1、BRITISH STANDARD BS EN 13652:2001 Soil improvers and growing media Extraction of water soluble nutrients and elements The European Standard EN 13652:2001 has the status of a British Standard ICS 65.080 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN 13652:2001 This Britis
2、h Standard, 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 38267 2 National foreword This British
3、 Standard is the official English language version of EN 13652:2001. 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
4、 to its secretary. 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
5、BSI Standards 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 e
6、nquirers 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 compr
7、ises a front cover, an inside front cover, the EN title page, pages 2 to 15 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 EN1365
8、2 September2001 ICS65.080 Englishversion SoilimproversandgrowingmediaExtractionofwatersoluble nutrientsandelements AmendementsdusoletsupportsdecultureExtraction deslmentsnutritifssolublesdansleau BodenverbesserungsmittelundKultursubstrateExtraktion wasserlslicherNhrstoffeundElemente ThisEuropeanStan
9、dardwasapprovedbyCENon11August2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonappli
10、cationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersar
11、ethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG Managem
12、entCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN13652:2001EEN13652:2001(E) 2 Contents page Foreword . 3 1 Scope 4 2 Normativereferences 4 3 Termsanddefinitions . 4 4 Principle . 4 5 Reagents 4 6 Apparatus.
13、 5 7 Testsample. . 5 8 Procedure. 5 9 Determinationofextractednutrientsandelements. . 6 10 Expressionofresults 6 11 Precision 6 12 Testreport 6 AnnexA (informative) Resultsofaninterlaboratorytrialtodeterminewatersolublenutrients andelements. . 7 AnnexB (informative) Methodsofanalysisusedintheinterla
14、boratorytrial. 14 Bibliography 15EN13652:2001(E) 3 Foreword ThisEuropeanStandardhasbeenpreparedbyTechnicalCommitteeCEN/TC223“Soilimproversand growingmedia“,thesecretariatofwhichisheldbyBSI. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidentical textorbyendorsem
15、ent,atthelatestbyMarch2002,andconflictingnationalstandardsshallbewithdrawnat thelatestbyMarch2002. TheannexesAandBareinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepubli
16、c,Denmark, Finland,France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal, Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN13652:2001(E) 4 SAFETYPRECAUTIONSCareshouldbetakenwhenhandlingsamplesthatmaycontainsharps orisofadustynature. 1Scope ThisEuropeanStandardspecifiesameth
17、odfortheroutineextractionofwatersolubleextractable nutrientsandelements(aslistedinannexB)insoilimproversorgrowingmedia. Themethodisnotapplicabletolimingmaterialsandpreformedmaterialssuchasmineralwoolslabsand foamslabs. NOTE Therequirementsofthestandardmaydifferfromthenationallegalrequirementsforthed
18、eclarationofthe productsconcerned. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications. Thesenormativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelisted hereafter.Fordatedreferences,subsequentamendmentstoorrevisio
19、nsofanyofthesepublications applytothisEuropeanStandardonlywhenincorporatedinitbyamendmentorrevision.Forundated referencesthelatesteditionofthepublicationreferredtoapplies(includingamendments). ENISO3696, WaterforanalyticallaboratoryuseSpecificationandtestmethods(ISO3696:1987). EN13039, Soilimprovers
20、andgrowingmediaDeterminationoforganicmattercontentandash. EN13040:1999, SoilimproversandgrowingmediaSamplepreparationforchemicalandphysicaltests, determinationofdrymattercontent,moisturecontentandlaboratorycompactedbulkdensity . 3 Termsanddefinitions Forthepurposesofthisstandardthetermsanddefinition
