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1、a Date: 29 November 2007 Origin: European Latest date for receipt of comments: 29 February 2008 Project no.: 2007/02480 Responsible committee: CII/37 Fertilisers and related chemicals Interested committees: Title: Draft BS EN 15452 : Fertilizers - Determination of chelating agents - Determination of
2、 iron chelated by o,p- EDDHA by reversed phase HPLC Supersession information: If this document is published as a standard, the UK implementation of it will supersede DDCEN/TS15452 : 2006 and partially supersede. NONE If you are aware of a current national standard which may be affected, please notif
3、y the secretary (contact details below). WARNING: THIS IS A DRAFT AND MUST NOT BE REGARDED OR USED AS A BRITISH STANDARD. THIS DRAFT IS NOT CURRENT BEYOND 29 February 2008. This draft is issued to allow comments from interested parties; all comments will be given consideration prior to publication.
4、No acknowledgement will normally be sent. See overleaf for information on commenting. No copying is allowed, in any form, without prior written permission from BSI except as permitted under the Copyright, Designs and Patent Act 1988 or for circulation within a nominating organization for briefing pu
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6、le from BSI Customer Services. Information on the co-operating organizations represented on the committees referenced above may be obtained from the responsible committee secretary. Cross-references The British Standards which implement International or European publications referred to in this draf
7、t may be found via the British Standards Online Service on the BSI web site http:/www.bsi-. Direct tel: 020 8996 7009 Responsible Committee Secretary: Committee Service Centre (BSI) E-mail: cscbsi- Draft for Public Comment Head Office 389 Chiswick High Road London W4 4AL Telephone: +44(0)20 8996 900
8、0 Fax: +44(0)20 8996 7001 Form 36 Version 7.0 DPC: 07/30171562 DC Licensed Copy: London South Bank University, London South Bank University, Thu Dec 20 03:19:14 GMT+00:00 2007, Uncontrolled Copy, (c) BSI b Introduction This draft standard is based on European discussions in which the UK has taken an
9、 active part. Your comments on this draft are welcome and will assist in the preparation of the consequent British Standard. If no comments are received to the contrary, then the UK will approve this draft and implement it as a British Standard. Comment is particularly welcome on national, legislati
10、ve or similar deviations that may be necessary. Even if this draft standard is not approved by the UK, if it receives the necessary support in Europe, the UK will be obliged to publish the official English Language text unchanged as a British Standard and to withdraw any conflicting standard. UK Vot
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14、m are available from the BSI web site at: http:/www.bsi- Template for comments and secretariat observations Date: xx/xx/200x Document: ISO/DIS xxxxx 1 2 (3) 4 5 (6) (7) MB Clause No./ Subclause No./ Annex (e.g. 3.1) Paragraph/ Figure/Table/ Note (e.g. Table 1) Type of com- ment Comment (justificatio
15、n for change) by the MB Proposed change by the MB Secretariat observations on each comment submitted 3.1 Definition 1 ed Definition is ambiguous and needs clarifying. Amend to read . so that the mains connector to which no connection . 6.4 Paragraph 2 te The use of the UV photometer as an alternativ
16、e cannot be supported as serious problems have been encountered in its use in the UK. Delete reference to UV photometer. Microsoft and MS-DOS are registered trademarks, and Windows is a trademark of Microsoft Corporation. Licensed Copy: London South Bank University, London South Bank University, Thu
17、 Dec 20 03:19:14 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM FINAL DRAFT prEN 15452 November 2007 ICS 65.080Will supersede CEN/TS 15452:2006 English Version Fertilizers - Determination of chelating agents - Determination of iron chelated by o,p-EDDHA
18、by reversed phase HPLC Engrais - Dosage des agents chlatants - Dosage du fer chlat par o,p-EDDHA par chromatographie liquide haute performance polarit de phase inverse Dngemittel - Bestimmung von Chelatbildnern - Bestimmung von Eisen-chelatisiertem o,p-EDDHA mit Umkehrphasen HPLC This draft European
