1、Designation: D6450 05 (Reapproved 2010)D6450 12Standard Test Method forFlash Point by Continuously Closed Cup (CCCFP) Tester1This standard is issued under the fixed designation D6450; 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. Scope Scope*1.1 This flash point test method is a dynamic method and depends on definite rates of temperature incr
3、ease. 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 property of materials tested. They are a function of the apparatus design, the conditionof the ap
4、paratus 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 obtained by different test methods or with test apparatus different from that specified.1.2 This te
5、st method covers the determination of the flash point of fuel oils, lube oils, solvents, and other liquids by acontinuously closed cup tester. The measurement is made on a test specimen of 1 mL.1.3 This test method utilizes a closed but unsealed cup with air injected into the test chamber.1.4 This t
6、est method is suitable for testing samples with a flash point from 10 to 250C.NOTE 2Flash point determinations below 10C and above 250C can be performed; however, the precision has not been determined below and abovethese temperatures.1.5 If the users specification requires a defined flash point met
7、hod other than this test method, neither this test method nor anyother method should be substituted for the prescribed 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 incl
8、uded in this standard.Temperatures are in degrees Celsius, and pressure is 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 practi
9、ces and determine the applicability of regulatorylimitations prior to use. Specific warning statements appear throughout the standard.2. Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petroleum an
10、d Petroleum ProductsD6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-ment System PerformanceD6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and LubricantsE300 Practice f
11、or Sampling Industrial Chemicals2.2 ISO Standards:3ISO Guide 34 Quality Systems Guidelines for the Production of Reference MaterialsISO Guide 35 Certifications of Reference Material General and Statistical Principles3. Terminology3.1 Definitions:1 This test method is under the jurisdiction of ASTM C
12、ommittee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.08 onVolatility.Current edition approved Oct. 1, 2010Dec. 1, 2012. Published November 2010March 2013. Originally approved in 1999. Last previous edition approved in 20052010 asD645005. 05 (2010). D
13、OI: 10.1520/D6450-05R10.10.1520/D6450-12.2 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 Ame
14、rican National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036.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
15、to adequately depict all 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 standardCopyrigh
16、t ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.1 dynamic, adjthe condition in which the vapor above the test specimen and the test specimen are not in temperatureequilibrium at the time at which the ignition source is applied.3.1.2 flash
17、 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 momentarily under specified conditions of the test.3.1.2.1 DiscussionFor the purpose of this test method, the test specimen is deemed
18、 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.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 1 6 0.1 mL te
19、stspecimen of a sample is introduced into the sample cup, ensuring that both specimen and cup are at a temperature at least 18Cbelow the expected flash point, cooling if necessary. The cup is then raised and pressed onto the lid of specified dimensions to formthe continuously closed but unsealed tes
20、t chamber with an overall volume of 4.0 6 0.2 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, an arc of defined energy is discharged
21、inside the testchamber at regular intervals. After each ignition, 1.5 6 0.5 mL of air is introduced into the test chamber to provide the necessaryoxygen for the next flash test.The pressure inside the continuously closed but unsealed test chamber remains at ambient barometricpressure, except for the
22、 short time during the air introduction and except at a flash point.4.3 After each arc, the instantaneous pressure increase above the ambient barometric pressure inside the test chamber ismonitored. When the pressure increase exceeds a defined threshold, the temperature at that point is recorded as
23、the uncorrectedflash point.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 properties that must be considered in assessing the overallf
24、lammability hazard of a material.5.2 Flash point is used in shipping and safety regulations to define flammable and combustible materials and classify them. Thisdefinition may vary from regulation to regulation. Consult the particular regulation involved for precise definitions of theseclassificatio
25、ns.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 hazard or fire risk of materials underactual fire conditions. However, resul
26、ts of this test method may be used as elements of a fire risk assessment, which takes intoaccount all of the factors that are pertinent to an assessment of the fire hazard of a particular end use.5.4 Flash point can also indicate the possible presence of highly volatile and flammable materials in a
27、relatively nonvolatile ornonflammable material, such as the contamination of lubricating oils by small amounts of diesel fuel or gasoline.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, th
28、e temperature of which is controlled electrically. Two temperature sensors for the specimen and thelid temperatures, respectively, two electrically insulated pins for a high voltage arc, and a connecting tube for the pressuremonitoring and the air introduction are incorporated in the lid. Associated
