1、BRITISH STANDARD BS EN 13651:2001 Soil improvers and growing media Extraction of calcium chloride/DTPA (CAT) soluble nutrients The European Standard EN 13651:2001 has the status of a British Standard ICS 65.080 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN 13651:2001 Th
2、is British 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 38266 4 National foreword Thi
3、s British Standard is the official English language version of EN 13651:2001. 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 o
4、n request 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” facilit
5、y of the 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 obligatio
6、ns. aid enquirers 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 docum
7、ent comprises a front cover, an inside front cover, the EN title page, pages 2 to 16, an inside back cover 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 NORME
8、EUROPENNE EUROPISCHENORM EN13651 September2001 ICS65.080 Englishversion SoilimproversandgrowingmediaExtractionofcalcium chloride/DTPA(CAT)solublenutrients AmendementsdusoletsupportsdecultureExtraction deslmentsnutritifssolublesdanslechlorurede calcium/DTPA(CAT) BodenverbesserungsmittelundKultursubst
9、rateExtraktion voninCalciumchlorid/DTPA(CAT)lslichenNhrstoffen ThisEuropeanStandardwasapprovedbyCENon11August2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsan
10、dbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnot
11、ifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFOR
12、STANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN13651:2001EEN13651:2001(E) 2 Contents page Foreword . 3 1 Scope 4 2 Normativer
13、eferences 4 3 Termsanddefinitions . 4 4 Principle . 4 5 Reagents 4 6 Apparatus. 5 7 Testsample. . 5 8 Procedure. 6 9 Determinationoftheextractednutrientsandelements. . 6 10 Expressionofresults 6 11 Precision 6 12 Testreport 7 AnnexA (informative) Resultsofaninterlaboratorytrialtodeterminecalciumchlo
14、ride/DTPA (CAT)solublenutrientsandelements. 8 AnnexB (informative) Methodsofanalysisusedintheinterlaboratorytrial. 15 Bibliography 16EN13651:2001(E) 3 Foreword ThisEuropeanStandardhasbeenpreparedbyTechnicalCommitteeCEN/TC223“Soilimproversand growingmedia“,thesecretariatofwhichisheldbyBSI. ThisEurope
15、anStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidentical textorbyendorsement,atthelatestbyMarch2002,andconflictingnationalstandardsshallbewithdrawnat thelatestbyMarch2002. TheannexesAandBareinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorgan
16、izationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark, Finland,France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal, Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN13651:2001(E) 4 SAFETYPRECAUTIONSCareshouldbetakenw
17、henhandlingsamplesthatmaycontainsharps orisofadustynature . 1Scope ThisEuropeanStandardspecifiesanextractionmethodfortheroutinedeterminationofcalcium chloride/DTPA(CATmethod)extractablenutrientsandelements(aslistedinannexB)insoilimprovers orgrowingmedia. Themethodisnotapplicabletolimingmaterialsandp
18、reformedmaterialssuchasmineralwoolslabs andfoamslabs. NOTE Therequirementsofthestandardmaydifferfromthenationallegalrequirementsforthedeclarationofthe productsconcerned. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications. Thesenormativeref
19、erencesarecitedattheappropriateplacesinthetext,andthepublicationsarelisted hereafter.Fordatedreferences,subsequentamendmentstoorrevisionsofanyofthesepublications applytothisEuropeanStandardonlywhenincorporatedinitbyamendmentorrevision.Forundated referencesthelatesteditionofthepublicationreferredtoap
