D 93 - 16a

Designation: D93  −  16a

Designation: 34/99

Standard Test Methods for

Flash Point by Pensky-Martens Closed Cup Tester 1 This standard is issued under the fixed designation D93; the number immediately following the designation indicates the year of original adoption adopt ion or, in the case of revis revision, ion, the year of last revision. A number in parentheses parentheses indicates indicates the year of last reapproval. reapproval. A super superscrip scriptt epsilon (´) indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies of the U.S. Department of Defense.

INTRODUCTION

This flash point test method is a dynamic test method which depends on specified rates of heating to be able to meet 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 some materials. There are flash point test methods with slower heating rates available, such as Test Method  D3941   (for paints, resins, and related products, and high viscosity products in the range of 0 °C to 110 °C), where the test conditions are closer to equilibrium. Flash point values are a function of the apparatus design, the condition of the apparatus used, and the operational operational procedure carried out. Flash point can theref therefore ore only be defined in terms of a standa standard rd test method, and no general valid correlation can be guaranteed between results obtained by different test methods, or with test apparatus different from that specified. 1. Sco Scope* pe*

1.3 Proced Procedure ure B is applicable to residual fuel oils, cutback  residua, used lubricating oils, mixtures of petroleum liquids with solids, petroleum liquids that tend to form a surface film under test conditions, or are petroleum liquids of such kinematic viscosity that they are not uniformly heated under the stirring and heating conditions of Procedure A.

1.1 These test methods methods cover the determination determination of the flash point of pet point petrol roleum eum pro produc ducts ts in the temp tempera eratur turee ran range ge fro from m 40 °C to 370 °C by a man manual ual Pen Pensky sky-Ma -Marten rtenss clo closed sed-cu -cup p appara app aratus tus or an aut automa omated ted Pen Pensky sky-Ma -Marte rtens ns clo closed sed-cu -cup p apparatus, appara tus, and the determination determination of the flash point of biodie biodiesel sel in the temperature range of 60 °C to 190 °C by an automated Pensky-Martens closed cup apparatus.

1.4 Proced Procedure ure C is applica applicable ble to biodiesel (B100). (B100). Since a flash point of residual alcohol in biodiesel is difficult to observe by manual flash point techni techniques, ques, automated apparatus apparatus with electronic flash point detection have been found suitable.

NOTE  1—Flash point determinations above 250 °C can be performed, however, the precision has not been determined above this temperature. For res residu idual al fue fuels, ls, pre precis cision ion has not bee been n det determ ermine ined d for flas flash h poi points nts above abo ve 100 °C. The pre precis cision ion of inin-use use lub lubric ricatin ating g oil oilss has not bee been n determined. determ ined. Some specifications specifications state a D93 minimum flash point below 40 °C, how howeve ever, r, the pre precis cision ion has not bee been n det determ ermine ined d bel below ow thi thiss temperature.

1.5 The These se test methods methods are applicab applicable le for the det detecti ection on of  contamination of relatively nonvolatile or nonflammable materials with volatile or flammable materials. 1.6 The values values stated in SI uni units ts are to be reg regard arded ed as the standard. 1.6.1   Exception— The The values given in par parent enthes heses es are for information only.

1.2 Procedu Procedure re A is app applica licable ble to dis distill tillate ate fue fuels ls (di (diesel esel,, biodiesel blend biodiesel blends, s, keros kerosine, ine, heating oil, turbin turbinee fuels) fuels),, new and in-use inuse lub lubric ricatin ating g oil oils, s, and oth other er hom homoge ogeneo neous us pet petrol roleum eum liquids not included in the scope of Procedure B or Procedure C.

NOTE 2—It has been common practice in flash point standards for many decadess to alt decade altern ernatel ately y use a C-s C-scale cale or an F-s F-scal calee the thermo rmomet meter er for temperature measurement. Although the scales are close in increments, they are not equivalent. Because the F-scale thermometer used in this procedure is graduated in 5 °F increments, it is not possible to read it to the 2 °C equivalent increment of 3.6 °F. Therefore, for the purposes of  application of the procedure of the test method for the separate temperature scale thermometers, different increments must be used. In this test method, the following protocol has been adopted: When a temperature is intend int ended ed to be a con conver verted ted equ equival ivalent ent,, it wil willl app appear ear in par parent enthes heses es following the SI unit, for example 370 °C (698 °F). When a temperature

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These test methods are under the joint jurisdiction of ASTM Committee D02 Committee D02 on  on Petroleum Products, Liquid Fuels, and Lubricants and are the direct responsibility of Subcommittee D02.08 Subcommittee  D02.08 on  on Volatility. In the IP, these test methods are under the  jurisdiction of the Standardization Committee. Current Curre nt editi edition on approv approved ed Oct. 1, 2016. Published Published October 2016. Originally Originally approv app roved ed in 192 1921. 1. Las Lastt pre previo vious us edi editio tion n app approv roved ed in 201 2016 6 as D93 – 16. 16. DOI DOI:: 10.1520/D0093-16A.

*A Summary of Changes section appears at the end of this standard Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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D93 − 16a 3.1.4.1   Discussion— This T his co cond ndit itio ion n ma may y no nott be fu full lly y achieved 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.

is intended to be a rationalized unit for the alternate scale, it will appear after “or,” for example, 2 °C or 5 °F.

standard d doe doess not purport purport to add addre ress ss all of the 1.7   This standar safetyy co safet conc ncer erns ns,, if an anyy, as asso socia ciate ted d wi with th its us use. e. It is th thee responsibility of the user of this standard to establish appro priate safety and health practices and determine the applicaspecifi cificc bilit bi lityy of reg egul ulat ator oryy lim limita itatio tions ns pr prio iorr to us use. e.   For spe warning statements, see 6.4 see 6.4,, 7.1  7.1,, 9.3  9.3,, 9.4  9.4,, 11.1.2  11.1.2,, 11.1.4  11.1.4,, 11.1.8  11.1.8,, 11.2.2,, and 11.2.2 and 12.1.2  12.1.2..

3.1.5  flash point, n—in flash point test methods , the lowest tempe tem pera ratu ture re of th thee te test st sp speci ecime men, n, ad adju just sted ed to acc accou ount nt fo forr variations in atmospheric pressure from 101.3 kPa, at which application of an ignition source causes the vapors of the test sample to ignite under specified conditions of test.

2. Referenc Referenced ed Documents Documents

4. Summa Summary ry of Test Method

2.1   ASTM Standards: 2 D56 Test D56  Test Method for Flash Point by Tag Closed Cup Tester D3941 Test Me Meth thod od fo forr Fl Flas ash h Po Poin intt by th thee Eq Equi uilib libri rium um Method With a Closed-Cup Apparatus D4057 Pr Pract actice ice fo forr Ma Manu nual al Sa Samp mplin ling g of Pe Petr trol oleu eum m an and d Petroleum Products D4177   Practice for Automatic Sampling of Petroleum and D4177 Petroleum Products E1   Specification for ASTM Liquid-in-Glass Thermometers E1 E300 Practice E300  Practice for Sampling Industrial Chemicals E502   Test Method for Selection and Use of ASTM StanE502 dards for the Determination of Flash Point of Chemicals by Closed Cup Methods

4.1 A brass test cup of specified specified dim dimens ension ions, s, fille filled d to the insi in side de ma mark rk wi with th tes testt sp spec ecim imen en an and d fitt fitted ed wi with th a co cove verr of  specifi spe cified ed dim dimens ension ions, s, is hea heated ted and the spe specim cimen en stir stirred red at specified rates, using one of three defined procedures (A, B, or C). An ignition source is directed into the test cup at regular intervals with simultaneous interruption of the stirring, until a flash is detected (see   11.1.8) 11.1.8). The flash point is reported as defined in 3.1.5 in  3.1.5.. 5. Signi Significanc ficancee and Use 5.1 The fla 5.1 flash sh po poin intt te temp mper eratu ature re is on onee mea measu sure re of th thee tendency of the test specimen to form a flammable mixture with air under controlled laboratory conditions. It is only one of a nu numb mber er of pr prop oper ertie tiess wh which ich mu must st be co cons nsid ider ered ed in assessing the overall flammability hazard of a material.

2.2   ISO Standards 3 Guide 34 General 34  General requirements for the competence of reference materia materiall prod producers ucers Guide 35 Reference 35  Reference material—General and statistical principles for certification

5.2 Flash point is used in shipping and safety regulation regulationss to define  flammable and  combustible  materials. One should consult the particular regulation involved for precise definitions of  these classifications.

3. Terminology

5.3 Th 5.3 Thes esee tes testt me meth thod odss sh shou ould ld be us used ed to me meas asur uree an and d describe descri be the properties of materia materials, ls, prod products, ucts, or assemb assemblies lies in resp re spon onse se to he heat at an and d an ig igni nitio tion n so sour urce ce un unde derr co cont ntro rolle lled d laboratory conditions and should not be used to describe or appraise the fire hazard or fire risk of materials, products, or assemblies assemb lies unde underr actual fire cond conditions. itions. However, However, result resultss of  thes th esee tes testt me meth thod odss ma may y be us used ed as ele eleme ment ntss of a fir firee ri risk  sk  assessment which takes into account all of the factors which are pertinent to an assessment of the fire hazard of a particular end use.

3.1   Definitions: 3.1.1   biodiesel, n— a fuel comprised of mono-alkyl esters of  long chain fatty acids derived from vegetable oils or animal fats, designated B100. 3.1.2   biodiesel blen end d of bi biod odies iesel el fu fuel el wi with th biodiesel blend blends, s, n— a bl petroleum-based diesel fuel. dynamic, adj—in petr petroleum oleum pr products oducts—in —in petr petroleum oleum 3.1.3   dynamic, —thee con conditi dition on whe where re the  product flash point test methods—th vapor above the test specimen and the test specimen are not in temperature equilibrium at the time that the ignition source is applied. 3.1.3.1   Discussion— This This is primarily caused by the heating of the test specimen at the constant prescribed rate with the vapor temperature lagging behind the test specimen temperature.

