“This tterostonelsondand as se 1 the etl x Sanda and Qa ( il ‘West Conshohocken, Pennsylvania | MAB Zig ses fei. Ts ibs et Bat) Tan ed Hie 19428-2858, | ee Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure’ “This nda sued under the ied designation DG esa immediately fellowing the esgnatonndetes the yar fia ‘Hopton or inthe eas fs, the year Flt revs, Amb in pce inte the year f ht eapponal sapere train (e) inc an ei change since the lst revision oF oppo ‘This standard hasbeen approved for nae hy agencies ofthe US Deparment of Defense L. Scope* 1.1 This test method covers the atmospheric distillation of | ppettaleum products and liquid fuels using a laboratory batch distillation unit to determine quantitatively the boiling range characteristics of such praduets as light and middle distillates, automotive spark-ignition engine fuels with or without oxy- ‘genates (see Note 1), aviation gasolines, aviation turbine fuels, diesel fuels, biodiesel blends up to 20 %, marine fuels, special petroleum ‘spirits, naphthas, white spirits, kerosines, and Grades 1 and 2 bumer fuels. [Note 1—Aa interlaboratory study was conducted in 2008 involving 11 ferent laboratories submitting 15 datasets and 15 differen sanples of cethanol-fel blends containing, 25 % volume, $0 % volume, and 75 5 ‘volume ethanol, The results indicate thatthe repeatability imits of these stunples are comparable or within the published repeatability of the method (th the exception of FBP of 75 % ethanol-fuel blends). On this basis, it can be concluded that Test Method D86 is applicable to Ihanolfel blonds such a E75 and EBS (Speciation DS798) or other thanol-foel blends with preter than 10-9 volume ethanol, Ses ASTM, RRDO2-1654 for supporting data" 1.2 ‘The test method is designed for the analysis of distillate fuels; it is not applicable 10 products containing appreciable ‘quantities of residual material. 1,3 This test method covers both manual and automated instraments. 1.4 Unless otherwise noted, the values stated in SI units are to be regarded as the standard. The values given in parentheses are provided far information only. 1.5 WARNING—Mercury has been designated by many regulatory agencies as a hazardous material that can cause central nervous system, kidney and liver damage. Mercury, of "his tet mato i ube the jutedon of ASTM Commitee DO2 on ‘lou Prods, Ligid Fak, and besa ds the dec responsi af Sbeommitce D020 en Vols. ne he equivalent est tod eps vader the dsignton I 2. Wise the jason of the Sandton Commie: Current edition approved My", 2017, Pulished June 2017. Oxignlly snprved in 1921 Las pevios eiion approved in 2016 as 036162. DOH Int se0ang- 17, ® Supporting dala have hen fed a ASTM ItratinatHeodques and my be btn by requesting Research Report RRM 194 fee ey es a ee Mee canon shoud taken when anling mse) ead ay conaling pur. See the applet ped Ma aa Seen bas Sect (MSDS) for etal and EFAS Aapalis Ricca vlaarerp fugit Te We ior teat Heald to aweroue slog a essing poaca a you sais Pot gy OA soy 6 pele by te “thly ? 6 Th standard does wot purpon 10 odessa of BALL Pited oolesmar perigee rourgr Ket ee iy ofthese of ths ender to estalsh fs nie priate safety and health practices and detennine the applica. Dility of regulatory limitations prior fo use. TF en 17 This international standard was developed in «car ——— dance with internationally recognized principles on standard teation established in the Decision on Principles for the Development of International Standards, Guides and Recon: ‘mendations issued by the World Trade Organization Technical Barriers 1o Trade (TBT) Commitee. 2, Referenced Documents 2.1 All standards are subject to revision, and parties to agreement on this test method are to apply the most recent edition of the standards indicuted below, unless otherwise specified, such as in contractual agreements or regulatory rules where earlier versions of the method(s) identified may be required. 2.2. ASTM Standards:* 'D97 Test Method for Pour Point of Petroleum Products 'D323 Test Method for Vapor Pressure of Petroleum Products (Reid Method) 14057 Practice for Manval Sampling of Petroleum and Petroleum Products 'D4175 Terminology Relating to Petroleum Products, Liquid Puels, and Lubricants “or refrened ASTM sand, vis ibe ASTM website, wuneasi. org. oF -onlct ASTM Caster Sesce at sersice asim. For Ania Book of ASTM ‘Strdands vol norman, fer the slatdat's Document Saninay page O° (te ASTM webs +4 Summary of Changes section appears atthe end of this standard ops © AS mana 10 8a Ha Oi, FO Sox C700, Wet Cncatote, PA E2248 Ud SesAy vss - 17 1D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products 1D4953 Test Method for Vapor Pressure of Gasoline and Gasoline-Oxygenate Blends (Dry Method) 1DS190 Test Method for Vapor Pressure of Petroleum Prod- uucts (Automatic Method) (Withdrawn 2012)* S191 Test Method for Vapor Pressure of Petroleum Prod- ucts (Mini Method) 1DS798 Specification for Ethanol Fuel Blends for Flexible- Fuel Automotive Spark-Ignition Engines DS842 Practice for Sampling and Handling of Fuels for Volatility Measurement 1DS949 ‘Test Method for Pour Point of Petroleum Products (Automatic Pressure Pulsing Method) 15950 Test Method for Pour Point of Petroleum Products, (Automatic Tilt Method) S985 Test Method for Pour Point of Petroleum Products, (Rotational Method) 1D6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lubricants 16708 Prectice for Statistical Assessment and Improvement ‘of Expected Agreement Between Two Test Methods that Purport to Measure the Same Property of a Material E1 Specification for ASTM Liquid-in-Glass Thermometers E77 Test Method for Inspection and Verification of ‘Ther- mometers E1272 Specification for Laboratory Glass Graduated Cylin- ders E1405 Specification for Laboratory Glass Distillation Flasks, 23 Energy Institute Standards:® LP 69 Determination of Vapour Pressure—Reid Method IP 123 Petroleum Products—Determination of Distillation Characteristics IP 394 Determination of Air Saturated Vapour Pressure IP Standard Methods for Analysis and Testing of Petroleum and Related Products 1996—Appendix A. 3. Terminology 3.1 Definitions: 3.te1 decomposition, n—of « hydrocarbon, the pyrolysis or cracking of a molecule yielding smaller molecules with lower boiling points than the original molecule 3.1.2 decomposition point, n—in distillation, the corrected teinperatute reading that coincides with the frst indications of {hetmal decomposition ofthe specimen, 3.1.3 dry point, n—in distillation, the corrected temperature reading at the instant the last drop of Liquid evaporates from the Towest point in the las. 3.14 dynamic holdup, in D86 distillation, the amount of ‘material present in the neck of the flask, inthe sidearm of the Mask, and in the condenser tube during the distillation, “The lat approved version of this hitvcal sanded is reeeaced on aailbe fom Kacey lst, 61 New Cavendish St, London, WIG TAR, U.K. epi enereynt ong 3.1.5 emergent stem effect, n—the offset in temperature reading caused by the use of total immersion mercury-in-glass thermometers in the partial immersion mode. 3.1.5.1 Diseussion—In the partial immersion mode, a por- tion of the mercury thread, that is, the emergent portion, is at a lower temperature than the immersed portion, resulting in a shrinkage of the mercury thread and a lower temperature reading, 3.1.6 end point (EP) or final boiling point (FBP), n—the ‘maximum corrected thermometer reading obtained during the test 3.1.6.1 Discussion—This usually oceurs after the evapora- tion of all liquid from the bottom of the flask, The term ‘maximum temperature is a frequently used synonym, 3.1.7 front end toss, n—toss due to evaporation during transfer from receiving cylinder to distillation flask, vapor loss «during the distillation, and uncondensed vapor in the flask at the end of the distillation 3.1.8 fuel ethanol (Ed75-Ed85), n—blend of ethanol and hydrocarbon of which the ethanol portion is nominally 75 % to 85 % by volume denatured fuel ethanol D475 3.1.9 initial boiling point (IBP), n—in D86 distillation, the corrected temperature reading at the instant the first drop of condensate falls from the lower end of the condenser tube. 3.1.10 percent evaporated, n—in distttation, the sum of the percent recovered and the percent loss, 3.1.10.1 percent foss, 1 in distilation, one hundred minus the pereent total recovery. 3.1.10.2 correeted loss, n—percent loss corrected for baro- metric pressure. 3.1.11 pereent recovered, n—in distillation, the volume of ‘condensate collected relative to the sample charge. 3.1111 percent recovery, n—in distillation, maximum per- cent recovered relative to the sample charge. 3.L.11.2 corrected percent recovery, n—in distillation, the petcent recovery, adjusted for the corrected pereent Toss 3.1.11.3 percent total recovery, n—in distillation, the com- bined percent recovery and percent residue, 3.1.12 percent residue, n—in distillation, the volume of residue relative to the sample charge, 3.1.13 rate of change (or slope), n—the change in tempera ture reading per percent evaporated or recovered, as deseribed in 13.2. 3.1.14 sample charge, n—the amount of sample used in a test 3.1.15 temperature lag, n—the offset between the tempera ture reading obtained by a temperature sensing device ancl the true temperature at that time, 3.1.16 semperaure measurement device, n—a thermometer, 1s described in 6.3.1, or a temperature sensor, as described in 63.2, 3.1.16.1 temperature reading, n—the temperature obtained by a temperature meusuring device or system that is equal t0 the thermometer reading described in 3.1,16.3,fly ves - 17 3.1.16.2 corrected temperature reading, n—the temperature reading, as described in 3.1.16.1, corrected for barometiic pressure. 3.1.16.3 thermometer reading (or thermometer result), ‘nthe temperature ofthe saturated vapor measured in the neck ff the flask below the vapor tube, as determined by the prescribed thermometer under the conditions of the test 31.164 corrected thermometer reading, n—the thermam= ‘ter reading, as described in 3.1.16.3, corrected for barometric pressure. 4, Summary of Test Method 4.1 Based on its composition, vapor pressure, expected IBP or expected EP, or combination thereof, the sample is placed in fone of four gtoups. Apparatus arrangement, condenser ‘temperature, and other operational variables are defined by the ‘group in which the sample falls, 4.2 A 100mL specimen of the sample is distilled under prescribed conditions for the group in which the sample falls. ‘The distillation is performed in a laboratory batch distillation unit at ambient pressure under conditions that are designed to provide approximately one theoretical plate fractionation. Sys- tematic observations of temperature readings and volumes of condensate are made, depending on the needs of the user of the data, ‘The volume of the residue and the losses are also recorded 43 At the conclusion ofthe distillation, the observed vapor temperatures can be corrected for barometric pressure and the data are examined for conformance to procedural requirements, such as distillation rates. The test is repeated if any specified condition has not been met. 4.4 Tost rsulls are commonly expressed a8 percent evapo- rated or percent recovered versus corresponding temperature, cither in a table or graphically, as a plot of the distil 5. Significance and Use 5.1 The basic test method of determining the bo of a petroleum product by performing a simple batch di tion hs been in use as long as the petroleum industry has existed. It is one of the oldest test methods under the jurisdi- tion of ASTM Committee DO2, dating from the time when it ‘vas still referred to as the Engler distillation. Since the test method has been in use for such an extended period, a {emendous number of historical data bases exis for estimating end-use sensitivity on produets and processes. 