ASTM_D_4793-09R2017.pdf

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations isued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.Designation:D4793-09(Reapproved 2017)INTERNATIONALStandard Test Method forSequential Batch Extraction of Waste with WaterThis standard is issued under the fixed designation D4793;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(8)indicates an editorial change since the last revision or reapproval.1.ScopeD420 Guide to Site Characterization for Engineering Design1.1 This test method is a procedure for the sequentialand Construction Purposes(Withdrawn 2011)leaching of a waste containing at least five percent solids toD653 Terminology Relating to Soil,Rock,and Containedgenerate solutions to be used to determine the constituentsFluidsleached under the specified testing conditions.D1129 Terminology Relating to WaterD1193 Specification for Reagent Water1.2 This test method calls for the shaking of a known weightD2216 Test Methods for Laboratory Determination of Waterof waste with water of a specified purity and the separation of(Moisture)Content of Soil and Rock by Massthe aqueous phase for analysis.The procedure is conducted tenD2234/D2234M Practice for Collection of a Gross Sampletimes in sequence on the same sample of waste and generatesof Coalten aqueous solutions.D2777 Practice for Determination of Precision and Bias of1.3 This test method is intended to describe the procedureApplicable Test Methods of Committee D19 on Waterfor performing sequential batch extractions only.It does notD3370 Practices for Sampling Water from Closed Conduitsdescribe all types of sampling and analytical requirements thatmay be associated with its application.3.Terminology1.4 The values stated in SI units are to be regarded as3.1 Definitions:standard.No other units of measurement are included in this3.1.1 For definitions of terms used in this test method,seestandard.Terminology D1129.3.2 Symbols:1.5 This standard does not purport to address all of the3.2.1 Variables listed in this test method are defined in thesafety concerns,if any,associated with its use.It is theindividual sections where they are discussed.A list of definedresponsibility of the user of this standard to establish appro-variables is also given in Section 11.priate safety,health and environmental practices and deter-3.2.2 Explanation of Variables:mine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-=total mean valueization established in the Decision on Principles for the=analytical mean value(calculated using data fromDevelopment of International Standards,Guides and Recom-analysis of standards)mendations issued by the World Trade Organization TechnicalS=total standard deviationBarriers to Trade(TBT)Committee.Sta=analytical standard deviationS=estimated standard deviation due to the extraction2.Referenced DocumentsprocedureS=total single operator standard deviation2.1 ASTM Standards:S=analytical single operator standard deviationD75/D75M Practice for Sampling AggregatesSoe=estimated single operator standard deviation due tothe extraction procedure This test method is under the jurisdiction of ASTM Committee D34 on Waste4.Significance and UseManagement and is the direct responsibility of Subcommittee D34.01.04 on Waste4.1 This test method is intended as a means for obtainingLeaching Techniques.Current edition approved Sept.1.2017.Published September 2017.Originallysequential extracts of a waste.The extracts may be used toapproved in 1988.Last previous edition approved in 2009 as D4793-09.DOI:estimate the release of certain constituents of the waste under10.1520/D4793-09R17.the laboratory conditions described in this test method.2 For 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 on3The last approved version of this historical standard is referenced onthe ASTM website.www.astm.org.Copyright ASTM Intemational,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesD4793-09(2017)2-L Plastic or Glass Bottles50-Watt Electric Motor0.5 HertzScrews for Holding Bottles4-L PlasticHinged CoverFoam Bonded to Coveror Glass BottleBox AssemblyPlywood ConstructionTotally EnclosedFan Cooled Motor0.5 Hertz,93 WattsFoam Inner Liner3PositionToggle SwitchFuse30cmFIG.1 Extractors7.2 Where no specific methods are available,sampling7.6 The time between collection and extraction of themethodology for material of similar physical form shall besample should be determined by the nature of the sample andused.the information desired.See Practices D3370 for guidance.7.3 The amount of sample to be sent to the laboratoryReport the length of time between sample collection andshould be sufficient to perform the solids content determinationextraction.as specified in 9.2 and to provide 100 g of sample on a dryweight basis for each extraction.8.Sample Preparation7.4 It is important that the sample of the waste be represen-8.1 For free-flowing particulate solid wastes,obtain atative with respect to surface area,as variations in surface areasample of the approximate size required in the test by quarter-would directly affect the leaching characteristics of the sample.ing the sample(Section 7)received for testing on an imper-Waste samples should contain a representative distribution ofmeable sheet of glazed paper,oil cloth,or other flexibleparticle sizes.material as follows:NoTE 4-Information on obtaining representative samples can also be8.1.1 Empty the sample container into the center of thefound in Pierre Gys Sampling Theory and Sampling Practice,Volumes Isheet.and II,by F.Picard.CRC Press.1989.8.1.2 Flatten out the sample gently