1、Designation: D7579 09 (Reapproved 2013)Standard 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 th
2、e 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. Scope1.1 This test method describes a filtration procedure fordetermining the pyrolysis solids
3、content of pyrolysis 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
4、all of thesafety concerns, 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 ma
5、terials. Reviewthem for hazards prior to usage. For specific warningstatements, 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 Practi
6、ce for Automatic 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
7、 the vapors of biomass 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 thep
8、yrolysis of biomass.3.1.4.1 DiscussionPyrolysis liquid biofuel is comprised ofa complex mixture of the decomposition products of ligno-cellulosic biomass including highly oxygenated organic com-pounds. It is produced from the pyrolysis of biomass, followedby the rapid condensation of its vapors.3.1.
9、5 pyrolysis solids, 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 filt
10、er system. After filtering, 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
11、 con-centrations. Increasing 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 t
12、em-perature of 105 6 3C.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.06 on Analysis of Lubricants.Current edition approved Oct. 1, 2013. Published October 2013. Originallyappro
13、ved in 2009. Last previous edition approved in 2009 as D7579 09. DOI:10.1520/D7579-09R13.2For 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 to the standards Document Summ
14、ary 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.pdfCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
15、1FIG. 1 Paper Filtration ApparatusD7579 09 (2013)26.5 Filtering Flask, 1L.6.6 Filter Holders, borosilicate glass.6.7 Filter Membrane, binder free glass microfiber, 1 m.6.8 Weighing Dish, aluminum.6.9 Balance, capable of weighing to the nearest 0.0001 g(0.1 mg) with a range of 300 g.6.10 Vacuum.7. Re
16、agents and Solvents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it 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 availabl
17、e.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use 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 gr
18、ade. (WarningFlammable. Toxic.May be harmful or fatal if ingested or inhaled. Avoid skincontact.7.3 Methanol (MeOH), reagent grade. (WarningFlammable. Toxic. May be harmful or fatal if ingested orinhaled. Avoid skin contact.7.4 Dichloromethane (DCM), reagent grade. (WarningFlammable. Toxic. May be h
19、armful or fatal if ingested orinhaled. Avoid skin contact.)7.5 Filter Paper, 1 m pore size, binder free glass microfi-ber.8. 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 shou
20、ld be well mixedto ensure homogeneity.9. Procedure9.1 Dry a clean filter membrane for 15 min in a desiccator,place in a labeled 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.
21、4 Using a disposable pipette, weigh approximately 15 g ofpyrolysis liquid sample into the beaker. Record the weight tothe nearest 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 Mou
22、nt the filter on a dry holder and apply a vacuum.Mount and securely clamp the filter funnel to the filter holder.9.7 Use methanol 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 c
23、arefully poor the solution into thecenter of the funnel. Thoroughly wash the beaker with MeOH-DCM solution and return the contents 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
24、are clean of any pyrolysissolids. If required, rinse any pyrolysis solids on the filter funnelonto the filter paper with methanol, 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, a
25、nd 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 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 pyroly
26、sis solids content of the pyrolysisliquid sample in accordance with Eq 1.Pyrolysis solids wt %! 5PS1!PL3100% (1)where:Pyrolysis solids = Pyrolysis solids content, wt %,PS1= Pyrolysis solids retained on 1 m filterpaper (g), andPL = Pyrolysis liquid sample taken for analysis(g).11. Report11.1 Report t
27、he pyrolysis oil solids content to two signifi-cant figures.12. Precision and Bias512.1 This interim precision statement represents replicateanalyses performed in two laboratories over ten successivedays by the same analyst on the same day on the sameinstrument.12.2 RepeatabilityThe difference betwe
28、en test results,obtained by the same operator using the same apparatus underconstant operating conditions on identical test material in ashort amount of time, would in the long run, in the normal and4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, D
29、C. 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.5Supporting data h
30、ave been filed at ASTM International Headquarters and maybe obtained by requesting Research Report: RR:D02-1664.D7579 09 (2013)3correct 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
31、 to allow a calculation forreproducibility.12.4 BiasNo 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 solidsASTM International takes no po
32、sition respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibi
33、lity.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to A
34、STM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, 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 addres
35、s 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D7579 09 (2013)4
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