinto the sample cup after sample introduction. The stirringmagnet shall have a diameter of 3 6 0.2 mm and a length
38、of 126 1 mm. The rotation speed of the driving magnet shall bebetween 250 and 270 rev/min.6.1.5 Air IntroductionThe apparatus shall have provisionsfor introduction of air immediately after each flash test. The airshall be introduced by a short air pulse from a small membranecompressor by means of a
39、T-inlet in the connecting tube to thepressure transducer. The volume of the introduced air, from 0.5to 2 mL, is dependent on the sample temperature (see Table 1).6.1.6 Electrical heating and thermoelectric cooling of the lid(see the Peltier element shown in Fig. A1.1) shall be used toregulate the te
40、mperature of the test chamber for the duration ofthe test. The temperature regulation shall have a minimumaccuracy of 6 0.2C.6.1.7 A high voltage electric arc shall be used for theignition of the flammable vapor. The energy of the arc shall be1.3 6 0.3 J (1.3 6 0.3 Ws) per arc and the energy shall b
41、eapplied within 19 6 2 m/s. (WarningBecause samplescontaining low flash material or having a flash point below thepreset initial temperature can oversaturate the vapor inside thechamber and hence prohibit the detection of a flash point in thechosen range, a precautionary arc set at 5C intervals isre
42、quired while the lid and sample cup temperatures areequalizing.)6.1.8 The pressure transducer for the flash point detectionshall be connected to the connecting tube in the lid and shallhave a minimum operational range from 80 to 177 kPa with aminimum resolution of 0.1 kPa and a minimum accuracy of 6
43、0.5 kPa. It shall be capable of detecting an instantaneouspressure increase above barometric pressure of a minimum of20 kPa within 100 m/s.NOTE 3The monitoring of the instantaneous pressure increase abovebarometric pressure is one of several methods to determine a flash insidethe test chamber. A pre
44、ssure increase of 20 kPa corresponds to a flamevolume of approximately 2.5 mL.NOTE 4An automatic barometric correction, which is performedaccording to the procedure described in 12.1, can be installed in the tester.The absolute pressure reading of the pressure transducer described in 6.1.8may be use
45、d for the correction.6.1.9 The introduction of a test specimen of 2.0 6 0.2 mLshall be accomplished by the use of a pipette or syringe of therequired accuracy.7. Reagents and Materials7.1 Purity of ReagentsUse only chemicals of purity speci-fied in Table X1.1. Unless otherwise indicated, it is inten
46、dedthat all reagents conform to the specifications of the Committeeon Analytical Reagents of the American Chemical Societywhere such specifications are available.6Other grades may beused, provided it is first ascertained that the reagent is ofsufficient purity to permit its use without lessening the
47、 accu-racy of the determination.7.1.1 Anisole(WarningSee 7.2.)7.1.2 Dodecane(WarningSee 7.2.)7.2 Cleaning SolventsUse only noncorrosive solvents ca-pable of cleaning the sample cup and the lid. Two commonlyused solvents are toluene and acetone. (WarningAnisole,dodecane, toluene, acetone, and many so
48、lvents are flammableand are health hazards. Dispose of solvents and waste materialin accordance with local regulations.)8. Sampling8.1 Obtain at least a 50 mL sample from a bulk test site inaccordance with the instructions given in Practice D4057,D4177,orE300. Store the sample in a clean, tightly se
49、aledcontainer at a low temperature.8.2 Do not store samples for an extended period of time ingas permeable containers, such as plastic, because volatilematerial may diffuse through the walls of the container.Discard samples in leaky containers and obtain new samples.8.3 Erroneously high flash points can be obtained whenprecautions are not taken to avoid loss of volatile material. Donot open containers unnecessarily. Do not make a transferunless the sample temperature is at least 18C below theexpected flash point. When possible, perform the flash