5.2 The distillation (volatility) characteristics of hydrocar bons have an important effect on their safety and performance, ‘especially in the case of fuels and solvents. The boiling range gives information on the composition, the properties, and the behavior of the fuel during storage and use. Volatility is the ‘major determinant ofthe tendency af a hydrocarbon mixture to produce potentially explosive vapors 5.3 The distillation characteristics are critically important, for both automotive and aviation gasolines, affecting starting, Warm-up, and tendeney 10 vapor lock at high operating, Burner =) remeron 6 FIG. 1 Apparatus Assembly Using Gas Burner temperature or at high altitude, or both, The presence of high point components in these and other fuels can signifi- canily affect the degree of formation of solid combustion deposits. 54 Volatility, as it affects rate of evaporation, is an impor tant factor in the application of many solvents, particularly those used in paints. 55 Disillation limits are often included in petroleum prod- uct specifications, in commercial contract agreements, process refinery/control applications, and for compliance to regulatory rules. 6. Apparatus 6.1 Basic Components of the Apparatus: 6.1.1 The basie components of the distillation unit are the distillation flask, the condenser and associated cooling bath, metal shield or enclosure for the distillation flask, the heat souree, the lask support, the temperature measuring device, and the receiving cylinder to collect the distillate. 6.1.2 Figs, | and 2 are examples of manual distillation units. 6.1.3 Inaddition tothe basic components described in 6.1.1 automated units also are equipped with a system to measure ‘and automatically record the temperature and the associated recovered volume in the receiving cylinder. 62 A detailed description of the apparatus is given in Annex Ad. 63 Temperature Measuring Device: 6.3.1 Mercury-in-glass thermometers, if used, shal be filled with an inert gis, graduated on the stem and enamel backed. ‘They shall conform to Specification E1 or IP Standard Methods for Analysis and Testing of Petroleum and Related Products oi al 5 fal,Front view Condenser ba) 28a coer {-Baih tergerauro sensor 48h ovariow 5-8an ain {&-Conconver ube shel B-Viowing window a-Volage regulator ‘9-Vainaar eset ‘Power suites ‘Power igh cate so-ven 16-Ehcto heer 17-700 or acting ve 1 soppn patio 18-Powe sous cord {0 RocoWver eyindsr 20-Recelve ooing bath 2i-Recover cara FIG. 2 Apparsius Assembly Using Electr Heaterfly bos - 17 im I [Be Fa 1 mensions in min FIG. 8 PTFE Contering Device for Ground Glass Joint 1996—Appendix A, or both, for thermometers ASTM 7CAP SC and ASTM 7F for the low range thermometers, and ASTM 8C/IP 6C and ASTM 8F for the high range thermometers, 6.3.1.1 Thermometers that have been exposed for an ex- tended period above an observed temperature of 370°C shall not be reused without a verification ofthe ice point or checked as prescribed in Specification E1 and Test Method E77, g of 370°C, the tempera- ture of the bulb is approsching. a eritical range in the glass snd the thermometer may lose Xs caltzation, 6.3.2 Temperature measurement systems other than those described in 6.3.1 are satisfactory for this test method, pro- vided that they exhibit the same temperature lag, emergent stom effect, and accuracy as the equivalent mercury-in-glass thermometer. 6.3.2.1 ‘The electronic circuitry or the algorithms, or both, used shall include the capability to simulate the temperature lag of a mercury-in-glass thermometer, 6.3.2.2 Alternatively, the sensor can also be placed in a ceasing with the tip of the sensor covered so that the assembly, because of its adjusted thermal mass and conductivity, has « temperature lag time similar t0 that of a mercury-in-glass thermometer. Nore 3-In a region where the temperature is changing ropidly during the distin, the temperature Jag ofa thermometer ean be as iach a8 3 6.3.3 In case of dispute, the referee test method shall be carried out with the specified mercury-in-glass thermometer 64 Temperature Sensor Centering Device 6.4.1 The temperature sensor shall be mounted through @ snug-fitting device designed for mechanically centering the sensor in the neck of the flask without vapor leakage. Examples ‘of acceptable centering devices are shown in Figs. 3 and 4, (Warning—The use of a plain stopper with a hole drilled through the center is not acceptable for the purpose deseribed in 64.1), Nore 4—Other centering devies ae also acceptable, a8 long. a they postion and bold the temperature sensing device in the proper postin it the neck of the dstiltion column, as showin Fig. Sane deseribed in os, [Nore $—When running the test by the manual metho, products with 8 low IBP may have one or more readings obscured by the centering device. See ako 10.14.31, Drilled out to fit. Pt 100 Probe Compression Nut (PTFE) Cone-shaped for —~ perfect centering in neck of distillation flask Compression without O-ring Single O-ring Viton or perfluoro elastomer FIG, 4 Example of Centering Device Designs for Straight Bore ‘Neck Flasks FIG. § Position of Thermometer In Distillation Flask 6.5 Automated equipment manufactured in 1999 and later shall be equipped with a device to automatically shut down power to the unit and to spray an inert gas or vapor in the chamber where the distillation flask is mounted in the event of fir. Nore Sone causes of fires are breakage of the disilition Ms, elec shorts an oaming ad sping of ii sampetroggh hs op pening of he Mask 6.6 Barometer—A pressure measuring device capable of measuring loca station pressure with an accuracy of 0.1 KPa (mm Ha) or better, atthe same elevation relative to ea level as the apparatis inthe laboratory. (Warning—Do not take readings from ordinary aneroid barometers, suchas those used at weather stations and aiport, since these ae precorected to give sea level readings.)ly ves - 17 TABLE 1 Group Characteristics ‘Group Goup? Grau Gioape Semple ‘crates Ditlare ype Vapor pressure at 78°C, Ha O55 ss ass 00°F, psi 25 95S 8 {fest Methods 0923, 04959, 05190, 05131, (5642, 69 oP 304) Dietation 18°C 100100 "F Se ae ec 3250 525052803280 Ea Saag S402 Sane Sa ‘Sampling, Storage, and Sample Conditioning 7.1 Determine the Group characteristics that correspond to the sample to be tested (see Table 1). Where the procedure is dependent upon the group, the section headings will be so marked 7.2 Sampling: 7.2.1 Sampling shall be done in accordance with Practice 14057 or D177 and as described in Table 2. 7.2.1.1 Group 1—Condition the sample container to below 10°C, preferably by filling the bottle with the cold liquid sample and discarding the first sample. If this is not possible ‘because, for instance, the product to be sampled is at ambient temperature, the sample shall be drawn into a bottle prechilled to below IDSC, in such a manner that agitation is Kept at a ‘minimum, Close the bottle immediately with a tight-fting closure, (Warning—Do not completely fill and tightly seal a cold bottle of sample because of the likelihood of breakage on warming.) 7.2.1.2 Groups 2, 3, and 4—Collect the sample at ambient temperature, After sampling, close the sample bottle immedi- ately with a tight-fiting closure, 7.2.1.3 If the sample received by the testing laboratory has ‘been sampled by others and itis not known whether sampling has been performed as described in 7.2, the sample shall be assumed! to have been so sampled. 7.3 Sample Storage: 7.3.1 If testing is not to start immediately after collection, store the samples as indicated in 7.3.2, 73.3, and Table 2. All ‘samples shall be stored away from direct sunlight or sources of direct heat. 73.2 Group IStore the sample at 2 temperature below 10°C. [Nowe 7—If there are no, or inadequate, facilites for storage below HOC, the sample may aso be sfored at a temperature below 20°C, provided the operator ensures thatthe sample container is ight closed nd leakeee 7.3.3 Group 2—Store the sample at a temperature below 10°C. Nore 8—it there are no, o inadequate, facilities for 1W°C, the sample may also be stored at tempera provided the operator ensues thatthe sample eonaince fs ight closed tnd leaksie, 7.34 Groups 3 and 4—Store the sample at ambient or lower temperature, 7.4 Sample Conditioning Prior to Analysis: 74.1 Samples. shall be conditioned to the temperature shown in Tuble 2 before opening the sample container. 7.4.14 Groups I and 2—Samples shall be conditioned to a temperature of less than 10°C (50°F) before opening the sample container, except when the sample isto be immediately tested and is already at the prescribed sample temperature in ‘Table 3, 74.1.2. Groups 3 and 4—If the sample isnot fluid at ambient temperature, itis to be heated to a temperature of 9 °C 10 21 °C above its pour point (Test Method D97, D5949, or D5985) prior to analysis. If the sample has partially or completely solidified during storage, it shall be vigorously sheken after melting prior to opening the sample container to ensure homogencity. 74.1.3 If the sample is not flvid at room temperature, the temperature ranges shown in Table 2 for the flask and forthe sample do not apply. 15 Wet Samples: 7.5.1. Samples of materials that visibly contain water are not suitable for testing. If the sample is not dry, obtain another sample that is free from suspended watet. 7.5.2 Groups I and 2—If such a sample cannot be obtained, the suspended water can be removed by maintaining the sample at 0°C to 10 °C, adding approximately 10 g of anhy- 4rous sodium sulfate per 100 mL of sample, shaking the mixture for approximately 2 min, and then allowing the mi ture to setle for approximately 15 min, Once the sample shows, no visible signs of water, use a decanted portion of the sample, ‘maintained between 1 °C and 10 °C, for the analysis. Note in the report that the sample has been dried by the addition of = desiccant Nore 9-Suspended water in hazy samples in Groups 1 and 2 ean be ‘emoved by the addition of anhydrous sodium sulfate and separating the liquid sample from the dying, agent by decanting without stalsiealy allecting the results of the test® 7.83 Groups 3 and 4—In cases in which a water-free sample is not practical, the suspended water can be removed by shaking the sample with anhydrous sodium sulfate or other suitable drying agent and separating it from the drying agent by ‘decanting. Note in the report that the sample has been dried by the addition of a desiccant. 