SIST EN ISO 6865:2001

• Abstract:

  Cette norme internationale prescrit une méthode de détermination de la teneur en cellulose brute par filtration intermédiaire. Elle décrit un mode opératoire manuel et un mode opératoire semi-automatique. Cette méthode est applicable aux aliments des animaux ayant une teneur en cellulose brute supérieure à 10 g/kg. ; NOTE Pour des aliments pour animaux contenant de la cellulose brute inférieure ou égale à 10 g/kg, la méthode décrite dans l'ISO 6541 doit être utilisée. Cette Norme internationale est également applicable aux céréales et aux légumes.»

• Status: Published
• Publication Date: 31-Jan-2001
• ICS: 65.120 - Animal feeding stuffs
• Technical Committee: KŽP - Agricultural food products
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-Feb-2001
• Due Date: 01-Feb-2001
• Completion Date: 01-Feb-2001
• Ref Project: EN ISO 6865:2000 - Animal feeding stuffs - Determination of crude fibre content - Method with intermediate filtration (ISO 6865:2000)

• Refers: SIST ISO 3696:1995 - Water for analytical laboratory use -- Specification and test methods
• Effective Date: 09-Feb-2026

SIST EN ISO 6865:2001 is the Slovenian standard from SIST that adopts EN ISO 6865:2000 / ISO 6865:2000 for determining crude fibre content. It specifies a filtration-based method with both manual and semi-automatic procedures for animal feeding stuffs with more than 10 g/kg crude fibre, and it also applies to cereals and pulses. The standard is written for laboratories and quality-control staff who need a repeatable result from sample preparation through reporting.

What does SIST EN ISO 6865:2001 specify?

SIST EN ISO 6865:2001 specifies the method used to determine crude fibre content by intermediate filtration. The document is organized into clauses for scope, references, term and definition, principle, reagents, apparatus, sampling, sample preparation, two test procedures, calculation, precision, and the test report.

The main structure is:

• Clause 1 - scope and applicability
• Clause 2 - normative references
• Clause 3 - term and definition
• Clauses 4 to 6 - principle, reagents, apparatus
• Clauses 7 and 8 - sampling and preparation of the test sample
• Clauses 9 and 10 - manual and semi-automatic procedures
• Clause 11 - calculation
• Clause 12 - precision
• Clause 13 - test report
• Annex A - interlaboratory precision results, for information only

The method is intended for feeds above 10 g/kg crude fibre. For samples at or below that level, the standard points to ISO 6541 as the alternative method. It also states that the method is applicable to cereals and pulses, so it is not limited to compound feed.

What are the key requirements of SIST EN ISO 6865:2001?

SIST EN ISO 6865:2001 requires a prepared, air-dry laboratory sample that is ground so it passes a 1 mm sieve and is mixed thoroughly. In practice, this means the sample must be reduced to a consistent particle size before testing, because uneven grinding can change the residue that remains after digestion.

Sample selection and decision path

SIST EN ISO 6865:2001 uses a decision path based on fat and carbonate content. If fat content is high, or if the fats cannot be removed directly with light petroleum, the sample is defatted before digestion. If carbonate content, expressed as calcium carbonate, is high, the sample is treated to remove carbonate before the acid digestion step.

Digestion, filtration, washing

SIST EN ISO 6865:2001 requires boiling treatment with dilute sulfuric acid followed by potassium hydroxide solution [KOH]. The residue is filtered, washed with hot water until neutral, then washed with acetone and dried. In practice, these steps remove digestible material so that the remaining mineral-corrected residue can be measured.

Drying, ashing and blank control

SIST EN ISO 6865:2001 requires drying the crucible and residue at 130 °C, then ashing at 500 °C to 525 °C until two successive weighings differ by no more than 2 mg. A blank determination with the same amount of filter aid is also required, and its ash loss must not exceed 2 mg. This protects the result from errors caused by the filter aid or the crucible.

Calculation and reporting

SIST EN ISO 6865:2001 calculates crude fibre content from the mass before and after ashing, relative to the test portion. The result is reported in g/kg and rounded to the nearest 1 g/kg. The test report must identify the sample, state the method used, record any optional details or incidents, and give the result or paired results when repeatability is checked.

Precision

SIST EN ISO 6865:2001 includes repeatability and reproducibility limits in Table 1, with supporting interlaboratory data in Annex A. In practice, this tells users how close two results should be when the same method is run in one laboratory or in different laboratories.

What terms does SIST EN ISO 6865:2001 define?

• Crude fibre content - the mass lost after ashing the dried residue from acid and alkaline digestion, divided by the mass of the test portion.
• Test portion - the weighed amount of the prepared sample used for the analysis.
• Blank determination - a run carried out with filter aid but without sample, used to check the mass loss from the materials themselves.
• Repeatability - the closeness of results obtained in the same laboratory by the same operator using the same equipment over a short time.
• Reproducibility - the closeness of results obtained in different laboratories by different operators using different equipment.
• KOH - potassium hydroxide, the alkaline digestion reagent used after the acid step.

