1、Designation: D7094 121Standard 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, the year of las
2、t revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEEditorially removed sole source of supply footnote from 6.1 in February 2014.1. Scope*1.1 This test method covers the determinat
3、ion of the flashpoint of fuels, lube oils, solvents and other liquids 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 minut
4、e must be runaccording to Test Method D6450.1.2 This flash point test 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 poin
5、t values are not a constant physical chemicalproperty of materials 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 cor
6、relation can be guaranteed between resultsobtained by different test 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
7、225C.NOTE 2Flash point determinations below 35C and above 225C maybe 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 sh
8、ould be substituted for the prescribed testmethod without obtaining 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. Temperatures are in degrees Celsius, pressure inkilo-Pa
9、scals.1.7 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 safety and health practices and determine the applica-bility of regulatory limitations prior to use. For spec
10、ificwarning statements, see 7.2, 8.5, and 10.1.2.2. Referenced 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 Products
11、D6450 Test Method for Flash Point by Continuously ClosedCup (CCCFP) TesterD6708 Practice for Statistical Assessment 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:3IS
12、O Guide 34 Quality Systems Guidelines for the Produc-tion of Reference MaterialsISO Guide 35 Certification of Reference MaterialsGeneraland 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 ig
13、nitionsource causes the vapors of a specimen of the sample to ignitemomentarily under specified conditions of the test.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.08 on Volati
14、lity.Current edition approved Dec. 1, 2012. Published March 2013. Originallyapproved in 2004. Last previous edition approved in 2009 as D709404(2009).DOI: 10.1520/D7094-12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For An
15、nual Book of ASTMStandards 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, http:/www.ansi.org.*A Summary of Changes section appears at the end of this stand
16、ardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.1.1 DiscussionFor the 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
17、 least 20 kPa inside the closed measuring chamber.3.1.2 dynamic, adjthe condition where the vapor abovethe 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 t
18、o a temperatureat least 18C below the expected flash point.A2 6 0.2 mL testspecimen of a sample is introduced into the sample cup. Bothspecimen 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 di
19、mensions 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, 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
20、 flash tests, a high voltage arc of defined energy isdischarged inside the test chamber at regular intervals. Aftereach ignition, a variable 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 clo
21、sed but unsealed test chamber remains at ambientbarometric pressure except for the short time during the airintroduction and at a flash point.4.3 After each arc application, the instantaneous pressureincrease above the ambient barometric pressure inside the testchamber is monitored. When the pressur
22、e increase exceeds 20kPa, the temperature at that point is recorded as the uncorrectedflash point, which is then corrected to barometric pressure.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 contro
23、lled laboratory conditions. It is only oneof a number of properties which must be considered inassessing the overall flammability hazard of a material.5.2 Flash point is used in shipping and safety regulations todefine flammable and combustible materials and for classifica-tion purposes. This defini
24、tion may vary from regulation toregulation. Consult the particular regulation involved for pre-cise definitions of these classifications.5.3 This test method can be used to measure and describethe properties of materials in response to heat and an ignitionsource under controlled laboratory condition
25、s and shall not beused to describe or appraise the fire hazard or fire risk ofmaterials under actual fire conditions. However, results of thistest 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 haza
26、rd of a particular end use.5.4 Flash point can also indicate the possible presence ofhighly volatile and flammable materials in a relatively non-volatile or nonflammable material, such as the contaminationof lubricating oils by small amounts of diesel fuel or gasoline.This test method was designed t
27、o be more sensitive to potentialcontamination than Test Method D6450.6. Apparatus6.1 Flash Point Apparatus, Continuously Closed CupOperationThe type of apparatus suitable for use in this testmethod employs a lid of solid brass, the temperature of whichis controlled electrically. Two temperature sens
28、ors for thespecimen and the lid temperatures, respectively, two arc pinsfor a high voltage arc, and a connecting tube for the pressuremonitoring and the air introduction are incorporated in the lid.Associated equipment for electrically controlling the chambertemperature is used, and a digital readou
29、t of the specimentemperature is provided. The apparatus and its critical elementsare shown in Figs. A1.1 and A1.2.6.1.1 Test ChamberThe test 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 an
30、d the sample cup shall provide good heatcontact but allow ambient barometric pressure to be maintainedinside the test chamber during the test. 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 r
31、esults in a pressure increase above ambient due to thetemperature and the vapor pressure of the sample. A poor heatcontact results in a bigger 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 simi
32、lar 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 dimensions 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 s
33、imilar) in stainless steel of 1 mm diameter with a responsetime of t(90)=3s.Itshall be immersed to a depth of at least2 mm into the specimen. It shall have a resolution of 0.1C anda minimum accuracy of 6 0.2C, preferably with a digitalreadout.6.1.4 Magnetic StirringThe apparatus shall have provi-sio
34、ns 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 of 126 1 mm. The rotation speed of the driving magnet shall b
35、ebetween 250 and 270 rev/min.6.1.5 Air IntroductionThe apparatus shall have provisionsfor introduction of air immediately after each flash test. The airTABLE 1 Volume of Introduced Air as a Function ofSample TemperatureSample TemperatureRange (C)Introduced Volumeof Air (mL)below 80 080 to below 150
36、0.5 0.15150 to below 200 1 0.2200 to below 300 1.5 0.3300 and above 2 0.4D7094 1212shall be introduced by a short air pulse from a small membranecompressor by means of a T-inlet in the connecting tube to thepressure transducer. The volume of the introduced air, from 0.5to 2 mL, is dependent on the s
37、ample 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 temperature of the test chamber for the duration ofthe test. The temperature regulation shall have a minimumaccuracy of 6 0.2C.6.1.7
38、 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 beapplied within 19 6 2 m/s. (WarningBecause samplescontaining low flash material or having a flash point below thepreset initial t
39、emperature 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 isrequired while the lid and sample cup temperatures areequalizing.)6.1.8 The pressure transducer for the flash point detectionshall b
40、e 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 60.5 kPa. It shall be capable of detecting an instantaneouspressure increase above barometric pressure of a minimum of20 kPa within
41、 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 pressure increase of 20 kPa corresponds to a flamevolume of approximately 2.5 mL.NOTE 4An automatic barometric correction, which is p
42、erformedaccording 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 used 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 syr
43、inge 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 intendedthat all reagents conform to the specifications of the Committeeon Analytical Reagents of the American Chemical Societywhere su
44、ch specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficient purity to permit its use without lessening the accu-racy of the determination.7.1.1 Anisole(WarningSee 7.2.)7.1.2 Dodecane(WarningSee 7.2.)7.2 Cleaning SolventsUse only noncorr
45、osive solvents ca-pable of cleaning the sample cup and the lid. Two commonlyused solvents are toluene and acetone. (WarningAnisole,dodecane, toluene, acetone, and many solvents are flammableand are health hazards. Dispose of solvents and waste materialin accordance with local regulations.)8. Samplin
46、g8.1 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 sealedcontainer at a low temperature.8.2 Do not store samples for an extended period of time ingas permeable containers, such as pla
47、stic, 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 mak
48、e a transferunless the sample temperature is at least 18C below theexpected flash point. When possible, perform the flash point asthe first test.8.4 Samples of very viscous materials may be warmed untilthey are reasonably fluid before they are tested. However, donot heat the unsealed sample above a
49、temperature of 18Cbelow its expected flash point.8.5 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, but it should not be heatedabove a temperature of 18C below its expected flash point.(WarningBecause samples containing volatile material willlose volatiles and then yield incorrectly high flash points, thetreatment described in 8.4 and 8.5 is not suitable for suchsamples.)9. Qu
