1、Designation:D656000 (Reapproved 2005) Designation: D6560 12Designation: IP 143/01Standard Test Method forDetermination of Asphaltenes (Heptane Insolubles) in CrudePetroleum and Petroleum Products1, 2This standard is issued under the fixed designation D6560; the number immediately following the desig
2、nation indicates the year oforiginal adoption or, in 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 a proc
3、edure for the determination of the heptane insoluble asphaltene content of gas oil, diesel fuel,residual fuel oils, lubricating oil, bitumen, and crude petroleum that has been topped to an oil temperature of 260C (seeA1.2.1.1).1.2 The precision is applicable to values between 0.50 and 30.0 % m/m. Va
4、lues outside this range may still be valid but maynot give the same precision values.1.3 Oils containing additives may give erroneous results.1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purpo
5、rt to address all of the safety concerns, if any, associated 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:3D86 Te
6、st Method for Distillation of Petroleum Products at Atmospheric PressureD1298 Test Method for Density, Relative Density (Specific Gravity), orAPI Gravity of Crude Petroleum and Liquid PetroleumProducts by Hydrometer MethodD4052 Test Method for Density, Relative Density, and API Gravity of Liquids by
7、 Digital Density MeterD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petroleum and Petroleum Products2.2 IP Standard: Energy Institute Standard:4Specifications for IP Standard Thermometers3. Terminology3.1 Definitions:3.1.1 asphaltenes,
8、 nwax-free organic material insoluble in heptane, but soluble in hot toluene (benzene).NOTE1Benzene is included in this definition solely on the basis of its classical references in the definition of asphaltenes. The precision of this testmethod when using toluene has been found to be the same as wh
9、en using benzene. (rarely used in the singular) in petroleum technology, representan oil fraction that is soluble in a specified aromatic solvent but separates upon addition of an excess of a specified paraffinic solvent.3.1.1.1 DiscussionIn this test method, the aromatic solvent is hot toluene and
10、the paraffinic solvent is heptane.3.1.1.2 DiscussionHistorically, benzene was the aromatic solvent, but benzene is not typically used now for health reasons.The precision of this test method when using toluene has been found to be the same as when using benzene.1This test method is under the jurisdi
11、ction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.14 onStability and Cleanliness of Liquid Fuels.Current edition approved Nov. 1, 2005. Published November 2005. Originally approved in 2000. Last previous edition approved in 2000 as
12、D656000. DOI:10.1520/D6560-00R05.Current edition approved April 15, 2012. Published May 2012. Originally approved in 2000. Last previous edition approved in 2005 as D656000(2005). DOI:10.1520/D6560-12.2This standard is based on material published in the IP Standard methods for Analysis and Testing o
13、f Petroleum and Related Products and British Standard 2000 Parts,copyright Energy Institute, 61 New Cavendish Street, London, W1M 8AR. Adapted with permission of Energy Institute.3For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. F
14、or Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.4Available from Energy Institute, 61 New Cavendish St., London, WIM 8AR, UK.1This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indi
15、cation 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 to be c
16、onsidered 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.4. Summary of Test Method4.1 A test portion of the sample is mixed with heptane and the
17、mixture heated under reflux, and the precipitated asphaltenes,waxy substances, and inorganic material are collected on a filter paper. The waxy substances are removed by washing with hotheptane in an extractor.4.2 After removal of the waxy substances, the asphaltenes are separated from the inorganic
18、 material by dissolution in hottoluene, the extraction solvent is evaporated, and the asphaltenes weighed.5. Significance and Use5.1 Asphaltenes are the organic molecules of highest molecular mass and carbon-hydrogen ratio normally occurring in crudepetroleum and petroleum products containing residu
19、al material. They may give problems during storage and handling if thesuspension of asphaltene molecules is disturbed through excess stress or incompatibility. They are also the last molecules in aproduct to combust completely, and thus may be one indicator of black smoke propensity. Their compositi
