1、Designation: D7344 17aStandard 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 characteristi
3、cs 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, all grades ofNo. 1 and No. 2 diesel fuels (as described in SpecificationD975), biodiesel (B100), biodiesel blends up to 30 % biodiesel,special petroleum spirits, pure petrochemical compounds,naphthas, white spirits, kerosenes
5、, furnace fuel oils, anddistillate marine fuels.NOTE 1The up to 10 % by volume ethanol limit in spark ignitionengine fuels (E10) was the range used in the supporting interlaboratorystudies. Spark ignition engine fuels containing 10 % by volume ethanoland up to 20 % by volume ethanol (E20) may be ana
6、lyzed, however thestated precision and bias does not apply.1.3 This test method is designed for the 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 g
7、iven in parentheses are for informationonly.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicab
8、ility of regulatory limitations prior to use.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the
9、World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products andLiquid Fuels at Atmospheric PressureD323 Test Method for Vapor Pressure of Petroleum Products(Reid Method)D975 Specification for Di
10、esel Fuel OilsD1160 Test Method for Distillation of Petroleum Products atReduced PressureD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4953 Test Method for Vapor Pressure of Gasoline andGasoline-Oxygenate
11、 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 Test Method for Vapor Pressure of Petroleum Prod-ucts (Mini MethodAtmospheric)D6300 Practice for Determin
12、ation 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 thatPurport to Measure the Same Property of a Material2.2 Energy Institute Standards:4IP 69 Determinatio
13、n of Vapour PressureReid MethodIP 394 Determination of Air Saturated Vapour Pressure1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.08 on Volatility.Current edition approved Dec.
14、15, 2017. Published February 2018. Originallyapproved in 2007. Last previous edition approved in 2017 as D7344 17. DOI:10.1520/D7344-17A.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume i
15、nformation, 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, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.*A Summary of Changes section appe
16、ars at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Princip
17、les for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.13. Terminology3.1 Definitions:3.1.1 decomposition, nof a hydrocarbon, pyrolysis orcracking of a molecule yielding smaller molecules with l
18、owerboiling 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 present in the distillation
19、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.3.1.4 initial boiling point (IBP), nin D7344 distillation,corrected temperature reading at the instant of the first detec-tion of conde
20、nsate 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 corrected loss, npercent loss corrected for baro-metric pressure.3.1.7 percent recovered, nin
21、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 distillation, thepercent recovery, adjusted for the corrected percent loss.3.1.8.2 pe
22、rcent 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 amount of sample used in atest.3.1.11 vapor temperature reading, ntemperature of thesatura
23、ted 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, corrected forbarometric pressure.4. Summary of Test Method4.1 Based on its composition,
24、vapor pressure, expected IBPor expected FBP, or a combination thereof, the sample is placedin one of five groups. Condenser temperature and otheroperational variables are defined by the group in which thesample falls.4.2 A specimen of the sample is distilled under prescribedconditions for the group
25、in which the sample falls. Thespecimen volume for distillation Groups 0 to 3 is 6 mL. ForGroup 4, the specimen volume is 5.5 mL. The distillation isperformed in an automatic, miniaturized distillation apparatusat ambient pressure under conditions that are designed toprovide approximately one theoret
26、ical 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 temperatures are auto-matically corrected for barometric pressure, using the pressurereading of a
27、 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 are commonly expressed as percent volumeevaporated or percent volume recovered versus c
28、orrespondingvapor 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 testing.5. Significance and Use5.1 The distillation (volatility) characteristics of hydrocar
29、-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 of the fuel during storage and use.Volatility is the major determinant of the tendency
30、 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 vapor lock at high operatingtemperatures or high altitude, or both. The presence of highb
31、oiling 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 application of many solvents, particu-larly those used in paints.5.4 Distillation limits
32、are often included in petroleum prod-uct specifications, in commercial contract agreements, processrefinery/control applications, and for compliance to regulatoryrules.5.5 This test method is suitable for setting specifications, foruse as an internal quality control tool, and for use in develop-ment
33、 or research work on hydrocarbon solvents.5.5.1 This test method gives a broad indication of generalpurity and can also indicate presence of excessive moisture. Itwill not differentiate between products of similar boiling range.6. Apparatus6.1 Automatic Distillation ApparatusThe type of appara-tus s
34、uitable 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, and a system tomeasure and
35、automatically record the vapor temperature, theD7344 17a2associated 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 automatically draw
36、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 be usedfor measu
37、ring 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 be60.1 kPa.6.6
38、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 of 0.1 kPa (1 mm Hg) or better, at the sameelevation relative to sea level as the apparatus in the laborator
39、y.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 (WarningFlammable and a health hazard) and hexadecane (see Section10). Unless otherwise indicated, it is intended th
40、at all reagentsconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society6where suchspecifications are available. Lower purities can be used,provided it is first ascertained that the reagent is of sufficientpurity to permit its use without lessening the acc
41、uracy of thedetermination.NOTE 2The chemicals in this section are suggested for quality controlprocedures (see Section 10) and are not used for instrument calibration.8. Sampling, Storage, and Sample Conditioning8.1 Determine the group characteristics that correspond tothe sample to be tested (see T
42、able 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 method.8.2.2 Sampling shall be done as described in Table 2 and inaccordance with Practice D4057 or D4177, exce
43、pt 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 this is notpossible because, for instance, the product to be sampled is atambient temperature, the sample shal
44、l 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 completely filland tightly seal a cold bottle of sample due to the likelihood ofbreakage upon warming.)8.2.2.2 Groups
45、 0, 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 laboratory hasbeen sampled by others and it is not known whether samplinghas been performed as described in 8.2, the s
46、ample 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 is not to start immediately after collection,store the samples as indicated in 8.3.2 and 8.3.3 and Table 2.All
47、 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 3If there are no, or inadequate, facilities for storage below orequal 10 C (50 F), the sample may also be stored at a temperature below20 C (68 F),
48、provided the operator ensures that the sample container istightly closed and leak-free.8.3.3 Groups 0, 3, and 4Store the sample at ambient orlower temperature.8.4 Sample Conditioning Prior to Analysis:8.4.1 Samples shall be conditioned to the temperatureshown in Table 2 before opening the sample con
49、tainer.8.4.1.1 Groups 1 and 2Samples shall be conditioned to atemperature of less than 10 C (50 F) before opening thesample container.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 careful consideration at a meetingof the responsible technical committee,1which you may attend.6Reagent Chemical