5.4 The These se test methods methods pro provid videe the only closed cup flash point test procedures for temperatures up to 370 °C (698 °F). 6. Appar Apparatus atus Pensky-Ma -Marte rtens ns Clo Closed sed Cup App Appara aratus tus (ma (manua nual) l) 6.1   Pensky This apparatus consists of the test cup, test cover and shutter,  — This stirring device, heating source, ignition source device, air bath, and top plate described in detail in  Annex A1. A1 .  The assembled manu ma nual al ap appa para ratu tus, s, te test st cu cup, p, tes testt cu cup p co cove verr, an and d te test st cu cup p assembly are illustrated in   Figs. A1.1-A1.4, A1.1-A1.4 ,   respectively. Dimensions are listed respectively.

3.1.4   equilibrium, n—in petroleum products—in petroleum  product flash point test methods—th —thee con conditi dition on whe where re the vapor above the test specimen and the test specimen are at the same temperature at the time the ignition source is applied.

6.2  Pensky-Martens Closed Cup Apparatus (Automated) 4— This apparatus is an automated flash point instrument that is

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For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [email protected]. For  Annual Book of ASTM  Standards volume information, refer to the standard’s Document Summary page on the ASTM website. 3 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.

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Supporting data regarding a variant of the cover locking mechanism have been filed at ASTM International International Headquarters Headquarters and may be obtai obtained ned by reque requesting sting Research Report RR:D02-1706.

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D93 − 16a capable of performing the test in accordance with Section 11 (Procedure (Proc edure A), Section 12 Section 12 (Procedure  (Procedure B), and 13 and  13 (Procedure  (Procedure C) of these test methods. The apparatus shall use the test cup, test cover and shutter, stirring device, heating source, and ignition source device described in detail in  Annex A1. A1 .

8.3 Succes Successive sive test specimens specimens can be taken from the same sample container. Repeat tests have been shown to be within the precision precisionss of the method method whe when n the second second spe specim cimen en is taken with the sample container at least 50 % filled. The results of flas flash h poi point nt det determ ermina inatio tions ns can be af affec fected ted if the samp sample le volume is less than 50 % of sample container capacity.

6.3   Temperature Thermometer having Temperature Measuring Device— Thermometer a range as shown in  Table 1   and conforming to the requirements prescribed in Specification E1   or in  Annex A3, A3, or an electronic electro nic temper temperature ature measuring device, such as resista resistance nce thermometers or thermocouples. The device shall exhibit the same temperature response as the mercury thermometers.

8.4 Err Errone oneous ously ly hig high h flas flash h poi points nts may be obt obtain ained ed if pre pre-cautions are not taken to avoid the loss of volatile material. Do not open containers unnecessarily, to prevent loss of volatile material or possible introduction of moisture, or both. Avoid storage of samples at temperatures in excess of 35 °C or 95 °F. Samples for storage shall be capped tightly with inner seals. Do not make a transfer unless the sample temperature is at least the equivalent of 18 °C or 32 °F below the expected flash point.

6.4   Ignition Source— Natural 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 deta iled in   Fig. A1. A1.4 4   requ requir ires es th thee us usee of th thee pi pilo lott fla flame me described describ ed in   A1.1.2.3. A1.1.2.3.   The The ele electri ctricc ign ignito itors rs sha shall ll be of the hotho t-wi wire re ty type pe an and d sh shall all po posit sitio ion n th thee he heate ated d se secti ction on of th thee ignitor in the aperture of the test cover in the same manner as the gas flame device. (Warning— (Warning—Gas Gas pressure supplied to the apparatus should not be allowed to exceed 3 kPa (12 in.) of  water pressure.)

8.5 Do not store samples in gas-permeable gas-permeable containers, containers, since volatile material may diffuse through the walls of the enclosure. Samples in leaky containers are suspect and not a source of valid results. 8.6 Sam Sample pless of very vis viscou couss mate materia rials ls sha shall ll be hea heated ted in their containers, with lid/cap slightly loosened to avoid buildup of dangerous pressure, at the lowest temperature adequate to liquefy any solids, not exceeding 28 °C or 50 °F below the expe ex pect cted ed fla flash sh po poin int, t, fo forr 30 mi min. n. If th thee sa samp mple le is th then en no nott completely liquefied, extend the heating period for additional 30 min periods as necessary. Then gently agitate the sample to provide prov ide mixing mixing,, such as orbit orbiting ing the contain container er horiz horizontally ontally,, before transferring to the specimen cup. No sample shall be heated hea ted and tra transf nsferr erred ed unl unless ess its temp tempera eratur tures es is mor moree tha than n 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 below the expected flash point before transferring.

6.5   Barometer— With With accuracy of  60.5 kPa. NOTE 3—The barometric pressure used in this calculation is the ambient pressu pres sure re fo forr th thee la labo bora rato tory ry at th thee ti time me of th thee tes test. t. Ma Many ny an aner eroi oid d barome bar ometer ters, s, suc such h as tho those se use used d at wea weathe therr sta statio tions ns and air airpor ports, ts, are precorrected to give sea level readings and would not give the correct reading for this test.

7. Reag Reagents ents and Materials Materials Cleaning Solven Solvents—  ts— Use 7.1   Cleaning U se su suita itabl blee so solv lven entt ca capa pabl blee of  cleaning out the specimen from the test cup and drying the test cup and cover. Some commonly used solvents are toluene and acetone. (Warning (Warning—T —Toluen oluene, e, aceton acetone, e, and many solve solvents nts are flammable and a health hazard. Dispose of solvents and waste material in accordance with local regulations.)

NOTE  4—Volatile vapors can escape during heating when the sample container is not properly sealed. NOTE 5—Some viscous samples may not completely liquefy even after prolonged periods of heating. Care should be exercised when increasing the heating temperature to avoid unnecessary loss of volatile vapors, or heating the sample too close to the flash point.

8. Samp Sampling ling 8.1 Obtain a sample in accordance with instructions given in Practices  D4057,,  D4177 Practices D4057  D4177,, or or E300  E300..

8.7 Samples Samples con contain taining ing dissolved dissolved or fre freee wat water er may be dehydr deh ydrated ated wit with h calc calcium ium chl chlori oride de or by filte filterin ring g thr throug ough h a qualitative filter paper or a loose plug of dry absorbent cotton. Warming the sample is permitted, but it shall not be heated for prolonged periods or greater than a temperature of 18 °C or 32 °F below its expected flash point.

8.2 Ensur Ensuree at least 75 mL of of sample is available so there is suffficie suf icient nt mate materia riall for the test test.. Whe When n obt obtaini aining ng a sam sample ple of  residual fuel oil, the sample container shall be from 85 % to 95 % full. For other types of samples, the size of the container shall be chosen such that the container is not more than 85 % full or less than 50 % full prior to any sample aliquot being taken tak en.. Fo Forr bi biod odies iesel el (B (B10 100) 0) sam sampl ples es,, a ty typi pica call on onee lit liter er container filled to 85 % volume is recommended.

NOTE 6—If the sample is suspected of containing volatile contaminants, the treatment described in 8.6 in 8.6  and  8.7  should be omitted.

TABLE 1 Temperature Measuring Device Temperature Range −5 °C to 110 °C (20 °F to 230 °F) +10 °C to 200 °C (50 °F to 392 °F) +90 °C to 370 °C (200 °F to 700 °F)

Thermometer Number ASTM 9C (9F)

Temperature Range −5 °C to 110 °C

Thermometer Number IP 1 5C

88C (88F)

+20 °C to 150 °C

1 01 C

10C (10F)

+90 °C to 370 °C

1 6C

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D93 − 16a (A1.1.2.3 A1.1.2.3)), an and d th thee an angl glee an and d po posit sitio ion n of th thee tem tempe pera ratu ture re measuring device (A1.1.2.4 (A1.1.2.4)). After any adjustment, repeat the test in 10.3 in  10.3 using  using a fresh test specimen, with special attention to the procedural details prescribed in these test methods.

9. Pre Prepara paration tion of Apparatus Apparatus 9.1 Supp Support ort the manual or automated apparatus apparatus on a level steady surface, such as a table. 9.2 Tes 9.2 ests ts ar aree to be pe perf rfor orme med d in a dr draf aftt-fr free ee ro room om or comp co mpar artm tmen ent. t. Tes ests ts ma made de in a lab labor orato atory ry ho hood od or in an any y location where drafts occur are not reliable.

10.6 The numerical values obtained obtained during the verifi verification cation check  (10.3  ( 10.3))  shall not be used to provide a bias statement, nor shall they be used to make any correction to the flash points subsequentl subse quently y determ determined ined using the appara apparatus. tus.

NOTE   7—A shield, of the appro approximat ximatee dimen dimensions sions 460 mm mm (18 in.) square and 610 mm (24 in.) high, or other suitable dimensions, and having an open front is recommended to prevent drafts from disturbing the vapors above the test cup. NOTE 8—With some samples whose vapors or products of pyrolysis are objectionable, it is permissible to place the apparatus along with a draft shield in a ventilation hood, the draft of which is adjustable so that vapors can be withdrawn without causing air currents over the test cup during the ignition source application period.

