1、BRITISH STANDARD BS EN 13650:2001 Soil improvers and growing media Extraction of aqua regia soluble elements The European Standard EN 13650:2001 has the status of a British Standard ICS 65.080 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN 13650:2001 This British Standar
2、d, having been prepared under the direction of the Consumer Products and Services Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 09 November 2001 BSI 09 November 2001 ISBN 0 580 38269 9 National foreword This British Standard
3、 is the official English language version of EN 13650:2001. The UK participation in its preparation was entrusted to Technical Committee AW/20, Top soil and other growing media, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its s
4、ecretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Stand
5、ards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers
6、to understand the text; present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a fr
7、ont cover, an inside front cover, the EN title page, pages 2 to 17 and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN13650 Septemb
8、er2001 ICS65.080 Englishversion SoilimproversandgrowingmediaExtractionofaquaregia solubleelements AmendementsdusoletsupportsdecultureExtraction dlmentssolublesdansleaurgale BodenverbesserungsmittelundKultursubstrateExtraktion voninKnigswasserlslichenElementen ThisEuropeanStandardwasapprovedbyCENon11
9、August2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCen
10、treortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbod
11、iesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,
12、36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN13650:2001EEN13650:2001(E) 2 Contents page Foreword . 3 1 Scope 4 2 Normativereferences 4 3 Termsanddefinitions . 4 4 Principle . 4 5 Reagents 5 6 Apparatus. 5 7 Testsamplepassingth
13、rougha500 msieve 6 8 Procedure. 6 9 Determinationofextractedelements . . 7 10 Expressionofresults 7 11 Precision 7 12 TestReport . 7 AnnexA (informative) Resultsofaninterlaboratorytrialtodetermineaquaregiasoluble elements. 9 AnnexB (informative) Methodsofanalysisusedintheinterlaboratorytrial 16 Bibl
14、iography 17EN13650:2001(E) 3 Foreword ThisEuropeanStandardhasbeenpreparedbyTechnicalCommitteeCEN/TC223“Soilimproversand growingmedia“,thesecretariatofwhichisheldbyBSI. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidentical textorbyendorsement,atthelatestbyMarch
15、2002,andconflictingnationalstandardsshallbewithdrawnat thelatestbyMarch2002. TheannexesAandBareinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark, Finland,Fra
16、nce,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal, Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN13650:2001(E) 4 SAFETYPRECAUTIONSCareshouldbetakenwhenhandlingsamplesthatmaycontainsharpsorareof adustynature. 1Scope ThisEuropeanStandardspecifiesamethodfortheroutineextrac
17、tionof aquaregiasolubleelements(aslistedin annexB)fromsoilimproversorgrowingmedia.Materialscontainingmorethanabout28%( m/m)organicmatter willrequiretreatmentwithadditionalnitricacid.Withhighsoluteconcentrationsinextractsolutions,spectral interferencesandbackgroundenhancementshouldbeexpected. Themeth
18、odisnotapplicabletolimingmaterialsandpreformedmaterialssuchasmineralwoolslabsandfoam slabs. NOTE1 Aquaregiawillnottotallydissolvemostsoilimproversorgrowingmedia,andtheefficiencyofextractionfor particularelementsdiffersfromelementtoelement.Suchefficiencymightalsodifferforthesameelementindifferentmatr
19、ic es. Elementsextractablein aquaregia cannottherefore,bedescribedas“Totals”;converselytheycannotberegardedasthe“bio available”fraction,astheextractionprocedureistoovigoroustorepresentanybiologicalprocess. NOTE2 Therequirementsofthestandardmaydifferfromthenationallegalrequirementsforthedeclarationof
20、theproducts concerned. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthe
21、sepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). ENISO3696, WaterforanalyticallaboratoryuseSpecificationandtestmethods (ISO3696:1987). EN13039, Soilimproversandgrowingm
22、ediaDeterminationoforganicmattercontentandash. EN13040:1999,SoilimproversandgrowingmediaSamplepreparationforchemicalandphysicaltests, determinationofdrymattercontent,moisturecontentandlaboratorycompactedbulkdensity. 3 Termsanddefinitions ForthepurposesofthisstandardthetermsanddefinitionsgiveninEN130
23、39andEN13040apply. 4Principle Thedriedsampleisfinelygroundandextractedwithahydrochloric/nitricacidmixturebystandingfor16hatroom temperature,followedbyboilingunderrefluxfor2h.Theextractisclarifiedandtheextractedelements determined. Thetestsampleshallbegroundtolessthan500 mpriorto aquaregia digestion.
