DIN EN 15962-2011 Fertilizers - Determination of the complexed micro-nutrient content and of the complexed fraction of micro-nutrients German version EN 15962 2011《肥料 复合微量营养含量和微量营养.pdf

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1、April 2011 Translation by DIN-Sprachendienst.English price group 10No 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).ICS

2、65.080!$nm“1757493www.din.deDDIN EN 15962Fertilizers Determination of the complexed micro-nutrient content and of thecomplexed fraction of micro-nutrientsEnglish translation of DIN EN 15962:2011-04Dngemittel Bestimmung des Gehalts an komplexgebundenen Spurennhrstoffionen und derkomplexgebundenen Fra

3、ktion von SpurennhrstoffenEnglische bersetzung von DIN EN 15962:2011-04Engrais Dosage de la teneur en oligo-lment complex et de la fraction complexe desoligo-lmentsTraduction anglaise de DIN EN 15962:2011-04www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be c

4、onsidered authoritative.03.11 16DIN EN 15962:2011-04 A comma is used as the 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/418 (Project management: Spain). The resp

5、onsible German body involved in its preparation was the Normenausschuss Lebensmittel und landwirtschaftliche Produkte (Food and Agricultural Products Standards Committee), Working Committee NA 057-03-02 AA Dngemittel. The DIN Standards corresponding to the International Standards referred to in this

6、 document are as follows, whereby EN ISO Standards are only listed below if these have not been published as DIN EN ISO Standards with the same number: EN ISO 3696 DIN ISO 3696 ISO 5725-2 DIN ISO 5725-2 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Sp

7、ecification and test methods DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15962 January 2011

8、 ICS 65.080 English Version Fertilizers - Determination of the complexed micro-nutrient content and of the complexed fraction of micro-nutrients Engrais - Dosage de la teneur en oligo-lment complex et de la fraction complexe des oligo-lments Dngemittel - Bestimmung des Gehalts an komplexgebundenen S

9、purennhrstoffionen und der komplexgebundenen Fraktion von Spurennhrstoffen This European Standard was approved by CEN on 3 December 2010. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a nationa

10、l 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 three official versions (English, French, German). A versio

11、n 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 bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Cze

12、ch 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 United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUR

13、OPEN 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 15962:2011: EEN 15962:2011 (E) 2 Contents Page Foreword 31 Scope 42 Norm

14、ative references 43 Principle 44 Interferences 45 Apparatus .46 Reagents .57 Preparation of the sample .58 Procedure .58.1 Preparation of the sample solution 58.2 Precipitation .68.3 Spectrometric determination 68.4 Water-soluble micro-nutrient content determination .69 Expression of results 79.1 Co

15、mplexed micro-nutrient content in the fertilizer 79.2 Complexed fraction of a micro-nutrient in the fertilizer.710 Precision .710.1 Inter-laboratory test .710.2 Repeatability .810.3 Reproducibility .811 Test report 8Annex A (informative) Results of the inter-laboratory test 10A.1 Test samples . 10A.

16、2 Inter-laboratory test procedure . 10A.3 Results and statistical interpretation 10Bibliography . 14DIN EN 15962:2011-04 EN 15962:2011 (E) 3 Foreword This document (EN 15962:2011) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held

17、 by DIN. This 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 July 2011, and conflicting national standards shall be withdrawn at the latest by July 2011. Attention is drawn to the possibility that som

18、e of the elements 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 has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. Acc

19、ording 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, Hungary, Iceland, Ireland, I

20、taly, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 15962:2011-04 EN 15962:2011 (E) 4 1 Scope This European Standard specifies a general method for the determination of the micronutr

21、ients complexed by complexing agents in fertilizers. The method allows the determination of the total concentration of each complexed micronutrient in complexes after subtraction of the chelated micro-nutrients content, but it does not identify the individual complexing agents. This procedure concer

22、ns EC-fertilizers which contain complexed micro-nutrients covered by Regulation (EC) No 2003/2003. The method is applicable to a mass fraction of the metal complexed of at least 0,07 %, 0,006 % and 0,035 % of Fe, Mn and Zn respectively (see 2). A lower limit of quantification has not been establishe

23、d for Cu and Co. 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 1482-2

24、, Fertilizers and liming materials Sampling and sample preparation Part 2: Sample preparation EN ISO 3696:1995, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) 3 Principle The method is based on the precipitation of the inorganic forms at pH 9. Then the complexed f

25、orms of an element remain in solution and are separated from the non complexed forms. The complexed forms are collected and their content determined by spectrometry, as well as the soluble element content. NOTE For additional information see 2 and 3. 4 Interferences Any substance combining with a mi

26、cro-nutrient to form a stable soluble compound (chelate or complex) at pH 9, will prevent the precipitation of the metal, and account for a certain degree of complexation. This is the case for chelating agents. If the presence of chelates is suspected the appropriate analytical method should be used

