1、August 2011 Translation by DIN-Sprachendienst.English price group 7No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS
2、65.080!$t2n“1811575www.din.deDDIN EN 15921Fertilizers Extraction of soluble phosphorus according to Petermann at 65 CEnglish translation of DIN EN 15921:2011-08Dngemittel Extraktion des lslichen Phosphors nach Petermann bei 65 CEnglische bersetzung von DIN EN 15921:2011-08Engrais Extraction du phosp
3、hore soluble selon Petermann 65 CTraduction anglaise de DIN EN 15921:2011-08SupersedesDIN SPEC 1100(DIN CEN/TS 15921):2010-02www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.908.11 DIN EN 15921:2011-08 A comma is used as the decimal
4、 marker. National foreword This standard has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials” (Secretariat: DIN, Germany) under the mandate M/335. The responsible German body involved in its preparation was the Normenausschuss Lebensmittel und landwirtschaftliche Pr
5、odukte (Food and Agricultural Products Standards Committee), Working Committee NA 057-03-02 AA Dngemittel. The method specified in this standard is based upon Regulation (EC) No 2003/2003 relating to fertilizers, Annex IV, method 3.1.5.1 (see Bibliography). DIN EN 15921 supersedes DIN SPEC 1100 (DIN
6、 CEN/TS 15921):2010-02, which has been adopted as a European Standard based on the results of the unique acceptance procedure. Amendments This standard differs from DIN SPEC 1100 (DIN CEN/TS 15921):2010-02 as follows: a) in Subclause 8.2, a normative reference to CEN/TS 15959 has been included relat
7、ing to the determination of phosphorus; b) normative references have been updated; c) the Bibliography has been updated; d) the standard has been editorially revised. Previous editions DIN SPEC 1100 (DIN CEN/TS 15921): 2010-02 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15921 June 2011 IC
8、S 65.080 Supersedes CEN/TS 15921:2009English Version Fertilizers - Extraction of soluble phosphorus according to Petermann at 65 C Engrais - Extraction du phosphore soluble selon Petermann 65 C Dngemittel - Extraktion des lslichen Phosphors nach Petermann bei 65 C This European Standard was approved
9、 by CEN on 29 April 2011. 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 stan
10、dards may be obtained on application to the CEN-CENELEC 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 n
11、otified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithu
12、ania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 C
13、EN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15921:2011: EEN 15921:2011 (E) 2 Contents Page Foreword 3 1 Scope 4 2 Normative references 4 3 Terms and definitions .4 4 Principle 4 5 Sampling .4 6 Reagents .5 7 Apparatus .6 8 Proce
14、dure .6 Bibliography 7 DIN EN 15921:2011-08 EN 15921:2011 (E) 3 Foreword This document (EN 15921:2011) 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 stand
15、ard, either by publication of an identical text or by endorsement, at the latest by December 2011, and conflicting national standards shall be withdrawn at the latest by December 2011. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent right
16、s. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes CEN/TS 15921:2009. 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
17、 Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
18、Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 15921:2011-08 EN 15921:2011 (E) 4 1 Scope This document specifies the procedure for the determination of soluble phosphorus in alkaline ammonium citrate. T
19、he method is applicable exclusively to precipitated dehydrated dicalcium phosphate (CaHPO4. 2H2O). 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 lates
20、t edition of the referenced document (including any amendments) applies. EN 1482-2, Fertilizers and liming materials Sampling and sample preparation Part 2: Sample preparation EN 12944-1:1999, Fertilizers and liming materials and soil improvers Vocabulary Part 1: General terms EN 12944-2:1999, Ferti
21、lizers and liming materials and soil improvers Vocabulary Part 2: Terms relating to fertilizers EN 15475, Fertilizers Determination of ammoniacal nitrogen CEN/TS 15959, Fertilizers Determination of extracted phosphorus 3 Terms and definitions For the purposes of this document, the terms and definiti
22、ons given in EN 12944-1:1999 and EN 12944-2:1999 apply. 4 Principle Extraction of phosphorus from the test portion at a temperature of 65 C with an alkaline solution of ammonium citrate (Petermanns solution) under the specified conditions. 5 Sampling Sampling is not part of the method specified in t