8, Preparation of Apparatus 8.1 Refer to Tuble 3 and prepare the apparatus by choosing the appropriate distillation flask, temperature measuring device, and flask support board, as directed for the indicated ‘group. Bring the temperature of the receiving cylinder, the flask, and the condenser bath to the indicated temperature, 8.2 Make any necessary provisions so that the temperature fof the condenser bath and the receiving cylinder will be ‘maintained at the required temperatures. The receiving cylin- ler shall be in a bath such that either the liquid level is at least as igh as the 100 mL. mark or the entite receiving cylinder is surrounded by an air circulation chamber, © Suppo dita hve been is at ASTM oration! Hendon andy be obey requesting Research Rept RRDOD-14,Ay ve TABLE 2 Sampling, Storage, 6-17 land Sample Coneltioning ‘Gopi Group? Grows Goons Tamporiur of canple bao © “10, * 0, “emporature of ered comple © s10* <0 ‘ambien ambient * “0! <3 ‘ambient ‘aitiont Temperature of sample ater © a0" io" ‘bien! oF airblentot condoning prior to ana '9°C 021°C cbove peu pant + <0 <0 ‘ambient or ‘bon or 48°F 10 70°F abowe pour point I sample is wot resampla rosampio ‘hy accodarce wth 7.53, itrasengl ssl wet? ‘dyin acondance wih 7.52 “Under eran ceumstancos, empl ean alco bo etred al torporatres blow 20°C (68°) cai presrbad in Tal 9,8 TABLE 9 Preparation of Apparatus and Specimen Gop ‘Geum? Gos Gems Fisk ni 135 125 25 25 ASTA dation theenometar rer, reur) a) scr 1 dtlatonthrmometer range ‘ow ‘ow tow high Frask euppot boas . s c c ‘te of hele, mn 8 2 0 50 Tomportu at lt fest ask © s9.0 118 118 rot above * 55-65 55-65 55-55 ‘ambient Flask uppon end lls at oboe ot above rot above ‘ambient ‘ambient ‘bert ecelvngeylnde and eagle “c soe isist taanbiea - 55-65 e508 ss-ambiea" See 103011 or eneptons 8.2.1 Groups 1, 2, and 3—Suitable media for low tempera {ure baths include, but are not limited to, chopped ico and ‘water, refrigerated brine, and refrigerated ethylene glycol 8.2.2 Group 4—Suitable media for ambient and higher bath temperatures include, but are not limited to, cold water, hot water, and heated ethylene glycol 8.3 Remove any residual liquid in the condenser tube by swabbing with epicce of soft, lint-free cloth attached to cord or wie, 9, Calibration and Standardization 9.1 Temperature Measurement System—Temperatare mea- surement systems using other than the specified mercury-in- lass thermometers shall exhibit the same temperature lag, emergent stem effect, and accuracy asthe equivalent mercury- in-glass thermometer. Confirmation of the calibration of these temperature measuring systems shall be made at intervals of Not more than six months, and after the system has boen replaced or repaired. 9.1.1 The accuracy and the calibration of the electronic circuitry or computer algorithms, or both, shall be vetted by the use of a standard precision resistance. bench, When pee- fouming tis verification, no algorithms shall be wed to correct the temperature for lag and the emergent stem effect (see ‘manufacturer's instruction). 9.1.2 Verification of the ealibration of temperature measur ing devices shall be conducted by distilling toluene in accor ance with Group 1 of this test method and comparing the ‘50% recovered temperature with that shown in Table 4, 9.1.2.1 If the temperature reading is not within the values shown in Table 4 for the respective apparatus being used (see Noto 11 and ‘Table 4), the temperature measurement system shall be considered defective and shall not be used for the test Nowe 10—Toluene is used aa verifieaton Mid fr calibration; twill yield almost 0 information on how well an elctonic measurement System simlates the temperature lag of liguidin-ass thermometer. 9.1.2.2 Reagent grade toluene and fhexadecane (cetane), ‘conforming to the specifications of the Committee on Analyt ‘eal Reagents of the American Chemical Society, shall be used. However, other grades may also be used, provided it is frst ascertained that the reagent is of sufficient purity to permit its use without Tessening the accuracy of the determination Nore I—At 101.3 kPa, toluene is shown in reference manuals as Doling at 10.6 °C when measured using & partial immersion thermon eter. Because this west method uses thermosneters. calibrated fer total Tnnmetson, the results (pically will be lower and, depending on the > Suppor date have ben fila t ASTM Intron Headquarters a nay te obtained by requctng Reacarch Report RR‘DOD 1580. "reagent Chemicals. Auerican Chemical Society Specifeuions, Aevican ‘Chemical Soses, Washngon, DC Fe Suggestions onthe testing of reagents rt Tsted by the American Chemical Soi, se Amina Stands for Labraery CChomial, BDH Lid Pole, Dor, Ua the United Sates Pharaacopcia ‘and National Formulary, US. Prarmaceeil Convention, Ie (USPC), Rosi % % "Aly 086 - 17 TABLE 4 True and Min and Max D86 $0 % Recovered Bolling Points (°CY* Manual ‘Aion Diniaton oe Daten DisiaTen a Dian cor ders min Oo condone Yer min 066 ‘one mae ‘50% bong ‘max O86 ‘s0%sboIng 089505 bot Point 50% teling point ng pit ASTIN we bot Gop) zara Group 1.2 Grow Zand eID Te, Teduene ng pol 3 rr 3 sna oe 059 18 7085 ‘007 ASTHMA tbo Groups rows Croup 4 Grom 4 Hexasneane Ing point 2810 2a aT ae aa ‘=the manual an avomated onperaures show ns abe are he velies fr ta 05 trance lava or ha 99% poulaton coverage, The proposed Wlrence \s approximately sa. Ifomaton cn the vahes hte can be found in RFD22-890, ‘thermometer and the situation, may be diferent foreach thermometer At 101.3 KPa, heradecane is shown in reference manuals boiling. 287.0 °C whon measured using 2 partial immersion thermometer. Because itis test method uses thermometers etibated for total immersion, the resuls(ypclly will be lower, and, depending onthe thermomeler and the ‘Station: may be efferent foreach thermometer, 9.1.3 A procedure (0 determine the magnitude of the tem: perature lag is described in Annex A3, 9.1.4 A procedure to emulate the emergent stem effect is described in Appendix XA. 9.1.5 To verify the calibration of the temperature measure ‘ment system at elevated temperatures, use hexadecane. The femperature measurement system shall indicate, at 50% recovered, a temperature comparable to that shown in Table 4 for the respective apparatus under Group 4 distillation condi tions, Nore 12—Because of the high melting point of bexadecane, Group 4 verfeation disillaions will have to be’ earied out with condenser femperatures 520°C. 9.2 Automated Method: 9.2.1 Level Follower—For an automated distillation apparatus, the level follower/recording mechanism of ‘the apparatus shall have a resolution of 0.1 S volume or better with a maximum error of 0.3 % volume between the 5 4% and 100 % volume points. The calibration of the assembly shall be verified in accordance with manufacturer’s instructions at intervals of not more than three months and after the system has been replaced or repaired, Nore 13—The typical caliation procedure involves verifying the curpat with the receiver containing 5% and 100% volume of material respectively, 9.2.2 Barometric Pressure—At intervals of not more than six months, and after the system has been replaced or repai the baromettic reading of the instrument shall be verified against a barometer, as deseribed in 6.6. 10. Procedure 10.1 Record the prevailing barometric pressure, 10.2 Groups I and 2—Ensure that the sample is conditioned in accordance with Table 2. Fit a low range thermometer provided with a snug-fiting cork or stopper of silicone rubber, ‘or equivalent polymeric material, tightly into the neck of the sample container and bring the temperature ofthe sample to the ‘temperature indicated in Table 3. 10.3 Groups 1, 2, 3, and 4—Check thatthe temperature of the sample isas shown in Table 3. Pour the specimen precisely to the 100 mL mark of the receiving eylinder, and transfer the contents of the receiving cylinder as completely as practical into the distillation flask, ensuring that none ofthe liga flows {nto tho vapor tube. ‘Nore 4—1is impodiant tat he diference baw he temperature of the specimen and th ermperatare ofthe ath around he eeiving einer is'at smal as practically posible. A diforence of $°C ean make a silence of 07 mL. 103.1 Groups 3 and 4—If the sample isnot fluid at ambient temperature, it is to be heated toa temperature between 9°C and 21°C shove its pour point (Test Methods 97, D549, 15950, oF DS985) prior to analysis. If the sample has parially cor completely solidified in the intervening petiod, it shall be vigorously shaken after melting, and prior to sampling, to ensure homogencity. 103.11 If the sample is not fluid at ambient temperatures, disregard the temperature range shown in Table 3 for the receiving cylinder and sample. Prior to analysis, heat the receiving cylinder to approximately the same temperature as the sample. Pour the heated specimen precisely tothe 100 mL. mark ofthe receiving cylinder, and transfer the contents of the receiving eylinder as completely as practical into the distilla- tion flask, ensuring that none of the liquid flows into the vapor tube. Nore 1S—Any material that evaporates during the transfer will contibute 1 the Joss; any material that remains in the eceving cylinder ‘ill contribute to the observed recovery volume atthe time of the TBP. 10.4 If the sample can be expected to demonstrate irregular boiling bchavior, that is, bumping, add a few boiling chips to the specimen. The addition ofa few boiling chips is acceptable for any distillation, 10.5 Fit the temperature sensor through a snug-fiting device, as described in 6.4, to mechanically center the sensor in the nock of the flask. In the case of a thermometer, the bull is centered in the neck and the lower end of the capillary is level ‘with the highest point on the bottom of the inner wall of the ‘vapor tube (see Fig. 5}. In the case of a thermocouple orFIG. 6 Example of One Manufacturer ‘of Pt-100 Probe Relative to Distillation ‘mated D86 Dist resistance thermometer, follow the manufacturer's instructions as to placement (see Fig. 6) Note 16-If vacuum gree ie used on the mating suise of the entering device. use the minimum amount of che tht presi 10.6 Fit the flask vapor tube, provided with a soug-fiting cork or rubber stopper of silicone, or equivalent polymeric ‘material, tightly ito the condenser tube. Adjust the flask in a vertical postion s0 that the vapor tube extends into the condenser tube fora distance from 25 mm to 50 mm. Raise and aust the flask support board to fit it snugly against the bottom of the flask, 10.7 Place the receiving cylinder that was used to measure the specimen, without drying the inside ofthe eylinder, into its temperature-contrlled bath under the lower end of the con- denser tube. The end ofthe condenser tube shall be centered in the receiving eylinder and shall extend therein fora distance of| at Teast 25,mm, but not below the 100 mL. mark. 10.8 Initial Botting Poin 10.8.1 Manual Method—To reduce evaporation loss of the distillate, cover the receiving cylinder witha piece of bloting Pape, or similar material, that as been cut to fit the condenser tube sougly. If a reciver deflector is being used, stat the distillation withthe tip ofthe deflector just touching the wall of the receiving cylinder. Ifa receiver deflector isnot used, keep the drip tip of the condenser away from the wall of the receiving cylinder, Note the start time. Observe and record the IBP to the nearest 05°C (1.0 °F). Ifa receiver deflector isnot being used, immediately move the receiving eylinder so that the tip of the condenser touches its inner wall Align top of P-100 coll nsde the Mask neck to lower portion ofthe inner side of flask arm, Recommended Placement lask Sldearm for Auto- lon Instrument 10,82 Automated Method—To reduce evaporat the distillate, use the device provided by the manufactuier for this purpose. Apply heat to the distillation flask and contents with the tip of the receiver deflector just touching the wall of the receiving eylinder. Note the start time. Record the IBP to the nearest 0.1 °C (0.2 °F) 10.9 Regulate the heating so that the time interval between the first application of heat and the IBP is as specified in Table 5. 