20、plies(includingamendments). ENISO3696, WaterforanalyticallaboratoryuseSpecificationandtestmethods (ISO3696:1987). EN13040:1999,SoilimproversandgrowingmediaSamplepreparationforchemicalandphysical tests,determinationofdrymattercontent,moisturecontentandlaboratorycompactedbulkdensity. 3 Termsanddefinit
21、ions ForthepurposesofthisstandardthetermsanddefinitionsgiveninEN13040apply. 4 Principle Asampleisextractedwithcalciumchloride/DTPAat22 C 3 Cinanextractionvolumeratioof1+5. Theextractednutrientsaredeterminedbyvariousmethodsasappropriate(seeannexB). 5Reagents 5.1General Allreagentsusedshallbeofrecogni
22、sedanalyticalqualityandwaterofgrade2accordingtoENISO 3696. 5.2 Dihydratedcalciumchloride, CaCl 2 .2H 2 O. 5.3 Diethylenetriaminepentaaceticacid(DTPA), C 14 H 23 N 3 O 10. 5.4 ConcentratedextractingsolutionCaCl 2 /DTPA,(CAT),dissolve14,7gCaCl 2 .2H 2 O(5.2)and 7,88gDTPA( 5.3)in800mlhotwater(temperatu
23、reapproximately80 C)withstirringonamagnetic stirrerina1000mlbeaker.At75 C 10 Cthereagentswilldissolvewithin2h.Allowtocoolto ambienttemperature.Transferthesolutiontoa1000mlflaskanddilutetothemarkwithwater.TheEN13651:2001(E) 5 solutionisstableatroomtemperatureforseveralweeks.Anyprecipitationthatoccurs
24、willdisappearwith warmingandstirring. 5.5 ExtractingsolutionCaCl 2 /DTPA,(CAT),dilutetheconcentratedextractingsolution(5.4)with waterintheproportionsonepartconcentratedsolutionwithninepartswater.Thefinalconcentrationof theextractingsolutionshouldbe0,01mol/lCaCl 2 and0,002mol/lDTPA.ThepHoftheextracti
25、ng solutionshouldbeadjustedifnecessarytobebetween2,6and2,65. 5.6 Nitricacid, c(HNO 3 )=15mol/l: 1,42g/ml;notlessthan65%mass/volume. 5.7 Nitricacid, c(HNO 3 )=0,5mol/l,dilute35mlnitricacid( 5.6)toonelitrewithwater. 6Apparatus 6.1 General NOTE Ithasbeenfoundconvenienttokeepseparatesetsofglasswareforth
26、edeterminationsgiveninannexB, inordertoreducethepossibilityofwithinlaboratorycontamination. Allglassapparatusandplasticvesselsusedintheprocedureshouldbesubjecttoanappropriate preparationprocedureinordertokeeptheriskofcontaminationaslowaspossible.Itisrecommended thatallvessels(glassandplastic)areclea
27、nsedbycarefullyimmersinginwarmnitricacid( 5.6)fora minimumof6handthenrinsedinwater. Rubberstoppers,whichmaycontaintracesofmetalsshallnotbeused.Itisrecommendedtouseplastic oranyotherstopperfreeofallsubstancestobeanalyzed. Borosilicateglasswareshallnotbeusedifboronistobedetermined. Theapparatusconsist
28、softheusuallaboratoryapparatus,andinparticularthefollowing: 6.2 Plasticbottlesorcontainers, sufficientlylarge(500mlto1500ml)withscrewcaptoaccommodate thevolumeofthesample,extractantandatleast10%airvolume. 6.3 Shakingormixingmachine, capableofholdingtheplasticbottlesorcontainers( 6.2)and maintainingt
29、hesampleinsuspensionwithoutdamagingthestructureofthesample.Theuseofa horizontaltableshakerisrecommended. 6.4 Filterpaper,cellulosebasedashlesstypes,withamediumporesizeofapproximately8 mand diameterof150mm. NOTE Centrifugationisanacceptablealternative. 6.5 Analyticalbalance withanaccuracyof10mg. 7 Te
30、stsample PreparethelaboratorysampleinaccordancewithEN13040:1999,clause8,anddeterminethe laboratorycompactedbulkdensityofthesampleinaccordancewithEN13040:1999,annexA.EN13651:2001(E) 6 8Procedure 8.1 Extraction 8.1.1Testsamplespassingthrougha20mmsieve Takeaweightequivalentto60mlofthesamplevolume(EN130
31、40:1999,clause8.5)tothenearest1g andtransfertothecontainer( 6.2).Add300mlofextractingsolution( 5.5),securethecapandshakefor 1hontheshakingmachine( 6.3) at22 C 3 C. 8.1.2Testsamplespassingthrougha40mmsieve Takeaweightequivalentto250mlofthesamplevolume(EN13040:1999,clause8.3)tothenearest1g andtransfer
32、tothecontainer( 6.2).Add1250mlofextractingsolution( 5.5),securethecapandshakefor 1hontheshakingmachine( 6.3) at22 C 3 C. 8.1.3Filtration Filterthroughfilterpaper( 6.4)discardingatleastthefirst10ml.Insomecasespaperfiltrationistooslow orevenimpossible.Insuchcasesalternativeproceduresforobtainingaclear
