1、Designation: E 1756 01Standard Test Method forDetermination of Total Solids in Biomass1This standard is issued under the fixed designation E 1756; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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-free basis. To
3、tal 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 include samples pre
4、pared in accor-dance with Practice E 1757 and extractive-free material pre-pared in accordance with Test Method E 1690. For particulatewood fuels, Test Method E 871 should be used.1.2 The values stated in SI units are to be regarded as thestandard.1.3 This standard does not purport to address all of
5、 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.2. Referenced Documents2.1 ASTM Standards:2E 871 Method for Moistur
6、e Analysis of Particulate WoodFuelsE 1690 Test Method for Determination of Ethanol Extrac-tives in BiomassE 1757 Practice for Preparation of Biomass for Composi-tional Analysis3. Terminology3.1 Descriptions of Terms Specific to This Standard:3.1.1 oven-dried solidsthe solids remaining after heatingt
7、he 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 inherenterror of this and any oven-drying procedure is that volatilesubstan
8、ces other than water are removed from the sampleduring drying.3.1.2 prepared biomassthe biomass that has been pro-cessed according to Practice E 1757.4. Significance and Use4.1 Moisture is a ubiquitous and variable component of anybiomass sample. Moisture is not considered a structural com-ponent of
9、 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 This procedure is not suitable for biomass samples thatvisibly chang
10、e 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 in Test Method B. Total solids in thesematerials should be done by
11、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).5.4 Moisture Analyzer,3infrared heated, 20 g capacity, 1 mgresolution (Test Method B only).5.5 D
12、rying Pans, disposable, aluminum, 10 cm diameter,suitable for moisture analyzer (Test Method B only).1This test method is under the jurisdiction of ASTM Committee E48 onBiotechnology and is the direct responsibility of Subcommittee E48.05 on BiomassConversion.Current edition approved November 10, 20
13、01. Published February 2002.Originally published as E1756-95. Last previous edition E1756-95.2For 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
14、Summary page onthe ASTM website.3A Denver Instruments, Model IR-100, available from Denver InstrumentCompany, 6542 Fig St.,Arvada, CO 80004, has been found to be satisfactory for thispurpose.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United S
15、tates.6. Sampling6.1 The sample is material prepared according to PracticeE 1757 or extractives-free material prepared according to TestMethod E 1690.7. Procedure: Test Method A7.1 This test method is suitable for either prepared biomasssamples or extractives-free material and employs drying thesamp
16、le at 105 6 3C in a drying oven.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 analyti
17、cal balance to thenearest 0.1 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, mi1.7.5 Place the sample in the drying oven at 105 6 3C for atleast 3 h but
18、not longer than 72 h. Allow 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 s
19、amples varies by less than 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! 3 100 % (1)where:%T105= mass percent of total solids based on 105C
20、 drymass,mt= tare mass of dried container,mi1= initial mass of container and biomass, andmf1= final mass of container and biomass after dryingat 105C.9. Procedure: Test Method B9.1 This test method is suitable for either prepared biomasssamples or extractives-free material and employs an automatedmo
21、isture analyzer. This test method 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
22、than 0.05 % in mass per minute.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
23、initial mass of theprepared 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 t
24、otal solids obtainedby drying at 105C as:%T1055 mf2/mi2! 3 100 %(2)where:%T105= mass percent total solids based on 105C drymass,mi2= initial mass of sample, andmf2= final mass of sample.11. Precision and Bias11.1 SummaryIn comparing two single observations fromthe analysis of hybrid poplar using Tes
25、t 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.4When analyzing washed, lyophilized ferme
26、ntationresidues 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, the4Vinzant, T. B., Ponfick, L., Nagle, N. J., Ehrman, C. I., Reynolds, J. B., andHimmel, M. E., “SSF Comparison of
27、Selected Woods From Southern Sawmills,”Applied Biochemistry and Biotechnology, Vol 45/46, 1994, pp. 611-626.TABLE 1 Critical Difference, Percent of Grand Average, For theConditions NotedA,BTest ConditionsNumber ofObservationsinEach AverageSingle OperatorPrecisionTest Method A, hybrid poplar 1 0.552
28、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 calculated with z = 1.960.BTo convert the values of the critical differences to units of measure, multiply thecritical differences by the
29、 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 ConditionsNumber ofObservationsinEach AverageSingle OperatorPrecisionTest Method A, hybrid poplar 1 0.392 0.28Test Method A, fer
30、mentation 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 convert the values of the critical differences to units of measure, multiply thecritical differences by the average of the two sp
31、ecific sets of data being comparedand divide by 100.E1756012difference should not exceed 0.56 and 0.89 %, respectively.The true total solids value can only be defined in terms of thisprocedure. Within this limitation, this test method has noknown bias.11.2 Critical DifferencesThe observed total soli
32、ds valuesshould be considered significantly different at the 95 % prob-ability level if the difference equals or exceeds the criticaldifferences given in Table 1.11.3 Confidence LimitsSingle averages of observed val-ues have the 95 % confidence limits given in Table 2.NOTE 1The values of the critica
33、l differences and confidence limitsshould be considered to be a general statement.11.4 BiasThe procedure in this test method has no biasbecause 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. Keywords
34、12.1 agricultural residue; biomass; fermentation residue;herbaceous; moisture; total solids; wastepaper; woodASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised
35、that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.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 reap
36、proved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you
37、 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).E1756013
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