1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 15923:2011Fertilizers Extraction ofphosphorus soluble in Jouliesalcaline ammonium citrateBS EN 15923:2011 BRITISH STANDARDNational forewordThis British Standard is the UK i
2、mplementation of EN 15923:2011. Itsupersedes DD CEN/TS 15923:2009 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee CII/37, Fertilisers and related chemicals.A list of organizations represented on this committee can beobtained on request to its secretary.
3、This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 72728 3ICS 65.080Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under
4、the authority of theStandards Policy and Strategy Committee on 30 June 2011.Amendments issued since publicationDate Text affectedBS EN 15923:2011EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15923 June 2011 ICS 65.080 Supersedes CEN/TS 15923:2009English Version Fertilizers - Extraction of pho
5、sphorus soluble in Joulies alcaline ammonium citrate Engrais - Extraction du phosphore soluble dans le citrate dammonium alcalin de Joulie Dngemittel - Extraktion des in alkalischem Ammoniumcitrat nach Joulie lslichen Phosphors This European Standard was approved by CEN on 29 April 2011. CEN members
6、 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
7、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 notified to the CEN-CENELEC Management
8、 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, Lithuania, Luxembourg, Malta, Netherlands,
9、 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 CEN All rights of exploitation in any
10、form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15923:2011: EBS EN 15923:2011EN 15923:2011 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Terms and definitions .44 Principle 45 Sampling .46 Reagents .57 Apparatus .58 Procedure .58.1 Test portion 58.2
11、Extraction .59 Application to fertilizers containing magnesium .6Bibliography 7BS EN 15923:2011EN 15923:2011 (E) 3 Foreword This document (EN 15923:2011) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held by DIN. This European Sta
12、ndard 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 standards shall be withdrawn at the latest by December 2011. Attention is drawn to the possibility that some of the elements
13、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 15923:2009. This document has been prepared under a mandate given to CEN by the European Commission and the European F
14、ree 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, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hu
15、ngary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 15923:2011EN 15923:2011 (E) 4 1 Scope This document specifies the procedure for the extraction of phospho
16、rus 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-calcic form. 2 Normative references The following referenced documents are indispensable for the application of this document
17、. 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, Fertilizers and liming materials Sampling and sample preparation Part 2: Sample preparation EN 12944-1:1999, Fertilizers and li
18、ming 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 fertilizers EN 15475, Fertilizers Determination of ammoniacal nitrogen CEN/TS 15959, Fertilizers Determination of extracted pho
19、sphorus 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 shaking vigorously with an alkaline solution of ammonium citrate of defined specification (and where appropriate in the presence
20、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 shall be carried out in accordance with EN 1482-2. Grinding of the laboratory sample is recommended for homogeneity reasons. BS E
21、N 15923:2011EN 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 citric acid and 153 g of NH3per litre. Its free ammonia content is approximately 55 g per litre. Prepare the solution according to
22、 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 litre). 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
23、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). Make 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 citrat
24、e 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. 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
25、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. 6.3 8-hydroxyquinoline (oxine), powdered. 7 Apparatus Use common laboratory equipment and glassware, in particular equipment accor
26、ding 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 minute. 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). A
27、dd 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 (6.2) and mix to a paste, leave it to settle for about 1 min. BS EN 15923:2011EN 15923:2011 (E) 6 Decant the liquid into a 500 ml g
28、raduated 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 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 pr
29、oduct 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 graduated 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 t
30、o 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 (6.1). Filter through a dry filter, discard the first portion of the filtrate and collect the clear filtrate in a dry flask. Continue th
31、e filtering until a sufficient quantity of filtrate is obtained to carry out the phosphorus determination according to CEN/TS 15959. 9 Application to fertilizers containing magnesium The use of oxine makes it possible to apply this method to fertilizers containing magnesium. This use is recommended
32、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. The use of oxine in the absence of magnesium is not, moreover, likely to interfere subsequently with the determination. In the known
33、absence of magnesium it is, however, possible not to use oxine. BS EN 15923:2011EN 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 2
34、003 relating to fertilisers, Official Journal L 304, 21/11/2003, P. 0001-0194, Annex IV, method 3.1.5.3 This page deliberately left blankThis page deliberately left blankBSI is the independent national body responsible for preparing British Standardsand other standards-related publications, informat
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