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    10 - STD Test Methods For Flash-Point by Pensky-Martens Closed

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    Gian Sanchez

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    © All Rights Reserved
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    334 diy Designation: D 93 - 97 IP® designation: b 34/88 METHODS OF SAMPLING AND TESTING 1 Standard Test Methods for Flash-Point by Pensky-Martens Closed Cup Tester? “his standard issued under the fa dsaton 19; the number mma folowing the designation indicates he yea of corsa adoption onthe cate of vision, the year fast sso, A number an parealhess dean the ear ast respyeval A Sopcrenp ean (fades an edo ange since the last evs ar eapva “This tot method has boon approved for we by agencies ofthe Departs of Befose. Caran the DoD Index of Speclastons and ‘Standards forthe specfe year of lsue which has been adopted By the Departmen of Dafense INTRODUCTION This flash point test method is a dynamic test method and depends on definite rates of ‘temperature increases to control the precision of the test method. The rate of heating may not in all cases give the precision quoted in the test method because of the low thermal conductivity of cercain materials, To improve the prediction of flammability, Test Method D 3941, an equilibrium, method, was developed in which the heating rate is slower. This allows the vapor above the test. specimen and the test specimen to be at about the same temperature. If your specification requires Test Method D93, do not substitute Test Method D 3941 or any other test method without obtaining comparative data and agreement from the specifier. This test method contains two procedures: Procedure A for fuel oils, lubricating oils, and other homogeneous liquids, and Procedure B for nonhomogeneous materials which are mixturcs of liquids with solids, liquids that tend to form a surface film under test conditions or are liquids with a kinematic viseosity which is not capable of uniform heating under the stirring and heating conditions of Procedure A, Procedure B provides a reduced heating rate and an increased stirring talc to improve thermal equilibrium, 1. Scope 1.1 This test method covers the determination of the flash point of petroleum products in the temperature range from 40 to 360°C by a manual Pensky-Martens closed-cup appa- ratus or an automated Pensky-Martens clasxl-cup appa- ratus. Note 1—Flash point determination as above 250°C can be per- formed, however, the precisions have not been delermined above this temperature. 1.2 ‘This test method is applicable to fuel oils, lube oils, liquids with suspensions of solids, liquids that tend to form a surface film under test conditions, and other liquids with viscosities of 5.5 mm 2/s (5.5 cSt) or more at 40°C (104°F). Nore 2—Liquids having kinematic viscosities less than 5,5 mm 2/s (6St) at 40°C (104°F), do not coniain suspended solids, or do not have a tendency to form a surface film while wador (eat conditions, can be tested in accordance with Test Method D 56, 1.3 This test method is applicable for the detection of contamination of relatively nonvolatile or nonflammable materials with volatile or flammable materials, "These test methods are under the joint inssction of ASIM Commitee D-2 ‘on Petroleum Products and Lubricants and are the diet respousibilty of ‘Subcommittee 02,08 on Volatility. Inthe I, these test methods sre der the jurisdiction of the Standardization Commits. ‘Current dition approved July 10, 1997, Published October 1997. Originally published as 98-21 T, Last previews edition DS = 96, 1.4 The values stated in ST units shall be regarded a sandard. The values given in parentheses are provide fi information only. 1.5 This standard does not purport to address all ofl safely concerns, if any, associated with its use. It is responsibility of the user of this standard to establish ase priate safety and health practices and determine the apis bility of regulatory limitations prior to use. For spoih hazards statements, sec Notes 3, 4,9, 11, 13, 14, 18,20, 2, 24, 25, 26, 28, and 29. 2. Referenced Documents 2.1 ASTM Standards: D56 Test Methods for Flash Point by Tag Closed Test 13941 Test Method for Flash Point by the Equilibria) Method with a Closed-Cup Apparatus? 4057 Practice for Manual Sampling for Petroleun a Petroleum Products* D417? Practice for Automatic Sampling of Petroleum: Petroleum Products* E | Specification for ASTM Thermometers? E 300 Practice for Sampling Industrial Chemical 2 Anant Book of AST Standards, Yol05.01. 8 Annual Book of ASTH Standards, Vol 06.01 + Annual Book of ASTI Standards, Vol 05.02. 3 Aral Book of ASTI Standards, Vol 14.03, © Annual Book of ASTM Standards, Vol 15.05. 22 180 Standards? Guide 34 Quality Systems Guidelines for the Production of Reference Materials Guide 35 Certification of Referen and Statistical Principles Material—General 4, erminology 4 Definitions: 41 flash point, n—in petrolewn products, the lowest temperature corrected to a barometric pressure of 101.3 kPa (160 mm Hg), at which application of an ignition source caus the vapors of a specimen of the sample to ignite under sociied conditions of test. LL. Discussion—The test specimen is deemed to have fibed when 2 flame appears and instantaneously propa- tus itself over the entire surface of the test specimen. 4.1.2 Discussion—When the ignition source is a test fine, he application of the test flame may cause a uc halo van enlarged flame prior to the actual flash point, This is tota fash point and shall be ignored 412 dynamic, adj—in petroleum products—the condi- ton where the vapor above the test specimen and the test ‘preimen are not in temperature equilibrium at the time that tteignition source is applied. 