with a suitable straight-7.5 In order to prevent sample contamination or constituentedge until it is spread uniformly to a depth at least twice theloss prior to extraction,keep samples in closed containersmaximum particle diameter.appropriate to the sample type and desired analysis.See8.1.3 Remix the sample by lifting a corner of the sheet andPractices D3370 for guidance.Record the storage conditionsdrawing it across,low down,to the opposite corner in a mannerand handling procedures in the report.that the material is made to roll over and over and does not3D4793-09(2017)merely slide along.Continue the operation with each corner,where:proceeding in a clockwise direction.Repeat this operation tenAmass of sample after drying,g.times.Boriginal mass of sample,g,and8.1.4 Lift all four corners of the sheet towards the centersolids content,g/g.and,holding all four corners together,raise the entire sheet intoAverage the two values obtained.Record the solids content.the air to form a pocket for the sample.8.1.5 Repeat8.1.2.9.3 Extraction Procedure-If the entire procedure cannot be8.1.6 With a straightedge(such as a thin-edged yard stick).conducted without interruption,at least the first four extractionsequences must be conducted without interruption.one at least as long as the flattened mound of sample,gentlydivide the sample into quarters.Make an effort to avoid using9.3.I Determine the mass of the extraction vessel to be usedpressure on the straightedge sufficient to cause damage to thein the extraction procedure to the nearest 0.I g.Record theparticles.mass of the extraction vessel,M.Use one extraction vessel8.1.7 Discard alternate quarters.per waste throughout the sequence of extractions.8.1.8 If further reduction of sample size is necessary,repeat9.3.2 Add 100 g(weighed to+0.I g)of solid waste on a dry8.1.3-8.1.7.Use a sample size to give 100 g of solid for eachweight basis to the extraction vessel.Calculate the amount ofwaste as received to add using the following equation:extraction.Provide additional samples for determination ofsolids content.If smaller samples are used in the test,report100M=S(2)this fact.NorE 5-For other acceptable methods for mixing and subsamplingwhere:free-flowing solid particulate wastes,see Pierre Gys Sampling TheoryM=mass of waste as received to add to the extractionand Sampling Practice,Volumes I and II,by F.Picard.CRC Press,1989.The method of subsampling should be determined by the physicalvessel to give 100 g(weighed to 0.1 g)of solidproperties of the waste,analytes of interest,and equipment available.waste.8.2 For field-cored solid wastes or castings produced in the9.3.2.1 If a mass of solid waste on a dry weight basis otherlaboratory,cut a representative section weighing approxi-than 100 g is used,Eq 2-4 must be modified to reflect the usemately 100 g for testing plus samples for determination forof a mass other than 100 g.Replace 100 in these equations withsolids content.Shape the sample so that the leaching solutionthe mass used.Use of a mass other than 100 g is notwill cover the material to be leached.recommended.8.3 For multiphasic wastes,mix thoroughly to ensure that a9.3.3 Add a volume in millilitres.V of test water(see 6.2)to the extraction vessel determined using the following equa-representative sample will be withdrawn.Take samples fortions:determination of solids content at the same time as the testsamplesM=M-100(3)where:9.ProcedureM=mass of moisture in the sample added to the extrac-9.1 Record the physical description of the sample to betion vessel,g.tested,including particle size so far as it is known.V.,=(20)(100)-Mm(4)9.2 Solids Content-Determine the solids content of two9.3.4 Agitate continuously for 18 0.25 h at 18 to 27C.separate portions of the sample as follows:Record the agitation time and temperature.9.2.1 Dry to a constant weight at 104+2C two dishes or9.3.5 Open the extraction vessel.Observe and record anypans of size suitable to the solid waste being tested.Cool in adesiccator and weigh.Record the values to t0.1 g.visible physical changes in the sample and leaching solution.Record the pH of the waste/leaching solution slurry.9.2.2 Put an appropriately sized portion of sample of thewaste to be tested into each pan.Scale the weight used to the9.4 Filtration-Transfer as much of the waste/leachingphysical form of the waste tested.Use a minimum of 50 g.butsolution as possible through a large glass funnel to a pressureuse larger samples where particles larger than 10 mm infiltration device equipped with a 0.45 or 0.8-um filter.Transferaverage diameter are being tested(see Test Methods D2216).the mixed slurry.Do not decant.Invert the extraction vessel9.2.3 Dry 16 to 20 h at 104+2 C.Record the temperatureover the filtration device and allow the liquid to drain from theand time of the drying period.solid remaining in the extraction vessel for I min.It is9.2.4 Cool to room temperature in a desiccator and reweigh.important to achieve as complete a transfer of fluid from theRecord the mass to 0.1 g.extraction vessel to the filtration device as possible.Pressurefilter the liquid through the filter using nitrogen gas.After the9.2.5 Repeat steps 9.2.3 and 9.2.4 until constant container-extract has passed through the filter,continue running nitrogensample masses are obtained.Discard the dried samples follow-gas through the filtration device at 30 psi for 3 min.The filtrateing completion of this step.obtained is the extract mentioned in this test method(see 9.59.2.6 Calculate the solids content of the sample from the10.8.and 10.9).Determine the volume of the