Who uses SIST EN ISO 6865:2001?

SIST EN ISO 6865:2001 is used by analytical laboratories testing animal feeding stuffs, and by quality-control teams in feed manufacturing and ingredient supply. It is also relevant to laboratories working with cereals and pulses when crude fibre content needs to be determined by a standardized wet-chemistry method. Buyers, inspectors, and auditors use it when they need comparable reported results from different laboratories.

Which standards are used with SIST EN ISO 6865:2001?

• ISO 3696 - specifies the water quality needed for analytical laboratory use.
• ISO 6498 - gives the preparation of test samples for animal feeding stuffs.
• ISO 6497 - provides a recommended sampling method for animal feeding stuffs.
• ISO 6541 - gives the alternative crude fibre method for samples with 10 g/kg crude fibre or less.
• ISO 4793 - supports the porosity grading of sintered filter plates used in the apparatus.
• ISO 6492 - is listed in the bibliography as the method for fat content, which is relevant when the sample must be defatted.

What does the SIST EN ISO 6865:2001 document contain?

SIST EN ISO 6865:2001 contains detailed manual and semi-automatic test procedures, reagent specifications, apparatus requirements, and the calculation method. It also includes a precision section with Table 1 for repeatability and reproducibility limits, plus Annex A with interlaboratory test results and statistical data. The document gives the step-by-step laboratory workflow needed for routine testing, method verification, and result reporting.

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Futtermittel - Bestimmung des Rohfasergehaltes - Verfahren mit Zwischenfiltration (ISO/FDIS 6865:2000)Aliments des animaux - Détermination de la teneur en cellulose brute - Méthode avec filtration intermédiaire (ISO/FDIS 6865:2000)Animal feeding stuffs - Determination of crude fibre content - Method with intermediate filtration (ISO 6865:2000)65.120KrmilaAnimal feeding stuffsICS:Ta slovenski standard je istoveten z:EN ISO 6865:2000SIST EN ISO 6865:2001en01-februar-2001SIST EN ISO 6865:2001SLOVENSKI
STANDARD
ReferencenumberISO6865:2000(E)©ISO2000INTERNATIONALSTANDARDISO6865Firstedition2000-10-15Animalfeedingstuffs—Determinationofcrudefibrecontent—MethodwithintermediatefiltrationAlimentsdesanimaux—Déterminationdelateneurencellulosebrute—MéthodeavecfiltrationintermédiaireSIST EN ISO 6865:2001

ISO6865:2000(E)PDFdisclaimerThisPDFfilemaycontainembeddedtypefaces.InaccordancewithAdobe'slicensingpolicy,thisfilemaybeprintedorviewedbutshallnotbeeditedunlessthetypefaceswhichareembeddedarelicensedtoandinstalledonthecomputerperformingtheediting.Indownloadingthisfile,partiesacceptthereintheresponsibilityofnotinfringingAdobe'slicensingpolicy.TheISOCentralSecretariatacceptsnoliabilityinthisarea.AdobeisatrademarkofAdobeSystemsIncorporated.DetailsofthesoftwareproductsusedtocreatethisPDFfilecanbefoundintheGeneralInforelativetothefile;thePDF-creationparameterswereoptimizedforprinting.EverycarehasbeentakentoensurethatthefileissuitableforusebyISOmemberbodies.Intheunlikelyeventthataproblemrelatingtoitisfound,pleaseinformtheCentralSecretariatattheaddressgivenbelow.©ISO2000Allrightsreserved.Unlessotherwisespecified,nopartofthispublicationmaybereproducedorutilizedinanyformorbyanymeans,electronicormechanical,includingphotocopyingandmicrofilm,withoutpermissioninwritingfromeitherISOattheaddressbeloworISO'smemberbodyinthecountryoftherequester.ISOcopyrightofficeCasepostal[e-mail]©ISO2000–AllrightsreservedSIST EN ISO 6865:2001

ISO6865:2000(E)©ISO2000–AllrightsreservediiiForewordISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISOmemberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnicalcommittees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhastherighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmental,inliaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnicalCommission(IEC)onallmattersofelectrotechnicalstandardization.InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,Part3.DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtothememberbodiesforvoting.PublicationasanInternationalStandardrequiresapprovalbyatleast75%ofthememberbodiescastingavote.AttentionisdrawntothepossibilitythatsomeoftheelementsofthisInternationalStandardmaybethesubjectofpatentrights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights.InternationalStandardISO6865waspreparedbyTechnicalCommitteeISO/TC34,Foodproducts,SubcommitteeSC10,Animalfeedingstuffs.AnnexAofthisInternationalStandardisforinformationonly.SIST EN ISO 6865:2001