3121 Discussion—This is primarily caused by the rating of the test specimen at the constant preseribed rate vith the vapor temperature lagging behind the test specimen fenperature. 413 equilitrium, n—in petroleum products—the condi- ‘ca where the vapor above the test specimen and the test fprimen are at the same temperature at the time the igition source is applied. 313.1 Discussion—This condition may not be fully uhieved in practice, since the temperature may not be uniform throughout the test specimen, and the test cover and shutter on the apparatus can be cooler. 4, Summary of Test Method 41 A TSemL test specimen is heated at a slow constant fale with continual stirring in a brass test cup of specified simensions with a cover of specified dimensions. An ignition source is directed into the test cup at regular intervals with Suultaneous interruption of the stirring. The Mash point is the lowest liquid temperature at which application of the ignition source causes the vapor of the test specimen of the sample to ignite, §, Signfieanoy and Use 5.1 Whe flash point temperature is one measure of the tendency of the test specimen to form a flammable mixture with air under controlled laboratory conditions. It is only one of a number of propertics which must be considered in sessing the overall flammability hazard of a material, 52 Flash point is used in shipping and safety regulations to define lanwmable and combustible materials. One should consult the particular regulation involved for precise defi tions ofthese classifications. "vale from American National tasdands Insitute, 11 W. 42nd St, 13th Four, New York, NY 10036, ~ 1 METHODS OF SAMPLING AND TESTING 335 4) p93 Nore 3—The US, Department of Trunsportation (DOT) and U.S, Department of Lahor (OSHA) have established that iquids with a flash point under 37.8°C (100°F) are flammable, as determined by this test ‘method, for those liquids which have a kinematic viscosity of 5.8 mm 2/s (cSt) or more at 37.8°C oF 9.5 mam 2/s (eSi) or more at 25°C (77°F), ‘or that contain suspended sald, or have a tendency to form a surface film while under test. Other classification flash points have been establised by diese departments for Hiquids using this test method. 5.3 This test method should be used to measure and describe the properties of materials, products, or assemblies in response to heat and an ignition source under controlled laboratory conditions and should not be used to deseribe or ‘appraise the fire hazard or fire risk of materials, products, or assemblies under actual fire conditions. However, results of this test method may be used as elements of a fire risk assessment which takes into account all of the factors which are pertinent to an assessment of the fire hazard of a particular end use. 5.4 This test method provides the only closed cup flash point test procedures for temperaturcs up to 370°C (698°F). 6. Apparatus .1 Bensky-Martens Closed Cup Apparatus (manual) — This apparatus consists of the test cup, test cover and shutter, stirring device, heating source, ignition source device, air bath, and top plate described in detail in Annex Al. ‘The assembled manual apparatus, test cup, lest cup cover, and. test cup assembly are illustrated in Jigs, Al.1, A1.2, A1.3, and AL.4, respectively. Dimensions are listed respectively. 6.2 Pensky-Mantens Closed Cup Apparatus (automated) — ‘This apparatus is an automated flash point instrument that is, capable of performing the test in accordance with Scetion 1, Procedure A, and Section 12, Procedure B, of this test method. The apparatus shall use the test cup, test cover and shutter, stirring device, Leating source, and ignition source device deseribed in detail in Annex Al 6.3 Temperature Measuring Device—Is « thermometer having a range as shown as follows and conforming to the requirements prescribed in Specification 1 or in Annex A3, or an electronic temperature measuring device, such as resistance thermometers or thermocouples. The device shall exhibit the same temperature response as the mercury thermometers. “Thermometer Nermber Tempecatune Range ASTM iP ~St0+110'C 9c lsc (20 102301 oy “19 1 200 BBC oc (50 103921 (any 490 16 310 100 16C (200 to 70°F) (io 6.4 Ignition Source—Natural gas flame, bottled gas flame, and electric ignitors (hot wire) have been found acceptable for use as the ignition source, The gas flame device described in detailed in Fig, A1.4 requires the use of the pilot flame described in A1.1.2.3. ‘The electric ignitors shall be of the hot-wire type and shall position the heated section of the ' Frinformation on US, Department of Transportation regulations roe Coder ‘of WS, Regulations 49 CER Chapler 1 aad the US, Deparment of Labor, se 29 (CER Chapter XVI, Each of thee ies is revised annul and may be procured fiom the Superintendent of Dociments, Goverament Printing Olfce, ‘Washington, DC 20402. 336 METHODS OF SAMPLING AND TESTING TH qh p93 ignitor in the aperture of the test cover in the same manner as the gas flame device. Note 4: Wamiag—Gas pressore supplied to the apparatus should not be allowed to exceed 300 mm (11.8 in.) of waler presire 7. Reagents and Materials 7.1. Cleaning Solvents—Use suitable solvent capable of cleaning out the specimen from the test cup and drying the test cup and cover. Some commonly used solvents arc toluene and acetone. Note 5: Waming—Toluene, acetone, and many solvents are fam= mable and « health hazard, Dispose of solvents and waste material ia ‘accordance with local regulations, 8. Sampling 8.1 Obtain a sample in accordance with instructions given in Practices D 4057, D 4177, or E 300. 8.2 At least 75 mL of sample is required for each test, Refer to Practice D 4057. 