POTW Sludge Sampling And Analysis Guidance Document

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United StatesEnvironmental ProtectionAgencyEPAOffice Of Water(4203)EPA 833-B-89-100August 1989POW Sludge Sampling AndAnalysis Guidance Document

TABLE OF CONTENTSPageviACKNOWLEDGEMENTS.1.INTRODUCTION .1-12.SLUDGE SAMPLING .2-12.1BACKGROUND INFORMATION.2-12.1.12.1.22-12-2SolidsContent and Viscosity.ProcessedSludge ions.Sample Point Representationofthe EntireSludge Stream .Availabilityof Flow Data and/orSolidsData .SamplePoints.2.3.2SamplingEquipment .Proper SamplingPracticesSAMPLE SIZE,2.5SAMPLE PREPARATION AND PRESERVATION Material.ContainerPreparation.Preservation.Time Priorto Analysis.PACKAGING AND SHIPPING.2.6.12.6.22-72-82-112-12SAMPLE TYPE, AND SAMPLING FREQUENCY. . 2-142.42.5.12-42-8SAMPLE COLLECTION .2.3.12.62-22-32-32-32-3SAMPLE POINT SELECTION .2.2.1.12.3AnaerobicallyDigestedSludge .AerobicallyDigestedSludge .Dewatered Sludges .Compost Product .Dried Powder .Packaging -22.2-222-22

TABLEOF Log Book 13.2PROCEDURES.CONVENTIONAL AND INORGANICMETALS tionAnalyticalDetectionMethods.3-23-63-63-83-83-9. . . . . . . . . . . . . . . 3-18Overviewof ATHOGENIC4.5.15.25.35.45.5POLLUTANTORGANICS . . . . . . . . . . 5C .625-S .MICROORGANISMS.3-26ASSURANCE.AND ities4-1COSTS.5-1REQUIREMENTS .ANALYTICALCOSTS .ANALYTICALCOSTS .EQUIPMENT COSTS .for Cost Savings tileSolidsA-1Reduction.B-1

LISTOF TABLESPageTable2-92.1SludgeFlow gContainers,Sample Volume din the HazardousMaterialsTable (49 CFR 172.101)Used by EPA forPreservationof Water, Effluent,Biological,Sedimentand Sludge Samples sisof3.3Comparison-Summary3.4Recommended InductivelyEstimatedInstrumental3.5Atomic AbsorptionDetectionLimitsPaintsDevices .2-9.Times,and Minimum2-15InterferencesAssociatedwithand Storage .Techniquesfor Conventionalin Sludge .Samplingand InorganicPreparationTechniquefor ElementalSludge Samples .ofICAP and AAS .CoupledDetection2-233-103-12WavelengthsandLimits .3-14Flame and Furnace Instrumentalfor WastewaterSamples .3-16AnalyticalTechniquesfor Determinationof PathogenicMicroorganismsin Sewage Sludge ntractSludgeNeeds .AnalyticalParametersCosts for Commonly.V5-5

nforcementalsoApplicationsManagermadeoftheTom Wall,No.peerwereunderOfficeEPA aluablepeerreviewed.reviewandEPA wishescommentsprovidedtobytheentities: EPA Region3 EPA Region5 EPA Region9 EPA Region10 EPA Environmental AMSA California Connecticut Eli Eugene LA County Missouri Nampa, Ohio Unified gineersofWashingtonAmericanSocietyCountyofQuality

orcompositionmay mittingsewageEPA hasPOTWs sampledetermine257on toAct1991.ThisthestandardsthetheEPA mustmeasuresa nsureamendmentstheEPA developdisposal,technicalotherthethatwhenNPDES tdisposalWaterofannuallysludgetomay ,isneededto40 CFR Part

In view of the variabilityof municipalsludge quality,appropriateproceduresmust be followedto collectand analyzesamples that accuratelyrepresenteach POTW's sludge quality.This manual was developedto providethat guidanceto POTWoperators,engineers,managers,chemistsand permitwriters.Itwas intendedto provideguidancein developingand implementingato gatherinformationon sludgesamplingand analysisprogram,Thisqualityand determinecompliancewith permitconditions.state-of-the-artfieldand laboratorymanual is based on current,practicesand thereforeis recommended for all sludge samplingand analysisprograms.1-2

