1、Designation: D 6450 05An American National StandardStandard Test Method forFlash Point by Continuously Closed Cup (CCCFP) Tester1This standard is issued under the fixed designation D 6450; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revi
2、sion, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This flash point test method is a dynamic method anddepends on definite rates of temperature incre
3、ase. 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 tested. They are a function of the apparatus design,the condition of the appar
4、atus 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 betweenresults obtained by different test methods or with test apparatus differentfrom that specified.1.2 This test met
5、hod covers the determination of the flashpoint of fuel oils, lube oils, solvents, and other liquids by acontinuously closed cup tester. The measurement is made on atest specimen of 1 mL.1.3 This test method utilizes a closed but unsealed cup withair injected into the test chamber.1.4 This test metho
6、d is suitable for testing samples with aflash point from 10 to 250C.NOTE 2Flash point determinations below 10C and above 250C canbe performed; however, the precision has not been determined below andabove these temperatures.1.5 If the users specification requires a defined flash pointmethod other th
7、an this test method, neither this test method norany other method should be substituted for the prescribedmethod without obtaining comparative data and an agreementfrom the specifier.1.6 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informat
8、iononly. Temperatures are in degrees Celsius, and pressure is inkilo-pascals.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 determ
9、ine the applica-bility of regulatory limitations prior to use. Specific warningstatements appear throughout the standard.2. Referenced Documents2.1 ASTM Standards:2D 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum P
10、roductsD 6299 Practice for Applying Statistical Quality AssuranceTechniques to Evaluate Analytical Measurement SystemPerformanceD 6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsE 300 Practice for Sampling Industrial Chemicals2.2
11、ISO Standards:3ISO Guide 34 Quality Systems Guidelines for the Produc-tion of Reference MaterialsISO Guide 35 Certifications of Reference Material Gen-eral and Statistical Principles3. Terminology3.1 Definitions:3.1.1 dynamic, adjthe condition in which the vapor abovethe test specimen and the test s
12、pecimen are not in temperatureequilibrium at the time at which the ignition source is applied.3.1.2 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 ignitemomentarily under specified co
13、nditions of the test.3.1.2.1 DiscussionFor the purpose of this test method, thetest specimen is deemed to have flashed when the hot flame of1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.08 on
14、Volatility.Current edition approved May 1, 2005. Published May 2005. Originallyapproved in 1999. Last previous edition approved in 1999 as D 645099.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandar
15、ds 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 10036.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr
16、Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.the ignited vapor causes an instantaneous pressure increase ofat least 20 kPa inside the closed measuring chamber.44. Summary of Test Method4.1 The lid of the test chamber is regulated to a temperatureat least 18C below the e
17、xpected flash point.A1 6 0.1 mL testspecimen of a sample is introduced into the sample cup,ensuring that both specimen and cup are at a temperature atleast 18C below the expected flash point, cooling if necessary.The cup is then raised and pressed onto the lid of specifieddimensions to form the cont
18、inuously closed but unsealed testchamber with an overall volume of 4.0 6 0.2 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 flash tests, an arc of
19、defined energy is discharged insidethe test chamber at regular intervals. After each ignition, 1.5 60.5 mL of air is introduced into the test chamber to provide thenecessary oxygen for the next flash test. The pressure inside thecontinuously closed but unsealed test chamber remains atambient baromet
20、ric pressure, except for the short time duringthe air introduction and except at a flash point.4.3 After each arc, the instantaneous pressure increaseabove the ambient barometric pressure inside the test chamberis monitored. When the pressure increase exceeds a definedthreshold, the temperature at t
21、hat point is recorded as theuncorrected flash point.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 that must be considered in
22、 assessingthe overall flammability hazard of a material.5.2 Flash point is used in shipping and safety regulations todefine flammable and combustible materials and classify them.This definition may vary from regulation to regulation. Consultthe particular regulation involved for precise definitions
23、ofthese 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 conditions and shall not beused to describe or appraise the fire hazard or fire risk ofmaterials under actual fire conditi
24、ons. However, results of thistest method may be used as elements of a fire risk assessment,which takes into account all of the factors that are pertinent toan assessment of the fire hazard of a particular end use.5.4 Flash point can also indicate the possible presence ofhighly volatile and flammable
25、 materials in a relatively non-volatile or nonflammable material, such as the contaminationof lubricating oils by small amounts of diesel fuel or gasoline.6. Apparatus6.1 Flash Point Apparatus, Continuously Closed CupOperationThe type of apparatus suitable for use in this testmethod employs a lid of
