1、Designation: D7579 09Standard Test Method forPyrolysis Solids Content in Pyrolysis Liquids by Filtrationof Solids in Methanol1This standard is issued under the fixed designation D7579; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision
2、, 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. Scope1.1 This test method describes a filtration procedure fordetermining the pyrolysis solids content of pyrolys
3、is liquid. Itis intended for the analysis of pyrolysis liquid with all rangesof pyrolysis solids concentrations.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety c
4、oncerns, if any, associated 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. Material SafetyData Sheets are available for reagents and materials. Reviewthe
5、m for hazards prior to usage. For specific warning state-ments, see 7.2, 7.3, and 7.4.2. Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4175 Terminology Relating to Petroleum, PetroleumProducts, and LubricantsD4177 Practice for Automatic
6、 Sampling of Petroleum andPetroleum Products2.2 Other Standards:3ESPOO 2001 A guide to physical property characterisationof biomass-derived fast pyrolysis liquids3. Terminology3.1 Definitions:3.1.1 See also Terminology D4175.3.1.2 char, nfine carbonaceous powder that is separatedfrom the vapors of b
7、iomass during pyrolysis.3.1.2.1 DiscussionPyrolysis liquid biofuel contains uni-formly suspended char at varying concentrations.3.1.3 pyrolysis, nchemical decomposition of organic ma-terials by heating in the absence of oxygen.3.1.4 pyrolysis liquid biofuel, nliquid product from thepyrolysis of biom
8、ass.3.1.4.1 DiscussionPyrolysis liquid biofuel is comprisedof a complex mixture of the decomposition products ofligno-cellulosic biomass including highly oxygenated organiccompounds. It is produced from the pyrolysis of biomass,followed by the rapid condensation of its vapors.3.1.5 pyrolysis solids,
9、 nsolid particles contained withinthe pyrolysis liquid biofuel.3.1.5.1 DiscussionPyrolysis solids consists of ash andchar.4. Summary of Test Method4.1 Apyrolysis liquid sample is dissolved in a methanol anddichloromethane solution (1:1), which is then filtered througha vacuum filter system. After fi
10、ltering, the filtrand is washedwith the solvent until the filtrate is clear. The filter is removed,dried and weighed. The pyrolysis solids content is calculatedbased on the original pyrolysis liquid sample.5. Significance and Use5.1 Pyrolysis liquid can be produced to various char con-centrations. I
11、ncreasing pyrolysis solids content can affect thepyrolysis liquid biofuel handling, atomization and storagestability in a negative manner.6. Apparatus (see Fig. 1)6.1 Smooth-tip Forceps.6.2 Beaker, 400 mL.6.3 Glass Stirring Rod.6.4 Oven, explosion-proof, capable of maintaining a tem-perature of 105
12、6 3C.6.5 Filtering Flask,1L.6.6 Filter Holders, borosilicate glass.6.7 Filter Membrane, binder free glass microfiber, 1 m.6.8 Weighing Dish, aluminum.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of Subcommittee
13、D02.06 on Analysis of Lubricants.Current edition approved Oct. 1, 2009. Published October 2009. DOI: 10.1520/D7579-09.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer t
14、o the standards Document Summary page onthe ASTM website.3Available from VTT Energy, New Energy Technologies, Biologinkuja 35, P.O.Box 1601, FIN-02044 VTT, Finland. http:/www.vtt.fi/inf/pdf/publications/2001/P450.pdf1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken
15、, PA 19428-2959, United States.FIG. 1 Paper Filtration ApparatusD7579 0926.9 Balance, capable of weighing to the nearest 0.0001 g(0.1 mg) with a range of 300 g.6.10 Vacuum.7. Reagents and Solvents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it
16、is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its u
17、se without lessening theaccuracy of the determination. If an industrial grade reagent isused, it shall be filtered using 0.45 m filter paper prior to use.7.2 Ethanol, reagent grade. (WarningFlammable. Toxic.May be harmful or fatal if ingested or inhaled. Avoid skincontact.7.3 Methanol (MeOH), reagen