2.BACKGROUND INFORMATION2.1DependingnecessaryInSLUDGE SAMPLINGtoorderforon thetousesamplesamplesamplingpractice,sludgetypesa elcharacteristicsorthebe awaresludgeofitmay bethroughoutthestream(s)a lidsinsolidsanda givencharacteristicsseparateintoisan appliedforce.proportionaltoofto20 percentthatsolidsrequirewithrelythebeon pumpscontentmanualofgrabSludgeswhichtosolida muchcontenta lwhichofa fluidisflowundersomewhataffectsthesampleThis propertya liquid,sinceliquidviscosity.general,content,may be useful20 percent.Othersampling.2-1by ctionInmay be conveyedby mechanicalthana ositysolidsconveyedsolidssample.content.a greaterandwithby utomaticallyup thedetermineTheisSludgemostarea terialanda erssludgesHowever,problemsasbycakessludgea

ispoint.Increasedcausea ionprecisionmay ewateredas ntthesludgedriedisentrainedhasa non-offensive2-2practices.areSome ofdescribedthebelow.ofslurryofgases.When welldigested,odor.The additionpriorto- mechanicaldigestedDepending8 percent.on rawa liquid,powder.typesludgeofsolidsofa thickandresiduetreatmentformsludgedependsSludgea ysludgethemay omparametersincreaseAnalyticalinwaterAlso,themay requireincreaselimits.precludeon thedigestedsludgemodesludgescontainsof30 todigesterrangesfrom 4of50

dsludgeis a dark-brown,flocculent,aerationof sludge.relativelyinertwaste producedby long-termThe suspensionis bulky and generallydifficultto thicken.TheTheodor of aerobicallydigestedsludge is not offensive.percentsolidsof aerobicallydigestedsludgeis less than thatof the influentsludge(if not decanted),because approximately50 percentof the volatilesolidsare convertedto gaseous SludgesDewateringconvertssludgefrom a flowingmixtureof liquidsand solidsto a cake-likesubstancemore readilyhandledas aThe characteristicsof dewateredsludge depend on thesolid.chemicalconditioning,and treatmentprocessestype of sludge,The percentsolidscontentof dewateredcake rangesemployed.Cake with a lower percentsolidsisfrom 15 to 40 percent.cake with a higherpercentsolidssimilarto a wet manure, whileis a chunky solid.2.1.2.4CompostProductCompostingis a processin which ionto a stableend product.composted sludgeis a sanitary,nuisance-free,humus-likeApproximately20 tomaterialcontaining75 to 80 percentsolids.to carbon dioxide30 percentof the volatilesolidsare convertedand water.2.1.2.5DriedPowderDried powder is the residuefrom heat dryingprocesses.Sludge dryingreduces water contentby vaporizationof waterweightreduction,and to preventsludge grinding,permit2-3to

continuedsludgeisbiologicalless thanaction.The moisture10 percent.contentofdriedIncineratorash is a productof the incinerationof sewageAsh is thereforenot covered under the samplingorsludge.analysisof sewage sludge.It is covered under RCRA SubtitleCif it is a hazardouswaste and if not it fallsunder SubtitleD.2.2SAMPLE POINT SJZLECTION2.2.1GeneralConsiderationsNPDES, pretreatmentand sludge program officialsneed sludgequalitydata in order to determinewhether sludge use or disposalmay pose a threatto publichealthor the environment.Thus, assludge samples should be drawn from ana generalrule,appropriatesamplingpointand in such a manner that the samplerepresents,as well as possible,the qualityof the sludge as itwillbe disposedof or used.When selectinga specificsamplethe followingtwo factorsshould be carefullyconsidered:point,0Does thestream?0AreThe tstreamrepresentflowtheentireor mass fluxsludgedataavailable?paragraphsexamine both factorsand presenton means to address each factor.SamplePointRepresentationof theEntireSludgeStreamOften it is not possibleto obtaina whollyrepresentativesample of a given wastestreamat any one time.Effortmust bemade, however,to ensure that a sample is obtainedthatis asrepresentativeas possible.Three cLncernsthat need to be2-4

