1、BRITISH STANDARD BS EN 13654-2:2001 Incorporating Corrigendum No. 1 Soil improvers and growing media Determination of nitrogen Part 2: Dumas method The European Standard EN 13654-2:2001 has the status of a British Standard ICS 65.080 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT
2、 LAWBS EN 13654-2:2001 This 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 5 December 2001 ISBN 0 580 38265
3、 6 National foreword This British Standard is the official English language version of EN 13654-2:2001. 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 c
4、ommittee can be obtained on 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 b
5、y using the “Find” facility 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 imm
6、unity 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 international and European developments and promulgate them in the UK. S
7、ummary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 8, 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 Comme
8、nts 13602 Corr. No. 1 5 December 2001 Corrects the header on the EN contents and EN foreword pages.EUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN136542 September2001 ICS65.080 Englishversion SoilimproversandgrowingmediaDeterminationofnitrogen Part2:Dumasmethod Amendementsdusoletsupportsdeculture
9、DterminationdelazotePartie2:MthodedeDumas BodenverbesserungsmittelundKultursubstrate BestimmungvonStickstoffTeil2:VerfahrennachDumas ThisEuropeanStandardwasapprovedbyCENon11August2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an St
10、andardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebyt
11、ra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,P
12、ortugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN136542:2
13、001EEN 13654-2:2001 (E) 2 Contents page Foreword. 3 1 Scope . 4 2 Normative references. 4 3 Terms and definitions 4 4 Principle. 4 5 Reagents 4 6 Apparatus 5 7 Test sample . 5 8 Procedure 5 9 Calculation 5 10 Expression of results . 6 11 Precision 6 12 Test Report 6 Annex A (informative) Results of
14、an interlaboratory trial to determine nitrogen (Dumas method)7 Bibliography. 8EN 13654-2:2001 (E) 3 Foreword This European Standard has been prepared by Technical Committee CEN/TC 223 “Soil improvers and growing media“, the secretariat of which is held by BSI. This European Standard shall be given t
15、he status of a national standard, either by publication of an identical text or by endorsement, at the latest by March 2002, and conflicting national standards shall be withdrawn at the latest by March 2002. Annex A is informative. According to the CEN/CENELEC Internal Regulations, the national stan
16、dards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom.EN136542:20
17、01(E) 4 SAFETYPRECAUTIONSCareshouldbetakenwhenhandlingsamplesthatmaycontain sharpsorisofadustynature. 1Scope ThisEuropeanStandardspecifiesamethodforthedeterminationofnitrogeninsoilimproversand growingmedia.ThedrycombustionmethodwasdevelopedoriginallyasamanualmethodbyDumas 5.Itsapplicationisimprovedg
18、reatlyduetotheuseofmodernautomatedequipmentandis applicabletoallformsofnitrogen. Themethodisnotapplicabletolimingmaterialsandpreformedmaterialssuchasmineralwoolslabs andfoamslabs. NOTE Therequirementsofthestandardmaydifferfromthenationallegalrequirementsforthedeclarationof theproductsconcerned. 2 No
19、rmativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromother publications.Thesenormativereferencesarecitedattheappropriateplacesinthetext,andthe publicationsarelistedhereafter.Fordatedreferences,subsequentamendmentstoorrevisionsofany ofthesepublicationsapplytothisE
20、uropeanStandardonlywhenincorporatedinitbyamendmentor revision.Forundatedreferences,thelatesteditionofthepublicationreferredtoapplies(including amendments). EN13040:1999, SoilimproversandgrowingmediaSamplepreparationforchemicalandphysical test,determinationofdrymattercontent,moisturecontentandlaborat
21、orycompactedbulkdensity. EN136541, SoilimproversandgrowingmediaDeterminationofnitrogenPart1:ModifiedKjeldahl method. 3 Termsanddefinitions ForthepurposesofthisstandardthetermsanddefinitionsgiveninEN13040apply. 4Principle Thenitrogencontentofthesample,pretreatedaccordingtoEN13040,isdeterminedbyheatin
22、gtoa temperatureofatleast900 Cinthepresenceofoxygengas.Mineralandorganicnitrogen compoundsareoxidizedand/orvolatilizedanddeterminedasdescribedbythemanufacturer. 5Reagents 5.1General Useonlyreagentsofrecognizedanalyticalgrade. 5.2 Forreduction,oxidation,removaland/orfixingofcombustiongases thatinterf
23、erewiththe analysis,refertothemanufacturersinstructions. 5.3 Calibrationsubstances,puresubstancesofknownnitrogencontent,forexampleacetanilide (C 8 H 9 NO),Lasparticacid(C 4 H 7 NO 4 ),oraminoacidsofknowncomposition. NOTE Thetotalcontentofnitrogenofthecalibrationsubstanceshouldbeassimilartothesamplen
