ASTM D7236-2006 Standard Test Method for Flash Point by Small Scale Closed Cup Tester (Ramp Method)《用小型闭杯试验器队闪点的标准试验方法(斜坡法)》.pdf

1、Designation: D 7236 06An American National StandardStandard Test Method forFlash Point by Small Scale Closed Cup Tester (RampMethod)1, 2This standard is issued under the fixed designation D 7236; the number immediately following the designation indicates the year oforiginal adoption or, in the case

2、of revision, 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.INTRODUCTIONThis flash point test method is a dynamic test method and depends on a definite rate of temp

3、eratureincrease to control the precision of the test method. The rate of heating may not in all cases give theprecision quoted in the test method because of the low thermal conductivity of certain materials. Theuse of an equilibrium method such as Test Methods D 3828, Method B improves the predictio

4、n offlammability for such materials, as the vapors above the test specimen and the test specimen are closerto thermal equilibrium.Flash point values are a function of the apparatus design, the condition of the apparatus used, andthe operational procedure carried out. Flash point can therefore only b

5、e defined in terms of a standardtest method, and no general valid correlation can be guaranteed between results obtained by differenttest methods or with test apparatus different than that specified.1. Scope1.1 This test method covers the determination of the flashpoint of aviation turbine fuel, die

6、sel fuel, kerosine and relatedproducts in the temperature range of 40 to 135C by a smallscale closed cup apparatus.1.2 This test method is only applicable to homogeneousmaterials that are liquid at or near ambient temperature and attemperatures required to perform the test.1.3 This test method is no

7、t applicable to liquids contami-nated by traces of highly volatile materials.1.4 This test method is a dynamic method and depends on adefinite rate of temperature increase. It is one of many flashpoint methods available, and every flash point test method,including this one, is an empirical one.1.5 I

8、f the users specification requires a defined flash pointmethod, neither this test nor any other method should besubstituted for the prescribed method without obtaining com-parative data and an agreement from the specifier.1.6 The values stated in SI units are to be regarded asstandard. No other unit

9、s of measurement are included in thisstandard.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 regul

10、atory limitations prior to use. For specific hazardstatements, see Section 7 and the Material Safety Data Sheetfor the product being tested.2. Referenced Documents2.1 ASTM Standards:3D 3828 Test Methods for Flash Point by Small Scale ClosedCup TesterD 4057 Practice for Manual Sampling of Petroleum a

11、ndPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 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 fo

12、r Petroleum Products andLubricantsE 300 Practice for Sampling Industrial Chemicals2.2 ISO Standards:4ISO Guide 34 Quality Systems Guidelines for the Produc-tion of Reference Materials1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the dire

13、ct responsibility of SubcommitteeD02.08 on Volatility.Current edition approved Jan. 1, 2006. Published March 2006.2This test method is being jointly developed and harmonized with the EnergyInstitute.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service

14、 at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.1Copyright ASTM International, 100 Barr Harbor Drive, P

15、O Box C700, West Conshohocken, PA 19428-2959, United States.ISO Guide 35 Certification of Reference MaterialGeneraland Statistical Principles3. Terminology3.1 Definitions:3.1.1 flash point, nlowest temperature corrected to apressure of 101.3 kPa, at which application of a test flamecauses the vapors

16、 of a test specimen of the sample to ignitemomentarily under the specified conditions of the test.3.2 Definitions of Terms Specific to This Standard:3.2.1 dynamic, adjthe condition where the vapor abovethe test specimen, and the test cup, are not in temperatureequilibrium at the time the test flame

17、is applied.4. Summary of Test Method4.1 A 2 6 0.1 mL test specimen is introduced into the testcup that is then heated automatically at a constant rate of 2 60.5C/min. A gas test flame is directed through an openingshutter, in the test cup lid, at specified temperature intervalsuntil a flash is detec

18、ted by the automatic flash detector. Theflash is reported as defined in 3.1.1.5. 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

19、that must be considered in 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.Consult the particular regulation involved for precise defini-tions of these classifications.5.3

20、 This test method can be used to measure and describethe properties of materials in response to heat and a test flameunder controlled laboratory conditions and shall not be used todescribe or appraise the fire hazard or fire risk of materialsunder actual fire conditions. However, results of this tes

