1、Designation: D 7344 08An American National StandardStandard Test Method forDistillation of Petroleum Products at Atmospheric Pressure(Mini Method)1This standard is issued under the fixed designation D 7344; the number immediately following the designation indicates the year oforiginal adoption or, i
2、n the case of 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
3、characteristics of petroleum productsin 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 containin
4、g up to 10 %ethanol, aviation gasolines, 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 distillateprodu
5、cts; 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 thesafety concerns, if any, as
6、sociated 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 Distillation of Petroleum Products
7、atAtmospheric PressureD 323 Test Method for Vapor Pressure of Petroleum Prod-ucts (Reid Method)D 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 4953 Test Method for Vapor Pressure of Gasoline andGasoline-
8、Oxygenate Blends (Dry Method)D 5190 Test Method for Vapor Pressure of Petroleum Prod-ucts (Automatic Method)D 5191 Test Method for Vapor Pressure of Petroleum Prod-ucts (Mini Method)D 5482 Test Method for Vapor Pressure of Petroleum Prod-ucts (Mini MethodAtmospheric)D 6300 Practice for Determination
9、 of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsD 6708 Practice for Statistical Assessment and Improve-ment of Expected Agreement Between Two Test Methodsthat Purport to Measure the Same Property of a Material2.2 Energy Institute Standards:3IP 69 Determination
10、of Vapour PressureReid MethodIP 394 Determination 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
11、 of a molecule yielding smaller molecules with lowerboiling points than the original molecule.3.1.2.1 decomposition point, ncorrected thermometerreading that coincides with the first indications of thermaldecomposition of the liquid in the specimen container.3.1.2.2 DiscussionCharacteristic indicati
12、ons of thermaldecomposition are evolution of fumes and erratic, typicallydecreasing, temperature readings that occur during the finalstages of the distillation.3.1.2.3 DiscussionThe decomposition point, as deter-mined under the conditions of this test method, does notnecessarily correspond to the de
13、composition temperature inother applications.3.1.3 dynamic holdup, namount of material present in thedistillation column, and in the condenser during the distillation.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibilit
14、y of SubcommitteeD02.08 on Volatility.Current edition approved Oct. 15, 2008. Published November 2008. Originallyapproved in 2007. Last previous edition approved in 2007 as D 734407.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.o
15、rg. For Annual Book of ASTMStandards 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.Copyri
16、ght ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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), ncorrected temperaturereading at the instant
17、 of the first detection of condensate in thereceiver.3.1.6 percent evaporated, nsum of the percent recoveredand the percent loss.3.1.7 percent loss, none hundred minus the percent totalrecovery.3.1.7.1 corrected loss, npercent loss corrected for baro-metric pressure.3.1.8 percent recovered, nvolume
18、of condensate observedin the receiver, expressed as a percentage of the charge volume,associated with a simultaneous temperature reading.3.1.9 percent recovery, nmaximum percent recovered.3.1.9.1 corrected percent recovery, npercent recovery,adjusted for the difference between the corrected loss and
19、 theobserved loss.3.1.9.2 percent total recovery, ncombined percent recov-ery and percent residue.3.1.10 percent residue, nvolume of residue in the speci-men container, expressed as a percentage of the charge volume.3.1.11 vapor temperature reading, ntemperature of thesaturated vapor measured in the
20、 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, vapor pressure, expected
21、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 falls.4.2 A specimen of the sample is distilled under prescribedconditions for the group in which the sample falls
22、. 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 ambient pressure under conditions that are designed toprovide approximately one theoretical plate fractionation.
23、 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 built-in pressure transd
24、ucer. 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 correspondingvapor tempera
25、ture, 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-bons have an important e
26、ffect on their safety 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 potenti
27、ally 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 highboiling point components in these and other
28、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 are often included in petroleum prod-uct sp
29、ecifications, in commercial 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 colum
30、n, 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 automatically record the vapor temperature, theassociated percent recovered volume in the receiver, the
31、condenser temperature, 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.
32、6.4 Temperature Measuring 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 Pres
33、sure TransducerA pressure 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 ofmeasurin
34、g local station pressure with an accuracy and a4The 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 Headqu
35、arters. Your comments will receive careful consideration at a meetingof the responsible technical committee,1which you may attend.D7344082resolution 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 Re
36、agentsUse 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 that all reagentsconform to the specification
37、s of the Committee on 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 chemica
38、ls 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 Table 1). Where the procedure isdependent up
39、on 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 D 4057 or D 4177, except do not usethe “Sampling by Water Displ
40、acement” section for fuelscontaining 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
41、 10C (50F), in such a manner 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 ambientt
42、emperature. 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 sample shall beassumed to have been so samp
43、led.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 samples shall be stored away from direct
44、sunlight orsources of direct 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 co
45、ntainer istightly closed 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 condit
46、ioned to atemperature of 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. I
47、f the sample is not dry, 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, sh
48、aking themixture for approximately 2 min, and then allowing themixture to settle for approximately 15 min. Once the sample5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemi
49、cal 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 ConditioningGroup 1 Group 2 Group 3 Group 4Temperature of sample bottle C 10F 50Temperature of sto