selectedwillprovideaddressedto ensure that the sample pointsrepresentativesamples of the entiresludge stream are:obtainingsamples that are representativeof the cross-sectionofobtainingwell mixed samples;and obtainingthe entireflow;samples of multiplesludge streams.A particularconcernin any samplingprogram is to obtainsamples which representthe entireflow past the sample pointEach discretesample shouldthroughoutthe sample period.representthe cross-sectionof the entireflow at the samplingEach compositesample of multiplecontributorystreamspoint.should representthe cross-sectionof the entireflow of thecombined stream.Samples should be obtainedfrom pointswhere the sludge isWhile some pollutantparametersare predominantlywell-mixed.associatedwith the solidsfraction(particularlyprecipitatedothersare more associatedvith the liquid-fractionmetals),Failureto acquirea sample with(many ionscan significantlyaffectThis is particularlythe analyticalresultsof a given sample.solidsand largefleetrue of sludgestreams wit:? high percentSince turbulenceensures mixed samples,theseparticles.recommendationsshould be followed:00In sludge processingtrains,samples from taps ,on thedischargeside of sludge pumps are well mixed sinceflow at thispointin the system is turbulentwith nosolidsseparationwithinthe flow stream.If a sample is drawn from a tap on a pipe containingsludge which is distantfrom the sludge pumps, theaverageflow velocitythroughthe pipe should beAveragegreaterthan 2 feet per second (fpsl.velocitiesof less than 2 fps resultin solidsand affectsamr;le solidsseparationand settling,dependingon the locationof the tap (top,content,2-5

side or bottom of the pipe).Given a choice,a tap onthe side of the pipe is preferable.In addition,thetap should be a large size to encouragedraw from theentirecross-sectionof flow when fullyopen.At times it may be necessaryto sample a poorlymixed openchannelflow.If thiscannot be avoided,then each sample mustbe a compositeconsistingof grabs taken at severallevels(l/4,l/2 and 3/4 depth,for example)in order to minimizesample biascaused by solidsstratification.For samplingsolidsludges(i.e.dewateredcake, compost,etc.),stratificationcan beavoided by not only samplingat variousdepths,but at numerouslocationsover the entiresludge pile.Althoughit is preferableto sample sludgejust priorto itsexitfrom the treatmentplantin a combined stream,sometimesthatis not possible.Therefore,a considerationin many sludgesamplingsituationsis the need to produce a compositesamplefrom confluentstreams.PLn example is the samplingof sludgeflows from severalparallelsources which latercombinedownstreamin an unsafe or inaccessiblelocation.Severaloptionsexistto accommodate multiplestreams.The mostappropriatechoice depends on the sludge flow and solidsfluxinformationavailable,the parametersbeing sampied and thepurpose of the generateddata.Severaloptionsare as follows:00The simplestoFtionis to withdrawequal volumes ofsample from each of the multiplesludge streamstccreatea compositesample.This approachis justifiedin the case of identicalunitsreceivingequal flowgeneratingequal sludge amounts.andA second optionis to weightthe grab samples in eachcompositeaccordingto the wastewaterflow to each unit(or in the case of filtercake, the thickenedsludgeflow to each unit;.This approachrecognizesthat fordifferentsized units;rith differentdesignflows,thevolume of sludge produced*dill theoreticallybe2-6

