1、December 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).IC
2、S 65.080!$xZM“1855542www.din.deDDIN EN 15925Fertilizers Extraction of total sulfur present in various formsEnglish translation of DIN EN 15925:2011-12Dngemittel Extraktion von Gesamtschwefel, der in verschiedener Form vorliegen kannEnglische bersetzung von DIN EN 15925:2011-12Engrais Extraction du s
3、oufre total prsent sous diffrentes formesTraduction anglaise de DIN EN 15925:2011-12SupersedesDIN SPEC 1111(DIN CEN/TS 15925):2010-02www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises pages11.118DIN EN 15925:2011-12 A comma is used as the
4、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 Normenausschuss Lebensmittel und landwirtschaftl
5、iche 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 8.2 (see Bibliography). DIN EN 15925 supersedes DIN SPEC 1111 (
6、DIN CEN/TS 15925):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 1111 (DIN CEN/TS 15925):2010-02 as follows: a) the DIN SPEC prestandard status has been changed to that of a European stand
7、ard; b) normative references have been updated; c) Clause 9 “Test report” has been added; d) the standard has been editorially revised. Previous editions DIN CEN/TS 15925: 2010-02 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15925 September 2011 ICS 65.080 Supersedes CEN/TS 15925:2009Engli
8、sh Version Fertilizers - Extraction of total sulfur present in various forms Engrais - Extraction du soufre total prsent sous diffrentes formes Dngemittel - Extraktion von Gesamtschwefel, der in verschiedener Form vorliegen kann This European Standard was approved by CEN on 18 August 2011. CEN membe
9、rs 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 applicatio
10、n 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 Manageme
11、nt 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, Netherland
12、s, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. 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 15925:2011: EEUROPEA
13、N COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG EN 15925:2011 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Terms and definitions .44 Sampling .45 Principle 46 Reagents .47 Apparatus .58 Procedure .59 Test report 5Bibliography DIN EN 1
14、5925:2011-12 6EN 15925:2011 (E) 3 Foreword This document (EN 15925:2011) 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 standard, either by publication of
15、an identical text or by endorsement, at the latest by March 2012, and conflicting national standards shall be withdrawn at the latest by March 2012. 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 h
16、eld responsible for identifying any or all such patent rights. This document supersedes CEN/TS 15925:2009. The following changes have been made to the former edition: a) the CEN Technical Specification has been adopted as a European Standard; b) Clause 9 “Test report“ has been added; c) the document
17、 has been editorially revised. 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 th
18、is European Standard: 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, Switzerlan
19、d and the United Kingdom. DIN EN 15925:2011-12 EN 15925:2011 (E) 4 1 Scope This document specifies a method for the extraction of the total sulfur contained in fertilizers in elemental form and/or in other chemical combinations. The method is applicable to EC fertilizers for which a declaration of t
20、he total sulfur present in various forms (elemental, thiosulfate, sulfite, sulfate) is provided. 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
21、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, Fertili
22、zers and liming materials and soil improvers Vocabulary Part 2: Terms relating to fertilizers EN 15749, Fertilizers Determination of sulfates content using three different methods 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 12944-1:1999 and EN 129
23、44-2:1999 apply. 4 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 is recommended for homogeneity reasons. 5 Principle Elemental sulfur is conve
24、rted in an alkaline medium into polysulfides and thiosulfate; these, together with any sulfites that can be present, are then oxidized with hydrogen peroxide. The various forms of sulfur are thus converted into sulfate that is determined by precipitation of barium sulfate. 6 Reagents Use only reagen
25、ts of recognized analytical grade and distilled or demineralized water. 6.1 Diluted hydrochloric acid. Mix one volume of hydrochloric acid (d = 1,18) with one volume of water. 6.2 Sodium hydroxide solution, NaOH 30 % minimum, d = 1,33. DIN EN 15925:2011-12 EN 15925:2011 (E) 5 6.3 Hydrogen peroxide s
26、olution, w = 30 %. 6.4 Barium chloride, aqueous solution of BaCl2 2H2O, = 122 g/l. 7 Apparatus 7.1 Electric hot plate, with adjustable temperature. 7.2 400 ml beaker. 7.3 600 ml beaker. 7.4 250 ml volumetric flask. 8 Procedure 8.1 Test portion Weigh to an accuracy of 1 mg a quantity of the laborator
27、y sample containing between 80 mg and 350 mg of sulfur (S) or 200 mg and 875 mg of SO3. As a rule (where S 15 %), weigh 2,5 g. Place the test portion in a beaker (7.2). 8.2 Oxidation Add 20 ml of sodium hydroxide solution (6.2) and 20 ml of water. Cover with a watch glass. Boil for 5 min on the hot
28、plate (7.1). Remove from the hot plate. Using a jet of hot water, collect the sulfur sticking to the sides of the beaker and boil for 20 min. Leave to cool. Add 2 ml increments of hydrogen peroxide (6.3) until no reaction is observed. 6 ml to 8 ml of hydrogen peroxide will be necessary. Allow oxidat
29、ion to continue for 1 h, and then bring to the boil for 0,5 h. Leave to cool. 8.3 Preparation of the solution to be analyzed Add approximately 50 ml of water and 50 ml of the hydrochloric acid solution (6.1). a) If the level of sulfur (S) is less than 5 %: Filter into a 600 ml beaker (7.3). Wash the
30、 residue on the filter several times with cold water. After washing, check for the absence of sulfate in the last drops of the filtrate using a barium chloride solution (6.4). The filtrate shall be perfectly clear. Sulfate is determined on the whole of the filtrate in accordance with EN 15749. b) If
31、 the level of sulfur (S) is at above 5 %: Transfer quantitatively into a 250 ml volumetric flask (7.4), make up to volume with water and mix. Filter through a dry filter into a dry container; the filtrate shall be completely clear. Stopper if the solution is not to be used immediately. Determine sul
32、fates on an aliquot of this solution by precipitation in the form of barium sulfate in accordance with EN 15749. 9 Test report The test report shall contain at least the following information: a) the test method used with a reference to this document; DIN EN 15925:2011-12 EN 15925:2011 (E) 6 b) all
33、information necessary for the complete identification of the sample; c) date of sampling and sampling procedure (if known); d) date when the extraction was finished; e) all operating details not specified in this document, or regarded as optional, together with details of any incidents that occurred
34、 when performing the method which might have influenced the test result(s). DIN EN 15925:2011-12 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, Pp. 1-194, Annex IV, method 8.2