8.3 Erroneously high flash points may be obtained if Precautions are not taken 10 avoid the loss of volatile material. Do not open containers unnecessarily, to prevent Joss of volatile material or possible introduction of moisture, or both, Do not make a transfer unless the sample tempera. ture is at least the equivalent of 18°C or 32°F below the expected flash point. When possible, flash point shall be the first test performed on a sample and the sample shall be stored at or below room temperature. Nore 6—Typically when the sume sample is Wo be used for vapor pressure analysis, the vapor pressuie specimen is obtained first 84 Do not store samples in plastic (polyethylene, polypropylene, etc.) containers, since volatile material may diffuse through the walls of the enclosure. Samples in leaky containers are suspect and not a source of valid resulls, 8.5 Samples of very viscous materials can be warmed until they are reasonably fluid before they are transferred: how ever, no sample shall be heated more than is absolutely ‘necessary. The sample shall not be heated and transferred unless its temperatures is mose than 18°C or 32°F below its expected flash point. When the sample has been heated above this temperature, allow the sample to cool until its temperature is at least 18°C or 32°F helow the expected flash point before transferring. Nore 7—Yolatte vanors can eseape during heating when the sample conlainer is not properly sealed 8.6 Samples containing dissolved or free water may be dehydrated with calcium chloride or by filtering through a qualitative filter paper or a loose plug of dry absorbent cotton. Warming the eample is permitted, but it shall not be heated for prolonged periods or greater than a temperature of 18°C 32°F below its expected flash point, Note 8—If the sample is suspected of containing volatile gontam: ‘nants, the tealment described in 8.5 and 8.6 should be omitted 9, Preparation of Apparatus 9.1 Support the manual or automated apparatus on a level steady table, 9.2 Tests are to be performed in a drafl-free room or Compartment, Tests made in a laboratory hood or in any location where drafts occur are not reliable. Note 9—A shiea, ofthe epprovimate dimensions 460 ma i stuare and 610 sam (24 i.) high, or other suitable dimen hving an open front is recommended to prevent dra fo dl the vapors above the tos cup. Note 10—With sou samples whose vapors or products fp ar objectionable, itis rermissble to place te appari ag ay sft shield ina venation hood, the daft of whith is adjust ‘eposs can be withdrawa without causing air curent over tan during the inition sours application peti. 9.3 Prepare the manual apparatus or the automalid apparatus for operation in accordance with the mamufactit ers instructions for calibrating, checking, and operat ing th equipment, Nore 4: Warning —Gas pressure should rot be allowed wel 300 mm (11.8 in.) of water pressure, 9.4 Thoroughly clean and dry all parts of the test cupsif its acoessories before starting the test, to ensure-the ronoa of any solvent which had been used to clean the appara Nore 12—Use suitable solvent capable of removing al ct specimen from the tet cup and dying the tet cup and eater Se Commonly used solvents are toluene and noctone, Nore 13: Waming—Tolueac, acetone, and many sevens ep tube, Health hard, Dispose of solvents aad. waste mate accordance with local regulations ; 10. Calibration and Standardization : 10.1 Adjust the automated flash point detection sygea (when used) in accordance with the manufacturer's int | tions, 10.2. Calibrate the temperature measuring device in ace dance with the manufacturer's instructions, 10.3. Verify the performance of the manual appacatus the automated apparatus at least once per year by dete mining the flash point of a certified reference muleit (CRM) such as those listed in Annex A4, which is reasouh close to the expected temperature range of the samples ile tested. The material shall be tested according to Proosdur 4 of this test method and the observed flash point obtanedia 11.1.8 oF 11.2.4 shall be corrected for barometric prsue (see Section 13), The flash point obtained shall be within the limits stated in Table 44.1 for the identified CRM or wit the limits calculated for an unlisted CRM (see Annex Ai) {0.4 Once the performance of the apparatus has bir Verified, the flash point of secondary working standats (SWSs) can be determined along with their control limis These secondary materials can then be utilized for nue frequent performance checks (see Annex Ad), Nore 14—The fash point temperature of 1,4-dimethylbenzeas ie relatively low temperaturz and may not allow the specified rf ‘heating to be achieved. Cooling the material to the specified spin {nsertion temperature may cave the material to erysalize, Ie aso Coordinating Commitee cn Flash Point isin the proces of deri rote suitable calibration fds 19.5 When the flash point obtained is not within te fimits stated in 10.3 or 10.4, check the condition ani operation of the apparatus to ensure conformity with th details listed in Annex A1, especially with regard to tghtoss of the lid (A1.1.2.2), the action of the shutter, the positin af the ignition source (A1.1.2.3), and the angle and position the temperature measuring device (ALL1.2.4). ‘After i) adjustment, repeat the test in 10.3 using a fresh ler specimen, with special attention to the procedural detat prescribed in this test method. Tm ‘METUODS OF SAMPLING AND TESTING 337 Il Procedure Ld Manual Apparatus: {LJ Fill the test cup with the test specimen to the filling ‘tikinsde of the test cup. The temperature of the test cup ‘nittst specimen shall be at least. 