1、Designation: D7344 11Standard Test Method forDistillation of Petroleum Products at Atmospheric 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 revision, the yea
2、r 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 characteristics of petroleum pr
3、oductsin the range of 20 to 400C (68 to 752F) using miniaturizedautomatic 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 containing up to 10 %ethanol, aviation g
4、asolines, aviation turbine fuels, regular andlow sulfur diesel fuels, biodiesel blends up to 20 % biodiesel,special petroleum spirits, naphthas, white spirits, kerosines,burner fuels, and marine fuels.1.3 This test method is designed for the analysis of distillateproducts; it is not applicable to pr
5、oducts 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 thesafety concerns, if any, associated with its use. It is th
6、eresponsibility 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 Distillation of Petroleum Products atAtmospheric PressureD323 Test
7、 Method for Vapor Pressure of Petroleum Prod-ucts (Reid Method)D4057 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 Blends (Dry Method)D5190
8、Test Method for Vapor Pressure of Petroleum Prod-ucts (Automatic Method)D5191 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 Determination of Precision and BiasData for Use in T
9、est Methods for Petroleum Products andLubricantsD6708 Practice for StatisticalAssessment and Improvementof Expected Agreement Between Two Test Methods thatPurport to Measure the Same Property of a Material2.2 Energy Institute Standards:3IP 69 Determination of Vapour PressureReid MethodIP 394 Determi
10、nation of Air Saturated Vapour Pressure3. Terminology3.1 Definitions:3.1.1 charge volume, nin petroleum products, in distilla-tion, volume of the liquid sample transferred to the specimencontainer.3.1.2 decomposition, nof a hydrocarbon, pyrolysis orcracking of a molecule yielding smaller molecules w
11、ith lowerboiling points than the original molecule.3.1.2.1 decomposition point, nin distillation, the cor-rected temperature reading that coincides with the first indica-tions of thermal decomposition of the specimen.3.1.3 dynamic holdup, nin D7344 distillation, amount ofmaterial present in the dist
12、illation column, and in the condenserduring the distillation.3.1.4 end point (EP) or final boiling point (FBP),nmaximum corrected temperature reading obtained duringthe test.3.1.5 initial boiling point (IBP), nin D7344 distillation,corrected temperature reading at the instant of the first detec-tion
13、 of condensate in the receiver.3.1.6 percent evaporated, nin distillation, sum of thepercent recovered and the percent loss.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.08 on Volatility.Curre
14、nt edition approved July 1, 2011. Published August 2011. Originallyapproved in 2007. Last previous edition approved in 2008 as D734408. DOI:10.1520/D7344-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of AS
15、TMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 1
16、00 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.7 percent loss, nin distillation, one hundred minus thepercent total recovery.3.1.7.1 corrected loss, npercent loss corrected for baro-metric pressure.3.1.8 percent recovered, nin distillation, the volume ofconden
17、sate collected relative to the charge volume.3.1.9 percent recovery, nin distillation, maximum percentrecovered relative to the charge volume.3.1.9.1 corrected percent recovery, nin distillation, thepercent recovery, adjusted for the difference between thepercent loss and the corrected percent loss.
18、3.1.9.2 percent total recovery, nin distillation, the com-bined percent recovery and percent residue.3.1.10 percent residue, nin distillation, the volume ofresidue relative to the charge volume.3.1.11 vapor temperature reading, ntemperature of thesaturated vapor measured in the distillation column b
19、elow 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, vapor pressure, expected IBPor expected FBP, or
20、 a combination thereof, the sample is placedin one of four 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 in which the sample falls. Thespecimen volume f
21、or 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 ambient pressure under conditions that are designed toprovide approximately one theoretical plate fractionation. Thevapor temperature
22、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 built-in pressure transducer. The data are exa
23、minedfor 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 correspondingvapor temperature, either in a tabl
24、e 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-bons have an important effect on their safety
25、and performance,especially in the case of fuels and solvents. The boiling rangegives information on the composition, the properties, and thebehavior of the fuel during storage and use. Volatility is themajor determinant of the tendency of a hydrocarbon mixture toproduce potentially explosive vapors.
