Gödselmedel Bestämning av olika former av kväve i ett prov där kväve föreligger som nitrat, ammonium, urea och cyanamid

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1 SVENSK STANDARD SS-EN 15604:2009 Fastställd/Approved: Publicerad/Published: Utgåva/Edition: 1 Språk/Language: engelska/english ICS: Gödselmedel Bestämning av olika former av kväve i ett prov där kväve föreligger som nitrat, ammonium, urea och cyanamid Fertilizers Determination of different forms of nitrogen in the same sample, containing nitrogen as nitric, ammoniacal, urea and cyanamide nitrogen SWEDISH STANDARDS INSTITUTE

2 Hitta rätt produkt och ett leveranssätt som passar dig Standarder Genom att följa gällande standard både effektiviserar och säkrar du ditt arbete. Många standarder ingår dessutom ofta i paket. Tjänster Abonnemang är tjänsten där vi uppdaterar dig med aktuella standarder när förändringar sker på dem du valt att abonnera på. På så sätt är du säker på att du alltid arbetar efter rätt utgåva. e-nav är vår online-tjänst som ger dig och dina kollegor tillgång till standarder ni valt att abonnera på dygnet runt. Med e-nav kan samma standard användas av flera personer samtidigt. Leveranssätt Du väljer hur du vill ha dina standarder levererade. Vi kan erbjuda dig dem på papper och som pdf. Andra produkter Vi har böcker som underlättar arbetet att följa en standard. Med våra böcker får du ökad förståelse för hur standarder ska följas och vilka fördelar den ger dig i ditt arbete. Vi tar fram många egna publikationer och fungerar även som återförsäljare. Det gör att du hos oss kan hitta över 500 unika titlar. Vi har även tekniska rapporter, specifikationer och workshop agreement. Matriser är en översikt på standarder och handböcker som bör läsas tillsammans. De finns på sis.se och ger dig en bra bild över hur olika produkter hör ihop. Standardiseringsprojekt Du kan påverka innehållet i framtida standarder genom att delta i någon av SIS ca 400 Tekniska Kommittéer. Find the right product and the type of delivery that suits you Standards By complying with current standards, you can make your work more efficient and ensure reliability. Also, several of the standards are often supplied in packages. Services Subscription is the service that keeps you up to date with current standards when changes occur in the ones you have chosen to subscribe to. This ensures that you are always working with the right edition. e-nav is our online service that gives you and your colleagues access to the standards you subscribe to 24 hours a day. With e-nav, the same standards can be used by several people at once. Type of delivery You choose how you want your standards delivered. We can supply them both on paper and as PDF files. Other products We have books that facilitate standards compliance. They make it easier to understand how compliance works and how this benefits you in your operation. We produce many publications of our own, and also act as retailers. This means that we have more than 500 unique titles for you to choose from. We also have technical reports, specifications and workshop agreements. Matrices, listed at sis.se, provide an overview of which publications belong together. Standardisation project You can influence the content of future standards by taking part in one or other of SIS s 400 or so Technical Committees.

3 Europastandarden EN 15604:2009 gäller som svensk standard. Detta dokument innehåller den officiella engelska versionen av EN 15604:2009. The European Standard EN 15604:2009 has the status of a Swedish Standard. This document contains the official English version of EN 15604:2009. Copyright/Upphovsrätten till denna produkt tillhör SIS, Swedish Standards Institute, Stockholm, Sverige. Användningen av denna produkt regleras av slutanvändarlicensen som återfinns i denna produkt, se standardens sista sidor. Copyright SIS, Swedish Standards Institute, Stockholm, Sweden. All rights reserved. The use of this product is governed by!the end-user licence for this product. You will find the licence in the end of this document. Upplysningar om sakinnehållet i standarden lämnas av SIS, Swedish Standards Institute, telefon Standarder kan beställas hos SIS Förlag AB som även lämnar allmänna upplysningar om svensk och utländsk standard. Information about the content of the standard is available from the Swedish Standards Institute (SIS), tel Standards may be ordered from SIS Förlag AB, who can also provide general information about Swedish and foreign standards. SIS Förlag AB, SE Stockholm, Sweden. Tel: Fax: sis.sales@sis.se Internet:

5 EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN January 2009 ICS Supersedes CEN/TS 15604:2007 English Version Fertilizers - Determination of different forms of nitrogen in the same sample, containing nitrogen as nitric, ammoniacal, urea and cyanamide nitrogen Engrais - Détermination des différentes formes d'azote dans un même échantillon contenant l'azote sous forme nitrique, ammoniacale, uréique et cyanamidique Düngemittel - Bestimmung verschiedener, nebeneinander anwesender Stickstoff-Formen in derselben Probe mit Stickstoff in Form von Ammonium, Nitrat, Harnstoff und Cyanamid This European Standard was approved by CEN on 6 December 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 CEN 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 CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15604:2009: E

6 SS-EN 15604: :2009 (E) (E) Provläsningsexemplar / Preview Contents Page Foreword Scope Normative references Terms and definitions Principle Reagents Apparatus Sampling and sample preparation Procedure Verification of the result Test report Bibliography

7 SS-EN 15604:2009 (E) Foreword This document (EN 15604:2009) has been prepared by Technical Committee CEN/TC 260 Fertilizers and liming materials, the secretariat of which is held by DIN. 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 July 2009, and conflicting national standards shall be withdrawn at the latest by July Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. This document supersedes CEN/TS 15604:2007. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. 3

8 SS-EN 15604: :2009 (E) (E) Provläsningsexemplar / Preview 1 Scope This European Standard specifies a method for the determination of any one form of nitrogen in the presence of any other form. The method is applicable to any fertilizer provided for in Annex I of the Regulation (EC) No 2003/2003 [1] containing nitrogen in various forms. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN , Fertilizers and liming materials Sampling and sample preparation Part 2: Sample preparation EN :1999, Fertilizers and liming materials and soil improvers Vocabulary Part 1: General terms EN :1999, Fertilizers and liming materials and soil improvers Vocabulary Part 2: Terms relating to fertilizers EN 15475, Fertilizers Determination of ammoniacal nitrogen EN 15562, Fertilizers Determination of cyanamide nitrogen EN ISO 3696:1995, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN :1999 and EN :1999 apply. 4 Principle 4.1 Total soluble and insoluble nitrogen According to the list of standard fertilizers given in Annex I of [1], this determination is applicable to products containing calcium cyanamide. In the absence of nitrates, the test sample is mineralized by direct Kjeldahl digestion. In the presence of nitrates, the test sample is mineralized by Kjeldahl digestion after reduction with the aid of metallic iron and stannous chloride. In both cases, the ammonia is determined according to EN NOTE If analysis shows an insoluble nitrogen content of more than 0,5 %, one concludes that the fertilizer contains other forms of insoluble nitrogen not included in the list in [1], Annex I. 4

9 SS-EN 15604:2009 (E) 4.2 Forms of soluble nitrogen General The forms of soluble nitrogen referred to in to are determined from different aliquots taken from the same solution of the test sample: Total soluble nitrogen In the absence of nitrates, by direct Kjeldahl digestion. The ammonia is then determined (by the same method as that described in EN 15475) In the presence of nitrates, by Kjeldahl digestion on an aliquot part taken from the solution after reduction according to Ulsch. The ammonia is then determined (by the same method as that described in EN 15475) Total soluble nitrogen with the exception of nitrate nitrogen By Kjeldahl digestion after elimination in an acid medium of nitrate nitrogen with ferrous sulfate. The ammonia is then determined (by the same method as that described in EN 15475) Nitrate nitrogen by difference In the absence of calcium cyanamide, by determining the difference between the nitrogen determined as summarized in and that determined as summarized in or between total soluble nitrogen (4.2.2) and the sum of ammoniacal nitrogen and ureic organic nitrogen ( ) In the presence of calcium cyanamide, by determining the difference between the nitrogen determined as summarized in and that determined as summarized in or between the nitrogen determined as summarized in and the sum of that determined as summarized in Ammoniacal nitrogen Solely in the presence of ammoniacal nitrogen and ammoniacal plus nitrate nitrogen, according to EN In the presence of urea nitrogen and/or cyanamide nitrogen by cold distillation after making slightly alkaline, the ammonia is absorbed in a standard solution of sulfuric acid and determined according to EN Urea nitrogen By conversion using urease, into ammonia which is titrated with a standard solution of hydrochloric acid. or By gravimetry with xanthydrol: the co-precipitated biuret can be counted with urea nitrogen without great error, its content remaining generally low in absolute value in compound fertilizers. or By difference according to Table 1. 5