18°C or 32°F below the gee flash point. If too much test specimen has been iid othe test cap, remove the excess using a syringe or ina device for withdrawal of fluid. Place the test cover on ite cup and place the assembly into the apparatus. Be ‘atte locating or locking device is properly engaged. Insert lrlemperature measuring device into its holder. IL..2 Light the test flame, and adjust it to a diameter of ‘Mito 48 mm (0.126 to 0.189 in,), or switch on the electric iniks and adjust the intensity in accordance with the ‘inuteturer’s instructions. An 15: Warning—Gas pressure should not he allowed to exceed lite (900 mm) of water pressure. Nae 16; Coution—Exercise care when using 2 gas test flame, If it ‘Sulibe extinguished it will not ignite the vapors in the test cup, and Beefs te et ame that then exes the vapor spe can inne rei Note 17: Warning—The operator should exercise and take appro- fiat sty precautions during the initial application of the ignition fur, ne text specimens containing lowlash material can glve an. itosmaly srong fash when the ignition source is first applied. ore 18: Warning—The operator should exercise and take appro- fia: slay procautons during the performance of this test method. Temperatures attained during this test method, up to 370°C (697), st ouidered hazardous. 1113 Apply the heat at such a rate that the temperature, indicated by the temperature measuring device, increases Sio6°C 0 to L1"FY/min. UL4 Turn the stirring device at $0 to 120 rpm, stirring itsdownward direction, Nit 19: Caution —Meticulous attention o all details relating tothe Ipion source, size of test flame of intensity ofthe electric ignitor, rate dleapetare increase, and rate of dipping le ignition source into the cathe tet specimen is desirable for geod results LS Application of Ignition Source: 11.5.1 If the test specimen is expected to have a flash Pont of 110°C or 230°F or below, apply the ignition source en the temperature of the test specimen is 23 # S°C or 41 EJF below the expected flash point and each time iheefler ata temperature reading that is a multiple of °C «PF, Discontinue the stirring of the test specimen and ‘oply the ignition source by operating the mechanism on the tel cover which controls the shutter so that the ignition source is lowered into the vapor space of the test cup in 0.5 s, Ith in its lowered position for 1's, and quickly raised to its Upward position. 1115.2 If the test specimen is expected to have a flash poi above {10°C or 230°F, apply the ignition source in the thaner described in 11.1.5.1 at each temperature increase of 2Cor StF, beginning at a temperature of 23 + 5°C or 41 JF below the expected flash point. 11.6 When testing materials to determine if volatile mafsial contamination is present, it is not necessary to qh p93 | ROCEDURE, A—DETERMINATION OF FLASH POINT OF FUEL OILS, LUBRICATING OILS AND OTHER HOMOGENEOUS LIQUIDS (sce Introduction) adhere to the temperature limits for initial ignition source application as stated in 11.1.5, 11.1.7 When testing materials where the expected flash point temperature is not known, bring the material to be ‘ested and the tester to a temperature of 15 S°C or 60 + 10°F, When the material is known to be very viscous at this temperature, heat the specimen to a starting temperature as described in’ 8.5. Apply the ignition source, in the manner described ia 11.1.5.1, beginning at least 5°C or 10°F higher than the starting temperature, Nore 20—Flash Point results determined in an “uakzown expected flash point mode” should be considered approximate. This value can be used asthe expected flash point when a fresh specimen i tested in the standard mode of operation 11.1.8 Record as the observed flash point the reading on the temperature measuring device at the time ignition source application causes a distinct ‘lash in the interior of the test, cup. Nore 21~The sample is deemed to have flashed when a large Name appears and instantancously propagates itself over the ertire surface of the test specimen. 11.1.9 When the ignition source is a test flame, the application of the test flame may cause a blue halo or an enlarged lame prior to the actual flash point, This is not a flash and shall be ignored. I1L1.10 When a flash point is detected on the first application, the test shall be discontinued, the result dis- carded, and the test repeated with a fresh test specimen, The first application of the ignition source with the fresh test specimen shall be 23 + 5°C or 41 + 9°F below the ‘temperature at which a flash point was detected on the first application, 111,11 When a flash point is detected at a temperature which is greater than 28°C or 50°F above the temperature of the first application of the ignition source, or when a flash point is detected at a temperature which is less than 18°C or 32°F abow: the temperature of the first application of the ignition source, the result shall be considered approximate, and the test repeated with a fresh test specimen. Adjust the expected flash point for this next test to the temperature of the approximate result. The first application of the ignition souroe with the fresh test specimen shall be 23 45°C or 41 + SF below the temperature at which the approximate result was found. 111.12 When the apparatus has cooled down to a safe handling temperature, less than 55°C (130°F), remove the test cover and the test cup and clean the apparatus as recommended by the manufecturer. Nove 22—Exercise care when cleaning and positioning the lid assembly #0 not to damage or dislocate the flash detection system or temperature measuring device. Set the manufacturer's instructions for proper care and maintenance, 11.2 Automated Apparatus: 11.2.1 The automated apparatus shall be capable of performing the procedure as described in 11.1, including 338, METHODS OF SAMPLING AND TESTING Th qh p93 control of the heating rate, stirring of the test specimen, application of the ignition source, detection of the flash point, and recording the flash point. 