10.10 Regulate the beating so thatthe time from IBP to 5 recovered is as indicated in Table 5, 10.11 Continue to regulate the heating so that the uniform average rate of condensation ftom 5% recovered to $m. residue in the fask is 4 mL to $ mL per minute, (Warning— ue to the configuration ofthe boiling flask and the conditions of the test, the vapor and liquid around the temperature sensor are not in thermodynamic equitibrium, The distillation rate will consoquently havo an effect on the measured vapor temper- ture. The distillation rate shall, therefore, be kept as constant as possible throughout the test.) 10.11.1 In the context of this test method, “uniform average rate of condensation” has the following intention. Heating of the boiling Mask shall be regulated (0 maintain as best as possible a uniform flow of condensation, which will then provide the most desired precision for tho test. However, some distillation tests can have one or more short-term rates of condensation which deviate from the 4 mL-Anin to $ m-Anin indicated in 10.11 and Table 5, this is acommon occurrence for some sample types. The periods ofthese short-term deviations % afons During Test Procedure ‘Growe cows Gu Temperature aang bal” =O Os os 0-60 © 3240 sao a0 Temperature ct bath around “0 mie 1318 3 recehing jie ca 65-08 8-65 3 of charge vanporte “Tine om ts pletion of hoa to ial boing po in s10 10 510 18 “Tne tom ial blig pont Toss recoveod,¢ 0-100 60-100 Uniform average ao of condensation trom 5 recovered 8 mk, In as, iin 4 4s os “s “Tin ocedod tom 6 mL eve ‘ond pont rin Snax Sma Sax 5 mox ‘Tho proper condenser bath temperate wil depond vpn he wax contort ho campo and ols lain Faatons. Tho toss gonaralyporored virgo ange condoncoromparae, Wax fomaton nthe conenser can De deduces Ham) op logs han what would bo exposed basod on hol el po of tho spaamon, of esldal iquidby sncing wih aoe doth e883), The minimum lonprat Inthe 0104 "Crange slate fer kerosive, Grace No. tut ol and Grade No. 1-0 ese a ol In some cases lnclving Grade No.2 al ol, Grado Ne. 20 esl tuatol gas cl and sia’ alates, it may be nocezsay to had th conconee bat tempat into 98 fo 60°C rane. may last for several percent of material condensed until the temperature slope becomes constant again, and may occur at several periods along the entire condensation range. ‘These ‘deviations will typically correct after the temperature slope again becomes constant, These short-term deviations shall not ‘occur over the entire range of condensation. Typically, these short-term deviations should not occur for more than ten contiguous percent volume. The precision of the temperature readings will be significantly affected during these periods. When the overall calculated average rate of condensation between 5% recovered and 5 mL. residue is within the pre- scribed rate, the requirement of 10.11 ancl Table 5 is satisfied. ‘As example, those samples containing a 10% ethanol-fuel bend or those that exhibit a significant change of temperature slope at points during the distillation can have a short-term rate of condensation which deviates from the 4mLnin to 5 mL_/min indicated in 10.11 and Table 5. Nove 17—When testing gasoline samples, its nt uncomnon to ee ‘he condcnsate suddenly for non-nscble iid phases and Bea up on the emperature measring device and in the neck of te bailing ask a ‘vapor temperate of around 160°C. This may be accmpanied by ashap {about 3 °C) dip inte vapor temperature ands drop into eecovery rat. “The phenomenon, which may be due to the presence of ace water in the supe, may lest for 10s 19308 before the fermperature recovers an the condensate stats fssng. smoothly again. This point 1s sometimes ollogually refered to os the Heston Point 10.12 Repeat any distillation that did not meet the require- rents deseribed in 10:2, 10.10, and 10.11. 10.13 If a decomposition point is observed, discontinue the heating and proceed as directed in 10.17. Nor: 18—Charuteristc indieations of thermal decomposition are ‘volition of fumes and erate, typically decreasing, temperature readings that eur daring the final sages ofthe distin, 10.14 In the interval between the IBP and the end of the distillation, observe and record data necessary for the ealcula- tion and reporting of the results of the test as required by the specification involved, or as previously established for the sample under test. These observed data can include tempera- ol wax parle nthe dee coming pt (igh atton a oebvery rate aed (Ue prosance of wax prices dug to remota parm eatsaciory operation ena be sod Io gerara abah om peraure ture readings at preseribed percentages recovered or percent ages recovered at prescribed temporature reangs, or both 10.14.1 Manual Method—Recotd all volumes in the grad- sted eylinder to the nearest 0.5 mL, and all temperature readings to the nearest 0.5 °C (1.0 °F). 10.142 Automated Method—Record all volumes in the reeciving cylinder to the nearest 0.1 mL, and all temperature readings to the nearest 0.1 °C (0.2°F). 10.143 Group 1, 2, 3, and 4—An cases in which no specific data requirements have been indicated, roord the IBP and the EP (FBP) or the dry point, or both, and temperature readings at 5%, 15%, 85%, and 95% recovered, and at cach 10% ‘multiple of volume recovered from 10 0 99, inclusive. 10.143.1. Group 4—When a high range thermometer is used in testing aviation turbine fuels and similar producs, pertinent thermometer readings canbe obscured by the contering device. If these readings are required, perform a second distillation in accordance with Group 3. In such eases, reading from a. low range thermometer ean be reported in place of the obscured high range thermometer readings, and the test report shall so indicat. If, by agreement, the obscured readings are waived, the test report shall so indicate 10.144 When it is required to report the temperature reading at a prescribed percent evaporated or recovered for a sample that has a rapidly changing slope of the distillation curve in the region of the prescribed percent evaporated ot recovered reading, record temperature readings at every 1% recovered, The slope is considered rapidly changing if the change in slope ( C) of the data points described in 10.14.2 in that particular area is greater than 0.6 (change of slope (F ) is, ‘greater than 1,0) as caleulated by Eq 1 (Eq 2). Change of Slope (C) a (Cy CMM Va — Vi) ~ (C5 Ca)¥5~ Ya) Change of Slope (F @ (Fa Fs = Yi) = (Fs Fas Ya)C, = temperature at the volume % recorded one reading prior to the volume % in question, °C, Cy = temperature atthe volume % recorded in question, °C, Cy = temperature at the volume % recorded following the volume % in question, °C, F, = temperature at the volume % recorded one reading prior fo the volume % in question, °F, Fz = lemperature at the volume % recorded in question, °F, Fy = temperature at the volume % recorded following the volume % in question, °F, V, = volume % recorded one reading prior to the volume % in question, V, = volume % recorded at the volume % in question, and Vy = volume % recorded following the volume % in ques lion, 10.15 When the residual liquid in the flask is approximately 5 mL, make a final adjustment of the heat, The time from the 5 mL of liquid residue in the flask to the EP (FBP) shall be within the Lis prescribed in Table 5. If this condition is not satisfied, repeat the test with appropriate modification of the final heat adjustment. Nore 19—Since itis iticult to determine when there is $ mL of boiling ligui left in the sk, this timo is determined by observing the ‘mount of liquid recovered inthe receiving eplinder. The dynamic holéup thas been determined o be approximately 1.5 mi at this poi If there are no frontend lost, the amount of SL inthe sk can be assumed to correspond with an amount of 93.5 mL in the reeiving eylinder. This mount has fo be adjusted forthe estimated amount of rot end os, 10.15.1 Ifthe actual front end loss differs more than 2 mL. from the estimated value, the test shall be rerun, 10.16 Observe and record the EP (FBP) or the dry point, oF both, as required, and discontinue the heating. Nore 20—The endpoint (final boiling pot), rather than the ry pint, jis intended for general use. The dry point can be reported in connection with special purpose naps, such those used in the paint irduty itis substi foe the end point (inal boiling pont) whenever the ‘sample is of sucha nature thatthe precision ofthe endpoint Fn boiling pint) cannot consistently mest the requirements given inthe precision Section, Nore 21—Groyps 1 and 2, onc the final heat adjustments made, the ‘vapor tempersturethermomeer reading wil coninge to increase. As the nears the end point (ial boiling poi) the distillation typically ‘ty pot fist, Ale the dry point has boca achieved the vapor {enmperaturefthstmomete reading should continve to increase, The botont fof the Mask will be dey but the sides and nock of the Nask and the temperature sensor will sill have vapor condensate preset. The vapor condensate may have the appearance of a white cloud of fumes. This ‘vapor condensstefeloud of fumes should otlly engulf the temmpertare- ‘measuring sensor before th vapor temperature stats to decrease IF these observations do not eur, the end point may not have been resched Tt ‘would be advisable to repeat the test adding addtional heat to the Final hat adjustment. Typically the vapor temperature wil eatinue to rise 38 the dry point is reached and the vapor cloud engulfs the temperature: measuring sensor, When the end poiat is near, the rate of emperstire increase will slow and level off. Once the endpoint is reached the vapor ‘enmperatre wil stat and continue to decrease. Ifthe vapor temperature stats to decrease but then increases and repeats this eye while the vapor ‘emperature continues to insceae you have added loo rach beal tothe est sting Gronps ) and 4, mary Group 3 and 4 samples will have the same ison erates fa regards. dy oi and epoint as Groops and 2. With simples tet conan higher temperature bling maces t tnay not be possible to detect dry point or a8 endpoint Before he ‘ecompostion pin occurs. 