21、sgiveninEN13039andEN13040apply. 4Principle Asampleisextractedwithwaterat22 C 3 Cinanextractionvolumeratioof1+5.Theextracted nutrientsaredeterminedbyvariousmethodsasappropriate. 5Reagents 5.1General Allreagentsusedshallbeofrecognisedanalyticalqualityandwaterofgrade2accordingtoENISO3696. 5.2 Nitricaci
22、d, c(HNO 3 )=15mol/l; 1,42g/ml;notlessthan65%mass/volume. 5.3 Nitricacid, c(HNO 3 )=0,5mol/l,35mlnitricacid( 5.2)diluterequiredvolumeofnitricacid( 5.2)with water.EN13652:2001(E) 5 6Apparatus 6.1 General NOTE IthasbeenfoundconvenienttokeepseparatesetsofglasswareforthedeterminationsgiveninannexB,in or
23、dertoreducethepossibilityofwithinlaboratorycontamination. Allglassapparatusandplasticvesselsusedintheprocedureshouldbesubjecttoanappropriate preparationprocedureinordertokeeptheriskofcontaminationtoaminimum.Itisrecommendedthatall vessels(glassandplastic)arecleansedbycarefullyimmersinginwarmnitricaci
24、d( 5.3)foraminimumof 6handthenrinsedinwater. Borosilicateglasswareshallnotbeusedifboronistobedetermined. Rubberstoppers,whichmaycontaintracesofmetalsshallnotbeused.Itisrecommendedtouseplastic oranyotherstopperfreeofallsubstancestobeanalyzed. Theapparatusconsistsoftheusuallaboratoryapparatus,andinpar
25、ticularthefollowing: 6.2 Analyticalbalance withanaccuracyof10mg. 6.3 Plasticbottlesorcontainers, sufficientlylarge(500mlto1500ml)withscrewcaptoaccommodate thevolumeofthesample,extractantandatleast10%airvolume. 6.4 Shakingormixingmachine, capableofholdingtheplasticbottlesorcontainers( 6.3)and maintai
26、ningthesampleinsuspensionwithoutdamagingthestructureofthesample.Theuseofa horizontaltableshakerisrecommended. 6.5 Filterpaper, cellulosebasedashlesstypes,withamediumporesizeofapproximately8 mand diameterof150mm. NOTE Centrifugationisanacceptablealternative. 7 Testsample Preparethelaboratorysampleina
27、ccordancewithEN13040:1999,clause8,anddeterminethe laboratorycompactedbulkdensityinaccordancewithEN13040:1999,annexA. 8Procedure 8.1 Extraction 8.1.1Testsamplespassingthrougha20mmsieve Takeaweightequivalentto60mlofthesample(EN13040:1999,clause8.5)volumetothenearest1g andtransfertothecontainer( 6.3).A
28、dd300mlofwater,securethecapandshakefor1hontheshaking machine( 6.4) at22 C 3 C. 8.1.2Testsamplespassingthrougha40mmsieve Takeaweightequivalentto250mlofthesample(EN13040:1999,clause8.3)volumetothenearest1g andtransfertothecontainer(6.3).Add1250mlofwater,securethecapandshakefor1honthe shakingmachine( 6
29、4) at22 C 3 C.EN13652:2001(E) 6 8.1.3Filtration Filterthroughfilterpaper( 6.5)discardingatleastthefirst10ml.Insomecasespaperfiltrationistooslow orevenimpossible.Insuchcasesalternativeproceduresforobtainingaclearsupernatantareacceptable andthetechniqueusedshallbereported. Thefilteredextractisstablef
30、orthreedaysinahermeticallyclosedpolyethylenebottleifstoredina refrigeratorat0 Cto5 C.Thefiltratecanbestoredforlongerperiodsinadeepfreezeratabout18 C. Beforeusingasolutionthathasbeenfrozen,thethawedsolutionshallbethoroughlymixedtoeliminate gradientseparationthatoccursonfreezingandsubsequentthawing. 8
31、2 Blank Thereagentblanktestshallbecarriedoutinparallelwiththedetermination,bythesameprocedureas outlinedin 8.1.1or8.1.2and 8.1.3,usingthesamequantitiesofallthereagentsasinthedetermination butomittingthetestportion. NOTE Themeasurementofablankisintroducedtodeterminethecontributionoftheextractingsolu
32、tion, glasswareandfilterpaperused. 9 Determinationofextractednutrientsandelements. SeeannexB. 10 Expressionofresults Subtractthevaluesdeterminedforreagentblankfromthoseobtainedforthesamples.Allresultsshallbe calculatedusingthedeterminedcompactedlaboratorybulkdensityandexpressedinmg/lsubstrateas rece