PROCEDURE A 11. Proced Procedure ure 11.1   Manual Apparatus: 11. 1.1. 1.1 1 En Ensu sure re th that at th thee sa samp mple le co cont ntai aine nerr is fill filled ed to th thee volumee capacit volum capacity y requir requirement ement specified in  8.2  8.2..  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. If the temperature measuring device is not already in place, insert the device into its holder. 11.1.2 11 .1.2 Lig Light ht the test flame, flame, and adjust adjust it to a diam diamete eterr of  3.2 mm to 4.8 mm (0.126 in. to 0.189 in.), or switch on the electric igniter and adjust the intensity in accordance with the manufacturer’s instructions. (Warning— (Warning—Gas Gas pressure should not be allowed to exceed 3 kPa (12 in.) of water pressure.) (Warning—  Exercise care when using a gas test flame. If it should be extinguished it will not ignite the vapors in the test cup, and the gas for the test flame that then enters the vapor space sp ace can in influ fluen ence ce th thee re resu sult. lt.)) (Warning— The ope operato ratorr Warning—The should exercise and take appropriate safety precautions during the initial application of the ignition source, since test specimenss con men contain taining ing low low-fla -flash sh mate materia riall can giv givee an abn abnorm ormally ally stro st rong ng fla flash sh wh when en th thee ig igni nitio tion n so sour urce ce is fir first st ap appl plied ied.) .) (Warning— The operator should exercise and take appropriate Warning—The safety precautions during the performance of these test methods. The temperatures attained during these test methods, up to 370 °C (698 °F), are considered hazardous.) ( Warning— As a Warning—As safety practice, when using automated or manual apparatus, it is strongly advised, before heating the test cup and specimen, to dip the ign ignito itorr to che check ck for the pre presen sence ce of une unexpe xpected cted volatilee materia volatil material.) l.) 11.1.3 11 .1.3 Apply the heat at such a rate that the temperature, temperature, as indicated indica ted by the temperature measuring measuring device device,, increa increases ses 5 °C to 6 °C (9 °F to 11 °F) ⁄min. 11.1.4 11 .1.4 Tu Turn rn the stir stirrin ring g dev device ice at 90 r ⁄mi ⁄min n to 120 r ⁄mi ⁄min, n, stirring in a downward direction. (Warning— ( Warning—Meticulous Meticulous attention to all details relating to the ignition source, size of test flame or intensity of the electric ignitor, rate of temperature increase, and rate of dipping the ignition source into the vapor of the test specimen is desirable for good results.) 11.1.5   Application of Ignition Source: 11.1.5.1 If the test specimen is expected to have have a flash point of 110 °C or 230 °F or below, apply the ignition source when the temperature of the test specimen is 23 °C 6 5 °C or 41 °F

9.3 Prepa Prepare re the manual apparatus apparatus or the automated automated apparatus for ope operat ration ion in acco accorda rdance nce with the man manufa ufactu cturer rer’s ’s instructions for calibrating, checking, and operating the equipment. men t. (Warning— Gass pr pres essu sure re sh shou ould ld no nott be all allow owed ed to Warning—Ga exceed 3 kPa (12 in.) of water pressure. ) 9.4 Thor Thoroughl oughly y clean and dry all parts of the test cup and its accessories before starting the test, to ensure the removal of  any solvent which had been used to clean the apparatus. Use suitable solvent capable of removing all of the specimen from the test cup and drying the test cup and cover. Some commonly used solvents are toluene and acetone. (Warning— ( Warning—Toluene, Toluene, acetone acet one,, and man many y sol solven vents ts are flam flammab mable. le. Heal Health th haz hazard ard.. Dispose Disp ose of sol solven vents ts and was waste te mat materia eriall in acc accord ordanc ancee with local regulations.) 10. Verification of Apparatus Apparatus 10.1 Adjust 10.1 Adjust the auto automate mated d flas flash h poi point nt det detecti ection on sys system tem (when used) in accord accordance ance with the manufacturer’s manufacturer’s instructions. 10.2 10. 2 Verif erify y that the tem temper peratu ature re mea measur suring ing dev device ice is in accordance with 6.3 6.3.. 10.3 Verify the performance performance of the manua manuall apparatus or the automated apparatus at least once per year by determining the flash point point of a cer certifie tified d ref refere erence nce material material (CR (CRM) M) suc such h as those tho se list listed ed in in   Annex A4, A4, whi which ch is rea reason sonably ably close close to the expected temperature range of the samples to be tested. The material shall be tested according to Procedure A of these test methods and the observed flash point obtained in   11.1.8 or 11.2.2  shall be corrected for barometric pressure (see Section 14). 14 ). The flash point obtained shall be within the limits stated in Table A4.1   for for th thee id iden enti tifie fied d CR CRM M or wi with thin in th thee li limi mits ts calculated for an unlisted CRM (see Annex (see  Annex A4). A4). 10.4 Once 10.4 Once th thee pe perf rfor orma manc ncee of th thee ap appa para ratu tuss ha hass be been en verifi ve rified ed,, th thee fla flash sh po poin intt of se seco cond ndar ary y wo work rkin ing g st stan anda dard rdss (SWSs) (SW Ss) can be det determ ermine ined d alo along ng with their con contro troll limi limits. ts. Thes Th esee se seco cond ndar ary y ma mater terial ialss ca can n th then en be ut utili ilized zed fo forr mo more re frequent frequ ent perfo performanc rmancee checks (see  Annex A4). A4 ). 10.5 When the flash point point obtained is not within the limits stated in 10.3 in  10.3 or  or 10.4  10.4,,  check the condi condition tion and operation of the apparatus to ensure conformity with the details listed in  Annex A1,, especially with regard to tightness of the lid ( A1.1.2.2 A1 A1.1.2.2), ), the actio act ion n of th thee sh shut utter ter,, th thee po posit sitio ion n of th thee ig igni niti tion on so sour urce ce 4

D93 − 16a 9 °F below the expected flash point and each time thereafter at a tem temper peratu ature re rea readin ding g tha thatt is a mul multipl tiplee of 1 °C or 2 °F °F.. Discont Disc ontinu inuee the stirring stirring of the test specimen specimen and apply the ignition source by operating the mechanism on the test cover which controls the shutter so that the ignition source is lowered into the vapor space of the test cup in 0.5 s, left in its lowered position for 1 s, and quickly raised to its upward position. 11.1.5.2 If the test specimen is expected to have a flash point abov ab ovee 110 °C or 23 230 0 °F °F,, ap appl ply y th thee ig igni nitio tion n so sour urce ce in th thee manner described in   11.1.5.1  at each temperature increase of  2 °C or 5 °F, beginning at a temperature of 23 °C 6  5 °C or 41 °F 6 9 °F below the expected flash point. ( Warning— As a Warning—As safety practice, when using automated or manual apparatus, it is str strong ongly ly adv advised ised that, for an exp expecte ected d flas flash h poi point nt abo above ve 130 °C, to dip the ignitor every 10 °C throughout the test until the sample temperature reaches 28 °C below the expected flash point and then follow the prescribed dipping procedure. This practicee has been shown to reduce the possi practic possibility bility of a fire, and, on ave averag rage, e, not to sig signifi nifican cantly tly af affect fect the res result ult.. A limi limited ted 5 study has shown that this dipping practice has no observable effect ef fect on test method repeatability repeatability.) .) 11.1.6 11 .1.6 When testing materials materials to determ determine ine if volatil volatilee material contamination is present, it is not necessary to adhere to the temperature limits for initial ignition source application as stated in 11.1.5 in  11.1.5.. 11.1 1.1.7 .7 When tes testing ting mat materia erials ls whe where re the exp expect ected ed flas flash h point temperature is not known, bring the material to be tested and the tester to a temperature of 15 °C 6  5 °C or 60 °F 6 10 °F. When the material is known to be very viscous at this tempera temp eratur ture, e, hea heatt the spe specim cimen en to a sta startin rting g temp tempera eratur turee as described describ ed in 8.6 8.6..   Apply Apply the ign ignitio ition n sou source rce,, in the man manner ner described in  in   11.1.5.1, 11.1.5.1, beginning at least 5 °C or 10 °F higher than the starting temperature.

11. 1.1. 1.10 10 Whe When n a fla flash sh po poin intt is de dete tect cted ed on th thee fir first st application, applic ation, the test shall be discontinued, discontinued, the result discarded, discarded, and an d th thee tes testt re repe peat ated ed wi with th a fr fres esh h te test st sp spec ecime imen. n. Th Thee fir first st application of the ignition source with the fresh test specimen shall be 23 °C 6 5 °C or 41 °F 6 9 °F below the temperature at which a flash point was detected on the first application. 11.1.1 11 .1.11 1 Whe When n a flas flash h poi point nt is det detecte ected d at a tem temper peratu ature re 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 above the temperature of the first application of the ignition source, sourc e, the result shall be consid considered ered approximate, 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 source with the fresh test specimen shall be 23 °C 6 5 °C or 41 °F 6 9 °F below the temperature at which the approximate result was found. 11. 1.1. 1.12 12 When th thee ap appa para ratu tuss ha hass co cool oled ed do down wn to a sa safe fe handling temperature, less than 55 °C (130 °F), remove the test cover and the test cup and clean the apparatus as recommended by the manufacturer.

6

NOTE  10—Exerc  10—Exercise ise care when cleaning and posit positioning ioning the lid assembly so not to damage or dislocate the flash detection system or temperature measuring device. See the manufacturer’s instructions for proper care and maintenance.

11.2   Automated Apparatus: 11.2.1 11 .2.1 The aut automa omated ted app apparat aratus us sha shall ll be cap capabl ablee of per per-forming the procedure as described in  11.1  11.1,,   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. 11.2.2 11 .2.2 Start the automated apparatus apparatus in accordance accordance with the manufacturer’s instructions. (Warning— (Warning—Failure Failure to install the sample temperature measuring device corre correctly ctly,, when using automated apparatus, can result in uncontrolled heating of the test portion and potentially a fire. Some automated apparatus includee provi includ provisions sions to avoid this occur occurrence. rence.)) The apparatus shall follow the procedural details described in 11.1.3 in  11.1.3 through  through 11.1.8.. 11.1.8

NOTE 9—Flash Point results determined in an “unknown expected flash point mode” should be considered approximate. This value can be used as the expected flash point when a fresh specimen is tested in the standard mode of operat operation. ion.