10.17 Allow the distillate to drain into the receiving cylinder, after heating has been discontinued 10.17.1. Manual Method—While the condenser tubs contin ues to drain into the graduated cylinder, observe and note the volume of condensate tothe nearest 0.5 ml. at 2 min intervals util two suecessive observations agree. Measure the volume inthe receiving eylinder accurately, and record it to the nearest 05 mL. 10,17.2 Automated Method—The apparatus shall continu- ally monitor the recovered volume until this volume changes bby no more than 0.1 mL. in 2 min, Record the volume in the receiving cylinder accurately to the nearest 0.1 mL. 10.18 Record the volume in tho receiving cylinder as percent recovery. If the distillation was previously disconti ued under the conditions of a decomposition point, deduct the ppeteent recovered from 100, report this difference as the sum of [percent residue and percent loss, and omit the procedure given in 10.19. 10.19 After the flask has cooled and no more vapor is ‘observed, disconnect the flask from the condenses, pour its contents into a Sml. graduated cylinder, and with the flask suspended over the cylinder, allow the flask to drain until no appreciable increase in the volume of liquid in the cylinder is observed, Measure the volume in the graduated eylinder to the nearest 0.1 mL, and record as percent residue. 10,19.1 If the SmL graduated cylinder docs not have graduations below I mL. and the volume of liquid is less than T mL, prefil the cylinder with | mL. of a heavy oil to allow a bter estimate of the volume of the material recovered 10.19.1.1. Ifa residue greater than expected is obtained), and the distillation was not purposely terminated before the EP, check whether adequate heat was applied towards the end of the distillation and whether conditions during the test con- formed to those specified in Table 5, If not, repeat test Nore 22—The disilation residues ofthis test method for gasoline, ‘rosin and isillate diesel ate ¢ypically 09 % to 1.2 %,.09% 60 1.3% and 1.0 % to 1.4% volume, respectively Nore 23—Tho tst method isnot designed forthe analysis of distillate fuels containing eppreciable quantities of residual material (se I.) 10.19.2 Groups 1, 2, 3, and 4—Record the volume in the SmL graduated cylinder, to the nearest 0.1 mL, as percent residue, 10.20 If the intent of the distillation is to determine the percent evaporated or percent recovered at a predetermined corrected temperature reading, modify the procedure to con- form to the instructions described in Annex Ad. 10.21 Examine the condenser tube and the side arm of the flask for waxy or solid deposits. If found, repeat the test after making adjustments described in Footnote A of Table 5.Ay vss - 17 TABLE 6 Approximate Thermometer Reading Correction ‘Corea por 13xPa G0 mm Fay Tempeialre Range ton pr 13a (0 a i % oF 10-00 3-06 Das 088 30-50 6-122 038 058 sor 2158 0.20 or 70-00 158-104 oa 076 Sono 104280 a oat sWo-190 230-288, oa 0.05 130-150 286-002 030 a3 40-170 902-398 O82 on 0-100» 336-574 O54 098 020 aAK10 oar oe 2102 HOE 080 to? 230-250 aise 082 ut 2s0-270 © asa-st8 ost 415 zro20 —B1aeet 08s 120 200-010 $54.00 088 424 310-000 00-626 on 128 50-350 626-662 on 133 sso-s70 652-808 076 137 s7o-so0aae-734 07 aah oto 74770 oot 448 ‘ats o bo added when baronatie pressure Halow 1013 ‘and obo eibacted whan Boromeir pres esbove 04.3 70 mm 5) 11, Calculations 11.1 The percent total recovery is the sum of the percent recovery (see 10.18) and the percent residue (sec 10.19). Deduct the percent total recovery from 100 to obtain the percent loss, 11.2 Do not correct the barometric pressure for meniscus depression, and do not adjust the pressure to what it would be at sea level Nor 24—The observed barometric reading docs not have 10 be comceted to a standard temperature and to sandaed graviy. Even without performing these corections, the corecied temperate readings forthe Same sample between laborstocies st two different locations inthe world will, in genera, flr less than 0.1 “Cat 100 °C, Almost all data obtained earlier have been reported at Baomettc pressures that have not been corrected to standard temperature and to standard gravity, 11.3 Correct temperature readings 0 101.3 KPa (760mm Hg) pressure, Obtain the correction to be applied to each cmperature reading by means of the Sydney Young equation as given in Eq 3, Eq 4, or Eq 5, as appropriate, or by the use of Table 6. For Celsius temperatures 6. = 0.0009 (101.3 ~ P,)(273+1,) eo ©, = 0.00012 (760 ~ P)(273+1,) o it temperatures: 6, = 0.00012 (760 ~ F) (4604) o where: i, the observed temperature reading in °C, % the observed temperature reading in °F, , and G, = corrections t0 be added algebraically to the “observed temperature readings, Py ‘= barometric pressure, prevailing at the time and location of the test, KPa, and P = barometric pressure, prevailing at the time and loc: of the test, mm Hg. ‘After applying the corrections and rounding each result to the nearest 0.5°C:(1.0°F) or 0.1 °C (0.2°R), as appropriate to the apparatus being used, use the corrected temperature read- ings in all further calculations and reporting. Nore 25—Temperature readings. are not eonected to 101.3 KPa (760 mm Hg) when product definition, specifications, oF agreements ‘between the parties involved indicate, specifically, hat sich corection is ot ruled or that coerecton shall be made ta some other hase presi 114 Correct the actual loss (0 101.3 kPa (760mm Hg) pressure when temperature readings are corrected to 101.3 kPa pressure, The corrected loss, Lis calculated from Eq 6 or Eq 7, a8 appropriate, or can be read from the tables presented as ig. X3.1 of Fig. X3.2. 5+ (L- 03) (1 +(1013~ 00) 05+ (L~ 08)41+ (760 ~ P)i600} o m observed loss, ‘corrected loss, pressure, kPa, and pressure, mm Ig Nove 26—Ea 6 and 7 above have been devived from the data in Table |A4.3 and Bas 3 and 6 in Test Method D6. ~ 95 and ear versions. lis probable that Ea 6 and 7 shown were the original empiial equations fem Which the table snd equations in the Test Method D8S~98 and ear vorsions were derived. 11.4.1 Calculate the corresponding corrected percent recov- ery in accordance with the following equation: R=RH(L-L) ® where: L__ = poteent loss or observed loss, L, = corrected loss, R= percent recovery, and R= corrected percent recovery. 11.5 To obtain the percent evaporated at a preseribed temperature reading, add the percent loss to each of the observed percent recovered at the prescribed temperature readings, and roport these results as the respective percent evaporated, that is: P= PAL ©) where: observed loss, percent evaporated, and pereent recovered. 11.6 To obtain temperature readings at prescribed percent evaporated, and if no recorded temperature data is available within 0.1 volume % of the prescribed percent evaporated, use either of the two following procedures, and indicate on the report whether the arithmetical procedure or the graphical procedure has been used. 11.6.1 Arithmetical Procedure—Deduet the observed loss from each prescribed percent evaporated to obtain the corre- sponding percent recovered. Calculate each required tempera- ture reading as follows: THT +(Ty— Ty) (P, PMP Pad 10)Af oss - 17 where: P, = peteent recovered corresponding to the prescribed percent evaporated, Pay = percent recovered adjacent to, and higher than P,, Poy = pervent recovered adjacent to, and lower than 2, temperature reading at the prescribed pe evaporated, Ty = temperature reading recorded at Py, and Ti, = tempermure reading recorded at P,,, ‘Values obtained by the arithmetical procedure are affected by the extent to which the distillation graphs are nonfinear, Intervals between successive data points can, at any stage of the test, be no wider than the intervals indicated in 10.18, In no ‘case shall « calculation be made that involves extrapolation. 11,62 Graphical Procedure—Using graph paper with uni= form subdivisions, plot each temperature reading corrected for barometric pressure, if required (See 11.3), against its corre- sponding percent recovered, Plot the IBP at 0% recovered, Draw a smooth curve connecting the points. For each pre- scribed percent evaporated, deduct the distillation loss 10 ‘obtain the corresponding percent recovered and take from the graph the temperature reading that this percent recovered indicates. Values obtained by graphical interpolation proce- dures are affected by the care with which the plot is made, Nore 27—See Appendix X1 for numerical examples Mustatng the axihetial procedure, 11.6.3 In most automated instruments, temperature-volume data are collected at 0.1 volume % intervals oF less and stored in memory. To report a temperature reading at a prescribed percent evaporated, neither of the procedures described 11.6.1 and 11.6.2 have to be used. Obtain the desired tempera ture directly from the database as the temperature closest to and within 0.1 % volume of the prescribed percent evaporated. 12, Report 12.1 Repott the following information (see Appendix. XS for examples of repor 12.2 Report the barometric pressure to the nearest 0.1 KPa. (mm Hg). 12.3 Repott all volumetric readings in percentages. 12.3.1 Manual Method—Report volumetric readings to the nearest 0.5, and all temperature readings to the nearest 0,5° C (.0°R), 123.2 Automated Method—Report volumetric readings to the nearest 0.1, and all temperature readings to the nearest one tenth degree. 12.4 After barometric corrections of the temperature read- igs have been made, the following data require no further calculation prior to reporting: IBP, dry point, BP (FBP), dlecomposition point, and all pairs of coresponding values involving percent recovered and temperature readings. 12.4.1 The report shall state if the temperature readings hhave not been comected for barometric pressure, 12.5 When the temperature readings have not been cor rected (0 101.3 kPa (760 mim Hg) pressure, report the percent residue and percent loss as observed in accordance with 10.19 and 11.1, respectively. 12.6 Do not use the corrected loss in the calculation of percent evaporated. 12.7 It is advisable to base the report on relationships between temperature readings and percent evaporated when the sample is a gasoline, or any other product classified under Group 1, or in which the percent loss is greater than 2.0. Otherwise, the report can be based on relationships between temperature readings and percent evaporated or percent recov- cred. Every report must indicate clearly which basis has been used. 12.7.1 In the manual method, i results are peroent evaporated versus temperature readings, report if the arithmeti- cal or the graphical procedure was used (See 11.6). 128 Report ifa drying agent, as described in 7.5.2 oF 7.5.3, was used. 12.9 Fig. X1.1 isan example ofa tabular repo It shows the percent recovered versus the corresponding temperature read- ing and versus the corrected temperature reading, It also shows the percent loss, the eorected loss, andthe percent evaporated versus the corrected temperature reading. 13, Precision and Bias 13.1 Precision (Group 1, 2, 3 ausomated)—The precision of this test method, as determined by the statistical exemination of the interlaboratory test results,” is as follows: [Note 28—The precision was derived from data produced by automted 86 apparatus. Typicel examples of precision for manual apparsius can be calculated from the information contained in Annex Ad (see A4.10), ‘Note 29—Information on the precision of percent evaporaled or percent recovered a »preseribed temperature can be found in Annex Ad [Note 30—For naphthas, solvents, and other sinilar materials where percent recovered ace reporied and the poreent Toss typiealy ess than ‘ne percent, the percent rocovered temperatures ean be considered denial to the percent evaporated femperatures and precision can be caleulated as shown for Group I, 2, 3 13.1.1 Repeatability—The difference between successive test results, obtained by the same operator using the same apparatus under constant operating conditions on identical test material, would in the long run, in the normal and comect ‘operation of this test method, exceed the values in Table 7 only in one ease in twenty. 