BS EN 13266-2002 Slow-release fertilizers - Determination of the release of the nutrients - Method for coated fertilizers《缓慢释放化肥 用涂层肥料法测定营养释放性能》.pdf

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