26、 solid brass, the temperature of whichis controlled electrically. Two temperature sensors for thespecimen and the lid temperatures, respectively, two electri-cally insulated pins for a high voltage arc, and a connectingtube for the pressure monitoring and the air introduction areincorporated in the
27、lid. Associated equipment for electricallycontrolling the chamber temperature is used, and a digitalreadout of the specimen temperature is provided. The appara-tus and its critical elements are shown in Fig. A1.1 and Fig.A1.2.56.1.1 Test ChamberThe test chamber is formed by thesample cup and the tem
28、perature controlled lid and shall have anoverall volume of 4 6 0.2 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 test. Critical dimensions areshown in Fig. A1.2. T
29、he 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 bigger temperature difference between thesample and
30、 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 4 mL and shallbe capable of containing 1 6 0.1 mL of sample. The criticaldimensions and requirements are shown in Fig. A1.2.6.1.3
31、Specimen Temperature SensorThe specimen tem-perature sensor (Fig. A1.1: Ts) shall be a thermocouple(NiCr-Ni or similar) in stainless steel of 1-mm diameter with aresponse time of t(90)=3s.Itshall be immersed to a depth ofat least 2 mm into the specimen. It shall have a resolution of0.1C and a minimu
32、m accuracy of 6 0.2C, preferably with adigital readout.6.1.4 Magnetic StirringThe apparatus shall have provi-sions for stirring the sample. A rotating magnet outside thesample cup shall drive a small stirring magnet, which isinserted into the sample cup after sample introduction. Thestirring magnet
33、shall have a diameter of 3 6 0.2 mm and alength of 12 6 1 mm. The rotation speed of the driving magnetshall be between 250 and 270 rev/min.6.1.5 Air IntroductionThe apparatus shall have provisionsfor introduction of 1.5 6 0.5 mL of air immediately after eachflash test. The air shall be introduced by
34、 a short air pulse froma small membrane compressor by means of a T-inlet in theconnecting tube to the pressure transducer.6.1.6 Electrical heating and thermoelectric cooling of the lid(Fig. A1.1: PE) shall be used to regulate the temperature of the4The method of detecting the flash point by monitori
35、ng the instantaneouspressure increase is covered by a patent. Interested parties are invited to submitinformation regarding the identification of an alternative(s) to this patented item toASTM Headquarters.Your comments will receive careful consideration at a meetingof the responsible technical comm
36、ittee, which you may attend.5The sole source of supply of the continuously closed cup testers meeting theserequirements known to the committee at this time is Grabner Instruments, A-1220Vienna, Dr. Otto Neurathgasse 1, Austria. If you are aware of alternative suppliers,please provide this informatio
37、n to ASTM International Headquarters. Your com-ments will receive careful consideration at a meeting of the responsible technicalcommittee1, which you may attend.D6450052test chamber for the duration of the test. The temperatureregulation shall have a minimum accuracy of 6 0.2C.6.1.7 A high voltage
38、electric arc shall be used for theignition of the flammable vapor. The energy of the arc shall be3 6 0.5 mJ (3 6 0.5 Ws) per arc, and the energy shall beapplied within 43 6 3 ms. (WarningBecause samplescontaining low flash material or having a flash point below thepreset initial temperature can over
39、saturate the vapor inside thechamber and hence prohibit the detection of a flash point in thechosen range, the design of the apparatus should incorporatestep-wise ignitions in steps of 10C, following the closing ofthe measuring chamber and before the sample reaches theinitial temperature of the test
40、.)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 of60.5 kPa. It shall be capable of detecting an instantaneouspress
41、ure increase above barometric pressure of a minimum of20 kPa within 100 ms.NOTE 3The monitoring of the instantaneous pressure increase abovebarometric pressure is one of several methods used to determine a flashinside the test chamber. A pressure increase of 20 kPa corresponds to aflame volume of ap
42、proximately 1.5 mL.NOTE 4An automatic barometric correction, which is performed inaccordance with the procedure described in 12.1, can be installed in thetester. The absolute pressure reading of the pressure transducer describedin 6.1.8 may be used for the correction.6.1.9 The introduction of a test
43、 portion of 1.0 6 0.1 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 re-quested in Table X1.1. Unless otherwise indicated, it isintended that all reagents conform to the specifications of
44、theCommittee on Analytical Reagents of the American ChemicalSociety where such specifications are available.6Other gradesmay be used, provided it is first ascertained that the reagent isof sufficient purity to permit its use without lessening theaccuracy of the determination.7.1.1 Anisole(WarningFla
45、mmable and a health hazard.Dispose of solvents and waste material in accordance withlocal regulations.)7.1.2 Dodecane(WarningFlammable and a health haz-ard. Dispose of solvents and waste material in accordance withlocal regulations.)7.2 Cleaning SolventsUse only noncorrosive solvents ca-pable of cle
46、aning the sample cup and the lid. Two commonlyused solvents are toluene and acetone. (WarningFlammableand a health hazard. Dispose of solvents and waste material inaccordance with local regulations.)8. Sampling8.1 Obtain at least a 50 mL sample from a bulk test site inaccordance and instruction give
47、n in Practice D 4057, D 4177,or E 300. Store the sample in a clean, tightly sealed containerat 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 sample
48、s 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. Whe
49、n 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 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 do not heat the sampleabove a temperature of 18C below its expected flash point.(Warn
