EN 13654 2 2001 64 e stf 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[.]
BRITISH STANDARD BS EN 13654-2:2001 Incorporating Corrigendum No 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 LAW BS EN 13654-2:2001 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: — 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 A list of organizations represented on this committee 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 by 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 immunity from legal obligations 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 Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 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 © BSI December 2001 ISBN 580 38265 Amd No Date Comments 13602 Corr No December 2001 Corrects the header on the EN contents and EN foreword pages EN 13654-2 EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM September 2001 ICS 65.080 English version Soil improvers and growing media - Determination of nitrogen Part 2: Dumas method Amendements du sol et supports de culture Détermination de l'azote - Partie 2: Méthode de Dumas Bodenverbesserungsmittel und Kultursubstrate Bestimmung von Stickstoff - Teil 2: Verfahren nach Dumas This European Standard was approved by CEN on 11 August 2001 CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Management Centre or to any CEN member This European Standard exists in three official versions (English, French, German) A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG Management Centre: rue de Stassart, 36 © 2001 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members B-1050 Brussels Ref No EN 13654-2:2001 E EN 13654-2:2001 (E) Contents page Foreword Scope Normative references Terms and definitions 4 Principle Reagents Apparatus Test sample Procedure Calculation 10 Expression of results 11 Precision 12 Test Report Annex A (informative) Results of an interlaboratory trial to determine nitrogen (Dumas method)7 Bibliography EN 13654-2:2001 (E) 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 the 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 standards 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 EN 13654-2:2001 (E) SAFETY PRECAUTIONS — Care should be taken when handling samples that may contain sharps or is of a dusty nature Scope This European Standard specifies a method for the determination of nitrogen in soil improvers and growing media The dry combustion method was developed originally as a manual method by Dumas [5] Its application is improved greatly due to the use of modern automated equipment and is applicable to all forms of nitrogen The method is not applicable to liming materials and preformed materials such as mineral wool slabs and foam slabs NOTE The requirements of the standard may differ from the national legal requirements for the declaration of the products concerned Normative references This European Standard incorporates by dated or undated reference, provisions from other publications These normative references are cited at the appropriate places in the text, and the publications are listed hereafter For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision For undated references, the latest edition of the publication referred to applies (including amendments) EN 13040:1999, Soil improvers and growing media - Sample preparation for chemical and physical test, determination of dry matter content, moisture content and laboratory compacted bulk density EN 13654-1, Soil improvers and growing media - Determination of nitrogen – Part 1: Modified Kjeldahl method Terms and definitions For the purposes of this standard the terms and definitions given in EN 13040 apply Principle The nitrogen content of the sample, pre-treated according to EN 13040, is determined by heating to a temperature of at least 900 C in the presence of oxygen gas Mineral and organic nitrogen compounds are oxidized and/or volatilized and determined as described by the manufacturer Reagents 5.1 General Use only reagents of recognized analytical grade 5.2 For reduction, oxidation, removal and/or fixing of combustion gases that interfere with the analysis, refer to the manufacturer’s instructions 5.3 Calibration substances, pure substances of known nitrogen content, for example acetanilide (C8H9NO), L-aspartic acid (C4H7NO4), or amino acids of known composition NOTE The total content of nitrogen of the calibration substance should be as similar to the sample nitrogen content as possible EN 13654-2:2001 (E) Apparatus Usual laboratory apparatus, and in particular the following : 6.1 Analytical balance, capable of weighing accurately to 1,0 mg 6.2 Dumas apparatus, used to determine the total nitrogen content by combustion of the sample at a temperature of at least 900 C, including a detector for measuring the nitrogen gas formed Consult the manufacturer’s manual for the setting up and use of the apparatus 6.3 Containers, of various size as applicable to the instrument Test sample Prepare the test sample in accordance with EN 13040:1999, clause Losses of