11.1.8 Record as the observed 11.1.8 observed flash point the reading on the tempera temp eratur turee mea measur suring ing dev device ice at the time ign ignitio ition n sou source rce application applica tion causes a distin distinct ct flash in the interio interiorr of the test cup. Thee sa Th samp mple le is de deem emed ed to ha have ve fla flash shed ed wh when en a la larg rgee fla flame me appears and instantaneously propagates itself over the entire surface of the test specimen. (Warning— ( Warning—For For certain mixtur mixtures es containing halogenated hydrocarbons, such as, methylene chloridee or tr rid trich ichlo loro roet ethy hylen lene, e, no di dist stin inct ct fla flash sh,, as de defin fined ed,, is observed. Instead a significant enlargement of the test flame (not halo effect) and change in color of the test flame from blue to yellowish-orange occurs. Continued heating and testing of  these samples above ambient temperature can result in significantt bu can burn rnin ing g of va vapo pors rs ou outs tsid idee th thee tes testt cu cup, p, an and d ca can n be a potential fire hazard. See  Appendix X1 and Appendix X2 for more information.) 11.1 1.1.9 .9 Whe When n the ignition ignition source source is a test flame, the app applilication of the test flame can cause a blue halo or an enlarged flame prior to the actual flash point. This is not a flash and shall be ignored.

PROCEDURE B 12. Procedur Proceduree 12.1   Manual Apparatus: 12.1 12 .1.1 .1 Ensure Ensure th that at th thee sa samp mple le co cont ntain ainer er is fil filled led to th thee volumee capacit volum capacity y requir requirement ement specified in  8.2  8.2..  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. If the temperature measuring device is not already in place, insert the device into its holder. 12.1.2 12. 1.2 Ligh Lightt the test flame and adj adjust ust it to a dia diamete meterr of  3.2 mm to 4.8 mm (0.126 in. to 0.189 in.), or switch on the electric igniter and adjust the intensity in accordance with the manufacturer’s instructions. (Warning— (Warning—Gas Gas pressure should

5

Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1652.

5

D93 − 16a not be allo allowed wed to exc exceed eed 3 kPa (12 in. in.)) of wat water er pre pressu ssure.) re.) (Warning— Exercise care when using a gas test flame. If it Warning—Exercise should be extinguished it will not ignite the vapors in the test cup and the gas for the test flame that then enters the vapor spac sp acee ca can n in influ fluen ence ce th thee re resu sult. lt.)) (Warning— The ope operat rator or Warning—The should exercise and take appropriate safety precautions during the initial application of the ignition source, since test specimens containing low-flash material may give an abnormally stron str ong g fla flash sh wh when en th thee ig igni niti tion on so sour urce ce is fir first st ap appl plie ied. d.)) (Warning— The operator should exercise and take appropriate Warning—The safety precautions during the performance of these test methods. The temperatures attained during these test methods, up to 370 °C (698 °F), are considered hazardous.) 12.1.3 12. 1.3 Tu Turn rn the stir stirrin ring g dev device ice at 250 r ⁄mi ⁄min n 6  10 r ⁄min, stirring in a downward direction. 12.1.4 12.1. 4 Apply the heat at such a rate that the temperature temperature as indicated by the temperature measuring device increases 1 °C to 1.6 °C (2 °F to 3 °F) ⁄min. 12.1.5 12.1. 5 Proce Proceed ed as prescribed in Section Section  11  11,,  with the exception of the pre preced ceding ing req requir uireme ements nts for rates of stir stirrin ring g and heating.

the initial application of the ignition source, since test specimenss con men contain taining ing low low-fla -flash sh mate materia riall can giv givee an abn abnorm ormally ally stro st rong ng fla flash sh wh when en th thee ig igni nitio tion n so sour urce ce is fir first st ap appl plied ied.) .) (Warning— The operator should exercise and take appropriate Warning—The safety precautions during the performance of these test methods. The temperatures attained during these test methods, up to 370 °C (698 °F), are considered hazardous.) 13.4 App 13.4 Apply ly the hea heatt at such a rate that the temperatur temperaturee as indicat ind icated ed by the tempera temperatur turee meas measuri uring ng dev device ice inc increas reases es 3.0 °C ⁄min 6 0.5 °C °C ⁄mi ⁄min. n. 13.5 Tur 13.5 urn n th thee st stir irri ring ng de devi vice ce at 90 r ⁄m ⁄min in to 12 120 0 r ⁄m ⁄min in,, stirring in a downward direction. (Warning— ( Warning—Meticulous Meticulous attention to all details relating to the ignition source, size of test flame, flam e, rat ratee of temp tempera eratur turee inc increa rease, se, and rate of dip dippin ping g the ignition source into the vapor of the test specimen is desirable for good results.) Application of Igniti Ignition on Sour Source—  ce— The 13.6   Application T he first test on the sample shall use an expected flash point of 100 °C.

13.7 Apply the ignition ignition source when the temperature temperature of the test specimen is approximately 24 °C below the expected flash point and each time thereafter at a temperature reading that is a multiple of 2 °C. Discontinue the stirring of the test specimen and apply the ignition source by operating the mechanism on the test cover which controls the shutter so that the ignition source is lowered into the vapor space of the test cup in 0.5 s, left in its lowered position for 1 s, and quickly raised to its upward position.

12.2   Automated Apparatus: 12.2.1 12. 2.1 The aut automa omated ted app appara aratus tus sha shall ll be cap capable able of per per-forming the procedure as described in  12.1  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 12.2. 2 Start the automated apparatus apparatus in accordance accordance with the manufacturer manuf acturer’s ’s instru instructions ctions.. The appar apparatus atus shall follow the procedural details in accordance with  12.1.3  12.1.3 through  through 12.1.5  12.1.5..

13.8 Record as the flash point point the reading on the temperature measuring device at the time the ignition source application causes a distinct flash in the interior of the test cup which is detected by the electronic device.

Procedure C 13. Procedur Proceduree

13.9 The application application of the test flame can cause cause a blue halo or an enlarged flame prior to the actual flash point. This is not a flash and shall be ignored.

Apparatus—  atus— Ensure 13.1   Automated Appar Ensure that the app appara aratus tus is equipped with an electronic measuring system for the detection of the flash point.

13.10 When a flash point is detected detected on the first application, application, the test shall be discontinued, the result discarded, and the test repeated repeat ed with a fresh test specime specimen. n. The first applic application ation of the ignition source with the fresh test specimen shall be approximately 24 °C below the temperature at which a flash point was detected on the first application.

13.2 Ensur Ensuree that the sample container container is filled to the volume capacity requirement specified in 8.2 in  8.2..  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 24 °C be belo low w th thee ex expe pect cted ed fla flash sh po poin int. t. If to too o mu much ch te test st 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. If the temperature measuring device is not already in place, insert the device into its holder.

13.11 When a flash point is detected 13.11 detected at a temper temperature ature which which is gr grea eate terr th than an 30 °C ab abov ovee th thee te temp mper erat atur uree of th thee fir first st applica app licatio tion n of the ign ignitio ition n sou source rce,, or when a flas flash h poi point nt is detected at a temperature which is less than 16 °C above 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 fir st ap appl plic icati ation on of th thee ig igni nitio tion n so sour urce ce wi with th th thee fr fres esh h te test st specimen specim en shall be appro approximatel ximately y 24 °C below the temper temperature ature at which the approximate result was found.

13.3 13 .3 Lig Light ht th thee te test st fla flame me,, an and d ad adju just st it to a di diame amete terr of  3.2 mm to 4.8 mm (0. (0.126 126 in. to 0.1 0.189 89 in.) or swi switch tch on the electric igniter and adjust the intensity in accordance with the manufacturer’s instructions. (Warning— (Warning—Gas Gas pressure should not be allo allowed wed to exc exceed eed 3 kPa (12 in. of wate waterr pre pressu ssure.) re.) (Warning— Exercise care when using a gas test flame. If it Warning—Exercise should be extinguished it will not ignite the vapors in the test cup, and the gas for the test flame that then enters the vapor spac sp acee ca can n in influ fluen ence ce th thee re resu sult. lt.)) (Warning— The ope operat rator or Warning—The should exercise and take appropriate safety precautions during

13.1 13 .12 2 Wh When en th thee ap appa para ratu tuss ha hass co cool oled ed do down wn to a sa safe fe handling temperature, less than 55 °C, remove the test cover and the test cup and clean the apparatus as recommended by the manufacturer. 6

D93 − 16a 16.1.3   Bias— Since Since there is no accepted reference material suitable suitab le for determ determining ining the bias for the proce procedure dure in these test methods, bias has not been determined. 16.1.4   Relative Bias— Statistical Statistical evaluation of the data did not detect any significant difference difference between the repro reproducib ducibilility variances of manual and automated Pensky-Martens flash point results for the samples studied. Evaluation of the data did not det detect ect any sig signifi nifican cantt dif differ ferenc encee bet betwee ween n ave averag rages es of  manual man ual and auto automate mated d Pen Pensky sky-Ma -Marte rtens ns flas flash h poi point nt 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.

NOTE  11—Exercise care when cleaning and positioning the lid assembly so not to damage or dislocate the flash detection system or temperature measuring device. See the manufacturer’s instructions for proper care and maintenance.