11.2.2. Fill the test cup with the test specimen to the filling mark inside of the test cup. The temperature of the test cup and test specimen shall be at least 18°C or 32°F below the expected flash point, If too much test specimen has been added to the test cup, remove the excess using a syringe or similar device for withdrawal of fluid. Place the test cover on the test cup and place the assembly into the apparatus. Be sure the locating or locking device is properly engaged, Insert the temperature measuring device into its holder 11.2.3 Light the test flame, when necessary, and adju toa diameter of 3.2 to 4.8 mm (0.126 to 0.189 in). Nori 23: Waming—Gas pressure should not be allowed tem! 40 kPa (300 mun) of water pressure, ‘Nove 24: Caution—Biercise care when using a gas tet fae should be extinguished it will not ignite the vapors in the tes cps ‘the gas for the test lame that then enters the Vspor space cad the result, Nore 25: Warning—The operator should exercise und te priate safety precautions during the initial application of the igi source, since test specimens containing low-flath material my um abnormally strang flash when the ignition souroe is first appli Nore 26: Warning—The operator should cxercisa and i we plate safety precautions doring the performance of this tes we ‘The temperatures attained during this test method, up to 370A are considered hazardous, 11.2.4 Start the automated apparatus in accordant the manufacturer's instructions. ‘The apparatus shill i the procedural details described in 11.1.3 through 118 PROCEDURE B—DETERMINATION OF FLASH POINT OF LIQUIDS THAT TEND TO FORM A SURFAG FILM, LIQUIDS WITH SUSPENSIONS OF SOLIDS AND NON-HOMOGENEOUS LIQUIDS (see Introductin) 12. Procedure 12.1 Manual Apparatus: 12.1.1 Fill the test cup with the test specimen to the filling ‘mark inside of the test cup. The temperature of the test cup and test specimen shall be at least 18°C or 32°F below the expected flash point. If too much test specimen has been added to the test cup, remove the excess using a syringe or similar device for withdrawal of fluid, Place the test cover on the test cup and place the assembly into the apparatus. Be sure the locating or locking device is properly engaged. Insert the temperature measuring deviee into its holder. 12.1.2 Light the test flame and adjust it to a diameter of 3.2 to 4.8 mm (0,126 to 0.189 in.), of switch on the electric igniter and adjust the intensity in accordance with the ‘manufacturer's instructions Nore 27: Warning—Gas pressare should nat be allowed to exceed 40 kPa (300 mm) of water pressur: Nore 28: Caution—Exercise care when using a gas test flame. If it should be extinguished it will not ignite the vapors in the test cup and de gas for the test flume that then enters the vapor space ean influence the result Nore 29: Waming—The operstor should excreise and take appro- priate safery precautions during the initial application of the ignition Souter, since test specimens contaning loveflash material may give an abnormally strong flash sshien the ignition source is first applied, Nore 30: Warning—The operztor should exercise and take anpro- priate safety precautions during the performance of this test method. ‘The temperatures sttained during this test method, up to 370°C (698°F), are considered hazardous. 12.1.3 Turn the stirring device at 250 -+ 10 rpm, stirring in a downward direction. 12.1.4 Apply the heat at such a rate that the temperature as indicated by the temperature measuring device increases 1 to LSC (2 to 3°F)/min, 12.1.5 Proceed as prescribed in Section 11, with the exception of the preceding requirements for rates of stirring and heating. 12.2 Automated Apparatus 12.2.1 The automated apparatus shall be capable of performing the procedure 2¢ described in 12.1, including control of the heating rate, stirring of the test specimen, application of the ignition’ source, detection of the flash point, and recording the flash point. 12.2.2 Fill the test cup with the test specimen to the fll) mark inside of the test cup, The temperature of the ts and test specimen shall be at least 18°C or 32°F belort expected flash point. If too much test specimen tas added to the test cup, remove the excess using a syne similar device for withdrawal of fluid. Place the test cov the test cup and place the assembly into the apparatus!) sure the locating or locking device is properly engaged ‘the temperature measuring device into its holder. 12.2.3 Light the test flame, when necessary, and adi toa diameter of 3.2 t0 4.8 mm (0.126 to 0.189 in), Nore 3: Warning—Cas pressure should rot be allowed 16 40 kPa (300 mu) of water pressure, Norn 32: Caution Txersise care when usiag a gas test ena shouldbe extinguished it will not ignite the vapors in the ts a ‘ths eas forthe test flame that then enters the vapor space can the result ‘Nore 33: Warning —The operator should exercise and tale pate safety precautions during the initial application af tbe source, since lest specimens containing low-flash material can pt atmarmally strong flash when the ignition souioe is frst appli Nore 34: Warning—The operator should exercise and tak palate safety precautions during the performance of this tt mh ‘The temperatures attained during this test method, upto 370C (6 are considered hazardous, 12.2.4 Start the automated apparatus in accordance’ the manufacturer's instructions. The apparatus shall il the provodural details in accordance with 12.1.3 thn. 1215. 13. Caleulation 13.1 Observe and record the ambient barometric pest (See Note 30) at the time of the test. When the pra’ differs from 101.3 kPa (760 mm He), correct the flash pi as follows: Corrected fash poitt = C+ 0.28 (1013 — K) w CConrct fish point F 4 0106 160 7) a (Corrected fash pot = C+ 0.033 (160 — P) oy where: C= observed flash point, A 5G; ‘observed flash point, "F, Je ambient barometric pressure, mm Hp, and {ambient barometric pressure, kPa Nov: 35The barometric pressure used in this calculation isthe ‘a pressure fr the laboratory atthe tne of the tet, Many aneroid Suman, such as those sed at weather stations and airports, are Janeted to give za level readings and would vot give the corect ‘ego ns te. 132 When the ambient barometric pressure. is bdow i013 kPa (760 mm), round up the corrected flash point to the nearest 0.5°C (1°F) and record. When the ambient fatometric pressure is above 101.3 kPa (760 mm), round ‘town the corrected flash point to the nearest 05°C and “record, 1, Report \4 Report the corrected flash point as the ASTM D§3-IP 34, Procedure A or Procedure B Pensky-Marens Closed Cup Flash Point of the test specimen. 