proportionalto the influentflow to the unit.However,factorssuch as unequalloadingrates,differencesin sludge collectionmechanisms,etc. canaffectsolidsremoval rates and sludge generationratesThis optionparalleltreatmentunits.by unequal,particularlyappliesto situationswhere no sludgeflowor solidsdata existsfor unequa: parallelflowstreams.02.2.1.2The thirdoptionis to weightgrabs from individualstreams based on sludge flow data or solidsflux data.Nhether to use sludge flow or solidsflux willdependon the sample streams,the parametersof interest,andFor example,ifthe planneduse of the resultingdata.filtercake is being monitoredfor compliance;ylith landapplicati.onlimits,solidsflux data would be used asthe criteriafor proportioninggrabs from parallellimitsdewateringsystems,since most land appiicationare based on dry weightapplicationrates.Availabilityof FlowDataand/orSolidsFluxDataThe availabilityof accuratesolidsflux data (weighti'time;or accurateflow data (volume/time)is an Inportanc,considerationMost informationin planninga sludge samplingprogram.requirementsrelatingto sludge characteristicsinvolve,at leastthe need for data on the solidsflux of 2o;lutantin part,parametersfound in sludge dischargedfrom a ?073 . T3e 3erclnt- - solidsshould be determinedon sludge sampies.flow monitoringdevicesare not well suitedtoPortableand most sludge prccessingstreamsarehigh-solidsflow streams,not designedin a manner which is physicall;rconduciveto the useit is necessarytc relyThus, in most cases,of these devices.Due toon existingintegratedflow monitoringequipment.flow meters are highdifficultiesin monitoringsludge flows,Frequent calibrationof sludge flowmetersismaintenanceitems.Thisnecessaryin order to ensure accurate flow measurement. Xhenagair ;tmass balance data.data should be cross -checkedultimateuse cr disposalpractices2-7dictatemonic,oringsludgewith

a ipment2.2.2liquidflow meters are replacedby gross2.1 summarizesthe types of flowemployed to monitorvarioussludge flows.Sludcre SamDle PointsThe determinationof the appropriatesludge samplingpointis dependent on the rationalebehind the sampling.For permitsenforcement,sludge samples must come from theand regulationtreatmentunit processimmediatelyprecedingdisposalor use.of its dewateredfiltercakes inFor example, if a POTS disposesthen samplingactivityfocuses on the outputa sanitarylandfill,sludge stream from the dewateringdevice(i.e.,vacuum filter,belt filter,etc.).The sludge treatmentprocessescommonlyemployed are le 2.2 surmnarizes samplingpointsforthermalreduction.these processes.Other sludgessamplingpointsmay be necessaryto examine the originor fate of pollutantswithina POT,, (i.e.,additionalsludgesamples from influentand outputof otherprocesses may be needed).2.3SAMPLE C3LLXTIONHaving selectedappropriatesamplingpointsfor a sludgesamplingprogram,it is then necessaryto determinethe methodand equipmentby which sampling*dillbe.carriedout.In ccingobjectivesshould be considered:so I the following000Each grab sample, or aliquotof a compositesample,must be as representativeas possibleof the totalstream flow passingthe samplingpointEffortsamplemust be made to minimizecontaminationThe selectedand e safe,convenjent

TABLE 2.1.SLUDGE FLOFi MEASUREMENT DEVICES9easurementAoplicationMeansVenturiFlow stingThermal ReductionBulkcontainerStabilizedSludgeTABLE 2.2.SludgeMeterDisplacementscalesor truckscalesSLUDGE SAMPLING POINTSSamplinsTvDePointfrom taps on the amplepositiveAerobicallyDigested-Sample from taps on dischargelinesIf batch digestionis used, sa-rtplefrom the digester.Twc cautions'areconcerningthis practice:sideoffrom pumps.directlyin order(1) If aeratedduringsampling,air .entrainsthe.sample.Volatileorganiccompounds maypurge with escapingair.(2) When aerationis shut off,solidsrapidlyin well digestedsludge.ThickenedSludges -Samplepositivefrom taps on the dischargedisplacementpmps.2-9sideseparateofin

TABLE 2.2.SludgeHeatSLUDGE SAMPLING POINTS(continued)SamolinsTvoeSample from taps on the dischargeside ofpositivedisplacementpumps afterdecanting.when samplingheat treatmentBe carefulsludge because of:Treatment(1) h temperatureof sample(frequently 60 C as sampled)cancause problemswith certainsamplecontainersdue to coolingandsubsequentcontractionof entrainedgases.collectionconveyorsSample from materialSample from manyand bulk containers.locationswithinthe sludge mass and atDewatered:Belt ge(platePressand frame)Sample from the storageDryingBedsDividebed into quarters,arab equalamounts of sample from the centerofeach quarterand combine to form agrab sample of the totalbed.Eachgrab sample should includez;?eentiredepth of the sludge( own tothe ur pointswithinthe storagebin,collectequal amount of sample fromeach pointand combine.pilesSample directlyfrom front-endloaderas the sludgeis beins loadedinto trucksto be hauled away.2-10

