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1、BRITISH STANDARD BS EN 15360:2007 Fertilizers Determination of dicyandiamide Method using high-performance liquid chromatography (HPLC) The European Standard EN 15360:2007 has the status of a British Standard ICS 65.080 ? Licensed Copy: London South Bank University, London South Bank University, Sun
2、 Jun 17 07:15:49 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS EN 15360:2007 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 29 June 2007 BSI 2007 ISBN 978 0 580 50881 3 National foreword This British Standard was published by BSI. It is the
3、UK implementation of EN 15360:2007. The UK participation in its preparation was entrusted to Technical Committee CII/37, Fertilisers and related chemicals. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include
4、all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. Amendments issued since publication Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank Un
5、iversity, Sun Jun 17 07:15:49 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15360 May 2007 ICS 65.080Supersedes CEN/TS 15360:2006 English Version Fertilizers - Determination of dicyandiamide - Method using high- performance liquid chromatography (HPL
6、C) Engrais - Dtermination de la teneur en dicyandiamide - Mthode par chromatographie liquide haute performance (HPLC) Dngemittel - Bestimmung von Dicyandiamid - Verfahren mit Hochleistungs-Flssigchromatographie (HPLC) This European Standard was approved by CEN on 13 April 2007. CEN members are bound
7、 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 to the CEN
8、 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 Management Centre has the same statu
9、s 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, Malta, Netherlands, Norway, Poland, Portugal, Romania,
10、 Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. 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 wor
11、ldwide for CEN national Members. Ref. No. EN 15360:2007: E Licensed Copy: London South Bank University, London South Bank University, Sun Jun 17 07:15:49 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15360:2007 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references4 3 Principle4 4 Reagents.4
12、 5 Apparatus .4 6 Sampling and sample preparation.5 7 Procedure .5 8 Calculation6 9 Precision.6 10 Notes on procedure.7 11 Test report7 Annex A (informative) Results of the inter-laboratory trial.8 Bibliography9 Licensed Copy: London South Bank University, London South Bank University, Sun Jun 17 07
13、:15:49 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15360:2007 (E) 3 Foreword This document (EN 15360:2007) 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
14、 standard, either by publication of an identical text or by endorsement, at the latest by November 2007, and conflicting national standards shall be withdrawn at the latest by November 2007. This document supersedes CEN/TS 15360:2006. This document has been prepared under a mandate given to CEN by t
15、he 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 Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finl
16、and, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: London South Bank University, London South Bank University, Sun Jun
17、17 07:15:49 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15360:2007 (E) 4 1 Scope This document specifies a method for the selective determination of dicyandiamide (DCD) in addition to all the other forms of nitrogen fixations, particularly in fertilizers to which DCD has been added as a nitrificat
18、ion inhibiting agent. 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 1
19、482-2, Fertilizers and liming materials Sampling and sample preparation Part 2: Sample preparation EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) 3 Principle The sample is dissolved or suspended in water using an ultrasonic bath. Methyl dicyandiamide
20、is added to the filtered solution as the internal standard. The solution is then transferred onto a C18 reversed-phase column using a bypass injector and then separated. For detection, a UV-detector is used at a wavelength of 220 nm. 4 Reagents Use only reagents of recognized analytical grade and wa
21、ter conforming to grade 2 of EN ISO 3696. 4.1 Dicyandiamide standard solution Weigh 50 mg of dicyandiamide of known purity into a 1 000 ml volumetric flask and dissolve in water; make up the volume to the mark. Pipette 10 ml of this solution into a 100 ml volumetric flask and, after having added 10
22、ml of internal standard solution (4.2), make up the volume to the mark with water. 4.2 Internal standard solution Weigh 50 mg of methyl dicyandiamide of known purity into a 1 000 ml volumetric flask, dissolve in water and make up the volume to the mark. 4.3 Methanol HPLC-grade purity 5 Apparatus 5.1
23、 Ultrasonic bath 5.2 Membrane filter 0,45 m, with the usual filtration equipment. Licensed Copy: London South Bank University, London South Bank University, Sun Jun 17 07:15:49 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15360:2007 (E) 5 5.3 HPLC apparatus UV-detector for variable wavelengths and
24、an electronic integrator, sample injection valve equipped with a 20 l bypass injector. 6 Sampling and sample preparation Sampling is not part of the method specified in this document; however, a recommended sampling method is given in EN 1482-1. Sample preparation shall be carried out in accordance
25、with EN 1482-2. 7 Procedure 7.1 Preparing the analytical solution Weigh to the nearest 0,001 g, between 0,8 g and 1,5 g of the ground and thoroughly homogenized test sample (corresponding to approximately 50 mg of DCD) and mix with 750 ml of water into a 1 000 ml volumetric flask and dissolve using
26、an ultrasonic bath (5.1). Those portions that have not dissolved after 5 min are disregarded. Make up the volume to the mark with water. Filter one part of the homogenized sample solution (approximately 50 ml) through the membrane filter (5.2) into a dry vessel. Pipette 10 ml of this filtrate into a
