1、Designation: D 1310 01 (Reapproved 2007)Standard Test Method forFlash Point and Fire Point of Liquids by Tag Open-CupApparatus1This standard is issued under the fixed designation D 1310; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisi
2、on, 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method cov
3、ers the determination by TagOpen-CupApparatus of the flash point and fire point of liquidshaving flash points between 18 and 165C (0 and 325F) andfire points up to 325F.1.2 This test method, when applied to paints and resinsolutions that tend to skin over or that are very viscous, givesless reproduc
4、ible results than when applied to solvents.NOTE 1In order to conserve time and sample, the fire point of amaterial may be determined by the Tag Open-Cup Method by continuingthe heating of the specimen to its fire point. Fire points may also bedetermined by Test Method D92, which should be used for f
5、ire pointsbeyond the scope of this test method.1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard should be used to measure and describethe properties of materials, products, or assemblies in responseto heat
6、and flame under controlled laboratory conditions andshould not be used to describe or appraise the fire hazard orfire risk of materials, products, or assemblies under actual fireconditions. However, results of this test may be used aselements of a fire risk assessment which takes into account allof
7、the factors pertinent to an assessment of the fire hazard of aparticular end use.1.5 This standard does not purport to address the safetyproblems associated with its use. It is the responsibility of theuser of this standard to establish appropriate safety and healthpractices and determine the applic
8、ability of regulatory limita-tions prior to use.2. Referenced Documents2.1 ASTM Standards:2D92 Test Method for Flash and Fire Points by ClevelandOpen Cup TesterD 850 Test Method for Distillation of Industrial AromaticHydrocarbons and Related MaterialsD 1015 Test Method for Freezing Points of High-Pu
9、rityHydrocarbonsD 1016 Test Method for Purity of Hydrocarbons fromFreezing PointsD 1078 Test Method for Distillation Range of VolatileOrganic LiquidsD 1364 Test Method for Water in Volatile Solvents (KarlFischer Reagent Titration Method)D 2268 Test Method for Analysis of High-Purity n-Heptaneand Iso
10、octane by Capillary Gas ChromatographyD2699 Test Method for Research Octane Number ofSpark-Ignition Engine FuelD 2700 Test Method for Motor Octane Number of Spark-Ignition Engine FuelE1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 Definitions:3.1.1 flash point, nthe lowest te
11、mperature, corrected to apressure of 760 mm Hg (101.3 kPa, 1013 mbar), at whichapplication of an ignition source causes the vapor of thespecimen to ignite by the procedure described.3.2 Definitions of Terms Specific to This Standard:3.2.1 fire point, nthe lowest temperature at which aspecimen sustai
12、ns burning for a minimum of5sbytheprocedure described.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, andApplications and is the direct responsibility ofSubcommittee D01.22 on Flammability and Safety.Current edition approved June 1, 2007. Pu
13、blished August 2007. Originallyapproved in 1952. Last previous edition approved in 2001 as D 1310 01.2For 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 D
14、ocument Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Summary of Method4.1 The specimen is placed in the cup of a Tag Open-CupApparatus and heated at a slow, but constant rate. A small testflame i
15、s passed at a uniform rate across the cup at specifiedintervals until a flash occurs. To determine the fire point, thetest is continued until the application of the test flame causesthe specimen to ignite and burn for at least 5 s.5. Significance and Use5.1 Flash point and fire point of a liquid are
16、 physicalproperties that may be used to define their flammabilityhazards. The flash point may be used to classify materials ingovernment regulations.6. Apparatus6.1 Flash TesterTag Open-Cup Apparatus (Fig. 1), asdescribed in detail in Annex A1.6.2 Shield, as described in detail in Annex A1.6.3 Therm
17、ometers, conforming to Specification E1,aslisted in Table 1.6.4 Flasks, 500-mL, two, with rubber stoppers.7. Materials7.1 Water-Glycol Solution (1 + 1), for flash points from 18to 93C (0 to 200F).7.2 Solid Carbon Dioxide-Acetone or other Coolant.7.3 Silicone Fluid, inert, high boiling, having a flas
18、h pointexceeding the test temperatures by at least 60C (110F) forflash and fire points from 93 to 165C (200 to 325F).7.4 n-Heptane,3for determination of flash points from 18to 16C (0 to 60F). See Annex A2 for specifications.7.5 p-Xylene,3for determination of flash points from 16 to93C (60 to 200F).
