1、BR I T I S H S TA N DA RD BS EN 13 26 6:2 00 1 Slow-release fertilizers Determination of the release of the nutrients Method for coated fertilizers T h e Eu ropean Stan dard EN 1 3266: 2001 ha s t he statu s of a B ritis h S tan dard ICS 65.08 0 BS EN 13266:2001 This British Standard, having been pr
2、epared under the direction of the Materials and Chemicals Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 15 August 2002 BSI 15 August 2002 ISBN 0 580 40277 0 National foreword This British Standard is the official English lan
3、guage version of EN 13266:2001. The UK participation in its preparation was entrusted to Technical Committee CII/37, Fertilizers and related chemicals, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Additional infor
4、mation The United kingdom voted against the acceptance of this standard at the Formal Vote stage. The principle UK objections were as follows: a) Criteria for the release conditions of slow release fertilizers are specified in the normative Annex A. This is outside of the scope of this test method.
5、b) The “stated release time” is defined, in 3.4, as a property determined by the test method, when it should be the time stated by the manufacturer. c) Clause 9 gives requirements for the precision of the test method described in the standard. The UK deemed the precision of the main method in 9 to b
6、e poor and that an “accelerated test” would be even less reliable. d) There are no details or references to the standard analytical methods for the determination of nutrient concentration as required in 7.3, 7.4 and B.3.3. e) Clause 7 describes the procedure for the determination of the release of t
7、he nutrients. 7.2 describes the time intervals at which to determine the nutrient content of the fertilizer. The example of the time intervals is given in 7.2 for a slow release fertilizer intended to release nutrients over eight months. It is deemed that the time intervals need to be spread beyond
8、the expected “longevity” in order that a more accurate value of nutrient content can be determined. f) The apparatus for controlling the temperature of the water, described in 5.4, could be further defined. g) A description of the “sensor system”, referred to in B.2.1.7 for use in the accelerated te
9、st of Annex B, is not provided. h) B.3.3 refers to the measurement of electrical conductivity, however no method is provided Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section
10、entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standard Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for their correct application. Comp
11、liance with a British Standard does not of itself confer immunity from legal obligations. 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 internationa
12、l and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 12, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last is
13、sued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN13266 October2001 ICS65.080 Englishversion SlowreleasefertilizersDeterminationofthereleaseofthe nutrientsMethodforcoatedfertilizers EngraislibrationlenteDterminationdumodede librationdesl
14、mentsnutritifsMthodeapplicableaux engraisenrobs LangsamfreisetzendeDngemittelBestimmungder FreisetzungsratevonNhrstoffenVerfahrenfrumhllte Dngemittel ThisEuropeanStandardwasapprovedbyCENon29September2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgi
15、vingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninany
16、otherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,
17、Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMember
18、s. Ref.No.EN13266:2001EEN13266:2001(E) 2 Contents page Foreword3 1 Scope 4 2 Normativereferences 4 3 Termsanddefinitions. .4 4 Principle4 5 Apparatus .5 6 Sampling.5 7 Procedure .5 8 Expressionofresults . .6 9 Precision.7 10 Testreport 8 AnnexA (normative) Criteriaforreleaseconditions .9 AnnexB (inf