19、 Standard is submitted to CEN members for unique acceptance procedure. It has been drawn up by the Technical Committee CEN/TC 260. If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this Europ
20、ean Standard the status of a national standard without any alteration. This draft European Standard was established by CEN 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 noti
21、fied to the CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Ma
22、lta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and shall not be referred to as a European Sta
23、ndard. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2007 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. prEN 15452:2007: E
24、Licensed Copy: London South Bank University, London South Bank University, Thu Dec 20 03:19:14 GMT+00:00 2007, Uncontrolled Copy, (c) BSI prEN 15452:2007 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references4 3 Principle4 4 Interferences 4 5 Reagents.4 6 Apparatus .6 7 Sampling and sample p
25、reparation.6 8 Procedure .6 9 Expression of results 8 10 Precision.8 11 Test report9 Annex A (informative) Typical chromatogram .10 Annex B (informative) Statistical results of the inter-laboratory test 11 Annex C (informative) Complete names of chelating agents .12 Bibliography13 Licensed Copy: Lon
26、don South Bank University, London South Bank University, Thu Dec 20 03:19:14 GMT+00:00 2007, Uncontrolled Copy, (c) BSI prEN 15452:2007 (E) 3 Foreword This document (prEN 15452:2007) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is h
27、eld by DIN. This document is currently submitted to the Unique Acceptance Procedure. This document will supersede CEN/TS 15452:2006. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. Licensed Copy: London South Bank Unive
28、rsity, London South Bank University, Thu Dec 20 03:19:14 GMT+00:00 2007, Uncontrolled Copy, (c) BSI prEN 15452:2007 (E) 4 1 Scope This European Standard specifies a method for the chromatographic determination of the amount of iron chelated by each of the individual isomers of the chelating agent or
29、tho-para EDDHA (o,p-EDDHA) in fertilizers. The method allows the identification of this chelating agent and the determination of the water soluble fraction of iron chelated by this chelating agent. The method is not applicable for the determination of the amount of free chelating agent. NOTE 1 This
30、method has been shown to be also suitable for the determination of the amount of iron chelated by each of the individual isomers of the chelating agent ortho-ortho EDDHA (o,o-EDDHA) in fertilizers. NOTE 2 o,o-EDDHA and o,p-EDDHA are abbreviations used in this European Standard for the sake of simpli
31、city. For complete names see Annex C. NOTE 3 The substances o,o-EDDHA and o,p-EDDHA both exist as different stereoisomers. For o,o-EDDHA a meso form and a d/l pair (the racemic isomers) exist, for o,p-EDDHA two different d/l pairs exist. All four stereoisomers are observed separately in this method.
32、 NOTE 4 Currently, an analytically pure standard only exists for o,o-EDDHA. The method for o,p-EDDHA has been developed with an o,p-EDDHA standard containing an uncertain concentration of o,p-EDDHA. 2 Normative references The following referenced documents are indispensable for the application of th
33、is 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, Fertilizers and liming materials Sampling and sample preparation Part 2: Sample preparation 3 Principle The techniqu
34、e used is reversed phase HPLC with UV detection at 277 nm. The sample is separated on a silica-based reversed phase column using sodium formate, c = 0,015 mol/l, pH = 3,0, and acetonitrile as mobile phase. For both o,p-EDDHA and o,o-EDDHA, two stereoisomer peaks are observed. The concentration of ir
35、on chelated by o,p-EDDHA (o,p-Fe) is determined according to the external standard method. 4 Interferences No interferences have been detected. Iron chelates with EDTA, HEDTA, DTPA and EDDHMA do not interfere. 5 Reagents 5.1 General a) all reagents shall be of recognized analytical grade. Licensed C