13.1.2 Reproducibility —The difference between two single tnd independent test results, obtained by different operators working in different laboratories on identical test material, \would in the long run, in normal and correct operation of this, test method, exceed the values in Table 7 only in one case in fon statements were derived from a 2010 interlaboratory cooperative test program. Twenty six labor tories participated and analyzed twenty one sample sets com- prised of; specification grade gasoline, both conventional and * Soppotng data have bon filed at ASTM lato Headqurs ond nay be obey requ Research Repon RROD 107, Contact ASTM Caster Serie a service oe,Ai vss - 17 TABLE 7 Repeatability and Reproducibility for Group 1, 2,3 (Automated) (Valid Range 20°C to 260°C) Percent Repesiaiiy «© Ropredsabiny 2F 5 tae 2aadsse+a2) 25 42.80.80 +020) fo 09+ 2a0.4386 +024 19+ 28(0488s +028) 2 09s 2.804382 +028) 20+ 2.804350 40.28) 50 03428104582 + 0.28) 43+ 2800008 +02 © Ope 2acaise saz) © 20 280.4550 40.20) 50 fosaaodsse+o2) © 19 + 204580 +020) € — asamoassc+o2) © 204 2804880 30.20) 7 1B428(0438> 402) 2.1 + 28(0498e + 020) 8 1442804885402 204+ 28104880 + 024) 80 184 2.8(0.4880 +028) 28 + 28L0BSe + 028) 85 204 28004985 +028) 8 + BBLOABSe + 0.24) ‘Se = opo orate of ehango of lomperature in dogres Coleus calelatod tng A101 oxygenated, some containing up to 20 % ethanol. The tem- perature range covered was 20 °C to 220 °C. Information on the type of samples and their average boiling points are in the research report 13.2 Precision (Group 4)—The precision of this test method, as determined by the statistical examination of the interlaboratory test results," is as follows: Nore 31—Information on the pression of percent evaporated or erent covered ala preseribed temperature canbe found in Annes A4 132.1 Repearabitiy—The difference between successive test results, obtained by the same operator using the same apparatus under constant operating conditions on identical test material, would in the long run, in the normal and correct ‘operation of this test method, exceed the following values in ‘Table 8 only in one ease in twenty. 13.22 Reproducibilty—The difference between two single and independent test results, obtained by different operators ‘working in different laboratories on identical test material, would in the long run, in normal and eorreet operation of th test method, exceed the following values in Table 8 only in one. case in twenty, "© Suppoting dita (sls ofthe 2008 Inersbarsory Caopeaive Test P= prin hve fee led at ASTM Iterations Hesdqtrs and may be ead By requesting Reseach Repo RRDO2- 162 TABLE 8 Repeatability and Reproducibility for Group 4 (automated) Percent Fepeaiabliy °C Repoduebtiy © vara Range Recovered 1B oor ‘0ST Sez 5% oer oat 1801 255 0% ‘0.00047 ouezt 60 1 265, 2% 00728 oa0at W751 278 sos .osaar oovest 185 1 205, 0% 008 oot 195 1 290 50% 40 30 F70t 205, oe 003571 cont 22010308 ne (05st oowst 20006315 aos esr oor 240 t9 325, os 007 01st 4006340, 95% © O01SteCT-14 oostos(T-140) 20010360, FBP 22 7 1954 965 soars T= porcont ecovered lemeraute wihin vat rang proserbos. Rete Anno At fo bles f cleat repeatability an reproduc. 13.23 ‘The precision statements were derived from @ 2005 terlaboratory cooperative test program.!? Sixteen laborato- ries participated and analyzed sample sets comprised of; specification grade diesel, with a BS and 120 biodiese!, specification grade heating oil, aviation turbine fuels, marine fuels, mineral spirits and toluene. The temperature range covered was 145°C to 365 °C. Information on the type of samples and their average boiling points are in the research report. 13.3 Bias: 133.1 Bias—Since there is no accepted reference material suitable for determining the bins forthe procedure in these test ‘methods, bias has not been determined. 13.3.2 Relative Bias between Manual and Automared Apparatus—An interlaboratory study’ conducted in 2003 using ‘manual and automated apparatus has conchided that there is no statistical evidence to suggest that there is a bias between, ‘manual and automated results, [Note 32—See 2.1 for information on the application and use of, borosilicate and quart stilton asks. 14, Keywords 14.1 batch distillation; distillates; distillation; laboratory : petroleum productsALI Tables Recovered OP Terperetue (6) 60, 55 100 v0 35 180 105 190 200 205 210 220 Recovered 8%. Temperature) 185 170 5 185 190 198 208 210 218 2 2s 2 2 20 20 5 Recovered 10% ‘organ (6) 1e 165 70 vs 16 188 160 20 0 20 25 225 20 235 288 Aly Des - 17 ANNEXES (Mandatory Information) AL, PRECISION TABLES FOR REPEATABILITY (+) AND REPRODUCIBILITY (R) 'aP_onPs peau R.086euio 261 798 27 925 an 889 288 880 207 908 300 935 348 96 324 990 333 1010 3a 1045 ast tare 360 ie 368 128 an 1155, aa 18 399 1210 Ts.0npe pasauo—-Raseuto 174 420 1% 495 ts 510 131 525 196 840 20 535 2or 570 21 8a 20 600 22 615 22 630 204 45 240 600 2a 075 2s a0 256 105 200 720 26 188 279 180 Bs 788 T10_GRPA pasauo RDBBaWto 150 382 155 303 reo am 165 305 ve 398 174 sor 179 an te a2 vee ao 183 ast ter 402 202 473 207 40 22 495 216 505 2a an 226 523 200 539 1s 288 260 295 Recovered 20% Temoerature CC) 178 a0 190 ir 200 205 SSRERESERENSS Recovered 3% ‘Tomperatre (C) 180 210 215 20 230 235 248 250 255 288 20 216 200 238 Recoveras 40% Temperature °C} 198 200 205 218 220 228 230 235 248, 250 240 se Bat 872 20 503 ‘r_6AP4 0968010 R_DDBoute war ‘68 435 305 138 295 12 408 146 46 138 425 1s 4a 1s 447 +60 450 te 05 te 4m 171 409 178 499 178 510 12 520 126 529 te0 Say 19 a] is Si 200 57 e0_GRPA .Dasaue R096 au 108 305 443 32 448 300 449 338 tee a7 125 355 128 353 431 an 434 a0 sar 308 te 44 146 a9 18 fat 1st 20 tet “ar ts 448 to a5 te fe 16 470 406A dasa R_086auio 095 273 ‘00 200 03 287 105 204 105 301 10 3.08 43 315 us 22 ie 320 12 338 123 343 138 350 ailly 086 - 17 a te ws 310 uw tz ie is ut 3S ia g i iB Me Fy a 3 = 138 a8 Recovered 90% T90_GAPS a 2 as pontrets 1 ons oats ms od bead 180 ove 270 0 1 - 185, 078 278 nce s0% tsa onP4 s om ie feet etna tate ie om iS mos i 20 20 om 300 ecw 0 Teo oR as ee a rere 1 ote0e toa a oa a8 1 a7 4 Be oo 350 = oe on 20 998 345 20 0 an Bs oe eas CH oe a 28 1.00 3.68 oo oe Be 250 103 a5 2 oe 8 = 1 a8 = ‘oe vo 200 107 300 * ie ey 265 to 398 os oe oe 270 an 405, 2 on Per 25 133 a3. Pa i a 200 435 420 o Ae ey 205 aa 428 a rey oe 200 138 438 2 3 & a in ‘s S is s ' s Eo te at = iB i becomes 70% rons a 'S te So eae teas s iB & oe Cee 2a By a 3 = oS a = a ‘S = oa 300 = 2 ‘a i oer ae = " fr = oe = ee iB SS 2 a 3 = on 38 cowed 8 ros ona = ost at Fonte eeu oto 275 0868 344 7° = Pei = oe 38 = g A % ‘e a = 3 oe 318 co a4 3 = bd reconros00% ro0.one4 i in os Rapes owes cess 2 Bi oA at eer oe 3 Es ts is oe 33 = zg 3 i oar xa S BS i S os io 2 & ae s a a is Bi i Fd 2 38 he is te a a 38 = in te a i am = ie te a a gi = r oe CA tos aa Recovered FAP. FaP_ORPA ee teu rr "porte roan one 900, 113 4.08 ba teoasl meAly pss - 17 perenne 0 2h O3 amie 254 3m 82 1S Ane on GERD. 1c, 125 mL Flask Han 168 Se aP mw 215430 £0439 22 05ma00, 1401S wa. 125 mL Flask with Ground Glass Joint FIG. A2.1 125 mL Flask and 125 mL. Flask with Ground Glass Joint A2, DETAILED DESCRIPTION OF APPARATUS 2.1 Distlaion Flasks—Flasks shall be of heat resistant glass, constructed to the dimensions and tolerances shown in Fig. A2.1 and Fig, A2.2. Flasks made of borosilicate glass shall comply with the requirements of Specification E1405, Flasks rade of quartz shall be composed of 99.9+ % SiO, Flasks ‘may also be constructed with a ground glass joint Nove A2.1—Sincethethemal response of broalliate glass and quartz canbe eifernt, consider sppropite sdjusiments forthe tl nd nal hea egulation wo atin the tne lin tte in the proses Nowe A22~For tess specifying dry pont, specially selected asks with Dotoms ant walls of uniform thickness sre desirable A2.Le1 Inralaboratory and interlaboratory data" for motor gasoline, kerosene, aviation turbine fucl, fuel cil, and diesel fuel were assessed by Practice D6708 indicating that some correction could improve the degree of agroement between quartz and borosilicate flask results. The level of conection ‘ould be considered practically not significant. Correction is !mote probable atthe IBP and FBP of both motor gasoline and distillate fuels. Optimizing D86 parameters for motor gasoline and distillate fuls may further minimize the differences in DB6 TBP and FBP when using borosilicate versus quartz ask. Bias cea conceivably occur for materials and temperatures not studied in this limited program, A2.L.1.1 For motor gasoline in the temperature range of 25°C to 220°C: Borosilicate = 1.0054 Quartz ~ 0.73 A2.1.1.2 For Kerosene, aviation turbine fuel, fuel oil, and diesel fuel in the temperature range of 140 °C to 350°C: opporing daa have ben filed a ASTAM Intertonal Headers ond may ‘be band by reusing Research Repor RR-D02-115, Contec ASTM Cone Serve at sevice @atmorg. Borosilicate = Quartz + 0.40 A2.2 Condenser and Condenser Bath—Typical types of condenser and condenser baths are illustrated in Figs. 1 and 2. ‘A2.2.1 The condenser shall be made of seamless noncorro- sive metal tubing, 560 + 5 mm in length, with an outside diameter of 14 mm and a wall thickness of 0.8 mm to 0.9 mm. Nore A2.3 Brass or stainless steel has been found to be a suitable material fe this prpose. A222 The condenser shall be set so that 393 mm 2 3 mn of the tube is in contact with the cooling medium, with 50 mm * 3:mm outside the cooling bath at the upper end, ancl with 114 mm * 3 mim outside atthe lower end. The portion of the tube projecting at the upper end shall be set at an angle of 75° + 3° with the vertical. ‘The portion of the tube inside the condenser bath shall be either straight or bent in any suitable continuous smooth curve. The average gradient shall be 15° = 1° with respect to the horizontal, with no 10 cm section having a gradient outside of the 15° + 3° range. The projecting lower Portion of the condenser tube shall be curved dawnward for a length of 76 mm and the lower end shall be cut off at an acute angle, Provisions shall be made to enable the flow of the distillate to run down the side of the receiving cylinder. This ‘can be accomplished by using a drip-deflector, which is attached to the outlet of the tube. Altematively, the lower portion of the condenser tube can be curved slightly backward to ensure contact with the wall of the receiving cylinder at a point 25 mm to 32 mm below the top of the receiving cylinder. Fig, A23 is a drawing of an acceptable configuration of the lower end of the condenser tube.Aly vss - 17 16.9 + 0.3 mm ID Woon awoe ree € SIZ eet 176 1.3mm }— 2.10.7 mm FIG, A2.2 Detall of Upper Neck Section A2.23 The volume and the design of the bath will depend ‘on the cooling medium employed. The cooling eapacity of the bath shall be adequate to maintain the required temperature for the desired