33、supernatantareacceptable andthetechniqueusedshallbereported.Thefilteredextractisstableforthreedaysinahermetically closedpolyethylenebottleifstoredinarefrigeratorat0 Cto5 C.Thefiltratecanbestoredforlonger periodsinadeepfreezeratabout 18 C. NOTE Beforeusingasolutionthathasbeenfrozen,thethawedsolutions
34、hallbethoroughlymixedtoeliminate gradientseparationthatoccursonfreezingandsubsequentthawing. 8.2 Blank Thereagentblanktestshallbecarriedoutinparallelwiththedetermination,bythesameprocedureas outlinedin 8.1.1or8.1.2and 8.1.3,usingthesamequantitiesofallthereagentsasinthedetermination butomittingthetes
35、tportion. NOTE Themeasurementofablankisintroducedtodeterminethecontributionoftheextractingsolution, glasswareandfilterpaperused. 9 Determinationoftheextractednutrientsandelements SeeannexB. 10 Expressionofresults Subtractthevaluesdeterminedforthereagentblankfromthoseobtainedforthesamples.Allresults
36、shallbecalculatedusingthedeterminedcompactedlaboratorybulkdensityandexpressedinmg/l substrateasreceivedbasis. 11Precision TherepeatabilityandreproducibilityofthecalciumchlorideDTPAsolublenutrientcontentinseparately preparedsamplesshouldbeinaccordancewithTablesA.1toA.6. Asummaryoftheresultsofaninterl
37、aboratorytrialtodeterminetheprecisionofthemethod,in accordancewithISO57252,isgiveninannexA. NOTE Thevaluesderivedfromthisinterlaboratorytrialmaynotbeapplicabletoconcentrationsandmatrices otherthanthosetested.EN13651:2001(E) 7 12 Testreport Thetestreportshallcontainthefollowinginformation: a)areferen
38、cetothisEuropeanStandard; b)allinformationnecessaryforcompleteidentificationofthesample; c)alltheanalyticalmethodsused; d)theresultsofthedetermination,expressedasmg/lfreshsample; e)detailsofanyoperationsnotspecifiedintheEuropeanStandardor regardedasoptional,aswellasanyfactorwhichmayhaveaffectedthere
39、sults; f)thelaboratorycompactedbulkdensityresult.EN13651:2001(E) 8 AnnexA (informative) Resultsofaninterlaboratorytrialtodeterminecalciumchloride/DTPA (CAT)solublenutrientsandelements Aninterlaboratorytrialwasorganizedin1997undertheauspicesoftheEuropeanCommitteefor Standardization,totesttheprocedure
40、sspecifiedinthisEuropeanStandard. InthistrialthenumberoflaboratoriesgivenintheTablesA.1toA.6determinedthecalciumchloride/DTPA solublenutrientandelementscontentinsixsampletypes. Allresultsarereportedonafreshbasis.EN13651:2001(E) 9 Asummaryoftheresultsoftheinterlaboratorytrialforthedeterminationofcalc
41、iumchloride/DTPA(CAT)solublenutrientsan delementsinsixsampletypes isgiveninTablesA.1toA.6. TableA.1Compostedbark Element No.oflabs after eliminating outliers No.of outliers (labs) Mean value mg/l Repeatability s r Repeatability StdDev% Repeatability limit r=2,8 s r Reproducibility s R Reproducibilit
42、y StdDev% Reproducibilitylimit R=2,8s R NH 4 N 19 0 1220,1 49,19 11,29 137,72 248,52 57,03 695,87 NO 3 N 13 2 13,6 2,27 46,65 6,35 13,96 287,18 39,08 P 20 0 290,0 14,59 14,09 40,85 108,99 105,22 305,17 K 21 0 2727,0 71,12 7,30 199,13 401,48 41,22 1124,15 Mg 20 1 170,4 7,33 12,05 20,52 57,22 94,04 16
43、0,21 SO 4 S 13 0 100,7 8,93 24,82 24,99 47,53 132,15 133,09 Na 19 0 389,7 7,83 5,63 21,93 59,44 42,71 166,42 B 13 0 1,8 0,09 14,14 0,25 0,74 117,42 2,06 Cu 18 1 1,1 0,08 20,68 0,23 0,25 63,39 0,70 Fe 17 2 14,0 0,92 18,48 2,58 2,31 46,28 6,47 Mn 18 1 10,7 0,48 12,72 1,36 1,78 46,79 4,99 Mo 9 1 0,1 0,
44、02 43,46 0,06 0,04 88,68 0,11 Zn 18 1 15,3 0,69 12,60 1,93 2,94 53,79 8,23 Cd 7 1 0,02 0,00 46,84 0,01 0,01 182,32 0,04 Pb 9 1 0,25 0,03 35,29 0,09 0,17 188,29 0,47 Element No.oflabs after eliminating outliers No.of outliers (labs) Mean value g/l Repeatability s r Repeatability StdDev% Repeatability limit r=2,8 s r Reproducibility s R Reproducibility StdDev% Reproducibilitylimit R=2,
