1、Designation:D734411 Designation: D7344 11aStandard 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
2、 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 determination of the distillation characteris
3、tics of petroleum products in therange of 20 to 400C (68 to 752F) using miniaturized automatic distillation apparatus.1.2 This test method is applicable to such products as: light and middle distillates, automotive spark-ignition engine fuels,automotive spark-ignition engine fuels containing up to 1
4、0 % ethanol, aviation gasolines, aviation turbine fuels, regular and lowsulfur 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 distillate products; i
5、t is not applicable to products containing appreciablequantities of residual material.1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.1.5 This standard does not purport to address all of the safety concerns, if any, assoc
6、iated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products at Atm
7、ospheric PressureD323 Test Method for Vapor Pressure of Petroleum Products (Reid Method)D4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petroleum and Petroleum ProductsD4953 Test Method for Vapor Pressure of Gasoline and Gasoline-Oxygena
8、te Blends (Dry Method)D5190 Test Method for Vapor Pressure of Petroleum Products (Automatic Method)D5191 Test Method for Vapor Pressure of Petroleum Products (Mini Method)D5482 Test Method for Vapor Pressure of Petroleum Products (Mini MethodAtmospheric)D6300 Practice for Determination of Precision
9、and Bias Data for Use in Test Methods for Petroleum Products and LubricantsD6708 Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purportto Measure the Same Property of a Material2.2 Energy Institute Standards:3IP 69 Determination of Vapour Pres
10、sureReid MethodIP 394 Determination of Air Saturated Vapour Pressure3. Terminology3.1 Definitions:3.1.1 charge volume, nin petroleum products, in distillation, volume of the liquid sample transferred to the specimencontainer.3.1.2decomposition, nof a hydrocarbon , pyrolysis or cracking of a molecule
11、 yielding smaller molecules with lower boilingpoints than the original molecule.3.1.2.11This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.08 onVolatility.Current edition approved JulyDec. 1, 2011
12、. Published August 2011.January 2012. Originally approved in 2007. Last previous edition approved in 20082011 asD734408.D734411. DOI: 10.1520/D7344-11A.2For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM S
13、tandardsvolume information, refer to the standards Document Summary page on the ASTM website.3Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, U.K., http:/www.energyinst.org.uk.1This document is not an ASTM standard and is intended only to provide the user of an ASTM standard
14、an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is
15、to be considered the official document.*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.1.1 decomposition point, nin distillation, the corrected temperature reading
16、that coincides with the first indications ofthermal decomposition of the specimen.3.1.33.1.2 dynamic holdup, nin D7344 distillation, amount of material present in the distillation column, and in the condenserduring the distillation.3.1.43.1.3 end point (EP) or final boiling point (FBP), nmaximum cor
17、rected temperature reading obtained during the test.3.1.53.1.4 initial boiling point (IBP), nin D7344 distillation, corrected temperature reading at the instant of the first detection ofcondensate in the receiver.3.1.63.1.5 percent evaporated, nin distillation, sum of the percent recovered and the p
18、ercent loss.3.1.73.1.6 percent loss, n in distillation, one hundred minus the percent total recovery.3.1.7.13.1.6.1 corrected loss, npercent loss corrected for barometric pressure.3.1.83.1.7 percent recovered, nin distillation, the volume of condensate collected relative to the charge volume.sample
19、charge.3.1.93.1.8 percent recovery, nin distillation, maximum percent recovered relative to the charge volume.sample charge.3.1.9.13.1.8.1 corrected percent recovery, nin distillation, the percent recovery, adjusted for the difference between thepercent loss and the corrected percent loss.3.1.9.2, t
20、he percent recovery, adjusted for the corrected percent loss.3.1.8.2 percent total recovery, nin distillation, the combined percent recovery and percent residue.3.1.103.1.9 percent residue, nin distillation, the volume of residue relative to the charge volume. , the volume of residue relativeto the
21、sample charge.3.1.10 sample charge, nthe amount of sample used in a test.3.1.11 vapor temperature reading, ntemperature of the saturated vapor measured in the distillation column below the vaportube, as determined by the prescribed conditions of the test.3.1.11.1 corrected vapor temperature reading,
22、 ntemperature reading, as described in 3.1.11, corrected for barometricpressure.4. Summary of Test Method4.1 Based on its composition, vapor pressure, expected IBP or expected FBP, or a combination thereof, the sample is placed inone of four groups. Condenser temperature and other operational variab
23、les are defined by the group in which the sample falls.4.2 A specimen of the sample is distilled under prescribed conditions for the group in which the sample falls. The specimenvolume for distillation Groups 1 to 3 is 6 mL. For Group 4, the specimen volume is 5.5 mL. The distillation is performed i
24、n anautomatic, miniaturized distillation apparatus at ambient pressure under conditions that are designed to provide approximately onetheoretical plate fractionation. The vapor temperature readings and volumes of condensate are monitored continuously. After thetest, specimen losses and residue are r
25、ecorded.4.3 After conclusion of the test, the temperatures are automatically corrected for barometric pressure, using the pressure readingof a built-in pressure transducer. The data are examined for conformance to procedural requirements, such as distillation rates. Thetest has to be repeated if any
26、 specified condition has not been met.4.4 Test results are commonly expressed as percent volume evaporated or percent volume recovered versus corresponding vaportemperature, either in a table or graphically, as a plot of the distillation curve.4.5 This test method uses a small specimen volume and mi
27、niaturized apparatus which can be portable for field testing.5. Significance and Use5.1 The distillation (volatility) characteristics of hydrocarbons have an important effect on their safety and performance,especially in the case of fuels and solvents. The boiling range gives information on the comp