29、 equipment for electrically controlling the chambertemperature is used, and a digital readout of the specimen temperature is provided. The apparatus and its critical elements areshown in Fig. A1.1 and Fig. A1.2.46.1.1 Test ChamberThe test chamber is formed by the sample cup and the temperature contr
30、olled lid and shall have an overallvolume of 4 6 0.2 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 chamber during the test. Critical dimensions are shown in Fig. A1.2.The pressure
31、inside the measuring chamber during the temperature increase is monitored. A seal that is too tight results in a4 The method of detecting the flash point by monitoring the instantaneous pressure increase is covered by a patent. Interested parties are invited to submit informationregarding the identi
32、fication of an alternative(s) to this patented item toASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsibletechnical committee, which you may attend.4 The sole source of supply of the continuously closed cup testers meeting these requirements known to th
33、e committee at this time is Grabner Instruments,A-1220 Vienna,Dr. Otto Neurathgasse 1, Austria. If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical com
34、mittee 1, which you may attend.D6450 122pressure increase above ambient due to the temperature and the vapor pressure of the sample.Apoor heat contact 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 aluminu
35、m or other material with similar heat conductivity.It shall have an overall volume of 4 mL and shall be capable of containing 1 6 0.1 mL of sample. The critical dimensions andrequirements are shown in Fig. A1.2.6.1.3 Specimen Temperature SensorThe specimen temperature sensor (Fig. A1.1: Ts) shall be
36、 a thermocouple (NiCr-Ni orsimilar) 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 least 2 mminto the specimen. 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 Stirri
37、ngThe apparatus shall have provisions for stirring the sample.Arotating magnet outside the sample cupshall drive a small stirring magnet, which is inserted into the sample cup after sample introduction. The stirring magnet shall havea diameter of 3 6 0.2 mm and a length of 12 6 1 mm. The rotation sp
38、eed of the driving magnet shall be between 250 and 270rev/min.6.1.5 Air IntroductionThe apparatus shall have provisions for introduction of 1.5 6 0.5 mLof air immediately after each flashtest. The air shall be introduced by a short air pulse from a small membrane compressor by means of a T-inlet in
39、the connectingtube 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 thetest chamber for the duration of the test. The temperature regulation shall have a minimum accuracy of 6 0.2C.6.1.7 A high volt
40、age electric arc shall be used for the ignition of the flammable vapor. The energy of the arc shall be 3 6 0.5mJ (3 6 0.5 Ws) per arc, and the energy shall be applied within 43 6 3 ms. (WarningBecause samples containing low flashmaterial or having a flash point below the preset initial temperature c
41、an oversaturate the vapor inside the chamber and henceprohibit the detection of a flash point in the chosen range, the design of the apparatus should incorporate step-wise ignitions in stepsof 10C, following the closing of the measuring chamber and before the sample reaches the initial temperature o
42、f the test.)6.1.8 The pressure transducer for the flash point detection shall be connected to the connecting 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 60.5 kPa.It shall be capable of detecting an instan
43、taneous pressure increase above barometric pressure of a minimum of 20 kPa within 100ms.NOTE 3The monitoring of the instantaneous pressure increase above barometric pressure is one of several methods used to determine a flash insidethe test chamber. A pressure increase of 20 kPa corresponds to a fla
44、me volume of approximately 1.5 mL.NOTE 4An automatic barometric correction, which is performed in accordance with the procedure described in 12.1, can be installed in the tester.The absolute pressure reading of the pressure transducer described in 6.1.8 may be used for the correction.6.1.9 The intro
45、duction of a test portion of 1.0 6 0.1 mL shall be accomplished by the use of a pipette or syringe of the requiredaccuracy.7. Reagents and Materials7.1 Purity of ReagentsUse only chemicals of purity requested in Table X1.1. Unless otherwise indicated, it is intended thatall reagents conform to the s
46、pecifications of the Committee onAnalytical Reagents of theAmerican Chemical Society where suchspecifications are available.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
47、 Anisole(WarningFlammable and a health hazard. Dispose of solvents and waste material in accordance with localregulations.)7.1.2 Dodecane(WarningFlammable and a health hazard. Dispose of solvents and waste material in accordance with localregulations.)7.2 Cleaning SolventsUse only noncorrosive solve
48、nts capable of cleaning the sample cup and the lid. Two commonly usedsolvents are toluene and acetone. (WarningFlammable and a health hazard. Dispose of solvents and waste material inaccordance with local regulations.)8. Sampling8.1 Obtain at least a 50 mLsample from a bulk test site in accordance a
49、nd instruction given in Practice D4057, D4177, or E300.Store the sample in a clean, tightly sealed container at a low temperature.8.2 Do not store samples for an extended period of time in gas permeable containers, such as plastic, because volatile materialmay 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 when precautions are not taken to avoid loss of volatile material. Do not opencontainers unnecessarily. Do not make a transfer unless the s