PRECISION, CALCULATION, AND REPORT FOR PROCEDURES A, B, OR C 14. Calc Calculati ulation on 14.1 Obser Observe ve and record the ambient barometric pressure pressure (see  Note 3) (see Note 3) at the time of the test. When the pressure differs from fr om 10 101. 1.3 3 kP kPaa (7 (760 60 mm Hg Hg), ), co corr rrec ectt th thee fla flash sh po poin intt as follows: Corrected flash point 5 C 1 0.25 ~ 101.3 2 K !

(1 )

Corrected flash point 5 F 1 0.06 ~ 760 2 P !

(2 )

Corrected flash point 5 C 1 0.033 ~ 760 2 P !

(3 )

NOTE 12—The precision statements were derived on clear liquids only. Refer to the research report6 for information regarding relative bias and types of samples. Additional studies are in progress concerning relative bias.

16.1.5 The precision 16.1.5 precision data were developed from a combined 1991 ASTM cooperative test program 6 using 5 samples of fuel and lubricating oils (Twelve laboratories participated with the manual man ual app appara aratus tus and 21 lab labora orator tories ies par partici ticipat pated ed wit with h the automated equipment) and a 1994 IP cooperative test program using usi ng 12 fue fuell sam samples ples and 4 pur puree che chemic micals. als. (T (Twen wentyty-six six laboratories labor atories participated participated with manual and automated equipment. The apparatus used either a gas test flame 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.6

where: C  = obs observ erved ed flash flash point, point, °C, °C, F  = obser observed ved flash flash point, point, °F °F,, P = ambien ambientt barometric barometric pressur pressure, e, mm Hg, Hg, and ambientt barometric barometric press pressure, ure, kPa. kPa. K  = ambien 14.2 14. 2 Aft After er cor correct rection ion for bar barome ometri tricc pre pressu ssure, re, rou round nd the temperature to the nearest 0.5 °C (1 °F) and record. 15. Repor Reportt 15.1 Rep 15.1 Report ort the cor correc rected ted flash poi point nt as the ASTM ASTM D93 D93,, Procedure A or Procedure B or Procedure C Pensky-Martens Closed Cup Flash Point of the test specimen.

17. Pre Precisi cision on and Bias (Procedur (Proceduree B) 17.1   Precision— The The precision of this procedure, as determined by the statistical examination of the interlaboratory test results, is as follows: 17.1.1   Repeatability— The The dif differ ferenc encee bet betwee ween n suc success cessive ive results obtained by the same operator with the same apparatus under constant operating operating condi conditions tions on identic identical al test materials would, in the long run, in the normal and correct operation of  the test method, exceed the following value in 1 case in 20:

16. Pre Precisi cision on and Bias (Pr (Proced ocedure ure A) 16.1   Precision— The The precision of this procedure as determined by the statistical examination of the interlaboratory test results, is as follows: 16.1.1   Repeatability— The The dif differ ferenc encee betw between een suc succes cessiv sivee results,, obtain results obtained ed by the same opera operator tor with the same appar apparatus atus under constant operating conditions on identical test material, would in the long run, in the normal and correct operation of  the test method, exceed the following values in 1 case in 20. r  5  AX ,

Residual fuel oil 2 °C Other types 5 °C

17.1.2   Reproducibility— The The difference between two single and independent results obtained by different operators working in different laboratories on identical material would, in the long run, exceed the following value only in 1 case in 20:

(4)

 A 5 0.029,  X  5 mean result in ° C, and

Residual fuel oil 6 °C Other types 10 °C

r  5 repeatability.

NOTE  13—The precisions of these standards were derived from interlaboratory studies conducted in degrees Celsius.

16.1.2   Reproducibility— The The difference between two single and independent results, obtained by different operators working in different laboratories on identical material, would in the long lo ng ru run, n, in th thee no norm rmal al an and d co corr rrec ectt op oper erat atio ion n of th thee tes testt method, exceed the following values only in 1 case in 20.  R 5  BX ,

17.1.3   Bias— Since Since there is no accepted reference material suitable suitab le for determ determining ining the bias for the proce procedure dure in these test methods, bias has not been determined. 17.1.4 17.1. 4 The precision precision data for residu residual al fuel oils were developed in a 1996 cooperative test program conducted by the IP

(5)

 B 5 0.071,  X  5 mean result in ° C, and

6

Suppor Sup portin ting g dat dataa (th (thee res result ultss of the 199 1991 1 int interl erlabo aborat ratory ory coo cooper perati ative ve tes testt program) have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:S15-1008.

 R 5 reproducibility.

7

D93 − 16a using 12 samples of residual fuel and 40 laboratories worldwide using both the manual and automated apparatus. Information on the type of samples and their average flash point are in the research report. 17.1.5 17.1. 5 The precision precision data for other sample types in Procedure B is not known to have been developed in accordance with RR:D02-1007.

ing in different laboratories on identical material would, in the long lo ng ru run, n, in th thee no norm rmal al an and d co corr rrec ectt op oper erati ation on of th thee te test st method, exceed the following value only in 1 case in 20: 14.7 °C

NOTE  15—The precisions of these standards were derived from interlaboratory studies conducted in degrees Celsius.

18.1.3   Bias— Since Since there is no accepted reference material suitable for determ suitable determining ining the bias for the proce procedure dure in these test methods, bias has not been determined.

NOTE   14—Proc 14—Procedu edure re B was not tes tested ted in the 199 1991 1 int interl erlabo aborat ratory ory program.

18. Pre Precisi cision on and Bias (Procedu (Procedure re C) 7

18.1.4 18.1. 4 The precision precision data for biodiesel were developed developed in a 2008 cooperative interlaboratory test program 7 using 9 samples of biodiesel (B100) of various source and 17 samples of the samee bio sam biodie diesel sel dos dosed ed wit with h con concen centra tratio tions ns of alco alcohol hol fro from m 0.1 % to 0.3 %. Various automated apparatus in 11 laboratories participated. The precision was calculated on the flash point range from 60 °C to 190 °C. The alcohol concentrations were verified in separate laboratories using EN 14110. Information on the type of samples and their average flash point are in the research report.

18.1   Precision— The The precision of this procedure, as determined by the statistical examination of the interlaboratory test results, is as follows: 18.1.1   Repeatability— The The dif differ ferenc encee betw between een suc succes cessiv sivee results obtained by the same operator with the same apparatus under constant operating conditions conditions on identi identical cal test materia materials ls would, in the long run, in the normal and correct operation of  the test method, exceed the following value in 1 case in 20: 8.4 °C

18.1.2   Reproducibility— The The difference between two single and independent results obtained by different operators work-

19. Keyw Keywords ords 19.1 automa automated ted flash poin point; t; auto automate mated d Pens Penskyky-Mar Martens tens closed cup; flammability; flash point; Pensky-Martens closed cup

7

Supportin Suppor ting g dat dataa (th (thee res result ultss of the 200 2008 8 int interl erlabo aborat ratory ory coo cooper perati ative ve tes testt program) have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1683.

ANNEXES (Mandatory Information) A1. APPARA APPARATUS TUS SPECIFICATIONS 4

A1.1 A typical A1.1 typical asse assembl mbly y of the app appara aratus tus,, gas heated, heated, is shown in Fig. in  Fig. A1.1. A1.1.  The apparatus shall consist of a test cup, cover, and stove conforming to the following requirements:

(3 ⁄ 32 32 in.) thick, operating on the plane of the upper surface of  the cover. The shutter shall be so shaped and mounted that it rotates on the axis of the horizontal center of the cover between two stops, so placed, that when in one extreme position, the openings A,  B , and C  in   in the cover are 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. A1.1.2.3   Flame-Ignition Device— The The flame-ignition device (Fig Fig.. A1. A1.4 4)   shall shall ha have ve a tip wi with th an op open enin ing g 0. 0.69 69 mm to 0.79 mm (0.027 in. 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 throug thr ough h the cen center ter of the lar larger ger opening opening A (Fig. A1.3). A1.3). An electric ignitor is also suitable. The electric ignitors shall be of 

A1.1.1   Cup— The The cup shall be of brass, or other nonrusting metal of equivalent heat conductivity, and shall conform to the dimensional dimens ional requir requirements ements in   Fig. A1.2. A1.2.   The The flan flange ge sha shall ll be equipped with devices for locating the position of the cup in the stove. A handle attached to the flange of the cup is a desirable accessory. The handle shall not be so heavy as to tip over the empty cup. A1.1.2   Cover: A1.1.2.1  Cover Proper— The The cover shown in Fig in  Fig.. A1. A1.3 3 shall be of brass (A1.1.1 (A1.1.1)) and shall have a rim projecting downward almost to the flange of the cup. The rim shall fit the outside of  the cup with a clearance not exceeding 0.36 mm (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 upper edge of the cup shall be in close contact with the inner face of the cover throughout its circumference. A1.1.2.2   Shutter— The The cover shall be equipped with a brass shutter shu tter (Fig Fig.. A1. A1.1 1 and   Fig. A1. A1.4 4), app approx roximat imately ely 2.4 mm

8

D93 − 16a

NOTE  1—Lid assembly can be positioned either right or left-handed. FIG. A1.1 Pensky-Martens Closed Flash Tester

the elec electri tricc res resista istance nce (ho (hot-w t-wire) ire) typ typee and sha shall ll pos positio ition n the heated section of the ignitor in the aperture of the test cover in the same manner as the gas flame device. A1.1.2.4   Pilot Flame— A pilot flame shall be provided for auto au toma matic tic re relig light htin ing g of th thee ex expo posu sure re fla flame. me. A be bead ad 4 mm 5 (  ⁄ 32 32 n.) in diameter can be mounted on the cover so that the size of the test flame can be regulated by comparison. The tip of the pilot flame shall have an opening the same size as the tip of the flame exposure device (0.69 mm to 0.79 mm (0.027 in. to 0.031 in.) in diameter).

