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!$t2o“1811576www.din.deDDIN EN 15923Fertilizers Extraction of phosphorus soluble in Joulies alcaline ammonium citrateEnglish translation of DIN EN 15923:2011-08Dngemittel Extraktion des in alkalischem Ammoniumcitrat nach Joulie lslichen PhosphorsEnglische bersetzung von DIN EN 15923:2011-08Eng
3、rais Extraction du phosphore soluble dans le citrate dammonium alcalin de JoulieTraduction anglaise de DIN EN 15923:2011-08SupersedesDIN SPEC 1109(DIN CEN/TS 15923):2010-02www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.908.11 DIN
4、EN 15923:2011-08 A comma is used as the decimal 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 Normenau
5、sschuss Lebensmittel und landwirtschaftliche Produkte (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 3.1.5.3 (see Bibliograp
6、hy). DIN EN 15923 supersedes DIN SPEC 1109 (DIN CEN/TS 15923):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 1109 (DIN CEN/TS 15923):2010-02 as follows: a) in Subclause 8.2, a normative re
7、ference to CEN/TS 15959 has been included relating 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 1109 (DIN CEN/TS 15923): 2010-02 2 EUROPEAN STANDARD NORME
8、EUROPENNE EUROPISCHE NORM EN 15923 June 2011 ICS 65.080 Supersedes CEN/TS 15923:2009English Version Fertilizers - Extraction of phosphorus soluble in Joulies alcaline ammonium citrate Engrais - Extraction du phosphore soluble dans le citrate dammonium alcalin de Joulie Dngemittel - Extraktion des in
9、 alkalischem Ammoniumcitrat nach Joulie lslichen Phosphors This European Standard was approved 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
10、 any alteration. Up-to-date lists and bibliographical references concerning such national standards 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 lan
11、guage made by translation under the responsibility of a CEN member into its own language and notified 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, Denma
12、rk, 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 COMIT EUROPEN DE NORMALISAT
13、ION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15923:2011: EEN 15923:2011 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 4
14、3 Terms and definitions .44 Principle 45 Sampling .46 Reagents .57 Apparatus .58 Procedure .58.1 Test portion 58.2 Extraction .59 Application to fertilizers containing magnesium .6Bibliography 7DIN EN 15923:2011-08 EN 15923:2011 (E) 3 Foreword This document (EN 15923:2011) has been prepared by Techn
15、ical 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 December 2011, and conflicting national stand
16、ards 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 rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes CEN/T
17、S 15923:2009. 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 Internal Regulations, the national standards organizations of the following countries are bound to implement this European Stand
18、ard: Austria, Belgium, Bulgaria, Croatia, 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
19、Kingdom. DIN EN 15923:2011-08 EN 15923:2011 (E) 4 1 Scope This document specifies the procedure for the extraction of phosphorus soluble in Joulies alkaline ammonium citrate. The method is applicable to all the straight and compound phosphate fertilizers, in which the phosphate occurs in an alumino-
20、calcic form. 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 1482-2, Fe
21、rtilizers 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, Fertilizers and liming materials and soil improvers Vocabulary Part 2: Terms relating to fe
22、rtilizers 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 definitions given in EN 12944-1:1999 and EN 12944-2:1999 apply. 4 Principle Extraction by shak
23、ing vigorously with an alkaline solution of ammonium citrate of defined specification (and where appropriate in the presence of oxine) at about 20 C. 5 Sampling Sampling is not part of the method specified in this document. A recommended sampling method is given in EN 1482-1. Sample preparation shal
24、l be carried out in accordance with EN 1482-2. Grinding of the laboratory sample is recommended for homogeneity reasons. DIN EN 15923:2011-08 EN 15923:2011 (E) 5 6 Reagents 6.1 Water, distilled or demineralized. 6.2 Joulies alkaline solution of ammonium citrate 6.2.1 This solution contains 400 g of
25、citric acid and 153 g of NH3per litre. Its free ammonia content is approximately 55 g per litre. Prepare the solution according to 6.2.2 or 6.2.3. 6.2.2 In a 1 l graduated flask, dissolve 400 g of citric acid (C6H8O7 . H2O) in approximately 600 ml of ammonia (d20= 0,925 g/ml i.e. 200 g of NH3per lit
26、re). Add citric acid successively in quantities of 50 g to 80 g maintaining the temperature below 50 C. Make up the volume to 1 l with ammonia. 6.2.3 In a 1 l graduated flask, dissolve 432 g of dibasic ammonium citrate (C6H14N2O7) in 300 ml of water (6.1). Add 440 ml of ammonia (d20= 0,925 g/ml). Ma
27、ke the volume up to 1 l with water (6.1). 6.2.4 Verify the total ammonia content as follows. Take an amount of 10 ml of the citrate solution and place it in a 250 ml flask. Make up the volume with water (6.1). Determine the ammoniacal nitrogen content on 25 ml of this solution according to EN 15475.
28、 1 ml of H2SO40,25 mol/l = 0,008 516 g of NH3. Under these conditions, the reagent is considered to be correct when the amount of millilitres found upon titration lies between 17,7 ml and 18 ml. If this is not the case, add 4,25 ml of ammonia (d20= 0,925 g/l) per 0,1 ml below 18 ml indicated above.
29、6.3 8-hydroxyquinoline (oxine), powdered. 7 Apparatus Use common laboratory equipment and glassware, in particular equipment according to 7.2 to 7.4. 7.1 Small mortar, glass or porcelain with pestle. 7.2 500 ml graduated flasks. 7.3 1 000 ml graduated flask. 7.4 Rotary shaker, 35 to 40 turns per min
30、ute. 8 Procedure 8.1 Test portion Weigh, to the nearest 0,000 5 g, 1 g of the prepared sample and place in a small mortar (7.1). Add about 10 drops of ammonium citrate solution (6.2) to moisten it and break it up very carefully with the pestle. 8.2 Extraction Add 20 ml of ammonium citrate solution (
31、6.2) and mix to a paste, leave it to settle for about 1 min. DIN EN 15923:2011-08 EN 15923:2011 (E) 6 Decant the liquid into a 500 ml graduated flask (7.2), straining off particles which might have escaped the preceding moist disintegration. Add 20 ml of citrate solution (6.2) to the residue, grind
32、as above and decant the liquid into the graduated flask. Repeat the process four times, so that by the end of the fifth time all the product can be poured into the flask. The total quantity of citrate used for these processes shall be approximately 100 ml. Rinse the pestle and mortar above the gradu
33、ated flask with 40 ml of water (6.1). Shake the stoppered flask for 3 h on the rotary shaker (7.4). Leave the flask standing for 15 h to 16 h, shake it again under same conditions for 3 h. The temperature during the whole process shall be kept at (20 2) C. Make up to the graduation mark with water (
34、6.1). Filter through a dry filter, discard the first portion of the filtrate and collect the clear filtrate in a dry flask. Continue the filtering until a sufficient quantity of filtrate is obtained to carry out the phosphorus determination according to CEN/TS 15959. 9 Application to fertilizers con
35、taining magnesium The use of oxine makes it possible to apply this method to fertilizers containing magnesium. This use is recommended when the ratio of magnesium and phosphoric anhydride contents is higher than 0,03 (Mg/P2O5 0,03). If this is the case, add 3 g of oxine to the moistened test portion
36、. The use of oxine in the absence of magnesium is not, moreover, likely to interfere subsequently with the determination. In the known absence of magnesium it is, however, possible not to use oxine. DIN EN 15923:2011-08 EN 15923:2011 (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 3.1.5.3 DIN EN 15923:2011-08