27、 100 ml volumetric flask and, after having added 10 ml of the internal standard solution (4.2), make up the volume to the mark with water. 7.2 HPLC conditions Eluent: Mixture of water and methanol (4.3), (99 + 1) parts by volume Separation column and packing: 250 mm x 4,6 mm C18 reversed-phase colum
28、n Column temperature: Room temperature Flow rate: 1,0 ml/min Wavelength: 220 nm 7.3 HPLC determination Alternately, transfer the standard solution (4.1) and the test solution (7.1) onto the separation column three times, applying the standard solution before the test solution. Measure the peak areas
29、 for DCD and methyl dicyandiamide. Licensed Copy: London South Bank University, London South Bank University, Sun Jun 17 07:15:49 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15360:2007 (E) 6 8 Calculation Calculate the proportion in the standard solution (4.1), Px according to the following equati
30、on: 2 1 x A A P= (1) where A1 is the peak area for DCD (4.1); A2 is the peak area of the internal standard. Calculate the proportion in the test solution (7.1), Px according to the following equation: 2 3 x A A P = (2) where A2 is the peak area of the internal standard; A3 is the peak area for DCD (
31、of 7.1). Take from each of the groups three values for Px and Px, the mean values PxM and PxM, and calculate the DCD content of the sample, expressed in g/100 g using the following equation: mPx mPx w = M M DCD (3) where PxM is the mean value of the proportions for the sample; PxM is the mean value
32、of the proportions for the standard; m is the mass of DCD in the standard solution (4.1) (50 mg), in milligrams; m is the mass of the sample in the aliquot part of the test solution (7.1) used, in milligrams. If necessary, correct the final result depending on the purity of the DCD used for the stan
33、dard solution. 9 Precision 9.1 General The precision of the method has been determined in an inter-laboratory trial, carried out and evaluated in 1997 according to ISO 5725-1. A summary of the results is given in Annex A. The values derived from this inter-laboratory trial might not be applicable to
34、 concentration ranges and matrices other than those given. Licensed Copy: London South Bank University, London South Bank University, Sun Jun 17 07:15:49 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15360:2007 (E) 7 9.2 Repeatability The absolute difference between two independent single test resul
35、ts obtained using the same method on identical test material in the same laboratory by the same operator using the same equipment within short time intervals, will exceed the values for the repeatability limit r, given in Table 1, on average in no more than 5 % of cases. 9.3 Reproducibility The abso
36、lute difference between two independent single test results obtained using the same method on identical test material in different laboratories by different operators using different equipment will exceed the values for the reproducibility limit R, given in Table 1, on average in no more than 5 % of
37、 cases. Table 1 Precision data Sample Level g/100 g r g/100 g R g/100 g No 1 (Alzon 27/1) 2,41 0,089 98 0,466 7 No 2 (Alzon 27/2) 2,18 0,073 7 0,329 10 Notes on procedure 10.1 As described, the method covers a range between 2 g and 10 g of DCD per 100 g. By variation of the weighed portion and the e
38、xtent of dilution, DCD contents of between (0,1 g and 100 g) per 100 g can be determined. 10.2 The method may also be carried out using an external standard. In this case the equation for the calculation has to be modified accordingly. 11 Test report The test report shall include at least the follow
39、ing information: a) information necessary for complete identification of the sample; b) test method used, making reference to this document, i.e. EN 15360; c) test results together with the units used to express them; d) date the test was finished; e) statement as to whether the requirement for the
40、repeatability limit has been fulfilled; f) procedural steps not specified in this document or carried out optionally, as well as details of any circumstances that occurred while carrying out the method that might have influenced the result(s). Licensed Copy: London South Bank University, London Sout
41、h Bank University, Sun Jun 17 07:15:49 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15360:2007 (E) 8 Annex A (informative) Results of the inter-laboratory trial The precision of the method was determined in 1997 during an inter-laboratory trial with respectively 13 and 12 laboratories participating
42、 and carried out on 2 samples of fertilizer. The statistical results are given in Table A.1. Table A.1 Statistical results of the inter-laboratory trial Parameter Sample No 1 Sample No 2 Year of the test 1997 Number of participating laboratories 13 12 Number of laboratories after eliminating outlier
43、s 13 12 Level mean value, (g/100 g) 2,41 2,18 Repeatability standard deviation sr, (g/100 g) 0,03 0,03 Coefficient of variation CVr (%) 1,348 1,218 Repeatability limit r (2,83 sr) (g/100 g) 0,089 98 0,073 7 Reproducibility standard deviation, sR (g/100 g) 0,168 4 0,118 7 Coefficient of variation CVR
44、 (%) 6,99 5,44 Reproducibility limit R (2,83 sR) (g/100 g) 0,466 7 0,329 Licensed Copy: London South Bank University, London South Bank University, Sun Jun 17 07:15:49 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15360:2007 (E) 9 Bibliography 1 Vilsmeier, K., 1984: Bestimmung von Dicyandiamid, Nitr
45、it und Nitrat in Bodenextrakten mit Hochdruckflssigkeitschromatographie. Zeitschrift fr Pflanzenernhrung, Dngung und Bodenkunde 147, page 264 to 268 2 ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions 3 EN 1482-1, Fertilizers
46、and liming materials Sampling and sample preparation Part 1: Sampling 4 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 Licensed Copy: London South Bank University, London South Ba
47、nk University, Sun Jun 17 07:15:49 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS EN 15360:2007 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe a
48、nd at the international level. It is incorporated by Royal Charter. Revisions British Standards are updated by amendment or revision. Users of British Standards 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
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