condenser performance. A single condenser bath may be used for several condenser tubes. A2.3 Metal Shield or Enclosure for Flask, (Manual units, only) A2A3.1 Shield for Gas Burner (see Fig. 1)—The purpose of this shield is (© provide protection for the operator and yet allow easy access to the burner and to the distillation flask uring operation. A typical shield would be 480 mm high, 280mm long, and 200mm wide, made of sheet metal of (0.8 mm thickness (22 gauge). The shield shall be provided with at Teast one window to observe the dry point atthe end of the lation, A232 Shield for Electric Heater (see Fig. 2)—A typical shield would be 440 mm high, 200 mm tong, and 200 mm wide, made of sheet metal of approximately 08 mm thickness (22 gauge) and with a window in the front side. The shield shallAy pes - 17 ‘mensions in mm Lower End of Condenser Tube FIG. A23. Lower End of Condenser Tube be provided with atleast one window to observe the dry point at the end of the distillation, A24 Heat Souree A2A.1 Gas Burner (sce Fig. 1), capable of bringing over the first drop from a cold start within the time specified and of continuing the distillation at the specified rate. A sensitive ‘manual control valve and gas pressure regulator t0 give comiplete control of heating shall be provided, A24.2 Electric Heater (see Fig. 2), of low heat retention, Nore A24-Heaters, adjustable from 0 W to 1000 W, have been foun to be suitable fortis purpose A25 Flask Support 25.1. Type Use a Type | flask support with a gas burner (sce Fig. 1). This support consists of either a ring support of the ‘ordinary laboratory type, 100 mm or larger in diameter, sup: ported on a stand inside the shield, or @ platform adjustable from the outside of the shicld. On this ring or platform is ‘mounted a hard board made of ceramic or other heat-resistant ‘material, 3 mm to 6 mm in thickness, with a central opening 76 mm to 100mm in diameter, and outside line dimensions slightly smaller than the inside boundaries of the shield, A2.5.2 Type 2—Use a Type 2 flask support assembly with clcctric heating (sec Fig. 2 as one example). The assembly ts ofan adjustable system onto Which the electric heater nounted with provision for placement of a flask support 19 board (see A2.6) above the electric heater."The whole assembly {adjustable from the outside of the shield A26 Flask Support Board—The flask support board shall be constructed of ceramic or other heat-resistant material, 3 mm to 6 mm in thickness, Flask support boards are classified as A, B, or C, based on the size of the centrally located ‘opening, the dimension of which is shown in Table 3, The flask ‘support board shall be of sufficient dimension to ensure that ‘thermal heat to the flask only comes from the central opening. and that extraneous heat (0 the flask other than through the central opening is minimized. (Warning —Asbestos- containing materials shall not be used in the construction of the flask support board.) 'A27 The flask support board can be moved slightly in different directions on the horizontal plane to position the distillation flask so that direct heat is applied to the flask only through the opening in this board. Usually, the position of the fiask is set by adjusting the length of the side-arm inserted into the condenser. A28 Provision shall be made for moving the flask support assembly vertically so that the flask support board is in direct contact with the bottom of the distillation Mask during the distillation, The assembly is moved down to allow for easy ‘mounting and removal of the distillation flask from the unit A29 Receiving Cylinders—The seceiving cylinder shall hhave a capacity to measure and collect 100 mL. + 1.0 mL. The shape of the base shall be such that the receiver does not topple ‘when placed empty on a surface inclined at an angle of 13° from the horizontal A29.1 Manual Method—The cylinder shall be graduated at intervals of I mL beginning at Teast at SmL. and have a gruduation at the 100 mL mark. Construction details. and tolerances for the graduated cylinder are shown in Fig. A2.4. A2.9.2 Automated Method—The cylinder shall conform to the physical specifications described in Fig. A24, except that graduations below the 100 mL: mark are permitted, as long as they do not interfere with the operation of the level follower Receiving cylinders for use in automated units may also have a metal base. A29.3 If requited, the receiving cylinder shall be immersed, during the distillation to above the 100 mL. graduation line in a cooling liquid contained in a cooling bath, such as a tall-form, beaker of clear glass or transparent plastic. Alternatively, the receiving cylinder may be placed in a thermostated bath air cireulation chamber, A210 Residue Cylinder—The graduated cylinder shall have a capacity of Sml.or 10mb, with graduations into 0.1 mL. subdivisions, beginning at 0.1 mL. The top of the cylinder may be flared, the other properties shall conform to Specification E1272,wass Nore 1-1 ml graduations ~ minimum $ mL to 100 mL. FIG, A24 100 mL Graduated Cylinder 3. DETERMINATION OF THE DIFFERENCE IN LAG TIME BETWEEN AN ELECTRONIC TEMPERATURE MEASURE- MENT SYSTEM AND A MERCURY.IN- A3.1 The response time of an electronic temperature mea- suring device is inherently more rapid than that of a mercury: in-glass thermometer. The temperature measuring device as- sembly in general use, consisting of the sensor and its cast ‘or an electronic system and its associated software, or both, so designed that the temperature measuring system will simu- late the temperature lag of the mercury-in-glass thermometer. A3.2 To determine the difference in lag time between such a temperature measuring system and a mercury-in-glass thermometer, analyze a sample such as gasoline, Kerosine, jot fuel, or light diesel fuel with the electronic temperature ‘measurement system in place and in accordance with the [procedures described in this test method. In most cases this is the standard distillation step performed with an automated unit 43.2.1 Do not use a single pure compound, a very narrow. boiling range product, or a synthetic blend of less than six ‘compounds for this test A3.2.2 Best tesults are obtained with a sample that is typical ‘of the sample load of the laboratory. Alternatively, use full-range mixture with a $ % to 95 % boiling range of atleast lao °c, {LASS THERMOMETER A33 Replace the electronic temaperature measuring, device with a low range or a high range mercury-in-glass thermometer, depending on the boiling range of the sample. ‘A34 Repeat the distillation with this thermometer, and manually record the temperature at the various percent recov- ered as deseribed in 10.14. ABS Caleulate the values for the repeatability for the observed slope (ATIAV) for the different readings in the test. ‘436 Compare the test data obtained using these two tem. perature measuring devices. The difference at any point shall ~ be equal to, or less than, the repeatability of the method at that point, If this difference is large, replace the electronic tem- perature measuring device or adjust the electrons involved, or both. »Ail vss - 17 ‘TABLE Ad.1 Precision for Percent Evaporated at a Prescribed Temporature—Gasoline (Consolidated Equation) ald Rango £70 - E1806 (Avionatod Apparat) Dee AiO har: x = parcont evaporated a the presebod emgeature ‘80085 T5O=% 7 D200 (10=X) ‘Ad, PROCEDURE TO DETERMINE THE PERCENT EVAPORATED OR PERCENT RECOVERED AT A PRESCRIBED TEM- PERATURE READING A. Many specifications require specific per ‘evaporated or recovered at prescribed temperature re cither as maxima, minima, or ranges. The procedures to determine these values are frequently designated by the terms xxx or Rxxx, where xxx is the desired temperature, Nore Aé.1—Regulatory standards on the eetfcation of reformulated gasoline under the complex model procedure require the determination of 1200 and E300, defined as the percent evaporated fuel at 93.3 °C (200 °F) and 148.9 °C (300°, respectively. E158, the percent evaporated at a Aisillation temperature of 70°C (158 °F), is also used in describing fuct volatlity characteristics. Other iypical temperatures are R200 for kero- sines nd R 250 and R350 for gas ols, where R'200, R250, and R 350, ae the percent ecovered fuel a 200 °C, 250 °C and 350 °C, respectively ‘A4.2 Detetmine the barometric pressure, and calculate the correction tothe desired temperature reading using Eq 3, Eq 4, or Bq 5 for t = axx°C (oF fy = X4X°R). A4.2.1 Manual Method—Determine this correction to 05°C (°F). A422 Automated Method—Determine this correction 10 04°C 02°), ‘A4.3 Deterinine the expected temperature reading to xxx °C (or xxx °F) after the barometric correction. To obtain the expected value, add the absolute valuc of the calculated correction fo the desired temperature ifthe barometrie pressure is above 101.3kPa. If the barometric pressure is below 101.3 kPa, subtract the absolute value of the calculated correc tion from the desired temperature. A44 Perform the distillation, as described in Section 10, while taking into account A4.5 and A4.6. A4S Manual Distillation ‘A4.5.1 Io the region between about 10°C below and 10 °C above the desired expected temperature reading determined in A4.3 record the temperature reading in intervals of 1 volume %, ‘A4.5.2 Ifthe intent of the distillation is to solely determine. the value of Exxx or Rxxx, discontinue the distillation after at least another 2 ml. of distillate have been collected. Otherwise, continue the distillation, as described in Section 10, and determine the observed loss, as described in 11. 4.5.2.1 If the intent of the distillation is to determine the value of Exxx and the distillation was terminated after about 2mL of distillate was collected beyond the desired a temperature, allow the distillate to drain into the receiving graduate. Allow the contents of the flask to cool to below approximately 40°C and then drain its contents into the receiving graduate, Note the volume of product in the receiving graduate (0 the nearest 0.5 mL. at 2 min intervals until two successive observations agree. A45.2.2 The amount recovered in the receiving graduate is the percent recovery. Determine the amount of observed loss by subtracting the percent recovery from 100.0, A4.6 Automated Distillation A4.6.1 In the region between about 10 °C below and 10 °C above the desired expected temperature reading determined ia ‘A4.3, collect temperature-volume data at 0.1 % volume inter- vals or less, ‘44.6.2 Continue the distillation, as described in Section 10, ‘and determine the percent loss, as described in 11.1 Ad.7 Caleulations A471 Manual Method—I @ volume percent recovered reading is not available at the exact temperature calculated in A43, determine the percent recovered by interpolation be- ‘ween the two adjacent readings. Bither the linear, as deseribed. in 11.6.1, or the graphical procedure, as described in 11.6.2, is permitted. ‘The percent recovered is equal to Rxxx. ‘A47.2. Automated Method—Report the observed volume to 0.1 % volume corresponding to the temperature closest t0 the expected temperature reading. This is the percent recovered, or Rxxx, A4.7.3 Manual and Automated Methods—To determine the value of Exxx, add the observed loss to the percent recovered, Rxxx, as determined in 447.1 or A4.7.2 and as described in Eq 9. A4.7.3.1 As presetibed in 12,6, do not use the corrected loss. A4S8 Precision—The statistical determination of the preci sion of the volume % evaporated or recavered at a prescribed temperature for automated apparatus were derived according to Practice D6300 from a 2005 interlaboratory program.'