1、Designation: D7344 14Standard Test Method forDistillation of Petroleum Products and Liquid Fuels atAtmospheric Pressure (Mini Method)1This standard is issued under the fixed designation D7344; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the procedure for the determi-nation of the distillation characteristic
3、s of petroleum productsand liquid fuels in the range of 20 C to 400 C (68 F to752 F) using miniaturized automatic distillation apparatus.1.2 This test method is applicable to such products as: lightand middle distillates, automotive spark-ignition engine fuels,automotive spark-ignition engine fuels
4、containing up to 10 %ethanol, aviation gasolines, aviation turbine fuels, regular andlow sulfur diesel fuels, biodiesel (B100), biodiesel blends up to20 % biodiesel, special petroleum spirits, naphthas, whitespirits, kerosines, burner fuels, and marine fuels.1.3 This test method is designed for the
5、analysis of distillateproducts; it is not applicable to products containing appreciablequantities of residual material.1.4 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.5 This standard does not purport to address all of the
6、safety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distilla
7、tion of Petroleum Products atAtmospheric PressureD323 Test Method for Vapor Pressure of Petroleum Products(Reid Method)D1160 Test Method for Distillation of Petroleum Products atReduced PressureD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling
8、 of Petroleum andPetroleum ProductsD4953 Test Method for Vapor Pressure of Gasoline andGasoline-Oxygenate Blends (Dry Method)D5190 Test Method for Vapor Pressure of Petroleum Prod-ucts (Automatic Method) (Withdrawn 2012)3D5191 Test Method for Vapor Pressure of Petroleum Prod-ucts (Mini Method)D5482
9、Test Method for Vapor Pressure of Petroleum Prod-ucts (Mini MethodAtmospheric)D6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsD6708 Practice for Statistical Assessment and Improvementof Expected Agreement Between Two Test Methods
10、 thatPurport to Measure the Same Property of a Material2.2 Energy Institute Standards:4IP 69 Determination of Vapour PressureReid MethodIP 394 Determination of Air Saturated Vapour Pressure3. Terminology3.1 Definitions:3.1.1 decomposition, nof a hydrocarbon, pyrolysis orcracking of a molecule yieldi
11、ng smaller molecules with lowerboiling points than the original molecule.3.1.1.1 decomposition point, nin distillation, the correctedtemperature reading that coincides with the first indications ofthermal decomposition of the specimen.3.1.2 dynamic holdup, nin D7344 distillation, amount ofmaterial p
12、resent in the distillation column, and in the condenserduring the distillation.3.1.3 end point (EP) or final boiling point (FBP),nmaximum corrected temperature reading obtained duringthe test.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lu
13、bricants and is the direct responsibility ofSubcommittee D02.08 on Volatility.Current edition approved Dec. 1, 2014. Published January 2015. Originallyapproved in 2007. Last previous edition approved in 2011 as D7344 11a. DOI:10.1520/D7344-14.2For referenced ASTM standards, visit the ASTM website, w
14、ww.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from Energy Institute,
15、61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.4 initial boiling point (IBP), nin D7344 dist
16、illation,corrected temperature reading at the instant of the first detec-tion of condensate in the receiver.3.1.5 percent evaporated, nin distillation, sum of thepercent recovered and the percent loss.3.1.6 percent loss, n in distillation, one hundred minus thepercent total recovery.3.1.6.1 correcte
17、d loss, npercent loss corrected for baro-metric pressure.3.1.7 percent recovered, nin distillation, the volume ofcondensate collected relative to the sample charge.3.1.8 percent recovery, nin distillation, maximum percentrecovered relative to the sample charge.3.1.8.1 corrected percent recovery, nin
18、 distillation, thepercent recovery, adjusted for the corrected percent loss.3.1.8.2 percent total recovery, nin distillation, the com-bined percent recovery and percent residue.3.1.9 percent residue, nin distillation, the volume ofresidue relative to the sample charge.3.1.10 sample charge, nthe amou
19、nt of sample used in atest.3.1.11 vapor temperature reading, ntemperature of thesaturated vapor measured in the distillation column below thevapor tube, as determined by the prescribed conditions of thetest.3.1.11.1 corrected vapor temperature reading,ntemperature reading, as described in 3.1.11, co