Except for limitationson the use of automaticsamplingdevices,the actual,samplingtechniquesfor sludgesare similarto those found in wastewatersampling.The followingsectionsdescribetwo importantconsiderationsfor equipmentand propersamplingpractices.2.3.1SamnlinsEa-uiomentIn general,automaticsamplingdevices,which are widelyusedfor wastewaterstreams,do not work well for sludge streamsbecause of the solidscontentand viscosityof sludges.Automaticsamplerswhich use pumps to draw samples up a suctionseparationif flow velocityin the suctionandtube cause solidsdischargetube iS too low.This increasespump head requirementsand limitsthe range of tubingdiameter.A second problemwhichoccurs in the use of automaticsamplersis foulingof tubingand/or pump structureby sludge solids.This resultsincontaminationof subsequentaliquotsduringcompositesampling.Sludge particlesmay also plug the sample tube or pumpAngmechanism and interruptsample collection.Yherefora,it ispreferableto sample liquidsludge streams manually,partic-Jlarlyif sample taps can be providedon pump dischargelines.Samplingequipmentmust be made of materials'Nihich vi11 notcontaminateor react with the sludge.The best materialchoicesare Teflon,glass,and stainlesssteelbecause they arerelativelyinert.When the cost of Teflonand stainlesssteelequipmentprohibitsor restrictstheiruse, plastic,steeland/oraluminum may be substitutedfor most samplingactivities.(Ifsteelequipmentis used, ensure that galvanizedor zinc coateditems are not used because these materialswillreadilyreleasezinc into the sample.12-11

Graduatedglass or plasticpitchersor cylindersare used todraw grabs for manuallycomposted samples.Stainlesssteelpitchersare also commerciallyavailable,and are used to grabsamples from taps and also can be affixedto lengthsof conduitto sample from open channelflows.Only aluminum conduitsshouldbe used since most commerciallyavailablesteelconduitisIn addition,galvanized.only stainlesssteelclamps should beused to attachthe sample containerto the ticesbelow are practicessludges:thatshouldbe followed;IhenClean all samplingequipmentbetween each sample periodto prevent ing with a laboratorydetergent,thoroughrinsingwith tap water and then ;rith at leastthreedistilledwater rinses.should be composted directlyintoSample aiiquotssample containers.Sample containers,preservationsample and allowableholdingtime pyiortc analysisin Section2.5.discussedofareWhen collectingsamples for oil and grease anal:Jsis,sample directlvinto the sample containersince cil andgrease tend to adhere to surfaces.Sample compositesshould be sent t,o the laboratoryas a seriesof grabsamples.Sampie collection proceduresshoulddocumented,as discussedin Secticnbe adequar,oly2.7.When collectingsamples for organicvolatilesor semivolatiles,carefullypour liquidsludgeinto ccntainerc; 1so as to avoid entrappingair *d:thinsample.-,,1containerto overflowingand screw on 11c!.Check airbubblesby turningcontainerupside down and tappinglid.If air bubblesrise,open containerand fillXlthadditionalsample.For sludge cake, care-fullypacksludge ir,:o containerso as to avoid air spaces.Fillthe containerto overflowingand screldon iid.2-i2

0When collectingsamples for dioxin/furan,containerto 4/5 fullto enable expansionwhen they are frozen.0When collectingsamples for pesticides/PCBs/herbicides,metalsand nonconventionals,fillcontainerto withinl/2 inch of the top to provideroom for expansionshould there be any gas productionduringsampleshipment.When sampling000To drawtap:sludges:a freshrepresentativesufficienttimeline of stagnantsludgefollowingsludge,samplefrompump startandaa)Allowclearb)Allow sludge to flow for severalseconds from tappriorto samplingin order to flushout stagnantsludge and solidsaccumulatedin the tap.Before drawinga sludge sample,rinseeach piecesamplingequipment3 times with sample to reducechance of contaminationfrom the previousgrab.up tooftheTo preventsolidsseparationin the sample,use glass,Teflon-coatedstirringrods, or stainlesssteelspoonsto mix the sample beforesplittingor transferringanyportionof it to anothercontainer(s.1.When sampling0liquidfilltheof samplessolidsludges:For eitherdewateredcakes, dried powdercombine equal amounts collected"atprcduct,locations/depthsfor each grab sample torepresentativesample.a)or compostvariousobtain a moreTo produce a sample from multiplesample locationstwo or more dewateringunits),combine the(e.g.,grab samples from each location(equal amounts orweightedbased on flow or solidsfluxdata)in aplasticor stainlesssteelpailand thoroughlymixthe sample (with a scoop or spoon),then transferit to sample containers.This is not appropriatefor volatileor microbialsamples.2-13