26、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 highboiling point components in these and other fuels can signifi-cant
27、ly 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 are often included in petroleum prod-uct specifications, in comme
28、rcial contract agreements, processrefinery/control applications, and for compliance to regulatoryrules.6. Apparatus6.1 Automatic Distillation ApparatusThe type of appara-tus suitable for this test method employs a heat source, aspecimen cup, a stainless steel distillation column, a tempera-ture meas
29、uring device, a thermoelectrically controlled con-denser and receiver system, a thermoelectrically controlledsample introduction and dosing system, and a system tomeasure and automatically record the vapor temperature, theassociated percent recovered volume in the receiver, thecondenser temperature,
30、 and the barometric pressure.46.2 A description of the apparatus is given in Annex A1.6.3 Sample Introduction and Dosing SystemA systemcapable to automatically draw sample from a sample containerand fill the specimen container cup with a specimen of 6 60.05 mL or 5.5 6 0.05 mL.6.4 Temperature Measur
31、ing DeviceA thermocouple(NiCr-Ni or similar) in stainless steel tube of 1 6 0.02 mmdiameter with a response time of t(90) = 3 6 1 s shall be usedfor measuring the temperature of the vapor. The minimumresolution shall be 0.1C (0.2F), and the minimum accuracy60.1C (0.2F).6.5 Pressure TransducerA press
32、ure transducer with aminimum range of 0 to 120 kPa with a minimum resolution of0.1 kPa shall be used. The minimum accuracy shall be 60.1kPa.6.6 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 pressu
33、re with an accuracy and aresolution of 0.1 kPa (1 mm Hg) or better, at the same elevationrelative 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 t
34、his test method are toluene (Warning4The 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. You
35、r comments will receive careful consideration at a meetingof the responsible technical committee,1which you may attend.D7344 112Flammable and a health hazard) and hexadecane (see Section10). Unless otherwise indicated, it is intended that all reagentsconform to the specifications of the Committee on
36、 AnalyticalReagents of the American Chemical Society5where 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 accuracy of thedetermination.NOTE 1The chemicals in this section ar
37、e 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 Table 1). Where the procedure isdependent upon the group, the sec
38、tion 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, except do not usethe “Sampling by Water Displacement” section for fu
39、elscontaining oxygenates.8.2.2.1 Groups 1 and 2Collect the sample as described in8.2.2 at a temperature below 10C (50F). If this is not possiblebecause, for instance, the product to be sampled is at ambienttemperature, the sample shall be drawn into a bottle prechilledto below 10C (50F), in such a m
40、anner that agitation is keptat a minimum. Close the bottle immediately with a tight-fittingclosure. (WarningDo not completely fill and tightly seal acold bottle of sample due to the of the likelihood of breakageupon warming.)8.2.2.2 Groups 3 and 4Collect the sample at ambienttemperature. After sampl
41、ing, 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 sample shall beassumed to have been so sampled.8.2.2.4 Follow the
42、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 samples shall be stored away from direct sunlight orsources of d
43、irect heat.8.3.2 Groups 1 and 2Store the sample at a temperaturebelow 10C (50F).NOTE 2If there are no, or inadequate, facilities for storage below orequal 10C (50F), the sample may also be stored at a temperature below20C (68F), provided the operator ensures that the sample container istightly close
44、d and leak-free.8.3.3 Groups 3 and 4Store the sample at ambient or lowertemperature.8.4 Sample Conditioning Prior to Analysis: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 o
45、f less than 10C (50F) before opening thesample container.8.4.1.2 Groups 3 and 4Samples shall be conditioned to atemperature not above ambient before opening the samplecontainer.8.5 Wet Samples:8.5.1 Samples of materials that visibly contain water are notsuitable for testing. If the sample is not dry
46、, obtain anothersample that is free from suspended water.8.5.2 Groups 1, and 2If such a sample cannot be ob-tained, the suspended water can be removed by maintaining thesample at 0 to 10C (32 to 50F), adding approximately 10 gof anhydrous sodium sulfate per 100 mLof sample, shaking themixture for ap
47、proximately 2 min, and then allowing themixture to settle for approximately 15 min. Once the sampleshows no visible signs of water, use a decanted portion of thesample, maintained between 1 and 10C (34 and 50F), for theanalysis. Note in the report that the sample has been dried bythe addition of a d
48、esiccant.NOTE 3Suspended water in hazy samples in Groups 1 and 2 can beremoved by the addition of anhydrous sodium sulfate and separating theliquid sample from the drying agent by decanting. For Test Method D86,5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, W
49、ashington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, 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 4Sample characteristicsDistillate typeVapor pressure at:37.8C, kPa $65.5 100F #212 212EP C #250 #250 250 250F #482 #482 482 482TABLE 2 Sampling, Storage, and Sample Condition
