EN 16032-2011 en Fertilizers - Extraction and determination of elemental sulfur《肥料 元素硫的萃取和测定》.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 16032:2011Fertilizers Extraction anddetermination of elementalsulfurBS EN 16032:2011 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 1

2、6032:2011. Itsupersedes DD CEN/TS 16032:2010 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee CII/37, Fertilisers and related chemicals.A list of organizations represented on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.This publication does

3、 not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 74621 5ICS 65.080Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theS

4、tandards Policy and Strategy Committee on 31 December 2011.Amendments issued since publicationDate Text affectedBS EN 16032:2011EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16032 November 2011 ICS 65.080 Supersedes CEN/TS 16032:2010English Version Fertilizers - Extraction and determination o

5、f elemental sulfur Engrais - Extraction et dosage du soufre lmentaire Dngemittel - Extraktion und Bestimmung von elementarem Schwefel This European Standard was approved by CEN on 29 October 2011. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the condition

6、s 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-CENELEC Management Centre or to any CEN member. This European Standard exists in

7、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 Centre has the same status as the official versions. CEN members are the national standards

8、 bodies of 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 Unite

9、d 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 form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16032:2011: E

10、BS EN 16032:2011EN 16032:2011 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Terms and definitions .44 Principle 45 Sampling and sample preparation .46 Reagents .57 Apparatus .58 Procedure .58.1 Test portion 58.2 Extraction of the sulfur .58.3 Determination of the purity of the ele

11、mental sulfur .59 Calculation and expression of the results 610 Test report 6Bibliography 7BS EN 16032:2011EN 16032:2011 (E) 3 Foreword This document (EN 16032:2011) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held by DIN. This

12、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 May 2012, and conflicting national standards shall be withdrawn at the latest by May 2012. Attention is drawn to the possibility that some of the element

13、s 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 16032:2010. The following has been added to the former edition of the European Standard: a) the CEN Technical Specif

14、ication has been adopted as a European Standard; b) the document 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 or

15、ganizations 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, Luxembourg, Malta, Netherlands, Norway, Poland,

16、Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 16032:2011EN 16032:2011 (E) 4 1 Scope This European Standard specifies a method for extraction and determination of the elemental sulfur contained in fertilizers. The method is applicable to EC fertilizer

17、s for which a declaration of the total sulfur in elemental form is provided for in Regulation (EC) Nr 2003/2003, Annex I 1. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For unda

18、ted 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 liming materials and soil improvers Vocabulary Part 1: General ter

19、ms EN 12944-2:1999, Fertilizers and liming materials and soil improvers Vocabulary Part 2: Terms relating to fertilizers 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 After the removal of soluble c

20、ompounds, elemental sulfur is extracted by using carbon disulfide, followed by gravimetric determination of the sulfur extracted. WARNING This method of analysis involves the use of carbon disulfide (CS2). Special safety measures shall therefore be taken, in particular with regard to: the storage of

21、 CS2; protective equipment for staff; occupational hygiene; prevention of fire and explosions; disposal of the reagent. This method requires a highly skilled staff and a suitably equipped laboratory. 5 Sampling and sample preparation Sampling is not part of the method specified in this European Stan

22、dard. A recommended sampling method is given in EN 1482-1. BS EN 16032:2011EN 16032:2011 (E) 5 Sample preparation shall be carried out in accordance with EN 1482-2. Grinding of the laboratory sample is recommended for homogeneity reasons. 6 Reagents 6.1 Carbon disulfide. 7 Apparatus 7.1 Extraction f

23、lask, capacity 100 ml, with ground glass stopper. 7.2 Soxhlet apparatus, with the appropriate filter elements. 7.3 Vacuum rotary evaporator. 7.4 Electric oven, fan assisted, set at (90 2) C. 7.5 Porcelain Petri dishes, 50 mm to 70 mm in diameter, not exceeding 50 mm in height. 7.6 Electric hot plate

24、, with adjustable temperature. 8 Procedure 8.1 Test portion Weigh to an accuracy of 1 mg, 5 g to 10 g of the laboratory sample and place the test portion (m) in the thimble of the Soxhlet apparatus (7.2). 8.2 Extraction of the sulfur Wash thoroughly the contents with hot water to remove all soluble

25、compounds. Dry in the electric oven (7.4) at 90 C for at least 1 h. Place the filter in the Soxhlet apparatus (7.2). Place a few glass beads in the flask of the apparatus (7.1) and weigh (m0), then add 50 ml of carbon disulfide (6.1). Connect the apparatus and leave the elemental sulfur to be extrac

26、ted for 6 h. Switch off the heat and, after cooling, disconnect the flask. Connect the flask to the rotary evaporator (7.3) and evaporate until the contents of the flask have solidified in a spongy mass. Dry the flask in the electric oven (7.4) at 90 C (generally 1 h is necessary) until a constant m

27、ass is obtained (m1). 8.3 Determination of the purity of the elemental sulfur Certain substances may have been extracted by the carbon disulfide at the same time as the elemental sulfur. The purity of the elemental sulfur is determined as follows: Homogenize the contents of the flask as thoroughly a