19、ormative) Acceleratedtestmethodsbasedonaelevatedtemperature.10 Bibliography 12EN13266:2001(E) 3 Foreword ThisEuropeanStandardhasbeenpreparedbyTechnicalCommitteeCEN /TC 260,“Fertilizersandliming materials“,thesecretariatofwhichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,
20、eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyApril2002,andconflictingnationalstandardsshallbewithdrawnatthelatestby April2002. AnnexAisnormativeandannexBisinformative. ThisstandardincludesaBibliography. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizatio
21、nsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden, SwitzerlandandtheUnitedKingdom.EN13266:2001(E) 4 1Scope ThisEuropeanStandardspecifiesameth
22、odforthedeterminationoftheslowreleasepropertiesofnutrientsfrom coatedfertilizers.pHdependenthydrolysisanddegradationbybiologicalormicrobialmechanismsareexcluded. Thespecifiedmethodisonlyapplicabletoproductsreleasinganynutrientsbymeansofanonbiologicalprocess (i.e.thosewherethenutrientsarereleasedbyap
23、hysicalmechanism).Microbialattackonthecoating(e.g.sulfur coatedfertilizers)andtheconsequencesthereofarenotmeasurablebythetechniquedescribed. Thismethodinvolvesalengthyprocesswhichmaynotbeappropriatefordaytodaytestingpurposes.Accelerated methodsmaybeusedprovidedtheyarecorrelatedwiththisstandard.Anexa
24、mpleofsuchanacceleratedmethod isdescribedinannex B.Regressionanalysismayalsobeusedforthispurpose. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelist
25、edhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). EN1482, Samplingofsolidfertilizersandlimingm
26、aterials. ENISO3696 ,WaterforanalyticallaboratoryuseSpecificationandtestmethods(ISO3696:1987). 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thefollowingtermsanddefinitionsapply. 3.1 release transferofanutrientfromthefertilizertothereceivingmedium(water) 3.2 slowrelease releaseunderthed
27、efinedconditionsmeetingeachofthecriteriasetoutinannexA 3.3 initialreleaseofanutrient themassfractioninpercentofanutrientreleasedduringthefirst24hafterthestartofthetest 3.4 statedreleasetime timeperiodbetweenthestartofthetestandthereleaseofagivenminimumpercentageofthespecifiednutrient NOTE Thismayals
28、obereferredtoaslongevity.SeeannexA. 3.5 coatedfertilizer fertilizerthatisencapsulated,bycoveringitwithawaterinsolublematerial,inordertoreduceitsreleaseratein water 4Principle Elutionofatestportionofafertilizerwithaspecifiedvolumeofwater.Determinationoftheconcentrationofthe nutrient(s),thathavebeendi
29、ssolvedindefinedtimeintervals.EN13266:2001(E) 5 5Apparatus Ordinarylaboratoryapparatusand,inparticular,thefollowing: 5.1Glassbeakers, ofcapacity800ml,withalid 5.2Onemarkvolumetricflask, 500mlcapacity 5.3Magneticstirrer, withamagneticrodwithasizeof25mm,oranyothersuitablestirrer 5.4Temperaturecontrole
30、quipment, capableofmaintainingthemediumatthetemperatureof(25 0,5)C 6Sampling SamplingandsamplepreparationshallbecarriedoutinaccordancewithEN1482. Themethodofsamplingandofsamplepreparationshallbeindicatedinthetestreport.Takecaretoavoiddamage to,ordestructionof,thecoating. Donotcrushorgrindthesample.
31、7Procedure 7.1Preparationofthetestsolution Transfer500mlofwater,conformingtograde3ofENISO3696,intoabeaker(5.1).Weigh,tothenearest0,01g, (10 0,1)gofthefertilizer,addittothewaterinthebeakerandrecordthetime.Weighthebeakertogetherwithits contents:thesampleoffertilizer,waterandstirringrod.Notethetotalmas
32、stothenearest1g.Startthestirrer(5.3) atarotationalfrequencyofapproximately300min 1 .Coverthebeakerwithalidtoavoidevaporationofwaterand maintainthetemperatureat(25 0,5)Cwiththetemperaturecontrolequipment(5.4). Eachtimeitisdesiredtomakeanutrientdetermination(see7.2),decantthesolutionintoanotherbeaker(