21、tmethod may be used as elements of a fire risk assessment, thattakes into account all of the factors that are pertinent to anassessment of the fire hazard of a particular end use.6. Apparatus6.1 Flash Point ApparatusThe apparatus consists of anelectrically heated test cup that is controlled automati

22、cally togive a temperature increase of 2.0 6 0.5C/min, a lid andshutter assembly, a pilot and test flame, an automatic flashdetector and a temperature display that displays and holds thetest temperature when a flash is detected. The key parts anddimensions are described in Annex A1 and illustrated i

23、n Fig.A1.1.6.2 Syringe, 2 mL, adjusted to deliver 2.00 6 0.1 mL.6.3 Barometer, accurate to 0.5 kPa. Barometers pre-corrected to give sea level readings, such as those used atweather stations and airports, shall not be used.NOTE 1Automatic barometric correction in accordance with 12.2 maybe installed

24、 in the apparatus.6.4 Cooling Bath or Freezer, for cooling the samples, ifrequired, and capable of cooling the sample to at least 10Cbelow the expected flash point. If a freezer is used, it shall beof explosion-protected design.6.5 Draft Shield, a shield fitted at the back and on two sidesof the ins

25、trument, for use in circumstances where naturalprotection from drafts does not exist.NOTE 2A shield 350-mm high, 480-mm wide, and 240-mm deep, issuitable.7. Reagents and Materials7.1 Cleaning SolventUse only noncorrosive solvents ca-pable of cleaning the test cup and lid assembly. Two commonlyused s

26、olvents are toluene and acetone. (WarningToluene,acetone and many solvents are flammable and a health hazard.Dispose of solvents and waste material in accordance withlocal regulations.)7.2 Butane or Natural GasFor use as the pilot and testflame. (WarningButane and natural gases are flammableand a he

27、alth hazard.)8. Sampling8.1 Obtain at least a 25 mL sample from a bulk test site inaccordance with Practices D 4057, D 4177, E 300 or othercomparable sampling practices.8.2 Store samples in clean, tightly sealed containers atnormal room temperature (20 to 25C) or colder. Ensure thatthe container is

28、85 to 95 % full.8.3 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.Samples in leaky containers are suspect and not a source ofvalid results.8.4 Erroneously high flash points can

29、be obtained whenprecautions are not taken to avoid loss of volatile materials. Donot open containers unnecessarily. Do not make a transferunless the sample temperature is at least 10C below theexpected flash point. Where possible perform the flash point asthe first test on the sample.8.5 Samples con

30、taining dissolved or free water may bedehydrated with calcium chloride. Warming the sample ispermitted, but do not heat the sample above a temperature of10C below its expected flash point. (WarningIf the sampleis expected of containing volatile components, the treatment asdescribed in 8.5 should be

31、omitted.)8.6 Cool or adjust the temperature of the sample and itscontainer to at least 10C below the expected flash point beforeopening to remove the test specimen. If an aliquot of theoriginal sample is to be stored prior to testing, ensure that thecontainer is filled to between 85 and 95 % of its

32、capacity.Gently mix the subsample to ensure uniformity while mini-mizing the possible loss of volatile components and light ends.NOTE 3Results of flash point tests may be affected if the samplevolume falls below 85 % of the containers capacity.9. Preparation of Apparatus9.1 Support the apparatus (An

33、nex A1) on a level and steadysurface in a draft-free position (see Notes 4 and 5).NOTE 4A draft shield (6.5) is recommended to be used when naturalprotection from drafts does not exist.D7236062NOTE 5When testing materials that may produce toxic vapors, theapparatus may be located in a fume hood with

34、 an individual control of airflow, adjusted such that the toxic vapors can be withdrawn withoutcausing air currents around the test cup during the test.9.2 Clean the test cup, cover, and its accessories with anappropriate solvent (7.1) to remove traces of gum or residuefrom the previous test.NOTE 6A

35、 stream of clean dry air may be used to remove the lasttraces of solvent used.NOTE 7The filler orifice may be cleaned with a pipe cleaner.10. Verification of Apparatus10.1 Verify that the temperature measuring device is inaccordance with A1.7.10.2 Verify the performance of the apparatus at least onc