24、itrogen contentaspossible.EN136542:2001(E) 5 6Apparatus Usuallaboratoryapparatus,andinparticularthefollowing: 6.1 Analyticalbalance, capableofweighingaccuratelyto1,0mg. 6.2 Dumasapparatus, usedtodeterminethetotalnitrogencontentbycombustionofthesampleat atemperatureofatleast900 C,includingadetectorfo
25、rmeasuringthenitrogengasformed.Consult themanufacturersmanualforthesettingupanduseoftheapparatus. 6.3 Containers,ofvarioussizeasapplicabletotheinstrument. 7 Testsample PreparethetestsampleinaccordancewithEN13040:1999,clause9. LossesofnitrogencanoccurwithsamplesofhighammoniumNcontentinalkalinesituati
26、onsand particularlywhenthesesamplesaredried.Ifthesampleasreceivedcontains(orissuspectedto contain)500mg/lNH 4 N,asdeterminedbyEN136512orEN136523,analyzethefresh materialusingthemethoddescribedinEN136541. 8Procedure 8.1 Calibrationoftheapparatus Calibratetheapparatusasdescribedinthemanufacturersmanua
27、l.Forthepurposeofcalibrationor establishingacalibrationscale,useoneofthesubstancesgivenin( 5.3). 8.2 Determinationofthenitrogencontent Theamountoftestsampleforanalysisdependsontheexpectedcontentofnitrogenandonthe samplecapacityoftheapparatusbeingused.Weighout m 1 gofthedriedgroundsampleorsub samplei
28、ntoacontainer( 6.3).Carryouttheanalysesinaccordancewiththemanufacturersmanual. NormallytheprimaryresultsaregivenasmgN (X 1 )permassofairdrygroundtestsampleused( m 1 ). 8.3 Residualmoisture Themoistureintheanalyzedsample( 8.2)isdeterminedinaccordancewithEN13040:1999,clause 10,using10gofthedriedsample
29、obtainedfromEN13040:1999,clause9. NOTE Poreswithinthetestsamplearefilledwithair,andtherefore,withnitrogengas.Nitrogengascan alsoenterthecombustioncellwhenitisopenedforsampleexchange.Bothfactscanleadtoanoverestimation ofthetotalNcontentofsoilimproversorgrowingmediumiftherehasbeeninsufficientpurgingby
30、gasbeforethe combustionstep. 8.4 Laboratorycompactedbulkdensity DeterminethelaboratorycompactedbulkdensityinaccordancewithEN13040:1999,annexA. 9 Calculation Thenitrogencontent( w n )inmilligramspergramdrymatterbasis,iscalculatedusingtheformula:EN136542:2001(E) 6 1 1 m X w n where: w n isthecontentof
31、nitrogeninmilligramspergramofdriedgroundtestsample; X 1 istheprimaryresultinmgnitrogen; m 1 isthemass,ingrams,ofdriedgroundtestsampleusedforanalysis. 10 Expressionofresults Reportallresultsonamass/massbasiscalculatedtoadrymatterbasis. 11 Precision Therepeatabilityandreproducibilityofthenitrogenconte
32、ntinseparatelypreparedsamplesshouldbe inaccordancewithTableA.1. Asummaryoftheresultsofaninterlaboratorytrialtodeterminetheprecisionofthemethod,in accordancewithISO57251,isgiveninannexA. NOTE Thevaluesderivedfromthisinterlaboratorytrialmaynotbeapplicabletoconcentrationsand matricesotherthanthoseteste
33、d. 12 TestReport Thetestreportcanbepreparedseparatelyorinconjunctionwiththetestreportofthesubsequent analyticalmethod. Thetestreportshallincludethefollowinginformation: a)areferencetotheEuropeanStandard; b)acompleteidentificationofthesample; c)alltheanalyticalmethodsused; d)astatementwhethergroundor
34、ungroundsamplehasbeenused; e)theresultsofthedeterminationexpressedasmass/massondrymatterbasis; f)thelaboratorycompactedbulkdensity; g)moisturecontent; h)anydetailsnotspecifiedintheEuropeanStandard,orwhichareoptional,aswellasanyother factor,whichmayhaveaffectedtheresults.EN136542:2001(E) 7 AnnexA (in
35、formative) Resultsofaninterlaboratorytrialtodeterminenitrogen(Dumasmethod) Aninterlaboratorytrialwasorganizedin1997undertheauspicesoftheEuropeanCommitteeforStandardization,totestthepr oceduresspecifiedinthisEuropeanStandard. InthistrialthenumberoflaboratoriesgiveninTableA.1determinedthenitrogenconte
36、ntusingtheDumasmethodinsixsampl etypes. Allresultsarereportedonadrymatterbasis. TableA.1 Asummaryoftheresultsoftheinterlaboratorytrialforthedeterminationofnitrogen(Dumasmethod) Sample No.oflabs after No.of outliers mean value Repeatability Repeatability Repeatability limit Reproducibility Reproducib
37、ility Reproducibility limit eliminating outliers (labs) mg/g s r StdDev% r=2,8 s r s R StdDev% R=2,8 s R Composted bark 10 1 19,5 0,45 6,50 1,27 1,32 18,91 3,68 Biowaste 12 0 13,21 0,36 7,70 1,02 1,10 23,40 3,09 Claypeat (fertilized) 11 1 9,2 0,25 7,67 0,71 0,63 19,21 1,78 Coarsepeat (fertilized) 11
38、 1 10,7 0,25 6,56 0,70 1,69 44,15 4,72 Composted sludge 15 1 29,90 0,96 8,97 2,68 2,97 27,77 8,30 Composted woodfibre 12 0 12,07 0,37 8,54 1,03 1,72 39,86 4,81EN136542:2001(E) 8 Bibliography 1 ISO5725:1994, Accuracy(truenessandprecision)ofmeasurementmethodsandresults. 2 EN13651, Soilimproversandgrow
39、ingmediaExtractionofcalciumchloride/DTPA(CAT)solublenutrients andelements. 3 EN13652, SoilimproversandgrowingmediaExtractionofwatersolublenutrientsandelements. 4 Dumas,J.B.A.(1831),Procdsdelanalyseorganique.Ann.Chim.Phys.247 , 198213.blankBS EN 13654-2:2001 BSI 389 Chiswick High Road London W4 4AL B
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