33、ivedbasis. 11Precision Therepeatabilityandreproducibilityofthewatersolublenutrientorelementcontentinseparately preparedsamplesshouldbeinaccordancewithTablesA.1toA.6. Asummaryoftheresultsofaninterlaboratorytrialtodeterminetheprecisionofthemethod,in accordancewithISO57252,isgiveninannexA. NOTE Thevalu
34、esderivedfromthisinterlaboratorytrialmaynotbeapplicabletoconcentrationsandmatrices otherthanthosetested. 12 Testreport Thetestreportshallcontainthefollowinginformation: a)areferencetothisEuropeanStandard; b)allinformationnecessaryforcompleteidentificationofthesample; c)alltheanalyticalmethodsused; d
35、)theresultsofthedetermination,expressedasmg/lfreshsample; e)detailsofanyoperationsnotspecifiedintheEuropeanStandardorregardedasoptional,aswellas anyfactor,whichmayhaveaffectedtheresults; f)thecompactedlaboratorybulkdensityresult.EN13652:2001(E) 7 AnnexA (informative) Resultsofaninterlaboratorytrialt
36、odeterminewatersolublenutrients andelements Aninterlaboratorytrialwasorganisedin1997undertheauspicesoftheEuropeanCommitteefor Standardization,totesttheproceduresspecifiedinthisEuropeanStandard. InthistrialthenumberoflaboratoriesgivenintheTablesA.1toA.6determinedthewatersolublenutrient contentinsixsa
37、mpletypes. Allresultsarereportedonafreshbasis.EN13652:2001(E) 8 Asummaryoftheresultsoftheinterlaboratorytrialforthedeterminationofwatersolublenutrientsandelementsinsixsamp letypesisgiveninTablesA.1toA.6. TableA.1Compostedbark Element No.oflabs after No.of outliers mean value Repeatability Repeatabil
38、ity Repeatability limit Reproducibility Reproducibility Reproducibility limit eliminating outliers (labs) mg/l s r StdDev% r=2,8 s r s R StdDev% R =2,8 s R NH 4 N 22 0 764,7 23,21 8,50 65,00 260,94 95,55 730,63 NO 3 N 18 2 25,1 1,50 16,68 4,19 45,54 507,93 127,50 P 18 3 236,2 6,53 7,74 18,28 67,73 8
39、0,28 189,65 K 23 0 1910,0 44,16 6,47 123,65 300,48 44,05 841,36 Ca 20 2 59,0 4,24 20,11 11,87 19,75 93,75 55,31 Mg 21 1 23,8 1,03 12,17 2,89 3,86 45,46 10,82 SO 4 S 13 0 109,4 7,01 17,94 19,62 53,73 137,57 150,43 Na 19 1 275,1 9,32 9,49 26,11 22,35 22,75 62,59 B 13 1 1,4 0,10 20,40 0,28 0,26 53,10 0
40、72 Cu 19 0 1,3 0,07 15,86 0,20 0,49 108,66 1,37 Fe 20 0 10,4 0,61 16,35 1,69 3,87 104,62 10,84 Mn 20 0 1,3 0,10 21,29 0,27 0,44 96,17 1,22 Mo 8 1 0,2 0,02 23,58 0,05 0,02 33,83 0,07 Zn 20 0 2,6 0,18 19,14 0,49 0,54 58,06 1,50 Cl 16 0 898,3 35,77 11,15 100,15 131,76 41,07 368,93 F 7 1 1,0 0,36 102,9
41、3 1,01 0,91 258,07 2,54 Element No.oflabs after No.of outliers mean value Repeatability Repeatability Repeatability limit Reproducibility Reproducibility Reproducibility limit eliminating outliers (labs) g/l s r StdDev% r=2,8 s r s R StdDev% R=2,8 s R CLBD a 14 1 392,8 8,3 5,9 23,3 22,1 15,8 61,9 a
42、CLBDCompactedlaboratorybulkdensityEN13652:2001(E) 9 TableA.2Biowaste Element No.oflabs after No.of outliers mean value Repeatability Repeatability Repeatability limit Reproducibility Reproducibility Reproducibility limit eliminating outliers (labs) mg/l s r StdDev% r=2,8 s r s R StdDev% R=2,8 s R NH
43、 4 N 20 1 115,4 2,45 5,94 6,85 60,70 147,25 169,97 NO 3 N 20 0 76,7 10,21 37,26 28,58 108,59 396,44 304,06 P 16 3 38,8 1,89 13,65 5,30 7,82 56,35 21,88 K 22 0 1430,8 50,35 9,85 140,97 267,66 52,38 749,45 Ca 20 1 101,2 8,34 23,08 23,36 37,37 103,34 104,62 Mg 20 1 31,6 2,77 24,58 7,76 14,44 128,01 40,
44、43 SO 4 S 11 1 56,9 2,23 10,97 6,24 15,28 75,26 42,79 Na 17 2 138,7 4,24 8,56 11,86 15,29 30,87 42,81 B 13 0 1,8 0,14 21,37 0,39 0,59 90,69 1,64 Cu 18 0 0,4 0,05 29,59 0,13 0,20 124,71 0,56 Fe 19 0 43,0 3,62 23,58 10,13 34,15 222,57 95,61 Mn 17 1 1,3 0,09 20,45 0,26 0,86 187,18 2,42 Mo 9 0 0,2 0,01 19,66 0,04 0,05 72,83 0,13 Zn 18 0 1,1 0,20 51,32 0,55 0,58 150,97 1,61 Cl 14 1 578,3 10,75 5,20 30,09 48,79 23,62 136,62 F 8 1 1,1 0,15 37,02 0,41 0,39 99,64 1,10 Element No.oflabs after No.of outliers mean value