28、osition, the properties, and thebehavior of the fuel during storage and use. Volatility is the major determinant of the tendency of a hydrocarbon mixture to producepotentially explosive vapors.5.2 The distillation characteristics are equally important for both automotive and aviation gasolines, affe
29、cting starting, warm-up,and tendency to vapor lock at high operating temperatures or high altitude, or both. The presence of high boiling point componentsin these and other fuels can significantly affect the degree of formation of solid combustion deposits.5.3 Volatility, as it affects the rate of e
30、vaporation, is an important factor in the application of many solvents, particularly thoseused in paints.5.4 Distillation limits are often included in petroleum product specifications, in commercial contract agreements, processrefinery/control applications, and for compliance to regulatory rules.D73
31、44 11a26. Apparatus6.1 Automatic Distillation ApparatusThe type of apparatus suitable for this test method employs a heat source, a specimencup, a stainless steel distillation column, a temperature measuring device, a thermoelectrically controlled condenser and receiversystem, a thermoelectrically c
32、ontrolled sample introduction and dosing system, and a system to measure and automatically recordthe vapor temperature, the associated percent recovered volume in the receiver, the condenser temperature, and the barometricpressure.46.2 A description of the apparatus is given in Annex A1.6.3 Sample I
33、ntroduction and Dosing SystemA system capable to automatically draw sample from a sample container and fillthe specimen container cup with a specimen of 6 6 0.05 mL or 5.5 6 0.05 mL.6.4 Temperature Measuring DeviceAthermocouple (NiCr-Ni or similar) in stainless steel tube of 1 6 0.02 mm diameter wit
34、ha response time of t(90) = 3 6 1 s shall be used for measuring the temperature of the vapor. The minimum resolution shall be 0.1C(0.2F), and the minimum accuracy 60.1C (0.2F).6.5 Pressure TransducerA pressure transducer with a minimum range of 0 to 120 kPa with a minimum resolution of 0.1 kPashall
35、be used. The minimum accuracy shall be 60.1 kPa.6.6 Balance, with a minimum range of 25 g and a minimum accuracy of 63 mg.6.7 Pressure Measuring Device for Calibration, capable of measuring local station pressure with an accuracy and a resolutionof 0.1 kPa (1 mm Hg) or better, at the same elevation
36、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 materials usedin this test method are toluene (WarningFlammable and a health hazard) and hexadecane (see Sec
37、tion 10). Unless otherwiseindicated, it is intended that all reagents conform to the specifications of the Committee on Analytical Reagents of the AmericanChemical Society5where such specifications are available. Lower purities can be used, provided it is first ascertained that thereagent is of suff
38、icient purity to permit its use without lessening the accuracy of the determination.NOTE 1The chemicals in this section are suggested for quality control procedures (see Section 10) and are not used for instrument calibration.8. Sampling, Storage, and Sample Conditioning8.1 Determine the group chara
39、cteristics that correspond to the sample to be tested (see Table 1). Where the procedure isdependent upon the group, the section headings will be so marked.8.2 Sampling:8.2.1 Only samples that are liquid at room temperature can be tested by this test method.8.2.2 Sampling shall be done as described
40、in Table 2 and in accordance with Practice D4057 or D4177, except do not use the“Sampling by Water Displacement” section for fuels containing oxygenates.8.2.2.1 Groups 1 and 2Collect the sample as described in 8.2.2 at a temperature below 10C (50F). If this is not possiblebecause, for instance, the
41、product to be sampled is at ambient temperature, the sample shall be drawn into a bottle prechilled tobelow 10C (50F), in such a manner that agitation is kept at a minimum. Close the bottle immediately with a tight-fitting closure.(WarningDo not completely fill and tightly seal a cold bottle of samp
42、le due to the of the likelihood of breakage upon warming.)4The sole source of supply of the apparatus known to the committee at this time is Grabner Instruments,A-1220 Vienna, Dr. Otto Neurathgasse 1,Austria. If you are awareof alternative suppliers, please provide this information toASTM Internatio
43、nal Headquarters. Your comments will receive careful consideration at a meeting of the responsibletechnical committee, which you may attend.5Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed b
44、ythe American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.TABLE 1 Group CharacteristicsGroup 1 Group 2 Group 3 Group 4Sample charact
45、eristicsDistillate typeVapor pressure at:37.8C, kPa $65.5 100F #212 212EP C #250 #250 250 250F #482 #482 482 482D7344 11a38.2.2.2 Groups 3 and 4Collect the sample at ambient temperature. After sampling, close the sample bottle immediately witha tight-fitting closure.8.2.2.3 If the sample received by
46、 the testing laboratory has been sampled by others and it is not known whether sampling hasbeen performed as described in 8.2, the sample shall be assumed to have been so sampled.8.2.2.4 Follow the manufacturers instructions for introducing the test specimen into the measuring chamber.8.3 Sample Sto
47、rage: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. Allsamples shall be stored away from direct sunlight or sources of direct heat.8.3.2 Groups 1 and 2Store the sample at a temperature below 10C (50F).NOTE 2If there are n
48、o, or inadequate, facilities for storage below or equal 10C (50F), the sample may also be stored at a temperature below 20C(68F), provided the operator ensures that the sample container is tightly closed and leak-free.8.3.3 Groups 3 and 4Store the sample at ambient or lower temperature.8.4 Sample Co
49、nditioning Prior to Analysis:8.4.1 Samples shall be conditioned to the temperature shown in Table 2 before opening the sample container.8.4.1.1 Groups 1 and 2Samples shall be conditioned to a temperature of less than 10C (50F) before opening the samplecontainer.8.4.1.2 Groups 3 and 4Samples shall be conditioned to a temperature not above ambient before opening the sample container.8.5 Wet Samples:8.5.1 Samples of materials that visibly contain water are not suitable for testing. If the sample is not dry, obtain another samp