36、eper year by determining the flash point of a Certified ReferenceMaterial (CRM) that has a certified flash point reasonably closeto the expected range of the samples to be tested. Examples ofmaterials that may be used to create CRMs are listed inAppendix X1. The flash point shall be determined using

37、 theprocedures stated in Section 11. Appendix X1 indicates typicallimits in Table X1.1 for a typical CRM and shows how tocalculate limits for an unlisted CRM.10.3 Once the performance of the apparatus has beenverified using a CRM, the flash point of Secondary WorkingStandards (SWS) can be determined

38、 along with their controllimits. These SWS can then be utilized for more frequentperformance checks. (See Appendix X1.)10.4 When the flash point obtained is not within the limitsstated in 10.2 or 10.3 check the condition and operation of theapparatus to ensure conformance to the details listed in An

39、nexA1, especially with regard to the action of the shutter, theposition and size of the test flame, the heating rate and thetemperature sensor readings. After any adjustment, repeat thetest in 10.2 or 10.3 using a fresh test specimen, with specialattention to the procedural details prescribed in the

40、 test method.11. Procedure11.1 Set the test cup temperature to 15 6 5C below theexpected flash point temperature.11.2 When the test cup is at the required temperature, chargea clean and dry syringe (6.2), adjusted to a temperature at least10C below the expected flash point, witha2mLtestspecimen. Clo

41、se the sample container immediately after with-drawal of the test specimen, to minimize any loss of volatilecomponents.11.3 Carefully transfer the syringe to the filler orifice anddischarge the test specimen into the test cup by fully depressingthe syringe plunger. Remove the syringe.11.4 Ignite the

42、 pilot and test flames. Adjust the test flame toconform to the size of the 4 mm gauge ring. Reset the flashdetector (A1.9). Start the test.NOTE 8The ignition of the test flame and control of the gas supplymay be automated on some instruments.11.5 The test cup is heated automatically at such a rate t

43、hatthe temperature, as indicated by the temperature sensor, in-creases by 1.5 to 2.5C/min. The test flame is dipped into thetest cup, as the shutter is slowly and uniformly opened andclosed overa2to3-speriod, at 1C intervals for temperaturesup to and including 100C and thereafter every 2C fortempera

44、tures over 100C.11.5.1 Observe the first two dips of the flame for continuousburning in the orifice. If a continuous luminous flame burns inthe orifice when the slide is opened and the test flame isintroduced, then the flash point lies considerably below the testtemperature. In such cases, discontin

45、ue the test and repeat thetest with a fresh test specimen using a lower expected flashpoint.11.5.2 Application of the test flame may cause a blue halo oran enlarged flame prior to the actual flash point. This is not aflash and is ignored by the flash detector.11.6 Record the displayed and held tempe

46、rature of thetemperature sensor when the application of the test flamecauses a flash to be automatically detected.11.7 Record the ambient barometric pressure using a barom-eter (6.3) in the vicinity of the apparatus at the time of the test.NOTE 9It is not considered necessary to correct the barometr

47、icpressure reading to 0C, although some barometers are designed to makethis correction automatically.11.8 When the temperature at which the flash is observed isless than 10C or greater than 30C from the start temperatureof the test, the result is not valid. Repeat the test using a freshtest specimen

48、 adjusting the temperature of the first applicationof the test flame until a valid determination is made.12. Calculation12.1 Barometric Pressure ConversionIf the barometricpressure reading is measured in a unit other than kilopascals,convert to kilopascals using one of the following equations:Readin

49、g in hPa 3 0.1 5 kPa (1)Reading in mbar 3 0.1 5 kPa (2)Reading in mmHg 3 0.1333 5 kPa (3)12.2 Correction of Detected Flash Point to Standard Atmo-spheric PressureCalculate the flash point corrected to astandard atmospheric pressure of 101.3 kPa, Tc, using thefollowing equation:Tc5 TD1 0.25 101.3 p! (4)where:TD= the detected flash point temperature at ambient baro-metric pressure, expressed in degrees Celsius, andp = the ambient barometric pressure, expressed in kilo-pascals.NOTE 10This equation is strictly correct only within the barometricpre