18, Precision and Bias 15.1 Precision—Procedtire A—The precision of this pro- tulure as determined by the statistical examination of the inedaboratory test results, is as follows: I5L1 Repeatahilty—The difference berween successive twalts, obtained by the same operator with the 81 :qmius under cmstant operating conditions on identical ist material, would in the long run, in the normal and sunect operation of the test method, exceed the Following valocs incase in 20. 1 24x, cy A =0.035, X = reported result in ‘C, and 1 = repeatability 15.12 Reproducibility —The difference between two single aad independent results, obtained by different operators sotking in different laboratories on identical material, would inthe long run, in the normal and correct operation of the ‘st method, exceed the following values anly in { ease in 20, R =BK, o B = 0.078, X= reported result in “C, and R ~ reproducibility 15.3 Bias—Since there is no accepted reference material sulable for determining the bias for the procedure in this test nathod, bias has not been determined, 1514 Relative Bias—Statistical evaluation of the data ‘6 not detect any significant difference between the repro- tacibility variances of manual and automated Pensky- Miarens fash point results for the samples studied. Evalua- ton of the data did not detect any significant difference 1 METHODS OF SAMPLING AND TESTING 339 qh p93 between averages of manual and automated Pensky-Martens flash point for the samples studied with the exception of cycle oil and fuel oil which showed some bias. In any case of dispute, the manual procedure shall be considered the referee test, Nore 36—The prevision statements were derived on clear tiguids only. Refer to the eseaech report for information regarding relative bias and types of samples, Additional stadies are in progres concerning relative bias 15.1.5 ‘The precision date were developed in a 1991 cooperative test program’ using $ samples of fucl and lubricating oils, Twelve laboratories participated with the manual apparatus and 21 laboratories participated with the automated equipment. The apparatus used either a pas test fame or an electric resistance (hot wire) device for the ignition source, Information on the type of samples and their average flash point are in the research report available at ASTM Headquarters. Request RR:1D02-1008, 15.2 Precision—Provedure B—The precision of this pro- cedure as determined by the statistical examination of the interlaboratory test results, is as follows: 15.2.1 Repeatability—The difference between successive results obtained by the same operator with the same appa. ratus under constant operating conditions on identical test materials would, in the long run, in the normal and correct, operation of the test method, exceed the following value in 1 ase in 20: Repeatability 15.2.2 Reproducibility—The difference between two single and independent results obtained by different opera. tors working in different latoratories on identical material ‘would, in the long run, exceed the following value only in 1 cease in 20 SCOP) Repmducibitity we usr) 15.2.3. Bias—Since there is no accepted reference material suitable for determining the bias for the procedure in this test method, bias has not been determined, 15.2.4 The precision data for Procedure B is not known to have been developed in accordance with RR:D02-1007. Nore 97—Procedure B was not tested in the 1991 interlaboratory program, Committee D-2 intends to conduct an intesiaboratory test utiiring Procedure B. 16. Keywords 16.1 aulomated flash point; automated Pensky-Martens closed cup; flammability; flash point; Pensky-Martens closed cup “The resus of the 1991 interiaboratory cooperative text program are ave liom ASTM Headquarters, Request ASTM RR:DO2 ~ 1008, 340 qh > ANNEXES (Mandatory Information) Al. APPARATUS SPECIFICATIONS Al. A typical assembly of the apparatus, gas heated, is shown in Fig. Al.1. The apparatus shall consist of a test cup, cover, and stove conforming to the following requirements: Por METHODS OF SAMPLING AND TESTING ue 93 AL.L1 Cup—The cup shall be of brass, or nonrusting metal of equivalent heat conductivity, and sl conform to the dimensional requirements in Fig, Al.2, smurteR nawout fo>TiowAL Ist nO" Tie eer ci SuRRES Dal¥E FLENOGE gar Ia €¥ DRE S@TIONAL) —— —— fh HS. Fame eros peace SEES es A & aegis eee B c | rest eur lawanael gf F wan twicewess — ven cuP anes TenetaL eunmouncins ee ree mm 9) i wemen reawe-rype * | a7 [S16 | @x7e | om Oe ezernit neglsrance 8 | aioe | 400 | (x5 | (ae “ise Fane Fre Sach | “ise | “ate | (aoe | ora >| a |e | daa, | Om & | sris | sree | easy | f ee | | Gas [No1e—Lis asso can be postoned ether right or handed, FIG. A1.1 Ponsky-Martens Closod Flesh Taster 1 METHODS OF SAMPLING AND TESTING 341 dh ps3 Jv am ™ nin oo ae 7 780 798 nn eta) 8 0 (o0H Ca ¢ 28 a6 (ot) ig, ° aire 21.86 (85s) (0.800) € 4547 4572 (1.790) (800) F 5072 50.85 (1997) @ 009) 6 58.75 56.00 (2195) (205) N 38. 