28、s possible, and remove 2 g or 3 g, weighed to an accuracy of 1 mg (n). Weigh the Petri dish (m2) and place the aliquot in it. Place on the hot plate (7.6) set at a temperature not exceeding 220 C so as not to cause combustion of the sulfur. Continue sublimation for 3 h or 4 h until a constant mass i

29、s obtained (m3). NOTE Only compounds with boiling point the temperature of the hotplate will be removed. BS EN 16032:2011EN 16032:2011 (E) 6 9 Calculation and expression of the results Calculate the mass fraction of impure elemental sulfur (S), wSi, in percent of the fertilizer according to Equation

30、 (1). 10001Si=mmmw (1) Calculate the purity of sulfur extracted, wp, in percent of the fertilizer according to Equation (2). (2) 10023=nmmwpCalculate the mass fraction of pure elemental sulfur (S), wSp, in percent of the fertilizer according to Equation (3). 100)(2301Sp=nmmmmmw (3) where m is the ma

31、ss of the test portion, in grams; m0is the mass of the Soxhlet flask, in grams; m1is the mass of the Soxhlet flask and the impure sulfur after drying, in grams; n is the mass of the impure sulfur to be purified, in grams; m2is the mass of the Petri dish, in grams; m3is the mass of the Petri dish aft

32、er sublimation of the sulfur, in grams. 10 Test report The test report shall contain at least the following information: a) all information necessary for the complete identification of the sample; b) the test method used with reference to this European Standard (i.e. EN 16032); c) the test results o

33、btained; d) date of sampling and sampling procedure (if known); e) date when the analysis was finished; f) whether the requirement of the repeatability limit has been fulfilled; g) all operating details not specified in this document, or regarded as optional, together with details of any incidents o

34、ccurred when performing the method, which might have influenced the test result(s). BS EN 16032:2011EN 16032:2011 (E) 7 Bibliography 1 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. 0001-01

35、94, Annex I and Annex IV, method 8.5 2 EN 1482-1, Fertilizers and liming materials Sampling and sample preparation Part 1: Sampling This page deliberately left blankThis page deliberately left blankBSI is the independent national body responsible for preparing British Standardsand other standards-re

36、lated publications, information and services. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter.British Standards Institution (BSI)raising standards worldwideBSI Group Headquarters389 Chiswick High Road London W4 4AL UKTel +44 (0)20 89

37、96 9001Fax +44 (0)20 8996 Standards are updated by amendment or revision. Users of British Stan-dards should make sure that they possess the latest amendments or editions.It is the constant aim of BSI to improve the quality of our products and serv-ices. We would be grateful if anyone finding an in

38、accuracy or ambiguity whileusing this British Standard would inform the Secretary of the technical com-mittee responsible, the identity of which can be found on the inside frontcover.Tel: +44 (0)20 8996 9001 Fax: +44 (0)20 8996 7001BSI offers Members an individual updating service called PLUS which

39、ensuresthat subscribers automatically receive the latest editions of standards.Tel: +44 (0)20 8996 7669 Fax: +44 (0)20 8996 7001Email: Buying standardsYou may buy PDF and hard copy versions of standards directly using acredit card from the BSI Shop on the website addition all orders for BSI, intern

40、ational and foreign standards publicationscan be addressed to BSI Customer Services.Tel: +44 (0)20 8996 9001 Fax: +44 (0)20 8996 7001Email: In response to orders for international standards, it is BSI policy tosupply the BSI implementation of those that have been publishedas British Standards, unles

41、s otherwise requested.Information on standardsBSI provides a wide range of information on national, Europeanand international standards through its Knowledge Centre.Tel: +44 (0)20 8996 7004 Fax: +44 (0)20 8996 7005Email: Various BSI electronic information services are also available whichgive detail

42、s on all its products and services. Tel: +44 (0)20 8996 7111 Fax: +44 (0)20 8996 7048Email: BSI Subscribing Members are kept up to date with standardsdevelopments and receive substantial discounts on the purchase priceof standards. For details of these and other benefits contact Membership Ad-minist

43、ration. Tel: +44 (0)20 8996 7002 Fax: +44 (0)20 8996 7001 Email: Information regarding online access to British Standards via BritishStandards Online can be found at information about BSI is available on the BSI website at www.bsi- subsists in all BSI publications. BSI also holds the copyright,in

44、the UK, of the publications of the international standardization bodies. Ex-cept as permitted under the Copyright, Designs and Patents Act 1988 no ex-tract may be reproduced, stored in a retrieval system or transmitted in anyform or by any means electronic, photocopying, recording or otherwise witho

45、ut prior written permission from BSI. This does not preclude the freeuse, in the course of implementing the standard of necessary details such assymbols, and size, type or grade designations. If these details are to be usedfor any other purpose than implementation then the prior written permissionof BSI must be obtained. Details and advice can be obtained from the Copy-right & Licensing Manager.Tel: +44 (0)20 8996 7070Email: