Designation: E1756 − 08 (Reapproved 2015)
Standard Test Method for
Determination of Total Solids in Biomass 1 This standard is issued under the fixed designation E1756; the number immediately following the designation indicates the year of original origin al adoption or, in the case of revis revision, ion, the year of last revision. revision. A number in paren parenthese thesess indicates the year of last reappr reapproval. oval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
INTRODUCTION
The total solids content is used to adjust the mass of the biomass so that all analytical results may be reported on a moisture-free basis. Total solids content may be determined by overnight drying at 105°C in a convection oven or with a loss-on-drying moisture analyzer.
1. Sco Scope pe
3. Terminology
1.1 This test method covers covers the determination determination of the amount of tot total al sol solids ids rem remaini aining ng aft after er dry drying ing a sam sample ple.. Mat Materia erials ls suitable for this procedure include samples prepared in accordance with Practi Practice ce E1757 and extrac extractive-f tive-free ree material pre in accordance with Test Method E1690 E1690.. For particulate pared in pared wood fuels, Test Method E871 E871 should should be used.
3.1 Definitions of Terms Specific to This Standard: 3.1.1 oven-dried solids— the the solids remaining after heating thee pr th prep epar ared ed bi biom omas asss at 10 105° 5°C C to co cons nstan tantt mas mass. s. Fo Forr th thee purposes of this procedure, the moisture content of a biomass sample is considered to be the amount of mass lost during the drying of the sample at 105°C to constant mass. An inherent error of this and any oven-drying procedure is that volatile substan sub stances ces oth other er tha than n wat water er are rem remove oved d fro from m the samp sample le during drying.
1.2 1. 2 Th Thee va valu lues es sta state ted d in SI un units its are to be re rega gard rded ed as standard. No other units of measurement are included in this standard.
prepared biomass— the 3.1.2 prepared t he bi biom omas asss th that at ha hass be been en pr proocessed according to Practice E1757 E1757..
standard d doe doess not purport purport to add addre ress ss all of the 1.3 This standar safet sa fetyy co conc ncer erns ns,, if an anyy, as asso socia ciated ted wi with th it itss us use. e. It is th thee responsibility of the user of this standard to establish appro priate safety and health practices and determine the applicability of regulatory limitations prior to use.
4. Signi Significanc ficancee and Use 4.1 Moistu Moisture re is a ubiqu ubiquitous itous and variable variable component component of any biomass sample. Moisture is not considered a structural component of biomass and can change with storage and handling of biomasss samples biomas samples.. The determ determination ination of the total solids content allows for the correction of biomass samples to an oven-dried solids mass that is constant for a particular sample.
2. Referenc Referenced ed Documents Documents 2.1 ASTM Standards:2 E871 Test Met Method hod for Moi Moistu sture re Ana Analys lysis is of Par Particu ticulate late Wood Fuels E1690 Test Metho Method d for Determ Determination ination of Ethan Ethanol ol Extractives in Biomass E1757 Pra Practic cticee for Pre Prepar paratio ation n of Bio Biomas masss for Com Compos posiitional Analysis
4.2 This procedure procedure is not suitable for biomass samples samples that visibly change on heating to 105°C, for example, unwashed acid-pretreated biomass still containing free acid. 4.3 Some materials materials that contain large amount amount of free sugars or pro protein teinss wil willl car carame amelize lize or bro brown wn und under er dir direct ect inf infrar rared ed heating elements used in Test Method B. Total solids in these materials should be done by Test Method A.
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Thiss tes Thi testt met method hod is und under er the jur jurisd isdict iction ion of AS ASTM TM Com Committ mittee ee E48 on Bioenergy and Industrial Chemicals from Biomass and is the direct responsibility of Subcommittee E48.05 Subcommittee E48.05 on Biomass Conversion. Current edition approved June 1, 2015. Published July 2015. Originally approved in 1995. Last previous edition approved in 2008 as E1756-08. DOI: 10.1520/E175608R15. 2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at
[email protected]. For Annual Book of ASTM Standards volume information, refer to the standard’s Document Summary page on the ASTM website.
5. Appar Apparatus atus and Materials Materials 5.1 Analytical Balance, sensitive to 0.1 mg. 5.2 Drying Oven, 105
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3°C (Test Method A only).
5.3 Desiccator, containing anhydrous calcium sulfate (Test Method Metho d A only) only)..
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E1756 − 08 (2015) TABLE 1 Critical Difference, Percent of Grand Average, For the Conditions Noted A,B Test Conditions
Test Method A, hybrid poplar Test Method A, fermentation residue Test Method B, hybrid poplar Test Method B, switchgrass
TABLE 2 Width of 95 % Confidence Limits, Percent of Grand Average, For the Conditions Noted A,B
Number of Observations Single Operator in Precision Each Average 1 2 1 2 1 2 1 2
Test Conditions
0 .5 5 0. 39 1 .3 5 0. 95 0 .5 6 0. 40 0 .8 9 0. 63
Test Method A, hybrid poplar Test Method A, fermentation residue Test Method B, hybrid poplar Test Method B, switchgrass
A
A
B
B
The critical differences were calculated with z with z = = 1.960. To convert the values of the critical differences to units of measure, multiply the critical differences by the average of the two specific sets of data being compared and divide by 100.
Number of Observations Single Operator in Precision Each Average 1 2 1 2 1 2 1 2
0 .3 9 0 .2 8 0 .9 5 0 .6 7 0 .4 0 0 .2 8 0 .6 3 0 .4 5
The critical differences were calculated with z with z = = 1.960. To convert the values of the critical differences to units of measure, multiply the critical differences by the average of the two specific sets of data being compared and divide by 100.
8. Calculation: Test Test Method A 5.4 Moisture Analyzer,3infrared heated, 20 g capacity, 1 mg resolution (Test Method B only).
8.1 Calculat Calculatee the mass percen percentt of the total solids obtained obtained by drying at 105°C as
5.5 Drying Pans, disposable, disposable, aluminum, 10 cm diamete diameter, r, suitable for moisture analyzer (Test Method B only).
% T 105 5 ~ m f 1 2 m t ! / ~ m i 1 2 m t ! 3 100 %
(1)
where: mass percent percent of total solids solids based based on 105°C dry dry %T 105 = mass mass, mt = tare mass of dried contain container, er, mi 1 = initial mass of contain container er and biomas biomass, s, and m f 1 = final mass of contain container er and biomas biomasss after dryin drying g at 105°C.
6. Samp Sampling ling 6.1 The sample is material prepared according according to Practice E1757 or E1757 or extractives-free material prepared according to Test Method E1690 Method E1690.. 7. Procedu Procedure: re: Test Test Method A
9. Procedur Procedure: e: Test Test Method B
7.1 This test method is suitable for either prepared prepared biomass biomass samples or extractives-free material and employs drying the sample at 105 6 3°C in a drying oven.
9.1 This test method is suitable for either prepared prepared biomass samples or extractives-free material and employs an automated moisture analyzer. This test method is not suitable for materials with bulk densities of less than 0.1 g/cm 3.
7.2 Uniqu Uniquely ely mark a suitab suitable le container, container, such as disposable aluminum aluminu m weighing pan or 50 mL beaker, for each sample and place in the drying oven at 105°C for at least one hour. Cool the containers to room temperature in the desiccator.
9.2 9. 2 Se Sett th thee sta stand ndby by tem tempe pera ratu ture re to 60 60°C °C an and d all allow ow th thee instrument to warm-up for 30 min. Set the drying temperature to 105°C. The drying program should be set to end when the sample mass changes less than 0.05 % in mass per minute.
7.3 Weig eigh h eac each h con contain tainer er on the ana analyti lytical cal bal balanc ancee to the nearest 0.1 mg. Record this as the tare mass, m t .
9.3 Tare a dispo disposable sable aluminum aluminum drying pan on the analyz analyz-er’s balance according to the manufacturer instructions.
7.4 Weigh a nominal 0.5 g of sample into the marked, tared container to the nearest 0.1 mg. Record the mass of the biomass plus container as the initial mass, m i 1.
9.4 Measur Measuree 2.0 2.0 6 0.2 g of sample onto the drying pan. The sample must be spread in a thin, even layer that completely covers the bottom of the pan. Record the initial mass of the prepared biomass, mi2, when the balance stabilizes.
7.5 Place the sample sample in the drying oven oven at 105 6 3°C for at least 3 h but not longer than 72 h. Allow the samples to cool to room temperature in a desiccator. Weigh each sample to the nearestt 0.1 mg and record this mass. After weighing, neares weighing, return the samples to the drying oven at 105°C for 1 h, cool again in the desiccator, and weigh again. Repeat this step until the mass of thee sa th samp mples les va vari ries es by le less ss th than an 0. 0.3 3 mg fr from om th thee pr prev evio ious us weighing. Record this mass as the final mass, m f 1.
9.5 Start the dryin drying g program according according to the manufacturmanufacturer’s instructions. instructions. Upon termina termination tion of the drying cycle, recor record d the final moisture-free solids mass, m f2. 10. Calculation: Test Test Method B 10.1 Calcula Calculate te the mass percen percentt of the total solids obtained obtained by drying at 105°C as: % T 105 5 ~ m f 2 / m i 2 ! 3 100 %
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The sole source of suppl supply y of the Denver Instruments, Instruments, Model IR-120 known to the committee at this time is Denver Instrument Company, 1401 17th St. Suite 750, Denver, CO 80202. If you are aware of alternative suppliers, please provide this information informa tion to ASTM Intern Internationa ationall Headq Headquarter uarters. s. Your comme comments nts will receiv receivee carefull consi carefu considerati deration on at a meeti meeting ng of the responsible responsible techni technical cal committee,1 which you may attend.
(2)
where: percent total solids solids based based on on 105°C 105°C dry dry mass, %T 105 = mass percent = initial initial mas masss of samp sample, le, and mi2 2
E1756 − 08 (2015) m f 2
The true total solids value can only be defined in terms of this proced pro cedure ure.. Wi Within thin thi thiss limi limitati tation, on, thi thiss test meth method od has no known know n bias.
= fina finall mas masss of sam sample ple..
11.. Pre 11 Precisi cision on and Bias
11.2 Critical Differences— The The observed total solids values should be considered significantly different at the 95 % probability abi lity level if the dif differ ferenc encee equ equals als or exc exceed eedss the cri critica ticall differences given in Table 1. 1.
11.1 Summary— In In comparing two single observations from thee an th analy alysis sis of hy hybr brid id po popl plar ar us usin ing g Tes estt Me Meth thod od A, th thee difference should not exceed 0.55 % of the average of the two observations in 95 out of 100 cases when both observations are taken by the same well-trained operator using this procedure and an d sp speci ecimen menss ra rand ndom omly ly dr draw awn n fr from om th thee sa same me sa samp mple le of material.4 When analyz analyzing ing washe washed, d, lyoph lyophilized ilized fermen fermentation tation residues by Test Method A, the difference should not exceed 1.35 %. In comparing two single observations from the analysis of hybrid poplar and switchgrass using Test Method B, the differen dif ference ce shoul should d not exceed 0.56 and 0.89 %, respec respectively tively..
11.3 Confidence Limits— Single Single averages of observed values have the 95 % confidence limits given in Table 2. 2. NOTE 1—The values of the critical differences and confidence limits should be considered to be a general statement.
11.4 Bias— The The procedure in this test method has no bias because the value of the total solids is defined in terms of the test method. Changes in the drying parameters may vary the observed total solids content. 12. Keyw Keywords ords
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Vinzant, T. B., Ponfick, L., Nagle, N. J., Ehrman, C. I., Reynolds, J. B., and Himmel, M. E., “SSF Comparison of Selected Woods From Southern Sawmills,” Applied Biochemistry and Biotechnology , Vol 45/46, 1994, pp. 611-626.
12.1 agricultural agricultural residu residue; e; bioma biomass; ss; fermen fermentation tation residu residue; e; herbaceous; moisture; total solids; wastepaper; wood
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