24、Suchgrindingisdesignedto a)giveamorehomogeneoussamplefromwhichasubsampleistaken; b)increasetheefficiencyofacidattackbyincreasingthesurfaceareaoftheparticles.EN13650:2001(E) 5 5Reagents 5.1General Allreagentsusedshallbeofrecognizedanalyticalquality.Usewaterofgrade2complyingwithENISO3696. Deionizedwat
25、ermaybeused,providingthatitmeetstherequirementsgivenabove.Itisrecommendedthatthe samebatchofwaterbeusedthroughoutagivenbatchofdeterminationsandthatblankdeterminationsarecarried out. 5.2Hydrochloricacid , c(HCl)=12mol/l; 1,18g/ml;37%mass/volume. 5.3Nitricacid, c(HNO 3 )=15mol/l; 1,42g/ml;notlessthan6
26、5%mass/volume. 5.4Nitricacid, c(HNO 3 )=0,5mol/l,35mlnitricacid( 5.3)isdilutedtoonelitreofwater. 6Apparatus 6.1 General NOTE Ithasbeenfoundconvenienttokeepseparatesetsofglasswareincludingantibumpinggranulesorroughenedbeads forthedeterminationsgiveninannexB,inordertoreducethepossibilityofwithinlabora
27、torycontamination . Cleanallnewglasswarebycarefullyimmersinginwarmnitricacid( 5.4)foraminimumof6handthenrinsein water. Theapparatusconsistsoftheusuallaboratoryapparatus,andinparticularthefollowing: 6.2 Grindingmill, capableofgrindingdriedsamplestoasizelessthan500 mwithoutcontaminationbythe elementst
28、obedetermined. Amillcausinglittleornocontaminationisessential,asisadequatecleaningbetweensamplestoeliminatememory effects.Bothagateandzirconiumoxidemillshavebeenfoundsuitable.5 6.3Testsieve ,ofaperturesize500 m,e.g.testsievewithgauzepreferablymadefromplasticmaterials,e.g. nylon. 6.4Desiccator, ofnom
29、inalvolume2l. 6.5Reactionvessel, ofnominalvolumeofnotlessthan250ml. NOTE1 IthasbeenfoundconvenienttouseformixingatwoneckErlenmeyertypereactionvesselofnominalvalue500ml withgroundglassjointsandadripfunnelofnominalvalue100mlwithconicalgroundglassjointsandstopper. NOTE2 Alargerreactionvesselmayberequir
30、edforsampleswhenasampleweightexceeding1gistakenforanalysesor excessivefrothingisexperienced. 6.6Refluxcondenser, straightthroughtype,withconicalgroundglassjoints. NOTE Watercooledcondenserswithaminimumeffectivelengthofatleast200mmhavebeenfoundsuitable.The effectivelengthistheinternalsurface,whichisi
31、ncontactwiththecoolingwater.Theoverallexternallengthofsuchconde nsers isusuallyatleast363mm. 6.7Roughenedglassbeads, diameter2mmto3mm(orantibumpinggranules). 6.8Temperaturecontrolledheatingapparatus, capableofheatingthecontentsofthereactionvesseltoreflux temperature. 6.9Funnel, ofdiameterapproximate
32、ly100mm. 6.10Volumetricflask ,ofnominalcapacity100ml.EN13650:2001(E) 6 6.11Filterpapers, cellulosebasedashlesstypes,withamediumporesizeofapproximately8 manddiameter of150mm. 6.12Analyticalbalance, capableofweighingaccuratelyto1,0mg. 7 Testsamplepassingthrougha500 msieve Takeapproximately5gofthesampl
33、epreparedinaccordancewithEN13040:1999,clause9,andgrindthesub sampleusingamill( 6.2)untilallthesubsamplehaspassedthroughthesieve( 6.3). 8Procedure 8.1 WARNINGDigestionswithhydrochloricandnitricacidarepotentiallyhazardousandlaboratory coats,glovesandsafetyspectaclesorgogglesshallbeused. Thedigestionsh
