1、Designation: E1756 08 (Reapproved 2015)Standard Test Method forDetermination of Total Solids in Biomass1This standard is issued under the fixed designation E1756; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.INTRODUCTIONThe total solids content is used to adjust the mass of the biomass so that all analytical results maybe reported on a moisture
3、-free basis. Total solids content may be determined by overnight drying at105C in a convection oven or with a loss-on-drying moisture analyzer.1. Scope1.1 This test method covers the determination of the amountof total solids remaining after drying a sample. Materialssuitable for this procedure incl
4、ude samples prepared in accor-dance with Practice E1757 and extractive-free material pre-pared in accordance with Test Method E1690. For particulatewood fuels, Test Method E871 should be used.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included
5、in thisstandard.1.3 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
6、.2. Referenced Documents2.1 ASTM Standards:2E871 Test Method for Moisture Analysis of ParticulateWood FuelsE1690 Test Method for Determination of Ethanol Extrac-tives in BiomassE1757 Practice for Preparation of Biomass for Composi-tional Analysis3. Terminology3.1 Definitions of Terms Specific to Thi
7、s Standard:3.1.1 oven-dried solidsthe solids remaining after heatingthe prepared biomass at 105C to constant mass. For thepurposes of this procedure, the moisture content of a biomasssample is considered to be the amount of mass lost during thedrying of the sample at 105C to constant mass. An inhere
8、nterror of this and any oven-drying procedure is that volatilesubstances other than water are removed from the sampleduring drying.3.1.2 prepared biomassthe biomass that has been pro-cessed according to Practice E1757.4. Significance and Use4.1 Moisture is a ubiquitous and variable component of anyb
9、iomass sample. Moisture is not considered a structural com-ponent of biomass and can change with storage and handling ofbiomass samples. The determination of the total solids contentallows for the correction of biomass samples to an oven-driedsolids mass that is constant for a particular sample.4.2
10、This procedure is not suitable for biomass samples thatvisibly change on heating to 105C, for example, unwashedacid-pretreated biomass still containing free acid.4.3 Some materials that contain large amount of free sugarsor proteins will caramelize or brown under direct infraredheating elements used
11、 in Test Method B. Total solids in thesematerials should be done by Test Method A.5. Apparatus and Materials5.1 Analytical Balance, sensitive to 0.1 mg.5.2 Drying Oven, 105 6 3C (Test Method A only).5.3 Desiccator, containing anhydrous calcium sulfate (TestMethod A only).1This test method is under t
12、he 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 2008 as E1756
13、-08. DOI: 10.1520/E1756-08R15.2For 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, 1
14、00 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.4 Moisture Analyzer,3infrared heated, 20 g capacity, 1 mgresolution (Test Method B only).5.5 Drying Pans, disposable, aluminum, 10 cm diameter,suitable for moisture analyzer (Test Method B only).6. Sampling6.1 The s
15、ample is material prepared according to PracticeE1757 or extractives-free material prepared according to TestMethod E1690.7. Procedure: Test Method A7.1 This test method is suitable for either prepared biomasssamples or extractives-free material and employs drying thesample at 105 6 3C in a drying o
16、ven.7.2 Uniquely mark a suitable container, such as disposablealuminum weighing pan or 50 mL beaker, for each sample andplace in the drying oven at 105C for at least one hour. Cool thecontainers to room temperature in the desiccator.7.3 Weigh each container on the analytical balance to thenearest 0.