18、t grade. (WarningFlammable. Toxic. May be harmful or fatal if ingested orinhaled. Avoid skin contact.7.4 Dichloromethane (DCM), reagent grade. (WarningFlammable. Toxic. May be harmful or fatal if ingested orinhaled. Avoid skin contact.)7.5 Filter Paper, 1 m pore size, binder free glass microfi-ber.8
19、. Sampling8.1 Obtain a sample using either Practice D4057 or PracticeD4177.8.2 Obtain a representative sample of the pyrolysis liquidfrom a well-mixed container. The sample should be well mixedto ensure homogeneity.9. Procedure9.1 Dry a clean filter membrane for 15 min in a desiccator,place in a lab
20、eled aluminum weighing dish, and weigh to thenearest 0.1 mg.9.2 Place a 400 mL beaker on the balance, and tare it.9.3 Vigorously shake the sample by hand for a minimum of15 s.9.4 Using a disposable pipette, weigh approximately 15 g ofpyrolysis liquid sample into the beaker. Record the weight tothe n
21、earest 0.1 mg.9.5 Add approximately 100 to 200 mL MeOH-DCM solu-tion (1:1) into the beaker and stir the mixture vigorously todissolve the pyrolysis liquid in the solvent.9.6 Mount the filter on a dry holder and apply a vacuum.Mount and securely clamp the filter funnel to the filter holder.9.7 Use me
22、thanol to wash the filter paper to properly sealthe latter to the bottom of the funnel.9.8 Filter the solution through the vacuum filter system on 1m filter paper. Quickly but carefully poor the solution into thecenter of the funnel. Thoroughly wash the beaker with MeOH-DCM solution and return the c
23、ontents to the funnel. Wash thefiltrand with methanol until the filtrate runs clear.9.9 Remove the filter funnel from the filter holder andensure the edges of the filter funnel are clean of any pyrolysissolids. If required, rinse any pyrolysis solids on the filter funnelonto the filter paper with me
24、thanol, ensuring no pyrolysissolids are lost.9.10 Release the vacuum, and using the smooth-tip forcepstransfer the filter membrane and filtrand to its original weigh-ing dish, and dry in the oven at 105 6 3C for 30 min.9.11 Remove the weighing dish and filter membrane andcool to room temperature in
25、a dessicator for a minimum of 1 h.9.12 Weigh the filter membrane and weighing dish andrecord the stabilized weight to the nearest 0.1 mg.10. Calculation10.1 Calculate the pyrolysis solids content of the pyrolysisliquid sample in accordance with Eq 1.Pyrolysis solids wt %!5PS1!PL3 100% (1)where:Pyrol
26、ysis solids = Pyrolysis solids content, wt %,PS1= Pyrolysis solids retained on 1 m filterpaper (g), andPL = Pyrolysis liquid sample taken for analy-sis (g).11. Report11.1 Report the pyrolysis oil solids content to two signifi-cant figures.12. Precision and Bias512.1 This interim precision statement
27、represents replicateanalyses performed in two laboratories over ten successivedays by the same analyst on the same day on the sameinstrument.12.2 RepeatabilityThe difference between test results,obtained by the same operator using the same apparatus underconstant operating conditions on identical te
28、st material in ashort amount of time, would in the long run, in the normal andcorrect operation of this test method, exceed 0.1303X wt %only in one case in twenty.12.3 ReproducibilityAt this time, no interlaboratory pre-cision data have been obtained to allow a calculation forreproducibility.12.4 Bi
29、asNo information can be presented on the bias ofthis procedure for measuring pyrolysis solids content becauseno accepted reference value is available.13. Keywords13.1 char; filtration; pyrolysis liquids; pyrolysis solids4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical S
30、ociety, Washington, 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,
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34、tee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D7579 094