20、rrected forbarometric pressure.4. Summary of Test Method4.1 Based on its composition, vapor pressure, expected IBPor expected FBP, or a combination thereof, the sample is placedin one of four groups. Condenser temperature and otheroperational variables are defined by the group in which thesample fal
21、ls.4.2 A specimen of the sample is distilled under prescribedconditions for the group in which the sample falls. Thespecimen volume for distillation Groups 1 to 3 is 6 mL. ForGroup 4, the specimen volume is 5.5 mL. The distillation isperformed in an automatic, miniaturized distillation apparatusat a
22、mbient pressure under conditions that are designed toprovide approximately one theoretical plate fractionation. Thevapor temperature readings and volumes of condensate aremonitored continuously. After the test, specimen losses andresidue are recorded.4.3 After conclusion of the test, the temperature
23、s are auto-matically corrected for barometric pressure, using the pressurereading of a built-in pressure transducer. The data are examinedfor conformance to procedural requirements, such as distilla-tion rates. The test has to be repeated if any specified conditionhas not been met.4.4 Test results a
24、re commonly expressed as percent volumeevaporated or percent volume recovered versus correspondingvapor temperature, either in a table or graphically, as a plot ofthe distillation curve.4.5 This test method uses a small specimen volume andminiaturized apparatus which can be portable for field testin
25、g.5. Significance and Use5.1 The distillation (volatility) characteristics of hydrocar-bons and other liquids have an important effect on their safetyand performance, especially in the case of fuels and solvents.The boiling range gives information on the composition, theproperties, and the behavior
26、of the fuel during storage and use.Volatility is the major determinant of the tendency of ahydrocarbon mixture to produce potentially explosive vapors.5.2 The distillation characteristics are equally important forboth automotive and aviation gasolines, affecting starting,warm-up, and tendency to vap
27、or lock at high operatingtemperatures or high altitude, or both. The presence of highboiling point components in these and other fuels can signifi-cantly affect the degree of formation of solid combustiondeposits.5.3 Volatility, as it affects the rate of evaporation, is animportant factor in the app
28、lication of many solvents, particu-larly those used in paints.5.4 Distillation limits are often included in petroleum prod-uct specifications, in commercial contract agreements, processrefinery/control applications, and for compliance to regulatoryrules.6. Apparatus6.1 Automatic Distillation Apparat
29、usThe type of appara-tus suitable for this test method employs a heat source, aspecimen cup, a stainless steel distillation column, a tempera-ture measuring device, a thermoelectrically controlled con-denser and receiver system, a thermoelectrically controlledsample introduction and dosing system, a
30、nd a system tomeasure and automatically record the vapor temperature, theassociated percent recovered volume in the receiver, thecondenser temperature, and the barometric pressure.56.2 A description of the apparatus is given in Annex A1.6.3 Sample Introduction and Dosing SystemA systemcapable to aut
31、omatically draw sample from a sample containerand fill the specimen container cup with a specimen of 6 mL 60.05 mL or 5.5 mL 6 0.05 mL.6.4 Temperature Measuring DeviceA thermocouple(NiCr-Ni or similar) in stainless steel tube of 1 mm 6 0.02 mmdiameter with a response time of t(90) = 3 s 6 1 s shall
32、be usedfor measuring the temperature of the vapor. The minimumresolution shall be 0.1 C (0.2 F), and the minimum accuracy60.1 C (0.2 F).6.5 Pressure TransducerA pressure transducer with aminimum range of 0 kPa to 120 kPa with a minimum resolu-tion of 0.1 kPa shall be used. The minimum accuracy shall
33、 be60.1 kPa.5The sole source of supply of the apparatus known to the committee at this timeis Grabner Instruments,A-1220 Vienna, Dr. Otto Neurathgasse 1,Austria. If you areaware of alternative suppliers, please provide this information to ASTM Interna-tional Headquarters. Your comments will receive
34、careful consideration at a meetingof the responsible technical committee,1which you may attend.D7344 1426.6 Balance, with a minimum range of 25 g and a minimumaccuracy of 63 mg.6.7 Pressure Measuring Device for Calibration, capable ofmeasuring local station pressure with an accuracy and aresolution