17、1 mg. Record this as the tare mass, mt.7.4 Weigh a nominal 0.5 g of sample into the marked, taredcontainer to the nearest 0.1 mg. Record the mass of the biomassplus container as the initial mass, mi 1.7.5 Place the sample in the drying oven at 105 6 3C for atleast 3 h but not longer than 72 h. Allow
18、 the samples to cool toroom temperature in a desiccator. Weigh each sample to thenearest 0.1 mg and record this mass. After weighing, return thesamples to the drying oven at 105C for 1 h, cool again in thedesiccator, and weigh again. Repeat this step until the mass ofthe samples varies by less than
19、0.3 mg from the previousweighing. Record this mass as the final mass, mf1.8. Calculation: Test Method A8.1 Calculate the mass percent of the total solids obtainedby drying at 105C as%T1055 mf12 mt!/mi12 mt! 3100% (1)where:%T105= mass percent of total solids based on 105C drymass,mt= tare mass of dri
20、ed container,mi 1= initial mass of container and biomass, andmf1= final mass of container and biomass after drying at105C.9. Procedure: Test Method B9.1 This test method is suitable for either prepared biomasssamples or extractives-free material and employs an automatedmoisture analyzer. This test m
21、ethod is not suitable for materialswith bulk densities of less than 0.1 g/cm3.9.2 Set the standby temperature to 60C and allow theinstrument to warm-up for 30 min. Set the drying temperatureto 105C. The drying program should be set to end when thesample mass changes less than 0.05 % in mass per minu
22、te.9.3 Tare a disposable aluminum drying pan on the analyz-ers balance according to the manufacturer instructions.9.4 Measure 2.0 6 0.2 g of sample onto the drying pan. Thesample must be spread in a thin, even layer that completelycovers the bottom of the pan. Record the initial mass of theprepared
23、biomass, mi2, when the balance stabilizes.9.5 Start the drying program according to the manufactur-ers instructions. Upon termination of the drying cycle, recordthe final moisture-free solids mass, mf2.10. Calculation: Test Method B10.1 Calculate the mass percent of the total solids obtainedby dryin
24、g at 105C as:%T1055 mf2/mi2! 3100% (2)where:%T105= mass percent total solids based on 105C dry mass,mi2= initial mass of sample, and3The sole source of supply of the Denver Instruments, Model IR-120 known tothe committee at this time is Denver Instrument Company, 1401 17th St. Suite 750,Denver, CO 8
25、0202. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.TABLE 1 Critical Difference, Percent of Grand Average, For theC
26、onditions NotedA,BTest ConditionsNumber ofObservationsinEach AverageSingle OperatorPrecisionTest Method A, hybrid poplar 1 0.552 0.39Test Method A, fermentation residue 1 1.352 0.95Test Method B, hybrid poplar 1 0.562 0.40Test Method B, switchgrass 1 0.892 0.63AThe critical differences were calculat
27、ed with z = 1.960.BTo convert the values of the critical differences to units of measure, multiply thecritical differences by the average of the two specific sets of data being comparedand divide by 100.TABLE 2 Width of 95 % Confidence Limits, Percent of GrandAverage, For the Conditions NotedA,BTest
28、 ConditionsNumber ofObservationsinEach AverageSingle OperatorPrecisionTest Method A, hybrid poplar 1 0.392 0.28Test Method A, fermentation residue 1 0.952 0.67Test Method B, hybrid poplar 1 0.402 0.28Test Method B, switchgrass 1 0.632 0.45AThe critical differences were calculated with z = 1.960.BTo
29、convert the values of the critical differences to units of measure, multiply thecritical differences by the average of the two specific sets of data being comparedand divide by 100.E1756 08 (2015)2mf2= final mass of sample.11. Precision and Bias11.1 SummaryIn comparing two single observations fromth
30、e analysis of hybrid poplar using Test Method A, thedifference should not exceed 0.55 % of the average of the twoobservations in 95 out of 100 cases when both observations aretaken by the same well-trained operator using this procedureand specimens randomly drawn from the same sample ofmaterial.4Whe
31、n analyzing washed, lyophilized fermentationresidues by Test Method A, the difference should not exceed1.35 %. In comparing two single observations from the analy-sis of hybrid poplar and switchgrass using Test Method B, thedifference should not exceed 0.56 and 0.89 %, respectively.The true total so
32、lids value can only be defined in terms of thisprocedure. Within this limitation, this test method has noknown bias.11.2 Critical DifferencesThe observed total solids valuesshould be considered significantly different at the 95 % prob-ability level if the difference equals or exceeds the criticaldif
33、ferences given in Table 1.11.3 Confidence LimitsSingle averages of observed valueshave the 95 % confidence limits given in Table 2.NOTE 1The values of the critical differences and confidence limitsshould be considered to be a general statement.11.4 BiasThe procedure in this test method has no biasbe
34、cause the value of the total solids is defined in terms of thetest method. Changes in the drying parameters may vary theobserved total solids content.12. Keywords12.1 agricultural residue; biomass; fermentation residue;herbaceous; moisture; total solids; wastepaper; woodASTM International takes no p
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38、ss 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), 6
39、10-832-9555 (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 Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ T. B., Ponfick, L., Nagle, N. J., Ehrman, C. I., Reynolds, J. B., andHimmel, M. E., “SSF Comparison of Selected Woods From Southern Sawmills,”Applied Biochemistry and Biotechnology , Vol 45/46, 1994, pp. 611-626.E1756 08 (2015)3