nitrogen can occur with samples of high ammonium-N content in alkaline situations and particularly when these samples are dried If the sample as received contains (or is suspected to contain) > 500 mg/l NH4 –N, as determined by EN 13651 [2] or EN 13652 [3], analyze the fresh material using the method described in EN 13654-1 Procedure 8.1 Calibration of the apparatus Calibrate the apparatus as described in the manufacturer’s manual For the purpose of calibration or establishing a calibration scale, use one of the substances given in (5.3) 8.2 Determination of the nitrogen content The amount of test sample for analysis depends on the expected content of nitrogen and on the sample capacity of the apparatus being used Weigh out m1 g of the dried ground sample or subsample into a container (6.3) Carry out the analyses in accordance with the manufacturer's manual Normally the primary results are given as mg N (X1) per mass of air dry ground test sample used (m1) 8.3 Residual moisture The moisture in the analyzed sample (8.2) is determined in accordance with EN 13040:1999, clause 10, using 10 g of the dried sample obtained from EN 13040:1999, clause NOTE Pores within the test sample are filled with air, and therefore, with nitrogen gas Nitrogen gas can also enter the combustion cell when it is opened for sample exchange Both facts can lead to an overestimation of the total N content of soil improvers or growing medium if there has been insufficient purging by gas before the combustion step 8.4 Laboratory compacted bulk density Determine the laboratory compacted bulk density in accordance with EN 13040:1999, annex A Calculation The nitrogen content (wn) in milligrams per gram dry matter basis, is calculated using the formula: EN 13654-2:2001 (E) X wn m1 where: wn is the content of nitrogen in milligrams per gram of dried ground test sample; X1 is the primary result in mg nitrogen; m1 is the mass, in grams, of dried ground test sample used for analysis 10 Expression of results Report all results on a mass/mass basis calculated to a dry matter basis 11 Precision The repeatability and reproducibility of the nitrogen content in separately prepared samples should be in accordance with Table A.1 A summary of the results of an interlaboratory trial to determine the precision of the method, in accordance with ISO 5725 [1], is given in annex A NOTE The values derived from this interlaboratory trial may not be applicable to concentrations and matrices other than those tested 12 Test Report The test report can be prepared separately or in conjunction with the test report of the subsequent analytical method The test report shall include the following information: a) a reference to the European Standard; b) a complete identification of the sample; c) all the analytical methods used; d) a statement whether ground or un-ground sample has been used; e) the results of the determination expressed as mass/mass on dry matter basis; f) the laboratory compacted bulk density; g) moisture content; h) any details not specified in the European Standard, or which are optional, as well as any other factor, which may have affected the results EN 13654-2:2001 (E) Annex A (informative) Results of an interlaboratory trial to determine nitrogen (Dumas method) An interlaboratory trial was organized in 1997 under the auspices of the European Committee for Standardization, to test the procedures specified in this European Standard In this trial the number of laboratories given in Table A.1 determined the nitrogen content using the Dumas method in six sample types All results are reported on a dry matter basis Table A.1 - A summary of the results of the interlaboratory trial for the determination of nitrogen (Dumas method) Sample No of labs No of after outliers eliminating (labs) outliers Composted 10 bark Biowaste 12 Clay peat 11 (fertilized) Coarse peat 11 (fertilized) Composted 15 sludge Composted 12 wood fibre mean value mg/g Repeatability Reproducibility Reproducibility sR Std Dev % Reproducibility limit R = 2,8 sR 19,5 0,45 6,50 1,27 1,32 18,91 3,68 13,21 9,2 0,36 0,25 7,70 7,67 1,02 0,71 1,10 0,63 23,40 19,21 3,09 1,78 10,7 0,25 6,56 0,70 1,69 44,15 4,72 29,90 0,96 8,97 2,68 2,97 27,77 8,30 12,07 0,37 8,54 1,03 1,72 39,86 4,81 sr Repeatability Repeatability limit r = 2,8 sr Std Dev % EN 13654-2:2001 (E) Bibliography [1] ISO 5725:1994, Accuracy (trueness and precision) of measurement methods and results [2] EN 13651, Soil improvers and growing media - Extraction of calcium chloride/DTPA (CAT) soluble nutrients and elements [3] EN 13652, Soil improvers and growing media - Extraction of water soluble nutrients and elements [4] Dumas, J.B.A (1831), Procédés de l’analyse organique Ann Chim Phys 247, 198-213 blank BS EN 13654-2:2001 BSI — British Standards Institution BSI is the independent national body responsible for preparing British Standards It presents the UK view on standards in Europe and at the international level It is incorporated by Royal Charter Revisions British 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