ASTM_E_1758_-_01_2015.pdf

Designation:E175801(Reapproved 2015)Standard Test Method forDetermination of Carbohydrates in Biomass by HighPerformance Liquid Chromatography1This standard is issued under the fixed designation E1758;the number immediately following the designation 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.INTRODUCTIONThe carbohydrates making up a major portion of biomass samples are polysaccharides constructedprimarily of glucose,xylose,arabinose,galactose,and mannose subunits.The polysaccharides presentin a biomass sample can be hydrolyzed to their component sugar monomers by sulfuric acid in atwo-stage hydrolysis process.These monosaccharides can then be quantified by ion-moderatedpartition HPLC.1.Scope1.1 This test method covers the determination of carbohy-drates present in a biomass sample,expressed as the percent,by mass,of each sugar on a 105C dried mass basis.NOTE1The percent sugar must be corrected for the water ofhydrolysis before calculating the actual mass percent of the polysaccha-ride in the original biomass sample.1.2 Sample materials suitable for this procedure includehard and soft woods,herbaceous materials(such as switchgrassand sericea),agricultural residues(such as corn stover,wheatstraw,and bagasse),wastepaper(such as office waste,boxboard,and newsprint),acid or alkaline-pretreated biomass(washed free of any residual acid or alkali),and the solidfraction of fermentation residues.All results are reportedrelative to the 105C oven-dried mass of the sample.1.3 The options for the types of samples to be analyzed inthis test method are as follows:1.3.1 Prepared Biomass Samples:1.3.1.1 Air Dried(%Tad)The percent,by mass,of totalsolids of the air-dried sample.1.3.1.2 45C Dried(%T45)The percent,by mass,of totalsolids of the 45C dried sample.1.3.1.3 Freeze Dried(%Tfd)The percent,by mass,of totalsolids of the freeze dried sample.1.3.2 Extractives-Free Sample(%Text)The percent,bymass,of total solids of the extracted sample determined at105C.1.4 The values stated in SI units are to be regarded as thestandard.1.5 This standard does not purport to address 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.Specific precau-tionary statements are given in Note 3 and Note 4.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE1690 Test Method for Determination of Ethanol Extrac-tives in BiomassE1721 Test Method for Determination of Acid-InsolubleResidue in BiomassE1756 Test Method for Determination of Total Solids inBiomassE1757 Practice for Preparation of Biomass for Composi-tional Analysis3.Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 as received biomassthe biomass material as it isreceived in its field or process collected state.3.1.2 oven-dried massthe moisture-free mass of a biomasssample dried at 105C as described in Test Method E1756.1This test method is under the jurisdiction of ASTM Committee E48 onBioenergy and Industrial Chemicals from Biomass and is the direct responsibility ofSubcommittee E48.05 on Biomass Conversion.Current edition approved June 1,2015.Published July 2015.Originally approvedin 1995.Last previous edition approved in 2007 as E175801(2007).DOI:10.1520/E1758-01R15.2For 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 Summary page onthe ASTM website.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 3.1.3 prepared biomassmaterial that has been treatedaccording to Practice E1757 in order to raise the total solidscontent above 85%,by mass,based on an oven-dried solidsmass.3.2 AbbreviationsAbbreviations of standards used in theprocedure,and definitions of terms used in the calculations areas follows:3.2.1 C1known concentration of sugar recovery standardbefore hydrolysis,in mg/mL.3.2.2 C2concentration of sugar recovery standard detectedby HPLC after hydrolysis,in mg/mL.3.2.3 Ccorr concentration of sugar in hydrolyzed samplecorrected for hydrolysis,in mg/mL.3.2.4 Cspl concentration of sugar in hydrolyzed sampledetected by HPLC,in mg/mL.3.2.5 CVS(calibration verification standard)standardsused in determining the quality of the calibration curve as wellas the quality of the standard reagents used in preparing thecalibration standards.3.2.6 m1initial mass of sample,in mg.3.2.7%extractivesthe percentage,by mass,of extractivesin the prepared biomass sample as described in Test MethodE1690.3.2.8%Rsrs percent recovery of sugar recovery standard,as determined in 13.2.3.2.9%su