35、of 0.1 kPa (1 mm Hg) or better, at the sameelevation relative to sea level as the apparatus in the laboratory.7. Reagents and Materials7.1 Purity of ReagentsUse chemicals of at least 99 %purity for quality control checks. Quality control check mate-rials used in this test method are toluene (Warning
36、Flammable and a health hazard) and hexadecane (see Section10). Unless otherwise indicated, it is intended that all reagentsconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society6where suchspecifications are available. Lower purities can be used,provided
37、 it is first ascertained that the reagent is of sufficientpurity to permit its use without lessening the accuracy of thedetermination.NOTE 1The chemicals in this section are suggested for quality controlprocedures (see Section 10) and are not used for instrument calibration.8. Sampling, Storage, and
38、 Sample Conditioning8.1 Determine the group characteristics that correspond tothe sample to be tested (see Table 1). Where the procedure isdependent upon the group, the section headings will be somarked.8.2 Sampling:8.2.1 Only samples that are liquid at room temperature canbe tested by this test met
39、hod.8.2.2 Sampling shall be done as described in Table 2 and inaccordance with Practice D4057 or D4177, except do not usethe “Sampling by Water Displacement” section for fuelscontaining oxygenates.8.2.2.1 Groups 1 and 2Collect the sample as described in8.2.2 at a temperature below 10 C (50 F). If th
40、is is notpossible because, for instance, the product to be sampled is atambient temperature, the sample shall be drawn into a bottleprechilled to below 10 C (50 F), in such a manner thatagitation is kept at a minimum. Close the bottle immediatelywith a tight-fitting closure. (WarningDo not completel
41、y filland tightly seal a cold bottle of sample due to the of thelikelihood of breakage upon warming.)8.2.2.2 Groups 3 and 4Collect the sample at ambienttemperature. After sampling, close the sample bottle immedi-ately with a tight-fitting closure.8.2.2.3 If the sample received by the testing laborat
42、ory hasbeen sampled by others and it is not known whether samplinghas been performed as described in 8.2, the sample shall beassumed to have been so sampled.8.2.2.4 Follow the manufacturers instructions for introduc-ing the test specimen into the measuring chamber.8.3 Sample Storage:8.3.1 If testing
43、 is not to start immediately after collection,store the samples as indicated in 8.3.2 and 8.3.3 and Table 2.All samples shall be stored away from direct sunlight orsources of direct heat.8.3.2 Groups 1 and 2Store the sample at a temperaturebelow 10 C (50 F).NOTE 2If there are no, or inadequate, faci
44、lities for storage below orequal 10 C (50 F), the sample may also be stored at a temperature below20 C (68 F), provided the operator ensures that the sample container istightly closed and leak-free.8.3.3 Groups 3 and 4Store the sample at ambient or lowertemperature.8.4 Sample Conditioning Prior to A
45、nalysis:8.4.1 Samples shall be conditioned to the temperatureshown in Table 2 before opening the sample container.8.4.1.1 Groups 1 and 2Samples shall be conditioned to atemperature of less than 10 C (50 F) before opening thesample container.8.4.1.2 Groups 3 and 4Samples shall be conditioned to atemp
46、erature not above ambient before opening the samplecontainer.8.5 Wet Samples:6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for Laborat
47、oryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE 1 Group CharacteristicsGroup 1 Group 2 Group 3 Group 4SamplecharacteristicsDistillate typeVapor pressure at:37.8 C, kPa $65.5 100F #21
48、2 212EP C #250 #250 250 250F #482 #482 482 482TABLE 2 Sampling, Storage, and Sample ConditioningGroup 1 Group 2 Group 3 Group 4Temperature of sample bottle C 10F 50Temperature of stored bottle C 10A10Aambient ambientF 50A50Aambient ambientTemperature of sample after C 10 10 ambient ambientconditioni
49、ng prior to analysis F 50 50 ambient ambientIf sample is wetBresample resample dryCdryCIf sample is still wetBdryDdryDAUnder certain circumstances, samples can also be stored at temperatures below20 C (68 F). See also 8.3.3.BIf sample is known to be wet, resampling may be omitted. Dry sample inaccordance with 8.5.2 and 8.5.3.CDry in accordance with 8.5.3.DDry in accordance with 8.5.2.D7344 1438.5.1 Samples of materials that visibly contain water are notsuitable for testing. If the sample is not dry, obtain anothers