19、See Annex A2 for specifications.7.6 Isopropanol (isopropyl alcohol),4for determination offlash points from 16 to 93C (60 to 200F). See Annex A2 forspecifications.7.7 Diethylene Glycol,5for determination of flash pointsfrom 93 to 165C (200 to 325F). See Annex A2 for specifi-cations.8. Assembly and Pr
20、eparation of Apparatus8.1 Place the tester in a level position on a solid table free ofvibration, in a location free of perceptible draft, and in a dimlight. Maintain a room temperature of 24 6 3C (75 6 5F)throughout the test. Other room temperatures may be specifiedon agreement between buyer and se
21、ller.NOTE 2For materials with vapors or products of pyrolysis that areobjectionable, it is permissible to place the apparatus with shield in a fumehood with the ventilation turned off. The ventilation can then be turned onat completion of the test, or when and if fumes become objectionable.8.2 Adjus
22、t the horizontal and vertical positions of the taperso that the jet passes on the circumference of a circle having aradius of at least 6 in. (150 mm). The jet should pass across thecenter of the cup at right angles to a diameter passing throughthe thermometer and in a plane18 in. (3.2 mm) above the
23、upperedge of the cup as measured from the center of the orifice.8.3 Using the leveling device as a gage, adjust the height ofthe taper so that the center of the orifice is exactly18 in. (3.2mm) above the top edge of the glass cup when it is in place. Itis imperative that this adjustment be made as a
24、ccurately aspossible. Raising or lowering the taper can be achieved bybending it slightly or preferably by adding and removing thinmetal shims as required from between the taper and the verticalsupporting member of the swivel holder.8.4 With the glass cup in place in the bath, adjust thethermometer
25、holder so that the thermometer is supported firmlyin a vertical position halfway between the center and edge ofthe cup and on a line passing through the center of the cup andthe pivot of the taper. Place the thermometer so that the bottomof the bulb is14 in. (6.4 mm) from the inner bottom of the cup
26、.8.5 Set the draft shield around the tester so that the sidesform right angles with each other and the tester is well towardthe back of the shield.9. Procedure9.1 Flash Points from 18 to 16C (0 to 60F) (WarningMeticulous attention to all details relating to the taper, size oftaper flame, rate of tem
27、perature increase, and rate of passingthe taper over the sample is necessary for good results.)9.1.1 Equip two 500-mLflasks with rubber stoppers throughwhich are inserted ASTM 33C (33F) thermometers. Cool aquantity of 1 + 1 water-glycol solution in one stoppered500-mL flask to approximately 30C (20F
28、) by immersingthe flask in a solid carbon dioxide-acetone bath or othercoolant. Use extreme care not to contaminate the water-glycolsolution with either acetone or carbon dioxide.9.1.2 Pour the cooled water-glycol solution into the testerbath to a predetermined level 3.2 mm (18 in.) below the topwhe
29、n the cup is in place. An overflow is desirable forcontrolling the liquid level in the bath.9.1.3 At the same time the water-glycol coolant is beingchilled, cool a portion of the sample to approximately 25C(10F) in the second stoppered 500-mL flask. If solid carbondioxide and acetone or other volati
30、le solvents are used as acoolant, extreme care must be exercised to avoid contamina-tion of the sample. Cool the glass cup and place it in the bath.Position the appropriate thermometer (Table 1) as described in8.4 and fill the cup with cooled sample to a depth approxi-mately 3.2 mm (18 in.) below th
31、e edge as determined by theleveling device.NOTE 3Remove all bubbles from the surface of the liquid beforestarting a determination.9.1.4 Light the ignition flame and adjust it to form a flameof spherical shape matching in size the532-in. (4.0-mm) sphereon the apparatus or the532-in. hole in the level
32、ing device.9.1.5 Make the final adjustment of the specimen level in thecup when the temperature is 20F (10C) below the anticipatedflash point. Two trial determinations may be necessary to select3Satisfactory n-heptane and p-xylene can be obtained from Special ProductsDivision, Chemical Department, P
33、hillips Petroleum Company, Drawer O, Borger,TX 79607.4Satisfactory isopropanol may be obtained from Exxon Chemical, Americus P.O. Box 3272, Houston, TX 77001, Shell Chemical Co., One Shell Plaza, Houston,TX 77002, or Union Carbide Co., P. O. Box 8361, South Charleston, WV 25303.5Satisfactory diethyl
34、ene glycol may be obtained from Union Carbide Co., S.Charleston, WV.D 1310 01 (2007)2the proper temperature at which to adjust the liquid level. Ahypodermic syringe or medicine dropper provides a convenientmeans of adding or removing sample from the cup.9.1.6 Allow the temperature of the specimen to