INTERNATIONALSTANDARDISO6865:2000(E)©ISO2000–Allrightsreserved1Animalfeedingstuffs—Determinationofcrudefibrecontent—Methodwithintermediatefiltration1ScopeThisInternationalStandardspecifiesamethodwithintermediatefiltrationforthedeterminationofthecrudefibrecontent.Amanualprocedureandasemi-automaticprocedurearedescribed.Themethodisapplicabletoanimalfeedingstuffswithacrudefibrecontentgreaterthan10g/kg.NOTEForanimalfeedingstuffswithacrudefibrecontentequaltoorlessthan10g/kg,themethoddescribedinISO6541[7]maybeused.ThisInternationalStandardisalsoapplicabletocerealsandpulses.2NormativereferencesThefollowingnormativedocumentscontainprovisionswhich,throughreferenceinthistext,constituteprovisionsofthisInternationalStandard.Fordatedreferences,subsequentamendmentsto,orrevisionsof,anyofthesepublicationsdonotapply.However,partiestoagreementsbasedonthisInternationalStandardareencouragedtoinvestigatethepossibilityofapplyingthemostrecenteditionsofthenormativedocumentsindicatedbelow.Forundatedreferences,thelatesteditionofthenormativedocumentsreferredtoapplies.MembersofISOandIECmaintainregistersofcurrentlyvalidInternationalStandards.ISO3696:1987,Waterforanalyticallaboratoryuse—Specificationandtestmethods.ISO6498:1998,Animalfeedingstuffs—Preparationoftestsamples.3TermanddefinitionForthepurposesofthisInternationalStandard,thefollowingtermanddefinitionapply.3.1crudefibrecontentlossinmassresultingfromashingofthedriedresidueobtainedafteracidandalkalinedigestionofthesamplebytheproceduredescribedinthisInternationalStandard,dividedbythemassofthetestportionNOTEThecrudefibrecontentisexpressedingramsperkilogram.Itmayalsobeexpressedasamassfractioninpercent.4PrincipleThetestportionistreatedwithboilingdilutesulfuricacid.Theresidueisseparatedbyfiltration,washedandthentreatedwithboilingpotassiumhydroxidesolution.Theresidueisseparatedbyfiltration,washed,dried,weighedandthenashed.Thelossinmassresultingfromashingcorrespondstothemassofcrudefibreinthetestportion.SIST EN ISO 6865:2001

ISO6865:2000(E)2©ISO2000–Allrightsreserved5ReagentsandmaterialsUseonlyreagentsofrecognizedanalyticalgrade.5.1Water,complyingwithatleastgrade3inaccordancewithISO3696.5.2Hydrochloricacid,c(HCl)=0,5mol/l.5.3Sulfuricacid,c(H2SO4)=(0,130,005)mol/l.5.4Potassiumhydroxidesolution,c(KOH)=(0,230,005)mol/l.5.5Acetone.5.6Filteraid:seasand,orCelite®1)545,ormaterialofanequivalentquality.Beforeuse,treatseasandwithboilinghydrochloricacid[c(HCl)=4mol/l],washwithwateruntilfreefromacidandheatatatemperatureof(50025)°Cforatleast1h.Beforeuse,heatotherfilteraidsatatemperatureof(50025)°Cforatleast4h.5.7Antifoamagent,forinstancen-octanol.5.8Lightpetroleum,boilingrange40°Cto60°C.6ApparatusUsuallaboratoryapparatusand,inparticular,thefollowing.6.1Grindingdevice,capableofgrindingthesamplesothatitpassescompletelythroughasievewith1mmapertures.6.2Analyticalbalance,withaccuracyofatleast0,1mg.6.3Filtercrucibles,ofquartz,porcelainorhardglass,withfusedsinteredfilterplatewithaporesizeof40mto100m(porositygradeP100accordingtoISO4793:1980[1]).Beforeusingforthefirsttime,carefullyandgraduallyheatanewfiltercrucibletoatemperaturenotexceeding525°Candleaveforafewminutesat(50025)°C.Stainless-steelcrucibleswithstainless-steelsieveplateswithanaperturesizeof90mofidenticalperformancecharacteristicsmaybeusedasanalternative.6.4Porcelainsieveplates.6.5Incinerationdishes.6.6Beakersorconicalflasks,of500mlcapacity,providedwithasuitablecoolingdevice,forexampleacondensororadish.1)Celite®isthetradenameofacommerciallyavailableproduct.ThisinformationisgivenfortheconvenienceofusersofthisInternationalStandardanddoesnotconstituteanendorsementbyISOofthisproduct.Equivalentproductsmaybeusediftheycanbeshowntoleadtothesameresults.SIST EN ISO 6865:2001