20、on normally includesa disproportionately high quantity of the sulfur, nitrogen, and metals present in the crude petroleum or petroleum product.6. Apparatus6.1 GeneralGround-glass joints from different sources may have one of two diameter to length ratios. For the purposes of thistest method, either
21、is suitable, and for some applications, the diameter itself can be one of two . However, it is critical that the maleand female parts of each joint are from the same series to avoid recession or protuberance.6.2 Condenser, with a coil or double surface, fitted with a 34/45 or 34/35 ground-glass join
22、t at the bottom to fit the top of theextractor. Minimum length is 300 mm.6.3 Reflux Extractor, conforming to the dimensions given in Fig. 1. Tolerances are 61 mm on the height and outer diameter(OD) of the extractor body and 60.5 mm on all other dimensions. The female ground-glass joint at the top s
23、hall match the maleat the bottom of the condenser, and the male ground-glass joint at the bottom shall match the female of the conical flask.6.4 Conical Flasks, of borosilicate glass of appropriate capacity (see 11.2 and Table 1), with ground-glass joints to fit the bottomof the extractor.NOTE2Sizes
24、 1Sizes 24/39, 24/29, 29/43, or 29/32 are suitable.6.5 Stopper, of borosilicate glass of a size to fit the conical flask.6.6 Evaporating Vessel, of borosilicate glass. Either a hemispherical dish of approximately 90 mm diameter, or another suitablevessel used in conjunction with a rotovapor.NOTE3A 2
25、A rotovapor in conjunction with a nitrogen atmosphere reduces the hazard of toluene evaporation (see 11.7).FIG. 1 ExtractorD6560 1226.7 Filter Funnel, of borosilicate glass, approximately 100 mm diameter.6.8 Filter Papers, Whatman5Grade 42, 110 or 125-mm diameter.6.9 Analytical Balance, capable of w
26、eighing with an accuracy of 0.1 mg.6.10 Forceps, of stainless steel, spade ended.6.11 Timing Device, electronic or manual, accurate to 1.0 s.6.12 Oven, capable of maintaining a temperature from 100 to 110C.6.13 Graduated Cylinders, of 50 and 100 mL capacity.6.14 Stirring Rods, of glass or polytetraf
27、luoroethylene (PTFE), 150 by 3-mm diameter.6.15 Cooling Vessel, consisting of either a dessicator without desiccant, or another suitable tightly-stoppered vessel.6.16 Mixer, high-speed, nonaerating.7. Reagents7.1 Toluene (methylbenzene) C6H5CH3, analytical reagent or nitration grade.7.2 Heptane C7H1
28、6, analytical reagent grade.8. Sampling8.1 Unless otherwise specified, take samples by the procedures described in Practice D4057 or D4177.9. Test Portion Preparation9.1 Test portions from the laboratory samples shall be drawn after thorough mixing and subdivision. Heat viscous samples ofresidual fu
29、els to a temperature that renders the sample liquid, but not above 80C, and homogenize, using the mixer (see 6.16) asnecessary.9.2 Heat samples of penetration grade bitumens to a temperature not exceeding 120C, and stir well before taking an aliquot.9.3 Samples of hard bitumens shall be ground to a
30、powder before an aliquot is taken.9.4 Samples of crude petroleum shall be prepared in accordance with the procedure described in the Annex A1, unless it isknown that the crude petroleum contains negligible quantities of material boiling below 80C.10. Apparatus Preparation10.1 Clean all glass flasks
31、(see 6.4) and dishes (see 6.6) by a means that matches the cleanliness obtained by the use of a stronglyoxidizing agent, such as chromosulfuric acid, ammonium peroxydisulfate in concentrated sulfuric acid at approximately 8 g/L, orsulfuric acid itself, soaking for at least 12 h, followed by rinses i
32、n tap water, distilled water, and then acetone, using forceps onlyfor handling. (WarningChromosulfuric acid is a health hazard. It is toxic, a recognized carcinogen as it contains Cr (VI)compounds, which are highly corrosive and potentially hazardous in contact with organic materials. When using chr
33、omosulfuricacid cleaning solution, eye protection and protective clothing are essential. Never pipette the cleaning solution by mouth.After use,do not pour cleaning solution down the drain, but neutralize it with great care, owing to the concentrated sulfuric acid present, anddispose of it in accord
34、ance with standard procedures for toxic laboratory waste (chromium is highly dangerous to the environment).Nonchromium containing, strongly oxidizing acid cleaning solutions are also highly corrosive and potentially hazardous in contactwith organic materials, but do not contain chromium, which has i