°Table ‘Ad.1 shows the consolidated equations for volume. percer evaporated for gasoline, Table Ad.2 shows the precision for volume percent recovered for diesel. ‘The precision is valid only for the range of temperatures stated, The estimation of 5 ti ‘etAf vss - 17 TABLE A4.2 Precision for Per nt Recovered at a Prescribed Temperature—Diesel (Rxxx) ‘Vad Rage F200 - R900" (Alomated Apparlus) 95 Auto precision for temperature points outside the stated range can be calculated from the procedures in 4.10 and the precision tables in Annex Al ‘M49 The statistical determination of the precision of the volume percent evaporated or recovered at a prescribed tem perature for manual apparatus has not been directly measured in an interlaboratory program. It ean be shown that the precision of the volume percent evaporated or recovered at a prescribed temperature is equivalent to the precision of the temperature measurement at that point divided by the rate of change of temperature versus volume percent evaporated or recovered. The estimation of precision becomes less precise at high slope values. A4.10 Calculate the slope or rate of change in temperature reading, Se (or $,), as described in A4.10.1 and Eq A4.1 and using temperature Values bracketing the desired temperature. 4.10.1 Slope or Rate of Change of Temperane: Noe AL2—The slope can have a dramatic inuence on precision for soine samples, pally that eonsiningoxygensts, andthe ealelated Preison obaied sig the values in Table A43 may nt refs hs a ailcases. This canbe due 0 the changing composition of the sample, the slope to change rapidly over a shrt nteral This change ma tcc either daring te data neremens por fo subsequent, he dl Prt under eaeulation A4.10.1.1 To determine the precision of a result, it is generally necessary to determine the slope or rate of change of ihe temperatuee at that particular point, This variable, denoted Se of Si equal tothe change in temperature, ether in °C ‘or in °F, respectively, per percent recovered or evaporated. A4.10.1.2 The precision of the IBP and EP does not require {ny slope calculation, ‘A4.10.1.3. With the exception stated in A4.10.1.2, te slope at any point during the distillation is calculated’ from the ‘equations, using the values shown in Table A4.3: Selor Sy) = (Ty THe Yad cagaay the slope, °Clvolume %, the slope, *Fivolume %, the upper temperature, °C (or °F), the lower temperature, °C (or °F), the volume % recovered or evaporated corresponding oTy. the vohime % recovered or evaporated corresponding to Tj, and ior 2 2006, R250G, ROO 26 Vee = the volume % recovered or evaporated corresponding to the end point. 44.10.14 In the event that the distillation end point occurs prior to the 95 % point, the slope at the end point is calculated as follows: Sel0e5,)= (Far TraVVar Ym) (42) where: Trp Of Tye = the temperature, in °C or °F, at the percent volume recovered indicated by the subscript, and Vep oF Vg = the volume S recovered Sibseripr EP = end point, and ‘Subscript HR = highest reading, either 80 % oF 90 %, prior to the end point A4.10.1.5 For points between 10 % to 85 % recovered that in Table A4.3, the slope is calculated as follows: Se 0" S,) = 0.05 (Tovey ~ Tv-m) (Atay A4.102 Calculate the repeatability, r or the reproducibility, R, from the slope, Se. (or Sp) and the data in Tables 4.4 and AAS. A4.103 Determine the repeatability or reproducibility, or both, of the volume % evaporated or recovered at a presctibed mperature from the following formulas: eauwa = Se (84) (aay Resa” RiSe(S;) (a4) where: Frolme % = repeatability of the volume percent evaporated or recovered, Rote = Reproducibility of the volume percent evapo- rated or recovered, r repeatability of the temperature at the pre- scribed temperature at the observed percent distilled, R reproducibility of the temperature at the pre- scribed temperature at the observed percent distilled, and Se (Sp) = rateof change in temperature retding in °C (°F) per the volume percent evaporated or recovered. A4.10.4 Examples on how to calculate the repeatability and the reproducibility are shown in Appendix X2.Ally vas - 17 TABLE A4.3 Data Points for Determining Slope, S¢ oF Se Sopeth PO Tats o 7 > 0 3. 040 50 00 70 9 S Tate 5 2 1% 4% > 9 7% Bw 8 S % Ven wee Bw SNe TABLE A4.4 Repeatability and Reproducibility for Group 1 anon Tana Sapo epi fenton ra = — as = oP 33, 5 36 0 5 1910686 aaoes, aust tse S001 7455 to ‘2r08es. 2208s, Bost nase Seis, 2 V2ioses, bhows Bovis, Seti 5, Soo V2vosese 2hows, Bouinese Senin, % 2rosese Paowsr Bout ss Seems, % 2v0268s boomer dost ese sats % Vavoa6ss Peomrer sieizese sons, oe 30 7 12 8 ‘Scr; the aworag dopo (orale el change calcusted In aocordance wah A104, Table AA preion data caine Gem Reidy ontahmanial and aaonaied 186 nie by Non Arran ad Parag ‘TABLE A4.5 Ropoatabilty and Reproductbility for Groups 2, 3 and 4 (Manual Method) Repoatabiy™ Feprodaabiiy™ 7. ca * F i T0038, THOS, 0S, 5000S, sa86% tovoaise teroaig, taviasge Baas, For oroses, 1310305, s1i048, 570.428, 2 yume at 07.0.9, o7its8is, ssi, 1519.20, tempera reading ‘£56 ste average slope (orale charg) ealeulale avordanco wi ALTO. Tabi AA hag boon dovved fom ho monographalh Figs. Gand 7 6 9-97 APPENDIXES, (Nonmandatory Information) XI. EXAMPLES ILLUSTRATING CALCULATIONS FOR REPORTING OF DATA X1.1 The observed distillation data used for the ealculation Ses of the examples below are shown in the first three columns of Fig. X11 X1.L.1 Temperature readings corrected to 101.3 kPa (760 mm Hg) pressure (ee 11.3) are as follows: coreetion (*€) = 00009 (101.3 ~ 98.6) (27344) C1.) 0012 (760 ~ 740) (460-4) X1.2) XI.1.2 Loss correction to 101.3 kPa (see 11.4) are as follows. The data for the exximples are taken from Fig. X11. coxrection (°F) comected oss = (05 + (4.7~05)) 4 «xiay {1 +1013 - 98.780) 6 X1.1.3 Recovery conection to 101.3 kPa (see 11.4.1) are as, comected recovery = 12+(49- 36) =953 (X14) 2Ai pas - 17 X12 Temperature Readings at Prescribed Percent Evaporated X1.2.1 Temperature reading at 10% evaporated (4.7 % observed loss = 5.3 % recovered) (See 11.6.1) are as follows: Tye (°C) = 387+ ((403 ~ 339) xis) (53-5) (10~s)]= 34126 Tree (°F) = 92.74 [(1088 ~ 92.9) (x16) (53 ~5)1 (10-5) = 93.41°F X1.2.2 Temperature reading at 50% evaporated (45.3 % recovered) (see 11.6.1) ate as follows: 39+ [(108.9 3.9) oan Toe (45:3 ~ 40) 1 (50~ 40)} = 101.9°C Tae (°F) = 201-+{(228 - 201) x18) (453 ~ 40) # (50~40)] = 215.9 X12.3 Temperature reading at 90 % evaporated (85.3 % recovered) (see 11.6.1) are as follows: Tye (°C) ~ 181.6+[(201.6~ 181.6) x9) (85.385) /(90~ 85) ]= 828°C Toys °F) = 398:9+[(3968~ 3589) (1.10) (853-85) /(90~88)] = 3610°F X1.24 Temperature reading at 90% evaporated (85.3 % recovered) not corrected to 101.3 KPa presure (see 11.61) are 1 follows: o (853 85} /(90~85)] = 181°C Tone (°F) = 387+{(392 ~ 357) (853— 85) / (90 - 85)) = 399.1°F Nore XI1—Results calculated from *C dala may not cortespond ‘exactly 10 reals ealelated from °F data ease of erors in rounding. (x1,12) X2. EXAMPLES OF CALCULATION OF REPEATABILITY AND REPRODUCIBILITY OF VOLUME % (RECOVERED OR EVAPORATED) AT A PRESCRIBED TEMPERATURE READING ‘TABLE X2-1 Distiltion Data from @ Group 1 Sample Manual Distlaton Diatitaion Polat ic ae oa Tempera iporstur F —_Reoovered at Unie ied 93.5" (200. 100 10 0 109 0 03 a0 0 wi 233 oka Cy ‘silaton Pont Qala Pont Temperature? Temperature’ F —_Eveporstod et porated, an Ta 10 9 02 20 4 2 30 103 a7 0 a 22 X2.1 Some specifications require the reporting of the vol- ume % evaporated or recovered at a prescribed temperature, ‘Table X2.1 shows the distillation data of a Group | sample as obtained by a manual uni X22 Example Calculation X2.2.1 Fora Group | sample exhibiting distillation charac- totstes as per Table X2.1, as determined by a manual unit, dhe reproducibility of the volume evaporated, "volume %, at 93.3 °C (200 °F) is determined as follows: X2.2.111 Determine first the slope at the desired tempera- cure: 5% = 01 (Tom ~ Tog) 2.1) 0.1 (94-83) 5,9 = 01 (Fon ~ Tra) =0.1 (201 ~ 182) =19 X22.2 From Table A4.4, determine the value of R, the reproducibility at the observed percentage distilled. In this ‘ease, the observed percentage distilled is 18 % and 204194(S)) 02.2) = 2.06 1.78% 11 =39 k= 35+ 1.24(5,) 364 LAX 19 =69 2.2.3 From the calculated value of R, determine the value of volume, as described in A4.10. 2 volume % = R/(S<) 02.3) aor 35 R volume 6 = RU(S;,) =69n19 “36# a8 8 $ 3 26 397 138 370 iy 8 Beg E i Bug & SSSSEES ZEGEESESSESEE' 1X3. TABLES OF CORRECTED LOSS FROM MEASURED LOSS AND BAROMETRIC PRESSURE. X3.1 The table presented as Fig. X3.1 can be used 0 _X3.2 ‘The table presented as Fig. X32 can be used t0 determine the corrected loss from the measured loss and the determine the corrected loss from the measured loss and the barometric pressure in kPa. barometric pressure in mm Hg. 25 at W bel adeoS OR 2 228S8E2EE89 2 eeenne SEGSSEES eaeceh BEREEES e 8 X3.2 Corrected Loss from Observed! Loss and Barometric Pressure mm Hg X4, PROCEDURE TO EMULATE THE EMERGENT STEM ERROR OF A MERCURY:IN- X4.1 When an electronic or other sensor without an emer- gent stem eror is used, the output of this sensor or the associated data system should emulate the output ofa mercury in-glass thermometer. Based on information supplied by four manufacturers of automated Test Method D86 equipment, the averaged equations shown in X4.2 and X4.3 have been reported to be in use, X4.1.1 The equations shown in X4,2 have limited applica. bility and are shown for information purposes only. In addition to the correction for the emergent stem, the electronic sensor and associated data system will also have to emulate the lag in response time observed for mercury-in-glass thermometers, X4.2. When a low range thermometer would have been used, no stem correction is 10 be applied below 20°C. Above this temperature, the correction is calculated using the following formula: {LASS THERMOMETER. ASTM 7€ T., = T, ~ 0.900162 x(7,~ 20"C)* (X41) X43 When @ high range thermometer would have been used, no stem correction is to be applied below 35°C, Above this temperature the correction is calculated using the follow- ing formula: AST 8C Tye, T,~ 0000131 (7,— 38°C)? (4.2) where: Toy = emulated temperature in °C for low range thermometers, Toye = emulated temperature in °C for high range thermometers, and T, = true temperature in °C.fly vss - 17 “Percent Recovered” Report Form SA TTS me bead [Ambient barometric pressure at the start of ‘ine tres Oo Nab donanats anata [eames gras aaah Soares Spentie ct te open each ees era fe “Kabiert temperature") T [Temperature measuring device readings See aeae ey fiahaccsroteho toca “Condenser temperature CC) —, 2 Se a add apa Co pap rex Foran Cored aE ae ene Percent Le ed] Timeor ear recovered | Fempeature | tye eC) Sia aa TT E eomeiosmin tot i Teas Teoria mene [nny gioar ons he tesa 4 20 Lare reached 3 vo 35

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