36、opy: London South Bank University, London South Bank University, Thu Dec 20 03:19:14 GMT+00:00 2007, Uncontrolled Copy, (c) BSI prEN 15452:2007 (E) 5 b) all water should conform to EN ISO 3696. c) when products with a declared purity of less than 99 % are used for the preparation of standard solutio
37、ns, a correction should be made in order to obtain the required concentration in the solution. 5.2 Sodium hydroxide solution c(NaOH) = 0,1 mol/l Dissolve 4 g of NaOH in pellet form in water in a 1 000 ml-volumetric flask. Dilute to the mark and homogenize. 5.3 Hydrochloric acid solution c(HCl) = 4 m
38、ol/l Dilute 395 g of concentrated hydrochloric acid (37 %) to 1 000 ml with water. 5.4 Hydrochloric acid solution c(HCl) = 0,1 mol/l Dilute 25 ml of hydrochloric acid (5.3) to 1 000 ml with water. 5.5 Iron (III) nitrate solution (Fe) = 4 200 mg/l Dissolve 3,04 g of iron (III) nitrate nonahydrate Fe(
39、NO3)3.9H2O in 80 ml of water. Add 1 ml of hydrochloric acid (5.3). Transfer to a 100 ml-volumetric flask. Dilute to the mark with water and homogenize. Check that the Fe concentration of this solution is 4 200 mg/ 100 mg/l for example by AAS or iodometric titration. This solution is stable for appro
40、ximately one week. 5.6 o,p-Fe-EDDHA standard solution (o,p-Fe) = 100 mg/l Weigh to the nearest 0,1 mg (64,5 1)*100/purity (%) mg of o,p-H4-EDDHA (mco,p, see 5.1c) in a 100 ml beaker. Add 5 ml of NaOH (5.2) and carefully dissolve the sample by stirring. Add, after complete dissolution, 35 ml of water
41、 and 2,5 ml of iron (III) nitrate solution (5.5). Adjust the pH of the solution to 3,0 with NaOH (5.2) or HCl (5.4). Transfer the solution quantitatively to a 100 ml-volumetric flask. Dilute to the mark with water and homogenize. 5.7 Eluent solution Dissolve 1,0 g of sodium formate in 800 ml of wate
42、r. Adjust the pH to 3,0 with HCl (5.3 or 5.4). Transfer the solution to a 1 000 ml-volumetric flask. Dilute to the mark with water and homogenize. Filter the solution through a 0,45 m membrane filter. Mix 915 ml of the sodium formate solution, pH 3,0, with 85 ml of acetonitrile. Homogenize and degas
43、 the solution. NOTE The quality and the status of the column may have an influence on the retention times. To adjust the retention times, it may be necessary to slightly change the ratio of sodium formate solution and acetonitrile. Licensed Copy: London South Bank University, London South Bank Unive
44、rsity, Thu Dec 20 03:19:14 GMT+00:00 2007, Uncontrolled Copy, (c) BSI prEN 15452:2007 (E) 6 6 Apparatus 6.1 General Usual laboratory equipment, glassware, and: 6.2 Magnetic stirrer Magnetic stirrer with magnets. 6.3 Chromatograph equipped with: a) isocratic pump delivering the eluent at a flow rate
45、of 1,0 ml/min; b) injection valve with a 20 l injection loop; c) C18 modified silica column (ODS-2); 2504,6 mm ID; dp = 5 m1); d) use of a C18 guard column (ODS-2) is recommended; e) UV/VIS-detector with a 277-nm-filter; f) integrator. 6.4 Membrane filters Micromembrane filters resistant to aqueous
46、solutions with porosity of 0,45 m. 7 Sampling and sample preparation 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. NOTE For the size reduction of samples with a
47、 high amount of chelating agents, it is not recommended to use a high speed laboratory mill. It is more convenient to grind the sample in a mortar to a particle size less than 1 mm. 8 Procedure 8.1 Preparation of the sample solution Weigh to the nearest 0,1 mg approximately (250 10) mg of sample (ms
48、) in a 250 ml-beaker. Add 200 ml of water and dissolve the sample by stirring for 30 min. Transfer the solution quantitatively to a 250 ml volumetric flask. Dilute to the mark with water and homogenize. 1) Spherisorb ODS-2 from Waters or Allsphere ODS-2 from Alltech are examples of suitable products
49、 available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by CEN of these products. Licensed Copy: London South Bank University, London South Bank University, Thu Dec 20 03:19:14 GMT+00:00 2007, Uncontrolled Copy, (c) BSI prEN 15452:2007 (E) 7 NOTE If the o,p-Fe concentration is lower than 0,5 % or higher than 5 % the concentration of these iron chelates will be outsid