A1.1.2.5   Stirring Device— The The cover shall be equipped with a stirring device ( device  (Fig. Fig. A1.4) A1.4)  mounted in the center of the cover and carrying two 2-bladed metal propellers. In  Fig. A1.4 lower A1.4  lower prop pr opell eller er is de desi sign gnate ated d by th thee let letter terss L, M , an and d N . Th This is 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 A, C , and G. This propeller measures approximately 19 mm, tip to tip, each of its two blades is also 8 mm in width with a pitch of 45°. Both propellers prop ellers are located on the stirrer shaft shaft in such a manner that, 9

D93 − 16a

mm

mm A B C D E F G H I J

D E F G H I J K L

(in.)

mi n

m ax

(min)

(max)

7 9. 0 1 .0 2 .8 2 1. 72 4 5. 47 5 0 .7 2 5 5 .7 5 3 .8 5 3 .9 0 2. 29

7 9 .8 ... 3 .6 2 1. 84 4 5. 72 5 0 .8 5 5 6 .0 0 4 .0 5 4 .0 2 2 .5 4

(3.11) (0.04) (0.11) (0.855) (1.790) (1.997) (2.195) (0.15) (2.122) (0.090)

(3.14) (...) (0.14) ( 0 .8 6 0 ) (0 ( 1 .8 0 0 ) (1 ( 2 .0 0 2 ) (2 ( 2 .2 0 5 ) (2 ( 0. 16 ) (0 (2.127) (2 (0.100)

(in.)

mi n

ma x

(min)

(max)

1 2 .7 4 .8 1 3. 5 2 3 .8 1 .2 7 .9 1 2. 00 1 6 .3 8 1 8. 65

1 3. 5 5 .6 1 4. 3 2 4 .6 2 .0 ... 1 2. 32 1 7 .0 0 1 9. 45

(0.50) (0.19) (0.53) (0.94) (0.05) (0.31) (0.472) (0.645) (0.734)

(0.53) (0.22) (0 (0.56) (0.97) (0.08) (0 (...) (0.485) (0 (0.669) (0.766) (0

FIG. A1.3 A1.3 Cover Proper Proper

that the temperatures of the bottom and the walls are approximately the same. In order that the air bath internal surfaces should be at a uniform temperature, it should not be less than 6.4 6. 4 mm (1 ⁄ 4 in in.) .) in th thic ickn kness ess un unles lesss th thee he heat atin ing g el elem emen entt is designed to give equal heat flux densities over all the wall and bottom surfaces. A1.1.2.9   Heater, Electric Resistance— If If the heater is of the electric resistance type, it shall be constructed so that all parts of the inte interio riorr sur surfac facee are hea heated ted uni unifor formly mly.. The wall and bottom of the air bath shall not be less than 6.4 mm ( 1 ⁄ 4 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 dis distrib tributi ution on sha shall ll hav havee the hea heatin ting g 5 elements positioned at least 4.0 mm (  ⁄ 32 32 in.) away from the internal surface of the air bath in conjunction with a minimum thickness of 1.58 mm ( 1 ⁄ 16 16 in.) for the wall and bottom of the air bath. A1.1.2.10   Top Plate— The 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 mm ( 3 ⁄ 16 16 in.), and they shall be not 3 more than 9.5 mm (  ⁄ 8 in.) in diameter.

FIG. A1.2 A1.2 Test Cup

when viewed from the bottom of the stirrer, the blades of one prop pr opel eller ler are at 0° an and d 18 180° 0° wh whil ilee th thee bl blad ades es of th thee ot othe herr propeller prope ller are at 90° and 270°. A stirrer stirrer shaft may be coupled to thee mo th moto torr by a fle flexi xibl blee sh shaf aftt or a su suit itab able le ar arra rang ngem emen entt of  pulleys. A1.1.2.6   Stove— Heat Heat shall be supplied to the cup by means of a prop properly erly designed designed stove which is equivalent to an air bath. The stove shall consist of an air bath and a top plate on which the flange of the cup rests. Bath—  h— The A1.1.2.7   Air Bat The air bat bath h sha shall ll hav havee a cyli cylindr ndrical ical interior and shall conform to the dimensional requirements in Fig. A1.1. A1.1.  The air bath may be either a flame or electrically heated metal casting (A1.1.2.8 (A1.1.2.8), ), or an electric-resistance element (A1.1.2.9 (A1.1.2.9)). In either case, the air bath must be suitab suitable le for use at the temperatures to which it will be subjected without deformation. A1.1.2.8   Heater, Flame or Electric— If If the heating element is a flame or an electric heater, it shall be so designed and used

10

D93 − 16a

mm A B C D E F G H IA J K L M N A

(in.)

mi n

max

(min)

(max)

1 8 .3 2 .3 8 7 .6 2 .0 0 .6 9 2 .0 6. 4 9 .6 4 3 .0 5 0. 0 . .. 1 .2 2 3 1. 8 7 .6

1 9 .8 3. 18 8. 4 2. 8 0. 79 2 .8 1 0 .4 11.2 4 6 .0 5 1. 6 0 .3 6 2 .0 6 4 4. 4 8. 4

(0.72) (0.094) (0.30) (0.08) (0.027) (0.08) (0.25) (0.38) (1.69) (1.97) (...) (0.048) (1.25) (0.30)

(0.78) (0.125) (0.33) (0.11) (0.031) (0.11) (0.41) (0.44) (1.81) (2.03) (0.014) (0.08) (1.75) (0.33)

Includes tolerance for length of thermometer given in Specification E1 Specification E1..

FIG. A1.4 Test Cup and Cover Assembly Assembly

11

D93 − 16a A2. MANUF MANUFACTURIN ACTURING G ST STANDARDIZ ANDARDIZA ATION OF THERMOMETER AND FERRULE

A2.1 The low-range low-range thermo thermometer meter,, which conforms conforms also to the spe specific cificatio ation n for the cup thermome thermometer ter in the tag clos closed ed tester (Test Method D56 Method  D56)) 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. Fig. A2.1) A2.1) to be used in the larger diameter collar of the Pensky-Martens apparatus. Differences in dimensions of these collars, which do not affect test results, are a source of unnecessary trouble to manufacturers and suppliers of instruments, as well as to users. A2.2 A2. 2 Dim Dimens ension ional al req requir uireme ements nts are sho shown wn in   Fig. A2.1. A2.1. Conformity Confor mity to the these se req requir uiremen ements ts is not man mandat datory ory,, but is desirab des irable le to use users rs as wel welll as sup suppli pliers ers of Pen Pensky sky-Ma -Marte rtens ns testers.

12

D93 − 16a

mm A B C D E F G H I J K L M N O P

(in.)

mi n

m ax

(min)

(max)

6 .2 0 1 7. 0 9 .8 0 11.92 1 .4 0 8 .5 6 1 2 .4 8 .5 6 8. 1 9 .9 8 .6 4 5 .1 1 7 .0 2 7. 4 7.11 9 .7 3

6 .5 0 1 8 .0 9 .8 5 1 2. 24 1 .6 5 8. 61 1 3 .0 8 .6 1 8 .6 1 0. 7 8 .6 9 5 .6 1 7 .5 2 8 .2 7 .1 6 9 .7 8

(0.244) (0.67) (0.386) (0.469) (0.055) (0.337) (0.49) (0.337) (0.32) (0.39) (0.340) (0.20) (0.67) (1.08) (0.280) (0.383)

(0.256) (0.71) (0.388) (0.482) (0.065) (0.339) (0.57) (0.339) (0.34) (0.42) (0.342) (0.22) (0.69) (1.11) (0.282) (0.385)

FIG. A2.1 Dimens Dimensions ions for Thermometer Thermometer Adapter, Adapter, Ferrule, and Packing Ring

A3. THERMOMETE THERMOMETER R SPECIFICATIONS SPECIFICATIONS

A3.1 A3. 1 See See Fig.  Fig. A3.1  a  and nd Tables  Tables A3.1-A3.4. A3.1-A3.4.

13

D93 − 16a

FIG. A3.1 Te Test st Gage for Checki Checking ng Enlargements Enlargements on Thermometers Thermometers TABLE A3.1 IP Thermometer Specifications

NOTE  1—The stem shall be made with an enlargement having a diameter of 1.5 mm to 2.0 mm greater than the stem and a length of 3 mm to 5 mm, the bottom of the enlargement being 64 mm to 66 mm from the bottom of the bulb. These dimensions shall be measured with the test gage shown in Fig. in  Fig. A3.1.. A3.1 Name Range Graduation Immersion, mm Overall length ±5 mm Stem diameter, mm B u l b s ha pe B u l b l e n g th , m m Bulb diameter, mm

Length of gradua graduated ted portion, mm Distance bottom of bulb to, mm L o n g e r l i n e s a t ea c h Figured at each E x p a n s i o n c h am b e r Top finish Scale error not to exceed ± S e e n o te s

IP 15C

IP 16C

IP 1 0 1 C

Pensky-Martens Low

Pensky-Martens High

Pensky-Martens Medium

−5 °C to + 110 °C 0 . 5 °C 57 290 6 .0 to 7 .0 cylindrical 9 to 1 3 n o t l e s s th a n 5 . 5 a n d not greater than s te m 1 40 t o 1 7 5

90 °C to 370 °C 2 °C 57 28 0 ± 1 0 6 .0 t o 7 . 0 cylindrical 7 to 1 0 n o t l e s s th a n 4 .5 a n d not greater than s t em 1 4 3 t o 18 0