b)2.4When samplingdryingbeds, divideeach bed intoquarters.From the centerof each quarter,collecta singlecore sample throughthe entiredepth of the sludge using a coringdevice.Usuallya small amount of sand willbe collected;Combine andavoid large amounts of sand.thoroughlymix in plasticor stainlesssteelpailand transferto sample containers.SAMPLE SIZE,SampleSAMPLE TYPE, AND SAMPLING FREQUENCYSizeA propersample is small enough to transportconvenientlyand handle carefullyin the laboratory,but large enough tocharacteristicsof the whole material.accuratelyrepresenttheMinimum sample sizes requiredfor accurateanalysisare specifiedTable 2.3 listsminimum sample sizesin each analyticalmethod.For methods not listedhere,for some common analyticalmethods.consultan analyticalmethods referenceor the laboratoryforfurtherguidance.SampleTvpeA grab sample collectedat a particulartime and locationcan representthe compositionof the source only at that time andIn the case of most sludges,singlegrab samples willlocation.adequatelyrepresentonly the instantaneouscompositionof thematerialbeing sampled.The qualityof a grab sample xi:1 beimprovedif it is comprisedof severalsmallersamples taken overa periodof a few minutes.A compositesample gives a betterreflectionof the timeand location-weightedaverage concentrationsthat are found inIn most cases, the term "compositethe sludge flow stream.to a mixtureof grab samples collectedat the s,nesample8' referssamplingpointat differenttimes.Althougha 24-hour composite2-14

'l'ABT,F 2. 3CONTATNERS, PRESERVATION, IIOI,D1‘NG TIMES,- n&Meta&ChromiumMercuryMetalsAND MINIMUM SAMPLE V6LUMES(')VIexcept.aboveQrqanic HC,haloethers,chlorinatedtlC and TCDD)Extr-actable(phenols)p,NoneNone2000 mLP,GP ,Gcool,4OCHN03 to pHt224 hours28 days300 mL500 mLP,GHN03 to pH 26 months1000 mLG, teflonlined capCool, 4OC0.008% Na2Y2037 days (ill40 days (a)1000 mLP, fordioxinandfuran 0111 Coo1 , 4OcLI2SO4 to pH 20.008% Na2S2031000 mLPurqeablcs(Halocarbons,lnd Aromatics 17 days b.qto)14 days indarkness 20 mLPuryeai) I es1.4 clays;20 ml,(AtrroleiinandAct-ylorl i t r i le )

TABLE 2.3CONTAINERS, PRESERVATION, HOLDING TIMES,Wide-mouthedParameterPesticidesContainer6, PCBsC! teflonlined septa(Continued)AND MlNIMUM SAMPLE VOLUMES('Preservative(*)Maximum (2)HoldingTimeCool 4Oc0.008% Na2S2031000 mL(1)40 CFR Part136(2)Preservativesshould he added to samplingcontainerspriorto actualsamplingepisodes.Holdingtimes commerlce upon additionof sample to samplingcontainer.Shippingof pre-preservedcontainersto the sample sitesmay be regulatedunderhazardous materialsregulations.Shippingof preservedsamples to the laboratoryis generallynot regulatedas a hazardousmaterial.(3)VariesP Plastic(; vativesPyrex)method.Consult40 CFR Part136,DOT

sample (consistingof a number of timeor flow-weightedgrabsamples)is more representativethan a grab sample,it can give apictureof only one day's sludge quality.Historicaldata isnecessaryto trulyrepresentthe s

2.1.1 Solids Content and Viscosity Two important physical characteristics of sludge with respect to sampling and analysis are viscosity and solids content. Solids content is the percent, by weight, of solid material in a given volume of sludge. Sludges have a much higher solids content than most wastewaters.

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