40 (025) (or) ' 5390 seme (212) azn 4 228 2.54 0.090) (0.100) FIG. A12 Tost Cup Tange shall be equipped with devices for locating the position of the cup in the stove, A handle attached to the fange of the cup is a desirable accessory. ‘The handle shall not be 0 heevy as to tip over the empty cup. ALL2 Cover: ALI21 Cover Proper—The cover shown in Fig. A1.3 shall be of brass (A1.1.1) and shall have a rim_ projecting, downward almost to the Mange of the cup. The rim shall fit the outside of the cup with a clearance not exceeding 0.36 rm (0.014 in.) on the diameter, There shall be a locating or locking device, or both, engaging with a corresponding device on the cup. The four openings in the cover, 4, B, C, and D, are shown in Fig. A1.3. The upper edge of the cup shall fe in close contact with the inner face of the cover throughout is circumference. ALL2.2 Shutter—The cover shall be equipped with a bass Gection 3) shutter (Fig. A1.4), approximately 2.4 mm (Jn in) thick, operating on the plane of the upper surface of the cover. The shutter shall he so shaped and mounted that it tolates on the axis of the horizontal center of the cover between two stops, so placed, that when in one extreme postion, the openings A, B, and C in the cover are ~ cl wo oH a wi (ra o 127 135 (040) (059) c 40 36 ig) (0.22) F 135 43 (053) (058) s 28 2 (028) on H 12 20 (0.05) (08) V 73 (oa) Ca a yaar row (4a) (0.488) k 1638 1868 (Osi) (0.656) L 18.85 19.45 orm (0.700) FIG, A1.8 Cover Proper completely closed, and when in the other extreme position, these openings are completely opened, The mechanism operating the shutter should be of the spring type and constructed so that when at rest the shutter shall exactly close the three openings. When operated to the other extreme, the three cover openings shall be exactly open and the tip of the exposure tube shall be fully depressed. ALL2.3 Flame-ignition Device—The fame-ignition de- vice (Fig. A1.4) shall have a tip with an opening 0.69 to 0.79 mm (0.027 to 0.031 in.) in diameter. This tip shall be made preferably of stainless steel, although it may be fabricated of other suitable metals. The flame-exposure device shall be equipped with an operating mechanism which, when the shutter is in the open position, depresses the tip so that the center of the orifice is between the planes of the under and upper surfaces of the cover proper at a point on a radius passing through the center of the larger opening A (Fig. AL.3}, An electric ignitor is also suitable. The electric ignitors shall be of the electric resistance (hot-wire) type and shall position the heated section of the ignitor in the aperture of the test cover in the same manner as the gas flame device. AL124 Pilot Flame—A pilot flamo shell be provided for automatic relighting of the exposure flame. A bead 4 mm (42 in.) in diameter can be mounted on the cover so that the size of the test flame can be regulated by comparison, The tip 342, METHODS OF SAMPLING AND TESTING 1 qh vos ME GTN Ef SHUTTER TEST LP — mm " ma (ay ra a 103 198 wry (078) B 230 18 (009) (0.125) c 18 Ba (030) (oa) 2 20 28 (008) (011) E os9 o7a (o027) (0.001) F 20 26 (008) on 6 ee 104 (025) (oa) H 38 112 (038) (0.42) i 430 400 (189) 8) 4 500 516. 97) 2.03) k 0.36 wy foo) L ize 206 toa) {o.08) M ot aa (225) (175) N 78. 34 (030) (233) “Includes toleance fr length of thermemeter given In Spaciioaton F 1 FIG. 14 Test Cup and Cover Assembly of the pilot fame shall have an opening the same size as the tip of the flame exposure device (0,69 to 0.79 mm (0.027 to 0.031 in.) in diameter) AL.1.2.5 Stirring Device—The cover shall be equipped with a stirring device (Fig. A1.4) mounted in the center of the cover and carrying two 2-bladed metal propellers. In Fig. 1.4 lower propeller is lesigmated by the letters L, M, and N. This propeller shall measure approximately 38 mm from tip to tip, with each of its two blades 8 mm in width with a pitch of 45°, The upper propeller is designated by the letters 4, C, and G. This propeller measures approximately 19 mm, tipty tip, each of its two blades is also 8 mm in width with a pth of 45°, Both propellers are located on the stirrer shaft in such 4 manner that, when viewed from the bottom of the sine, the blades of one propeller are at 0 and 180° while the blats of the other propeller are at 90 and 270°. A stirrer shaft may be coupled to the motor by a flexible shaft or a suitable arrangement of pulleys. 1.1.2.6 Stove—Heat shall be supplied to the cup by ‘means of a properly designed stove which is equivalent to 133 METHODS OF SAMPLING AND TESTING M3 ab pes sirbath. The stove shall consist of an air bath and a top plate ‘wvhich the flange of the cup rests. ALL27 Air Bath—The air bath shall have a cylindrical inlrior and shall conform to the dimensional requirements in Fig, ALJ. The air bath may be either a flame or thetrically heated metal casting (A1.1.2.8), or an electric~ mitance element (A1.1.2.9). In either ease, the air bath ‘must be suitable for use at the temperatures to which it will besubjected without deformation. ALL28 Heater, Flame or Flectric—If the hecting ele- rent is a flame or an electric heater, it shall be so designed tnd used that the temperatures of the bottom and the walls te approximately the same. In order that the air bath intemal surfaces should be at a uniform tmperature, it ‘Gould not be less than 6.4 mm (¥/4 in.) in thickness unless ite heating cloment is designed to give equal heat flux densities over all the wall and bottom surfaces. ALL.29 Heater, Bleciric Resistance the heater is of the electric resistance type, it shall be constructed so that all parts of the interior surface are heated uniformly. The wall and bottom of the air bath shall not be less than 6.4 mm (/+ in.) in thickness unless the resistance heating elements are distributed over at least 80 % of the wall and all the bottom of the air bath. A heater having such a distribution of the heating elements positioned at least 4.0 mm ($42 in.) away from the internal surface of the heating unit can be used in conjunction with a minimum thickness of 1,58 mm (ie in.) for the wall and bottom of the air bath, ‘AL.1.2.10 Top Plate—The