34、allbecarriedoutinawellventilatedfumecupboardwiththerefluxdigestionona temperaturecontrolledheatingapparatus.Itisessentialtoaddantibumpinggranules(orroughened glassbeads)bothtotheblankandthesamplestopreventbumpingandlossofsolution.Itisimportantto maintaingentlereflux,bothoftheblankandthetestsamples,t
35、oavoidtemperaturefluctuations,which couldcauselocalsuperheating. Thetoxicityorcarcinogenicityofeachreagentusedinthismethodhasnotbeenpreciselydefined; however,eachchemicalcompoundneedstobetreatedasapotentialhealthhazard.Fromthisviewpoint, reduceexposuretothesechemicalstothelowestpossiblelevelbywhatev
36、ermeansavailable. Toxicfumesareevolvedbynitricacid.Alwaysusetheconcentratedacidinafumecupboard. 8.2Digestion Weighapproximately1gto3g,tothenearest0,001g,ofthefinelygroundtestsample( clause7 )intothereaction vessel( 6.5).Moistenwithabout0,5mlto1,0mlwater.Addwhilemixing,21mlofhydrochloricacid( 5.2)fol
37、lowed by7mlofnitricacid( 5.3),dropbydropifnecessarytoreducefoaming.Allowtostandfor16hatroomtemperature toallowforslowoxidationoftheorganicmatterinthesample. NOTE1 Itiscommonpracticetoaddhydrochloricaciddirectlytothereactionvessel,followedbythenitricacid,andto assumethatthe aquaregiaformsinthereactio
38、nvessel.However,problemshavebeenencounteredwithmaterialsrichin carbonates,whereasubstantialportionofthehydrochloricacidhasbeenconsumedbeforethenitricacidcanbeadded.Under suchcircumstances,thecorrectformationof aquaregia isdoubtful. Theamountof aquaregiaissufficientonlyforoxidationofabout0,85goforgan
39、icmatter.Ifthereisanydoubt abouttheamountoforganicmatterpresent,carryoutadeterminationaccordingtoEN13039.Ifthereismorethan 0,85goforganicmatter(correspondingtoabout0,5goforganiccarbon)inthetestsamplereducethequantityof sampleanalyzedorproceedasfollows. Allowthefirstreactionwith aquaregia tosubside.T
40、henaddanextra1mlofnitricacid( 5.3)onlytoevery0,17gof organicmatterabove0,85g.Donotaddmorethan10mlofnitricacidatanytime,andallowanyreactionto subsidebeforeproceedingfurther. Addafewroughenedglassbeads( 6.7)andplacethereactionvesselonacoolheatingapparatus( 6.8). Raisethe temperatureofthereactionmixtur
41、eslowlyuntilrefluxconditionsarereachedandmaintainfor2hensuringthatthe condensationzoneislowerthan1/3oftheheightofthecondenser,thenallowtocool. Transferthecontentsofthereactionvesseltoa100mlvolumetricflask( 6.10).Washthereactionvesselatleast threetimeswithwaterdecantingeachwashingintothevolumetricfla
42、skbeforeaddingthenext.Dilutetothemark withwaterandmix.Allowtostandsothatmostofanyinsolubleresiduesettlesoutofsuspension.Decantthe relativelysedimentfreesupernatantontoafilterpaper( 6.11),discardingatleastthefirst10mloffiltrate. NOTE2 Theflaskcontainingtheextractcouldrequiretheadditionofreleasingagen
43、tsdependingontheelement(s)of interest,andthespectroscopicmethodchosen.EN13650:2001(E) 7 8.3Reagent blank Thereagentblanktestshallbecarriedoutinparallelwiththedetermination,bythesameprocedure,usingthe samequantitiesofallthereagentsasinthedeterminationbutomittingthetestportion. NOTE Themeasurementofablankisintroducedtodeterminethecontributionoftheextractingsolution,glasswareand filterpaperused. 8.4 Residualmoisture Themoisturecontentofthesampleisdetermined