23、his document. A recommended sampling method is given in EN 1482-1. Sample preparation shall be carried out in accordance with EN 1482-2. Grinding of the laboratory sample is recommended for homogeneity reasons. DIN EN 15921:2011-08 EN 15921:2011 (E) 5 6 Reagents 6.1 Water, distilled or demineralized
24、 having the same characteristics as distilled water. 6.2 Petermanns solution 6.2.1 Characteristics of the Petermanns solution citric acid (C6H8O7. H2O): 173 g/l; ammonia: 42 g/l of ammoniacal nitrogen; pH between 9,4 and 9,7. 6.2.2 Preparation from diammonium citrate Dissolve 931 g of diammonium cit
25、rate (molecular mass 226,19) in about 3 500 ml of water (6.1), in a 5 l standard flask. Stand in a bath of running water, mix and cool and add in small amounts ammonia. For example, for d20= 0, 906 g/ml corresponding to a level of 20,81 % by mass of ammoniacal nitrogen, it is necessary to use 502 ml
26、 of ammonia solution. Adjust the temperature to 20 C, make up to volume with water (6.1) and mix. 6.2.3 Preparation from citric acid and ammonia Dissolve 865 g of citric acid monohydrate in about 2 500 ml of water (6.1) in a container of about 5 l capacity. Place the container in an ice bath, and ad
27、d in small amounts, shaking constantly, ammonia solution using a funnel, the stem of which is immersed in the citric acid solution. For example, for d20= 0, 906 g/ml corresponding to a level of 20,81 % by mass of ammoniacal nitrogen, it is necessary to add 1 114 ml of ammonia solution. Adjust the te
28、mperature to 20 C, transfer to a 5 l standard flask, make up to the mark with water (6.1) and mix. 6.2.4 Checking of the ammoniacal nitrogen content Transfer 25 ml of the solution into a 250 ml standard flask and make up to volume with water (6.1) and mix. Determine the ammoniacal content on 25 ml o
29、f this solution according to EN 15475. If the solution is correct, an amount of 15 ml of c = 0,25 mol/l H2SO4 shall be used. If the strength of ammoniacal nitrogen is greater than 42 g/l, NH3can be expelled by a stream of inert gas or by moderate heating to bring back the pH to 9,7. Carry out a seco
30、nd determination. If the strength of ammoniacal nitrogen is less than 42 g/l, it will be necessary to add a mass M in grams of ammonia solution: 20,815002,8)(42 = nM (1) n is the volume of the sulfuric acid c=0,25 mol/l, in millilitres or a volume, V, at 20 C: 0,906MV = (2) If V is less than 25 ml,
31、add it directly to the 5 l flask with a mass of V 0,173 g powdered citric acid. DIN EN 15921:2011-08 EN 15921:2011 (E) 6 If V is greater than 25 ml, it will be convenient to prepare a new litre of reagent in the following way. Weigh 173 g of citric acid. Dissolve it in 500 ml of water. And, taking t
32、he precautions indicated, add not more than 225 + V 1 206 ml of ammonia solution which was used to prepare the 5 l of reagent. Make up to volume with water and mix. Mix this volume of 1 l with the 4 975 ml previously prepared. 7 Apparatus 7.1 Common laboratory equipment and glassware, in particular
33、equipment according to 7.2 to 7.4. 7.2 Water bath, which can be maintained at a temperature of (65 1) C. 7.3 500 ml graduated flask, e.g. Stohmann. 7.4 Dry fluted filter paper, free from phosphates. 8 Procedure 8.1 Test portion Weigh, to the nearest 0,001 g, 1 g of the prepared laboratory sample and
34、 transfer it to the graduated flask (7.3). 8.2 Extraction Add 200 ml of alkaline ammonium citrate solution (6.2). Stopper the flask and shake vigorously by hand to avoid the formation of lumps and to prevent any adherence of the substance to the sides. Place the flask in the water bath set at 65 C (
35、7.2) and shake every 5 min during the first 0,5 h. After each shaking, raise the stopper to equilibrate the pressure. The level of water in the water bath ought to be above the level of solution in the flask. Allow the flask to remain in the water bath a further 1 h at 65 C and shake every 10 min. R
36、emove the flask, cool to a temperature of about 20 C, make up to a volume of 500 ml with water. Mix and filter through a dry fluted filter paper (7.4), rejecting the first portion of filtrate. Continue the filtering until a sufficient quantity of filtrate is obtained to carry out the phosphorus dete
37、rmination according to CEN/TS 15959. DIN EN 15921:2011-08 EN 15921:2011 (E) 7 Bibliography 1 EN 1482-1, Fertilizers and liming materials Sampling and sample preparation Part 1: Sampling 2 Regulation (EC) No 2003/2003 of the European Parliament and of the Council of 13 October 2003 relating to fertilisers, Official Journal L 304, 21/11/2003, P. 0001-0194, Annex IV, method 3.1.5.1 DIN EN 15921:2011-08