20 °C to 150 °C 1 °C 57 2 90 6 .0 to 7 .0 cylindrical 9 to 1 3 n o t l e s s th a n 5 . 5 a n d not greater than s te m 1 4 0 to 1 7 5

0 °C 85 to 95 1 °C and 5 °C 5 °C required ring 0.5 °C

90 °C 80 to 90 10 °C and 20 °C 2 0 °C required ring 1 °C to 260 °C 2 °C above 260 °C 1 and Table and  Table A3.2 for A3.2  for emergent stem temperatures

20 °C 85 to 95 5 °C 5 °C required ring 1 °C

1 and Table A3.2 for A3.2  for emergent stem temperatures

14

1 and and Table  Table A3.2 for A3.2  for emergent stem temperatures

D93 − 16a       -     e     s     c     o     t      4      i     n     t     o     m     o      M      6      D     t     a      B     t

     t     n     e     m     e     g     r     a      l     n      E     m     e      t      S

     4     o     6      6     t      6

    A

     0  .      5

    A      5  .     o     0  .      2     t      5

     h      t     g     n     e      L

     L

     5  .      2

    o      t

     D      O

     5  .      K      7

    o      t

     5  .      8

     5  .     o     5  .      7     t      8

    o      t

     7      3      2

     7      5     o     4      2     t      2      2

     t         b      t     n      f      l      i     o     e     o    m     c     o     o     u     t     o      I      B     t      B      P

     t     n      i     e     o     l      P    a     c     e     S     c      I

    e     g     n     a      R    -     e     s     c      i     n      D     t     a

     H

     1      G      2      2

        b     e      t      f      l     o     n     t     o    m     a     o     o     u     t      i      B     t      B      L

    n     o      i      t     a     c     o      L     e      l     a     c      S

    e     c     n     a      t     s      i      D

    o      t

     C      °      0      6      3

     8      9

     6     o     9      8     t      9

     C      °      0      1      1

     F      °      2      3

     C      °      0

     F      °      0      8      6

     F      °      0      3      2

     D      O

    r     e     n      t      t     a     a     m     e      E     o     n    e      t      t     r      h     s     g

     h      t     g     n     e      L

     0  .      D      9

    o      t

     3      1

     0      0  .     o  .      8     t      0      1

    m     e     D      t      O      S

     0  .      C      6

    o      t

     0  .      7

     0  .     o     0  .      6     t      7

     l      h      t     a     g     5      t     o     n    ±      T    e      L

     7      B      8      2

     b      l     u      B

          n     n    m    r     a     o    a     e     p     i      h     b     x     s      E      C

     F      °      2      1      2

     C      °      0      0      1

     F      5      8

        t      l     o     e      f      b     n     t     o    m      i     o     u     t     a     o      t      B      B      L

     t         i     o      t      t     m     r     a     e     e    g     n      P     H     i

     l        a     i     p      i     c     r     n     o     e     c      i      t     p     s     n      S     I

 ,     e     r      l     x     a     o     a     r     c     r     m      S     E

    s     n     o      i      t     a     u      d     a     r      G

     6      6

 ,    -     e     s     c     o    p     x      i     n     t     o     a      J      D     t     a      T    m    -  ,     n    -     e     s     c     o     t      i      I      i     n     t     o     m     o    m      D     t     a      B     t

    n    r     o    e      i      t      b     c     a     r     m      t     a     n     h     o     C      C

    s     r     e  .      t     e     e     r     u     m      t     o     a     r     m     r  .     e     e    s     p      h    r     e    m      T     t     e     e     T      M    m    n      i      T     l      l     o      t      S     i      i      A    m    a     z     r     i     n     i     o      d     r      f     e    a      d     s    r     a     n     n     a     o    s     t      i      t     n     S     o     a     i     r     c    s     o      fi    n     f      i     c    e     3     e     i     m  .     p     d     3      A      S     l      l     e      l      2      A  .      3      b     a      A      T      E     e      L     e      B      S      A      T

    o      t

     5  .     o     0  .      4     t      6

     7      8      2      F      °      0      2      3

     C      °      0      6      1      M      T      S      A

    C

    r      M    o     F    m      T     C     0     m      M      S     0     1     7      M      I      A     1      5

    r     o     F    m      M     m      C     9     7     M      9      5     I

     C      °      5  .      0

     F      °      1

    B

    D

        h     c     m    r     e     t     a     a     u     b      E      N

     C      °      5

     F      °      0      1

     C      °      0      2

     F      °      0      5

    g     s      h     n     e     t     c     n    a     a     o     i      L     L      E

     C      °      1

     F      °      5

     C      °      0      1

     F      °      5      2

    s    -     n     o      b     i     u     i     s      S     i     v      d

     C      °      5  .      0

     F      °      1

     C      °      2

     F      °      5

   -     n    -     r     o     m    e     i      I     m    s

     7      5

     7      5

    r      t      t     o     s     e    a      F     T     e     g     n     a      R

    o      t      C      °      5    –

    r     e     e      M      T     b     d     n     m     m      S    u    a     a      A     N      N

     2      6         C      9

15

     C      °      0      1      1     +        y      k     s     n     e      P

    o      t      F      °      0      2      (

     )      F      °      0      3      2

    s      d     r      2     n    -     e     e     6     g     e     e     w    g      t      t        a     s     r     o    n     o     s     e     F     a     L    a     T     l      9      T      R      C      M

    o      )      t      C      F      °      F      °      C     °     o      0      0      °      7      0     t      0      0     3      (      2      0      7      9  ,         2     y     s    -     e     2     n      6     g     6    -      k        s     e     h     g    n     F      C    n     t     r      i     a     0      0     e     a     H     R      1      1     P     M

    e      h      t      d      l     u     o      h     s     s     e     c     n     a      t     s     m     u     c     r      i     c     o     n     r     e      d     n     u      d     n     a     ;     s     n     o  .      i      t      1  .     a     r      3      A     a     p  .     e     g     s      i      F     y     r     n     u      i     c     r     n     w     e     o     m      h     g     s     n     e      i     n     g      i     a      j     o     g      f      t     o     s     e     e      t     s     e     o      h     p      t     r     u      h      t     p      i     w     e      h      d      t     e     r     r     o     u      f     s      t     a     o     e     n     m     s      i     e      t      b      I  .      l      l     s     a     e      h     r     s      t     u      b     a      l     r     u     e      b     p     e     m      h     e      t      t      f     r     o     e      h     m      i     g     o      t      h      t      t     o     a      b      b     e      l      h     u      t      b     o      t     e      t      h     n      t     e      f     m     o     e     n     g      i     o     r      t     r     a      l     o     n      t     s     e      i      d     e      h      d      t      i      f     o     o     v     a     m     o     o      t  .      t      t     g     e     o     r      i     n      b     u     d     s     e     a     s      h      t     e    e     r     r     m     p    e  .     o     s     r     u     F     r      °      f  .     a     t     a     g      0     e     C     f     r     e     0     c     °     n     0     o    p     5     a     6     f     m    r      t     e      i      t     s     2     l     e     e      i     v     e      d    r     r     o     e      t     e    v     r     s      F     e      h      °     o     o      t      f      h     g     5      d     C      d     i  .     n     °     e     h     3     a     2     d     ;     e     F  ,     ;      i     v     h      t      t      °     o     n     C     e     0     e     °     r      0     p    v     0     m     o     5     s      6     e     2     i      b     o     g     a     t     r     o     r     e     a     t      b     d     p      l     e     u     n    p     m     e    u     a     t     a     F     e     C     h    e     °      h      t      °     c     h     5  .      f      1     n    e     2     o    :      i     o     b     :     r     s     r     r      h     e     o      t     o     r     r     n     t     r     g    r     a     n    e     p    e     e     e    e     x     m    e      l      l     e    o     l     a     e    a      h    c     n    m     r     c      T     S     A    e     S      t     D     A     B     C      h

D93 − 16a TABLE A3.3 Standardization Temperatures

NOTE  1—The emergent column temperatures are those attained when using the thermometers in the test equipment for which the thermometers were originally designed. In some cases these temperatures originally temperatures are markedly different different from those realize realized d durin during g standa standardizat rdization. ion. Temperature

Average Temperature of Emergent Column

Thermometer 9C (−5 °C to + 100 °C) 0 °C 1 9 °C 3 5 °C 2 8 °C 7 0 °C 4 0 °C 1 0 5 °C 5 0 °C IP 15C (−7 °C to 110 °C) 0 °C 1 9 °C 2 0 °C 2 0 °C 4 0 °C 3 1 °C 7 0 °C 4 0 °C 1 0 0 °C 4 8 °C

Temperature

Average Temperature of Emergent Column

Average Temperature of Emergent Column

Temperature

Thermometer 9F (20 °F to 230 °F) 3 2 °F 6 6 °F 100 °F 8 6 °F 160 °F 1 0 6 °F 2 2 0 °F 123 °F IP 15F (20 °F to 230 °F) 3 2 °F 6 6 °F 7 0 °F 7 0 °F 100 °F 8 6 °F 150 °F 1 0 4 °F 2 1 2 °F 118 °F

Thermometer 10C (90 °C to 370 °C) 100 °C 6 1 °C 2 0 0 °C 71 °C 3 0 0 °C 8 7 °C 370 °C 1 0 4 °C IP 16C (90 °C to 370 °C) 100 °C 6 1 °C 1 5 0 °C 6 5 °C 2 0 0 °C 71 °C 2 5 0 °C 7 8 °C 300 °C 8 7 °C 350 °C 9 9 °C

Temperature

Thermometer 10F (200 °F to 700 °F) 212 °F 141 °F 390 °F 159 °F 570 °F 180 °F 700 °F 220 °F IP 16F (20 °F to 700 °F) 200 °F 140 °F 300 °F 149 °F 400 °F 160 °F 500 °F 175 °F 600 °F 195 °F 7 0 0 °F 220 °F