filtrate collecteddata obtained in 9.2.2 and 9.2.4 as follows:and report it as Vfor that extraction step.Measure the pH of theS=A/B(1)extract immediately,remove the volume of filtrate necessaryD4793-09(2017)for determination of total dissolved solids content in 9.5,and10.2 Calculate the mass of the solid in grams lost throughthen preserve the extract in a manner consistent with thedissolution,M,using the following equation:chemical analyses or biological testing procedures to beM=(TDS)(V)(0.001)(6)performed(Practices D3370,Section 15).where:NoTE 6-It is recommended that all filtrations be performed in a hood.V=volume of filtrate collected in that extraction,L,andNoTE 7-Analytical results may be affected by the type of filter used.M=mass loss through dissolution.If a 0.8-um filter pore size is used,the resulting extract should be digestedprior to elemental analysis.If the filter is composed of material that may10.3 Calculate the mass of the solid corrected for TDScontaminate the extract during filtration,the filter should be washed in theremaining for the next extraction step,M.,using the followingfiltration device in a manner consistent with the chemical analyses orequation:biological testing procedures to be performed on the extract.For example,for elemental analysis of the extract,if a filter composed of borosilicateM,=M.-M(7)glass fiber is used,it should be washed in the filtration device with a dilutewhere:acid solution and rinsed with approximately 2 L of water prior to filtrationto prevent contamination.M.-=mass of the solid extracted in the current extractionstep,g.NoTE 8-Prefilters can be used only if it is absolutely necessary(if theNoTE 10-For example,in beginning the first extraction,M.-willfiltrate for analysis or testing cannot be obtained unless a prefilter is used)equal 100 g,and to calculate the mass of solid remaining for the seconddue to loss of sample trapped in the pores of the prefilter and theextraction step,M,will equal 100 g-Mpossibility of the prefilter disintegrating during rinsing.10.4 Calculate the combined mass of the solid and the9.5 Total Dissolved Solids Content(TDS)-Transfer aresidual liquid in the extraction vessel,M.,using the following10.0-mL sample of the extract to each of two pre-weighedequation:crucibles(weighed to 0.1 mg),previously dried at 110 2 C.Place the samples in a drying oven at 110 2C for 3 h.M=M-M-M(8)Record the drying oven temperature and drying time.Remove10.5 Calculate the mass of liquid adhering to the solids inthe crucibles and let cool in a desiccator.Reweigh the cruciblesthe extraction vessel,M,using the following equation:and record their weights to 0.1 mg.M1=M-M(9)NoTE 9-Only one drying is performed to limit the contact time10.6 Calculate the volume in millilitres of new test water tobetween the solid and the rinse water in the extraction vessel prior to thenext extraction step(see 9.6 and Section 10).be added to the extraction vessel.Test Water Volume,TWV.9.6 Quantitatively transfer the damp solid from the filterusing the following equation:back to the original extraction vessel,including the filter.UseTWV=(M,)(20)-M,-M.(10)water(see 6.2)from a pre-weighed wash bottle to assist in this10.7 Add to the extraction vessel the amount of new testtransfer and to rinse the filtration device.No more than 500 mLwater,TWV,determined in 10.6,and repeat 9.3.4-10.7 so thatof water should be used for rinsing.Use the smallest volume often extractions are done in sequence.wash water possible to achieve a thorough transfer.Usingtweezers or a similar device,recover the filter and rinse theNoTE 11-This procedure assumes that the amount of waste that isadhering solid into the extraction vessel with water from thetrapped in the filters after rinsing is negligible.pre-weighed wash bottle.Do not leave the filter in the10.8 Analyze the extracts for specific constituents or prop-extraction vessel.Reweigh the wash bottle to determine theerties or use the extracts for biological testing procedures asamount of water used in the transfer.Record this value as M.desired using appropriate ASTM test methods.Where noWeigh the extraction vessel following the transfer describedappropriate ASTM test methods exist,other methods may beabove and record this value as M.The extraction vessel mayused and recorded in the report.Where phase separation occursbe sealed until a feasible time for addition of new extractionduring the storage of the extracts,appropriate mixing should befluid.This is to enable filtration during the next sequence at aused to ensure the homogeneity of the extracts prior to their usereasonable time during the day.If the slurry is stored for longerin such analyses or testing.than 6 h in the extraction vessel prior to the addition of new10.9 Compensation for Carry-Over-For each constituentextraction fluid,the data generated by the analysis of thein each of the extracts generated in the extraction sequence,theextracts should be plotted to check for perturbation of the datacontribution to concentration from the residual liquid from thecurve.previous extraction step,C,can be calculated using thefollowing equation:10.CalculationC,=M120(M,一)C,(11)10.1 Calculate the total dissolved solids contents,TDS,inmilligrams per litre of the filtrate using the following equation:where:TDS=(M-M)(100)(5)C=concentration of the constituent in the filtrate fromthe previous extraction step,where:M=M from the previous extraction step,andM=mass of the crucible and dried solids,mg,andM.=mass of solid extracted in the current extraction stepM.=mass of the crucible,mg.(see Note 10).5