33、5.1), takingcaretoavoidanyoftheundissolvedfertilizerbeingcarriedover.Refillthebeaker(5.1)withwater (conformingtograde 3ofEN ISO 3696)at25Csoastoachievethepreviouslyrecordedmass.Continue extractionimmediately. Continuetheextractionprocedureuntilmorethan75%ofthenominalquantityofwatersolublenutrientsha
34、sbeen leached. NOTE Themassratiooffertilizertestportiontowaterislimitedtoamaximumof2%toavoidconcentrationeffects 7.2Timeintervalsforperiodicdeterminationsofnutrientcontent Determinethenutrientcontentatabouttentimeintervalsuntilthestatedreleasetime(forreleasecondition3).The firstdeterminationshallbem
35、adeafter(24 0,25)h(forreleasecondition1),anotheroneshallbemadeatday28 fromthebeginningoftheelution(forreleasecondition2).Choosetheintervalsfortakingthesampleswithrespect totheamountsofleachednutrientconcentrationandtheirdetectionlimits(forslowreleasecriteria1,2,3see annexA). EXAMPLE Determinationint
36、ervalsforaslowreleasefertilizerintendedtoreleasenutrientsovereightmonths: 1) D 1 after24h(day1); 2) D 7 atday7afterstart,periodfromday1today7; 3) D 14 atday14,periodfromday7today14; 4) D 21 atday21,periodfromday14today21;EN13266:2001(E) 6 5) D 28 atday28(week4,1month),periodfromday21today28; 6) D 56
37、 atday56(week8,2months),periodfromday28today56; 7) D 84 atday84(week12,3months),periodfromday56today84; 8) D 112 atday112(week16,4months),periodfromday84today112; 9) D 168 atday168(week24,6months),periodfromday112today168; 10) D 224 atday224(week32,8months),periodfromday168today224. 7.3Determination
38、ofthenutrientcontent Takealiquotsasappropriatetodeterminetheconcentrationsofthenutrients,usingstandardanalyticalmethods, andcalculatethetotalextractedamountofnutrients. Notetheresultas“ D n +nutrientsymbol“foreachnutrientunderexamination. 7.4Determinationofthetotalwaterextractablenutrientcontent Tra
39、nsfer500mlofwater(conformingtograde3ofENISO3696)intoabeaker(5.1).Weigh,tothenearest0,01g, (10 0,1)gofthefertilizer,groundortreatedinsomeotherappropriatemannertodestroyanycoatingandaddit tothewaterinthebeaker.Startthestirrer(5.3)atarotationalfrequencyofapproximately300min 1 ,coverthe beakerwithalidto
40、avoidevaporationofwaterandmaintainthetemperatureat(25 0,5)Cwiththetemperature controlequipment(5.4)forabout24h.Takealiquotsasappropriatewithoutanyundissolvedparttodeterminethe concentrationsofthenutrientsextractedasdesired,usingstandardanalyticalmethods.Notetheresultas“ C + nutrientsymbol“foreachnut
41、rientunderexamination. 8 Expressionofresults Theinitialrelease,m 1 ,expressedasmassfractioninpercentoftotalwaterextractablenutrient(s)isgivenby equation(1). C D m 1 1 100 (1) Thelongevity d 75% ,expressedindays,isgivenbytheinterpolationequation(2): l h l l h l 75% 75 m m m d d d d (2) Thereleasedmas
42、sfractionwithin ndays, m n ,expressedasapercentage,isgivenbyequation(3). ) n 1 i ( i 100 n to C D m (3) where m n isthereleasedmassfractionwithin ndays; C isthetotalwaterextractablenutrientcontent(7.4),givenasmassfractioninpercent; D n isthenutrientcontentofthesampleatday n(releasedbetweenday n1andd
43、ay n); n isthenumberofdays;EN13266:2001(E) 7 d l isthedayuntillessthan75%ofnutrient(s)arereleased; d h isthedayuntilmorethan75%ofnutrient(s)arereleased; m l isthereleasedmassfractionuntil d l ; m h isthereleasedmassfractionuntil d h . 9Precision 9.1General Theprecisiondataofthismethodhasbeenestablis
44、hedbyaninternationalinterlaboratorytest(see ISO5725:1986 1) ). Inthistest,eightsamplesofdifferentorigin,nutrientcompositions,coatingandlongevitywereinvestigatedand slowreleasepropertiesweredeterminedbymeasurementoftheelectricalconductivityanddeterminationofthe nitrogencontentby11laboratoriesinsixcountries. Forthevaluesobtainedforrepeatabi