TABLE A3.4 Specifications for Medium-Range Pensky-Martens ASTM No. 88F (88C) Vegetable Oil Flash Thermometer Name Reference Fig. No. Range For test at A Immersion, mm Graduations: S u b di v i s i o ns L o n g l i ne s at e a c h Numbers at each Scale error, max Special inscription

B C D E

F G

H I J K L M A

Expansion chamber: Permit heating to Total length, mm Stem OD, mm B u l b l e n gt h, m m Bulb OD, mm Scale location: B o tt o m o f b u l b to l i n e a t Distance, mm Length of graduated portion, mm Ice-point scale: Range Bott Bo ttom om of bu bulb lb to ic icee-po poin int, t, mm Contraction chamber: Dist Di stan ance ce to bo bott ttom om,, mi min, n, mm Dist Di stan ance ce to to top, p, ma max, x, mm Stem enlargement: OD, mm L e n g th , m m D i s ta n c e to b o t to m , m m Di

Medium-Range Pensky-Martens 5 50 °F–392 °F

10 °C–200 °C

57 1 °C 5 °C 1 0 °C 1 °C

2 °F 1 0 °F 2 0 °F 2 °F ASTM 88F (88C) 57 mm IMM

2 5 0 °C

4 9 0 °F 2 8 2 to 2 9 2 6 . 0 to 7 . 0 9 >stem

1 0 °C

5 0 °F 7 5 to 9 0 1 4 3 to 1 7 7

7 .5 t o 8 . 5 2.5 to 5.0A 6 4 to 6 6

Bulb OD shall be greater than 4.5 mm and less than the outside diameter of the stem (C).

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Average Temperature of Emergent Column

D93 − 16a A4. VERIFICA VERIFICATION TION OF APPARA APPARATUS TUS PERFORMA PERFORMANCE NCE

Certifi tified ed Refe Refere rence nce Mate Materia riall (CR (CRM) M)—CRM is a A4.1 Cer stable, pure (99 + mole % purity) hydrocarbon or other stable petroleum petrol eum product with a metho method-spe d-specific cific flash point established by a method method-speci -specific fic interl interlaborat aboratory ory study follo following wing ASTM RR:D02-1007 guidelines or ISO Guide 34 and 35.

for each material of the current production batch. Calculation of the limits for these other CRMs can be determined from the reproducibility value of these test methods multiplied by 0.7. This value provides a nominal coverage of at least 90 % with 95 % confid confidence. ence.

A4.1.1 A4. 1.1 Valu alues es of the flas flash h poi point nt cor correc rected ted for bar barome ometri tricc pressure for some reference materials and their typical limits are given in Table in  Table A4.18 (see (see Note  Note A4.1). A4.1). Suppliers of CRMs will prov provide ide certific certificates ates stating the method method-speci -specific fic flash point

NOTE A4.1—Materials, purities, flash point values, and limits stated in Table A4.1 A4.1   were dev develo eloped ped in an AST ASTM M int interl erlabo aborat ratory ory pro progra gram m to determ det ermine ine sui suitab tabilit ility y of use for ver verific ificati ation on flui fluids ds in flas flash h poi point nt tes testt methods. Other materials, purities, flash point values, and limits can be suitable when produced according to the practices of ASTM RR:D021007 100 7 or ISO Gui Guides des 34 and 35. Cer Certifi tificat cates es of per perfor forman mance ce of suc such h materials should be consulted before use, as the flashpoint value will vary dependent on the composition of each CRM batch.

8 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:S15-1010.

Secondary dary Working Standard Standard (SWS)—SWS is a A4.2 Secon stable, pure (99 + mole % purity purity)) hydro hydrocarbo carbon, n, or other petro petro-leum product whose composition is known to remain appreciably stable.

TABLE A4.1 D93 Typical Flash Point Values and Typical Limits for CRM

NOTE  1—Supporting data for the interlaboratory study to generate the flash point in Table in  Table A4.1 can A4.1  can be found in research report RR:S15-1010.8 Hydr Hy droc ocar arbo bon n n –decane n –undecane n –tetradecane n –hexadecane

Puri Pu rity ty,, mo mole le %

Flas Fl ash h Po Poin int, t,°°C

Tolerance Limits (0.7R), °C

99 + 99 + 99 + 99 +

5 2 .8 6 8 .7 1 0 9 .3 1 3 3 .9

2 .6 3 .4 5 .4 6. 7

A4.2.1 Establish A4.2.1 Establish the mea mean n flas flash h poi point nt and the statist statistical ical contro con troll limi limits ts (3σ) fo forr th thee SW SWS S us usin ing g st stan anda dard rd st stati atisti stical cal 9 techniques. (See ASTM MNL 7).

9  Manual on Presentation of Data and Control Chart Analysis, ASTM MNL, 6th ed., ASTM International, W. Conshohocken, 1990.

APPENDIXES (Nonmandatory Information) X1. FLASH POINT MASKING MASKING PHENOMENON

X1.1 A condition condition during flash point testing can occur with certain mixtures whereby the nonfl nonflammable ammable component component of the sample tends to inert the vapor space above the liquid, thus preventing a flash. Under this condition, the flash point of the material is masked resulting in the reporting of incorrect high flash point or no flash point.

test flame fro from m blu bluee to yel yellow low-or -orang angee lam lamina inarr flam flamee is observed. X1.4 Under this condition, condition, continued heating and testing for flash point at temperatures above ambient temperature, have resulted in significant burning of the ignitable vapor outside the test cup, often above the test flame. This can be a potential fire hazard if not recognized.

X1.2 This flash point masking phenomenon most frequently frequently occurs with ignitable liquids that contain certain halogenated hydrocarbon hydro carbonss such as dichlo dichlorometh romethane ane (methy (methylene lene chlor chloride) ide) and trichloroethylene.

X1.5 It is recommended recommended that if this condition is encountered encountered during the flash point testing of these type of materials, testing should be discontinued.

X1.3 Und X1.3 Under er thi thiss con condit dition ion,, no distinct distinct flas flash h as defi defined ned in 3.1.5   of these test methods is observed. Instead a significant enlargement of the test flame and a change in the color of the

X1.6 Furth Further er commentaries commentaries regarding flash point test and flammability of mixtures can be found in Test Method  E502  E502..

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D93 − 16a X2. FLASH POINT TEST AND FLAMMABILITY FLAMMABILITY OF MIXTURES

X2.1 While X2.1 While th thee fla flash sh po poin intt ca can n be us used ed to in indi dica cate te th thee flammability of liquid materials for certain end uses, flash point does do es no nott re repr prese esent nt th thee mi mini nimu mum m tem tempe pera ratu ture re at wh which ich a material can evolve flammable vapors.

flammable flammab le vap vapors ors und under er cer certain tain con conditi ditions ons and yet will not exhibit exh ibit a clo closese-cup cup flash point. point. Thi Thiss phe phenom nomeno enon n is not noted ed when a nonflammable component is sufficiently volatile and present in sufficient quantity to inert the vapor space of the close clo sed d cu cup, p, th thus us pr prev even entin ting g a fla flash sh.. In ad addi ditio tion, n, th ther eree ar aree certain instances where an appreciable quantity of the nonflammable component will be present in the vapor, and the material will exhibit no flash point.

X2.2 The X2.2 There re are ins instan tances ces with pure mate materia rials ls whe where re the abse ab senc ncee of a fla flash sh po poin intt do does es no nott en ensu sure re fr free eedo dom m fr from om flammab flam mabilit ility y. Inc Includ luded ed in this cate categor gory y are mate materia rials ls tha thatt require large diameters for flash propagation, such as trichloroethylene. This material will not propagate a flame in apparatus the size of a flash point tester, however, its vapors are flammable and will burn when ignited in apparatus of adequate size.

X2.4 Liq X2.4 Liquid uidss con contain taining ing a hig highly hly vol volatil atilee non nonflam flammab mable le component or impurity, which exhibit no flash point because of  the influence of the nonflammable material, may form flammable mixtures if totally flash vaporized in air in the proper proportions.

X2.3 When a liquid contains flammable and nonflammable nonflammable compon com ponent ents, s, the there re are cas cases es whe where re thi thiss liq liquid uid can evo evolve lve

SUMMARY OF CHANGES Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue (D93 – 16) that may impact the use of this standard. (Approved Oct. 1, 2016.) and Table  Table A4.1. A4.1. (1)  Updated subsection  A4.1.1 and

8.2   regarding sampling. (2)  Updated subsection 8.2

Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue (D93 – 15a) that may impact the use of this standard. (Approved June 1, 2016.) (1)  Updated definition of   flash point .

Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue (D93 – 15) that may impact the use of this standard. (Approved Oct. 15, 2015.) (1)   Added new 10.6 new  10.6.. (2) The format format of SI uni units ts (an (and d non non-SI -SI units) were rev revised ised editorially throughout. ASTM International International takes no positi position on respecting the validi validity ty of any patent rights assert asserted ed in connec connection tion with any item mentio mentioned  ned  in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk  of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and  if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards  and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the  responsible respon sible technical technical committee, which you may attend. If you feel that your comments have not receiv received ed a fair hearing you should  make your views known to the ASTM Committee on Standards, at the address shown below. This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above  address addr ess or at 610610-832832-9585 9585 (pho (phone), ne), 610610-832832-9555 9555 (fax (fax), ), or serv service@ ice@astm astm.org .org (e-m (e-mail) ail);; or thro through ugh the ASTM webs website  ite  (www.astm. (www .astm.org). org). Permission Permission rights to photocopy the standa standard rd may also be secure secured d from the Copyri Copyright ght Clearance Center, Center, 222  Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/ 

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