top plate shall be of metal, and shall be mounted with an air gap between it and the air bath, It may be attached to the air bath by means of three screws and spacing bushings, The bushings should be of proper thickness to define an air gap of 4.8 mim (Ye in.), and they shall be not more than 9.5 mm (% in.) in diameter 34 METHODS OF SAMPLING AND TESTING 13 Gb pes ; A2, MANUFACTURING STANDARDIZATION OF THERMOMETER AND FERRULE A2.1 ‘The low-range thermometer, which conforms also to the specification for the cup thermometer in the tag closed tester (Test Method D 56) and which frequently is fitted with a metal ferrule intended to fit the collar on the cover of the tag flash tester, can be supplemented by an adapter (Fig. ‘A2.1) to be used in the larger diameter collar of the Pensky- Martens apparatus, Differences in dimensions of these col- CLAMP NUT tars, which do not affect test results, are a sour d unnecessary trouble 10 manufacturers and suppliers oli. struments, as well as 10 users. 2.2 Dimensional requirements are shown in Fig. All Conformity to these requirements is not mandatory, biti desirable to users as well as supplicrs of Pensky-Mare ‘testers. __ Seam NUT-STAINLESS STECL Houne raweay [ek packine nines | SOFT ALUMINIUM /- ser FERRULE STAINLESS STEEL 7 mm cr rin ima ‘ey ra x 620 650 (0244) 10256) B 170 180 (sn or) © 9.80 9.85 (0388) (0.388) ° 1219 s224 (0.420) (0.482) E 140 105 (0.055) {o.005) FE 356 eat (0.87) (0.008) 6 124 130 (0.49) (057) 4 8.56 861 (o.sa7 (0.08) t 84 86 (0.92) (034) 4 99 107, (0.39) (a2) « roy 880 240) os, L 51 58 joo) (22) M 179 175 1067) (0.65) N ara 262 1.06) Gy ° 71 7316 (0.280) (0.262) P ira 278 (0.383) (0.365) FIG. A21 Dimensions for Thermometer Adapter, Ferrule, and Packing Ring 17 MICEHODS OF SAMPLING AND TESTING 345 4h v93 A3. THERMOMETER SPECIFICATIONS ‘TABLE Ad.1_ IP Thermometer Specifications Tho stem shall be mad with an enlargement having aclamater of 1.5 1 2.0 mm feng 40 68 mr trom the bottom ofthe bulb. These clmenslons sll be measured with or than te stom anes feng oo 8 mm, the bot oF bw enkryement test yage shown in Fig. Rt. % PSC Pa Pie Pons Marton Law Ponsky- Martens High Pensky arene Medium ie Sto +1108 10 570° 200 160°C Sahaton asre. re ve nee, mm a ar 87 ‘real ength 25 mm 20 230% 10 230 ‘en gemete, en sow ro 0070 0070 200 duro oyinsical ‘fncical nical Aubingt, re 91013 te 10 91019 “gamete, men ot less than 5.5 and notless than 4.5 and rotless than 5.5 and ot greater than not greater than ot greater than sem stom stem Lung of graduated portion, 140 19175 49 to 180 sate 178 Ditaee bottom of bub t, oe sore voc. tm Bb 1095 an 90 as toes Ler nos a out Lana 5° iO ana 20°C sc Fain al cat sc 20% 5°C Fsgasin chnber rexuired ‘eguled reques Tes fish ong, ‘ng ng Sele nee natto exceed = °C 1 260°C. re PC above 260°C Seoraes 1 and Tablo A2.3 for 1 and Table AB tor 1nd Table A or femeigent stem “omergont stom ‘aon sen temperatures temperatures temperatures FIG. A3.1_ Test Gage for Checking Enlargements on Thermometers METHODS OF SAMPLING AND TESTING 346 qh p93 YO fy W umoys 805 7 tn Ui posnzeous 9g ILA gna au Jo OR oA 6} UBLILEILA Bi JO WEHOY a og aOUELAE oly UE WUEWABIEU ain JO.ABUeE aL @ “Sujpaas eamesaduey ou og evoge paused aq aeyewoULio 8 anew Ssoueuros 04 Jepun aue‘suanesedos danse Bue! je ebodind ay 20) su 811 “ounteveduoy SUE ye ana au 7 uoRUORED OAD m ounsseed See ya jones, papacad | ogulye LEBLEdRO Uy» "4.009 J0r0 3,6 4009 01 dn 4407 2009 O05 ‘25082 1919 O52 ‘94082 01 A Del aa BOS y a [sos fase | us % | ons | oe a “a | | se fae + onte jocot | out | us dak faadt [26s | 2h | %» | os | se a |" @ ouoli~, fomeg sz se 2.80 [0.5 lout jovso| us | es-| 008 a 1 wet 3 63 | ag 08 e |e | Ses & | 8001 | 00 22a [ssi ou ea vou | yuo 8 un | ae “um an a3 saxo | stun | 2 2028 wt | oa maa seaustiie uae sis METHODS OF SAMPLING AND TESTING 347 qi) p93 TABLE A3.3 Standardization Temperatures ‘nenergant column temperatures er those attuned when using th themnometersn ths tes equipment for which the thermometers were orginally designed, ace tea amperes are markedly dle fom those realized during standerzation. ‘wore? ‘Average ood ‘aeerage Tempers: Tompera emnpera- Tompora- ela ust ogee: tet “emoere ture of ‘Tempore: ture of he: Emsargent we. Emeraont La Emergent we Eergent our ‘column ‘column ‘Calum Tramonater £6 “Thermometer 9F “Thommeameter 100 Thermornetor 10F (3t0 400°), {20 0 230°F) (@0 370°C) (200 10 700°) 1 sec aur 56°F 100° sire aie tater ssc 208 00°F aor 200°C Tree. 00°F 158¢F me aoc 60°F 106" 300°C arc BIO 180 8 50° 2200F 320 are 008 700" 220F PECPTO HOC) IP 18F @0 we 230°F) TP 160 (0 10 70°0), 1 16F @O 10 700"F) te we: ser bor 008 sie 200% aoe 0c 20°C 70 70°F 150°C esr. 800° v498F we aie 10°F aerr 200°C me 400° s60%F me 4ore 10°F 108°F 250°C re. 50°F ATSeF od eC Aer ser 300%¢ are Go0eF 195°F 350°C sore 00°F BOF 10-200°¢ esrion chambor: Pei enng oleae, rn $6000, Fb wet | ib 00. rm ‘a beats ‘Bator of bub to tho at 20% Disc, mm | Lao eraduatd portion, mm port cake 20sec Range ton of bulb to cept, mm ‘racton chamber: Tpstanoe to barter in, mm Distance o top, max, mm Ste: enargomont ‘0. Length in Distance to ott, nen AA Certified Reference Material (CRM)—CRM is a ‘sable, pure (99+ mole % purity) hydrocarbon or other stable prtrolcum product with a method-specific flash point estab- fished by a method-specific interlaboratory study following ASTM RR:D02-1007 guidelines or ISO Guide 34 and 35. ‘Ad.L.L Values of the flash point corrected for barometric ‘resare for some reference materials and their typical limits ‘ae given in Table A4.1 (see Note 4.1). Suppliers of CRMs TABLE A3.4 Specifications for Medium-Range Pensky-Martens, "ASTIN No. BSF (80) Vogotabw Ol Fash Thernomoter cium Range Panelay-Marens 5 S0-302°F 5 ve SF asim FBC) ST rm IMM. 400° 205 295 01070 Bow 120 DAS und

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