10 SS-EN 15604: :2009 (E) (E) Provläsningsexemplar / Preview Table 1 Determination of urea nitrogen by difference Case Nitrate nitrogen Ammoniacal nitrogen Cyanamidic nitrogen Difference 1 Absent ( ) ( ) 2 (4.2.3) ( ) 3 Absent Absent ( ) ( ) 4 Absent (4.2.3) ( ) Cyanamide nitrogen By precipitation as a silver compound, the nitrogen being determined in the precipitate by the Kjeldahl method. 5 Reagents 5.1 General Use only reagents of recognized analytical grade and distilled or de-mineralized water of grade 3 according to EN ISO 3696: Potassium sulfate p.a. 5.3 Iron powder, reduced with hydrogen. The prescribed quantity of iron shall be able to reduce at least 50 m g of nitrate nitrogen. 5.4 Potassium thiocyanate, p.a. 5.5 Potassium nitrate, p.a. 5.6 Ammonium sulfate, p.a. 5.7 Urea, p.a. 5.8 Diluted sulfuric acid Dilute one volume of sulfuric acid ( 20 = 1,84 g/ml) in one volume of water. 5.9 Standard solution of sulfuric acid, c = 0,1 mol/l Sodium hydroxide solution, aqueous solution of about 30 % (mass concentration), free from ammonia Standard solution of sodium or potassium hydroxide, c = 0,2 mol/l, free from carbonates. 6

11 SS-EN 15604:2009 (E) 5.12 Stannous chloride solution Dissolve 120 g of SnCl 2. 2H 2 O in 400 ml of concentrated hydrochloric acid ( 20 = 1,18 g/ml) and make up to 1 l with water. The solution shall be perfectly clear and prepared immediately before use. It is essential to check the reducing power of stannous chloride: dissolve 0,5 g of SnCl 2. 2H 2 O in 2 ml of concentrated hydrochloric acid ( 20 = 1,18 g/ml) and make up to 50 ml with water. Then add 5 g of Rochelle salt (potassium sodium tartrate), then a sufficient quantity of sodium bicarbonate for the solution to be alkaline to litmus paper. Titrate with an iodine solution (I 2 ) of c = 0,05 mol/l in the presence of a starch solution as an indicator. 1 ml of iodine solution (I 2 ) of c = 0,05 mol/l corresponds to 0,01128 g of SnCl 2. 2H 2 O. At least 80 % of the total tin present in the solution thus prepared shall be in bivalent form. For the titration at least 35 ml of the c = 0,05 mol/l iodine solution (I 2 ) should be used Sulfuric acid, 20 = 1,84 g/ml Diluted hydrochloric acid Mix one volume of hydrochloric acid ( 20 = 1,18 g/ml) with one volume of water Acetic acid, 96 % to 100 % Sulfuric acid solution, containing about 30 % of H 2 SO 4 (mass concentration) Ferrous sulfate, crystalline, FeSO 4. 7H 2 O Standard sulfuric acid solution, c = 0,05 mol/l Octyl alcohol 5.20 Saturated solution of potassium carbonate 5.21 Standard solution of sodium or potassium hydroxide, c = 0,1 mol/l (free from carbonates) Saturated solution of barium hydroxide 5.23 Sodium carbonate solution, at 10 % (mass concentration) Hydrochloric acid, c = 2 mol/l Standard solution of hydrochloric acid, c = 0,1 mol/l Urease solution Suspend 0,5 g of active urease in 100 ml of water. Using hydrochloric acid 0,1 mol/l (5.25), adjust the ph to 5,4, measured by a ph-meter. 7

SWEDISH STANDARDS INSTITUTE

SWEDISH STANDARDS INSTITUTE SVENSK STANDARD SS-EN ISO 5983-2:2009 Fastställd/Approved: 2009-06-15 Publicerad/Published: 2009-08-18 Utgåva/Edition: 2 Språk/Language: engelska/english ICS: 65.120 Animal feeding stuffs Determination