35、 increasespontaneouslywithout applying any heatuntil the rate oftemperature rise decreases to 2F (1C)/min. At this point,Metric Equivalentsin. mm21316 71.43316 81678 174.5FIG. 1 Tag Open-Cup ApparatusD 1310 01 (2007)3apply heat to maintain an increase in temperature at a rate of 26 0.5F (1 6 0.25C)/
36、min.NOTE 4With viscous materials, this rate of heating cannot always bemaintained.9.1.7 Determine the approximate flash point by passing thetaper flame across the specimen at intervals of 2F (1C). Makethe first pass of the taper flame immediately after the finaladjustment of the specimen level, as i
37、n 9.1.5. The time requiredto pass the ignition flame across the surface of the liquid shouldbe 1 s. Each pass must be in one direction only, and the tapershould be kept in the “off” position at one or the other end ofthe swing except when the flame is applied to the specimen. Incase the material ten
38、ds to “creep” over the edge of the cup,carefully wipe the edge with absorbant tissue to remove frostand liquid, just prior to passage of the taper over the cup.NOTE 5When determining the flash point or fire point, or both, ofviscous liquids and those liquids that tend to form a surface film, thefoll
39、owing procedure is suggested: About 15 s before the taper is passedover the surface, insert the end of a stirring rod to a depth of about12 in.(15 mm) in approximately a vertical position. Move the rod fromside-to-side of the cup for three or four complete passes followingapproximately the path of t
40、he taper, remove, and make the test.NOTE 6Discontinue heating and checking flash point if the specimenboils before flashing. Record that the material has no flash point prior toboiling.9.1.8 Continue with procedure in 9.4.9.2 Flash Points from 60 to 200F (16 to 93C) (See 9.1and Notes 3-5):9.2.1 Fill
41、 the bath with cold water or water-glycol solutionto a predetermined level18 in. (3.2 mm) below the top whenthe cup is in place. The bath liquid should be at least 30F(17C) below the anticipated flash point.9.2.2 If necessary, cool a portion of the sample to at least20F (10C) below the anticipated f
42、lash point. Exercise ad-equate care to avoid contamination of the sample with coolantliquid or vapors. Fill the glass cup with the cooled sample to adepth approximately18 in. (3.2 mm) below the edge asdetermined by the leveling device, with the proper thermom-eter (see Table 1) positioned as describ
43、ed in 8.4.9.2.3 For final adjustment of the specimen level, see 9.1.5.9.2.4 Light the ignition flame and adjust it as described in9.1.4.9.2.5 Apply heat to the liquid bath and adjust so that thetemperature of the specimen increases at a rate of 2 6 0.5F (16 0.25C)/min.9.2.6 Determine the approximate
44、 flash point by passing thetaper flame across the specimen at intervals of 2F (1C) asdescribed in 9.1.7.9.2.7 Continue with procedure in 9.4.9.3 Procedure for Flash Points from 200 to 325F (93 to165C) (See 9.1 and Notes 3-5):9.3.1 Fill the bath with a high-boiling inert silicone fluid toa predetermi
45、ned level18 in. (3.2 mm) below the top when thecup is in place.9.3.2 With the appropriate thermometer (see Table 1) prop-erly positioned (8.4), fill the glass cup with sample at roomtemperature to a depth slightly more than18 in. (3.2 mm)below the edge as determined by the leveling device.9.3.3 For
46、final adjustment of the specimen level, see 9.1.5.9.3.4 Light the ignition flame and adjust it as described in9.1.4.9.3.5 Apply full heat to the liquid bath; when the tempera-ture of the specimen reaches approximately 190F (90C),adjust the heat input so that the temperature of the specimenincreases
47、at a rate of 2 60.5F (1 6 0.25C)/min.NOTE 7The heaters on some testers do not have sufficient capacity tomaintain the proper rate of heating when the temperature approaches250F (120C) or above. The heat input to the liquid bath may beincreased if necessary by using a variable transformer to increase
48、 thevoltage to the heater or by wrapping the bath with electrical heating tape.The application of suitable insulation to the outside of the bath to preventheat loss is also permissible. The important factor is to maintain the rateof temperature increase of the specimen at 2 6 0.5F (1 6 0.25C)/min.9.
49、3.6 Determine the approximate flash point by passing thetaper flame across the specimen at intervals of 2F (1C) asdescribed in 9.1.7.9.4 Determine and record not less than three test values, asfollows:9.4.1 After the initial test to determine the approximate flashpoint of the materials, repeat the procedure by cooling a freshportion of the sample, the glass cup, the bath solution, and thethermometer to more than 20F (10C) below the approximateflash point. When the temperature of the specim