ISO6865:2000(E)©ISO2000–Allrightsreserved36.7Dryingoven,electricallyheatedandventilated,capableofbeingmaintainedatatemperatureof(1302)°C.6.8Desiccator,containingbluesilicagelasdesiccant,providedwithaperforatedplate,preferablyofaluminiumorstainlesssteel,ofthickness2mmto3mm.6.9Mufflefurnace,electricallyheated,providedwithaircirculationandtemperaturecontrolcapableofmaintainingthetemperaturearoundthecruciblestothenearest25°Cattemperaturesof475°Cto525°C.Thereadingofthepyrometerofthemufflefurnacecannotalwaysbetrusted:deviationsmayoccur.Therefore,thetemperatureinthemufflefurnaceshouldbecheckedregularly.Dependingonthesizeandtypeofthemufflefurnace,temperaturesinthefurnacemaydifferfromoneplacetoanotherplace.Whentheovendoorisclosed,adequateairsupplyshouldbeguaranteed.Thevolumeflowrateofairshouldnotbesogreatthatmaterialiscarriedawayfromthecrucibles.6.10Cold-extractiondevice,providedwithasupportforthefiltercrucible(6.3);adischargepipewithataptothevacuumandliquidoutlet;andconnectingringsforconnectingthefiltercrucible(6.3).6.11Heatingdevice(formanualmethod),providedwithasuitablecoolingdevicecapableofmaintainingthevolumeconstantduringboiling.6.12Heatingdevice(forthesemi-automaticmethod)foracidandalkalinedigestion,providedwithasupportforthefiltercrucible(6.3);adischargepipewithataptothevacuumandliquidoutlet;aboilingcylinderofatleast270mlcapacity,witharefluxcondenser;connectingringsforconnectingtheheatingdevicetothefiltercrucible(6.3)andtheboilingcylinder;andoptionally,provisionforcompressedair.Beforeuse,preheattheapparatuswithboilingwaterfor5min.7SamplingSamplingisnotpartofthemethodspecifiedinthisInternationalStandard.ArecommendedsamplingmethodisgiveninISO6497[6].Itisimportantthatthelaboratoryreceiveasamplewhichistrulyrepresentativeandhasnotbeendamagedorchangedduringtransportorstorage.8PreparationoftestsamplePreparethetestsampleinaccordancewithISO6498.Usingthegrindingdevice(6.1),grindtheair-drylaboratorysamplesothatitpassescompletelythroughasievewith1mmapertures.Mixthoroughly.SIST EN ISO 6865:2001

ISO6865:2000(E)4©ISO2000–AllrightsreservedForthemanualmethod,proceedinaccordancewithclause9.Forthesemi-automaticmethod,proceedinaccordancewithclause10.9Procedureformanualmethod9.1TestportionWeighabout1gofthepreparedtestsample(clause8)tothenearest0,1mg(m1).Ifthefatcontentofthesampleexceeds100g/kg,orifthesamplecontainsfatswhichcannotbeextracteddirectlywithlightpetroleum(5.8),transferthesampletoacrucible(6.3)andproceedinaccordancewith9.2.Ifthefatcontentofthesampledoesnotexceed100g/kg,transferthesampletoabeaker(6.6)andproceedinaccordancewith9.3ifthecarbonatecontent,expressedascalciumcarbonate,exceeds50g/kg.Ifthisisnotthecase,proceedinaccordancewith9.4.9.2PreliminarydefattingInthecold-extractiondevice(6.10),defatthesamplethreetimesundervacuumwith30mloflightpetroleum(5.8)eachtime.Drytheresiduebysuctionaftereachwashing.Transfertheresiduetoabeaker(6.6).Ifthecarbonatecontent,expressedascalciumcarbonate,exceeds50g/kg,proceedinaccordancewith9.3.Ifnot,proceedinaccordancewith9.4.9.3RemovalofcarbonatePour100mlofhydrochloricacid(5.2)overthesample.Stircontinuouslyfor5min.Carefullypourthemixtureintoafiltercrucible,thebottomofwhichiscoveredwithathinlayeroffilteraid(5.6).Decanttwicewith100mlofwatereachtime.Takecaresothataslittlematerialaspossibleendsuponthefilter.Transferthecontentsofthecrucibletotheoriginalbeakerandproceedinaccordancewith9.4.9.4AciddigestionPour150mlofsulfuricacid(5.3)overthesample.Bringtotheboilasquicklyaspossibleandcontinuesteadyboilingfor(301)min.Atthebeginningofboiling,swirlafewtimes.Iffoamingoccurs,addafewdropsofantifoamagent(5.7).Duringboiling,maintainaconstantvolumebyusingasuitablecoolingdevice(see6.6and6.11).9.5FirstfiltrationInthefiltercrucible(6.3)applyalayeroffilteraid
...