35、ts own special disposal problems.)10.2 For routine analysis, use a proprietary laboratory detergent to clean the glassware, followed by the rinses described in 10.1.When the detergent cleaning no longer matches the cleanliness required based on visual appearance, use a strong oxidizing agent.10.3 Af
36、ter rinsing, place the glassware in the oven (see 6.12) for 30 min, and cool in the cooling vessel (see 6.15) for 30 minbefore weighing.11. Procedure11.1 Estimate the asphaltene content of the sample, or residue obtained from the procedure inAnnexA1, and weigh the quantity,5The sole source of supply
37、 of the filter papers known to the committee at this time is Whatman Int. Ltd., Maidstone, UK. If you are aware of alternative suppliers, pleaseprovide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical comm
38、ittee, whichyou may attend.TABLE 1 Test Portion Size, Flask, and Heptane VolumesEstimated AsphalteneContent%m/mTest PortionSizegFlask VolumemLHeptane VolumemLLess than 0.5 10 6 2 1000 300 6 600.5to2.0 86 2 500 240 6 60Over 2.0 to 5.0 4 6 1 250 120 6 30Over 5.0 to 10.0 2 6 1 150 60 6 15Over 10.0 to 2
39、5.0 0.8 6 0.2 100 25 to 30Over 25.0 0.5 6 0.2 100 25 6 1D6560 123to the nearest 1 mg for masses above 1 g and to the nearest 0.1 mg for masses of 1 g and below (see Table 1), into a flask (see6.4) of appropriate capacity (see Table 1).11.2 Add heptane (see 7.2) to the test portion in the flask at a
40、ratio of 30 mL to each1gofsample if the expected asphaltenecontent is below 25 % m/m. For samples with an expected asphaltene content of above 25 % m/m, a minimum heptane volumeof 25 mL shall be used (see Table 1).11.3 Boil the mixture under reflux for 60 6 5 min. Remove the flask and contents at th
41、e end of this period, cool, close witha stopper (see 6.5), and store in a dark cupboard for 90 to 150 min, calculated from the time of removal from reflux.11.4 Place the filter paper, folded as shown in Fig. 2 (so as to prevent loss of asphaltenes by creeping), in the filter funnel, usingforceps. Th
42、ereafter, handle the filter paper only with forceps. Without agitation, decant the liquid into the filter paper, and thentransfer the the residue in the flask as completely as possible with successive quantities of hot heptane, using the stirring rod (see6.14) as necessary. Give the flask a final ri
43、nse with hot heptane, and pour the rinsings through the filter. Set the flask aside, withoutwashing, for use as specified in 11.6.11.5 Remove the filter paper and contents from the funnel, and place in the reflux extractor (see 6.3). Using a flask differentfrom that used initially, reflux with hepta
44、ne (see 7.2) at a rate of 2 drops/s to 4 drops/s from the end of the condenser for anextraction period of not less than 60 min, or until a few drops of heptane from the bottom of the extractor leave no residue onevaporation on a glass slide.11.6 Replace the flask by the one used initially, and to wh
45、ich has been added 30 to 60 mL of toluene (see 7.1), and continuerefluxing until all the asphaltenes have been dissolved from the paper.11.7 Transfer the contents of the flask to a clean and dry (see Section 10) evaporating vessel (see 6.6), weighed to the nearest0.2 mg by tare against a similar dis
46、h. Wash out the flask with successive small quantities of toluene to a total not exceeding 30mL. Remove the toluene by evaporation on a boiling water bath, or by evaporation in a rotovapor under an atmosphere of nitrogen.(WarningPerform the evaporation in a fume hood.)11.8 Dry the dish and contents
47、in the oven (see 6.12) at 100 to 110C for 30 min. Cool in the cooling vessel (see 6.15) for 30to 60 min and reweigh by tare against the dish used previously for this purpose, and which has been subjected to the same heatingand cooling procedure as was the dish containing asphaltenes.NOTE 43Asphalten
48、es are very susceptible to oxidation, and it is important that the procedure specified in the final drying stage is adhered to exactlyas regards to temperature and time 61 min.12. Calculation12.1 Calculate the asphaltene content, A, in % m/m, of petroleum products as follows:A 5 100 M/G! (1)D6560-12
49、_1where:M = is the mass of asphaltenes, in grams, andG = is the mass of test portion, in grams.12.2 Calculate the asphaltene content, C, in % m/m, of crude petroleum prepared in the manner described in the Annex, asfollows:D6560-12_2where:M = is the mass of asphaltenes, in grams,R = is the mass of the residue from distillation, in grams,G = is the mass of the residue aliquot, in grams, andD = is the mass of crude petroleum sample distilled, in grams.FIG. 2 Filter PaperD6560 12413. Report13.1 Report the following information:13.1.1 The heptane insoluble