27、 (see Bibliography) to identify and quantify the amount of element chelated, that should be subtracted from the amount of the element given by this method in order to obtain the actual amount of element complexed. 5 Apparatus All glassware, filters, and equipment parts coming in contact with samples

28、 and solutions, should be appropriate for micro-nutrient analysis, be very clean and free from contamination, especially by the elements Co, Cu, Fe, Mn, and Zn. Usual laboratory equipment, glassware and in particular the following: 5.1 Magnetic stirrer. 5.2 Balance, capable for weighing to an accura

29、cy of 1 mg. 5.3 pH-meter, equipped with a glass electrode; the system shall be calibrated with pH 7 and pH 10 calibration buffers. 5.4 Membrane filters, micro-membrane filters resistant to aqueous solutions, with porosity of 0,45 m. DIN EN 15962:2011-04 EN 15962:2011 (E) 5 5.5 Cellulose filters, fas

30、t filtration quantitative cellulose filters. 6 Reagents All reagents shall be of recognized analytical grade. 6.1 Water used for the preparation of standard solutions. Water used for the preparation of standard solutions, and sample solutions shall conform to EN ISO 3696:1995, grade 1 and be free of

31、 organic contaminants. 6.2 Hydrogen peroxide, H2O2, 30 % to 33 %. 6.3 Sodium hydroxide solution, c(NaOH) = 0,5 mol/l. Carefully dissolve 20,0 g of NaOH in water and dilute to 1 l. This solution is also available commercially. 6.4 Sodium hydroxide solution, c(NaOH) = 0,05 mol/l. Carefully dissolve 2,

32、0 g of NaOH in water and dilute to 1 l. This solution is also available commercially. 6.5 Buffer solution, pH = 7,0. 6.6 Buffer solution, pH = 10,0. 7 Preparation of the sample Sampling is not part of the method specified in this document. A recommended sampling method is given in EN 1482-1. Sample

33、preparation shall be carried out in accordance with EN 1482-2. NOTE For the size reduction of samples with a high amount of complexing agents, it is not recommended to use a high speed laboratory mill. It is more convenient to grind the sample to a particle size less than 1 mm by the use of a mortar

34、 and pestle. 8 Procedure 8.1 Preparation of the sample solution Weigh, to the nearest 1 mg, a quantity of the fertilizer between 5 g and 10 g, depending on the declared content of the metal complex, into a 250 ml or 500 ml beaker. Add 200 ml or 400 ml of water. Stir using a magnetic stirrer (5.1) fo

35、r 1 h. Transfer quantitatively into a 250 ml or 500 ml volumetric flask. Dilute to the mark with water and homogenize. The mass of the test sample and volume of extract should be taken according to Table 1. DIN EN 15962:2011-04 EN 15962:2011 (E) 6 Table 1 Preparation of sample solution Parameter Dec

36、lared content of complexed micro-nutrient in the fertilizer 0,5 % 0,5 % Mass of test portion (g) 10 5 Mass of element in the sample (mg) 50 25 Volume of the extract (ml) 250 500 Concentration of the element in the extract after precipitation (mg/l) 40 10 If insoluble matter is observed, filter immed

37、iately after the final volume has been reached using cellulose filters (5.5). 8.2 Precipitation Pipette 20 ml of the solution (8.1) into a 50 ml beaker. Add two drops of H2O2(6.2), stir and rise pH, with NaOH 0,5 mol/l (6.3) or 0,05 mol/l (6.4), to 9,0 as fast as possible in order to avoid reaction

38、with atmospheric carbon dioxide. Cover the beaker. Rise pH again to 9,0 after 30 min and cover the beaker again. Let the solution stand for a minimum of 18 h and a maximum of 24 h in the dark. Readjust the pH to 9,0, transfer the sample to a 100 ml volumetric flask and dilute to the mark with water

39、(6.1). Filtrate the solution through the membrane filter (5.4). If precipitation is observed and filtration is difficult then samples may be centrifuged at 7 500 min-1at 20 C to 25 C for 10 min before filtration. The acidification of the solution required for the spectrometric determination (8.3) sh

40、ould be made as soon as possible after the precipitation process, in order to stabilize the solution. 8.3 Spectrometric determination Determine the micro-nutrient concentration in the filtrate after precipitation procedure (8.2) by atomic absorption spectrometry (AAS) or by inductively coupled plasm

41、a emission spectrometry (ICP-ES). The AAS determination may be carried out in accordance with the appropriate methods (see Regulation (EC) No 2003/2003). If flame AAS is used, removal of the organic compounds is required, and should be made in accordance with method 9.3 (1) using H2O2(6.2) and HCl 0

42、,5 mol/l for the digestion of the samples and 0,5 % La as La(NO3)3, 0,2 % Cs as CsCl and 5 % HCl as matrix modifier. Let d(i)be the micro-nutrient concentration of the filtrate, in milligrams per litre. 8.4 Water-soluble micro-nutrient content determination Extract following method 9.2 (1). The same

43、 sample solutions 8.1 may be used in some cases. Determine the water-soluble micro-nutrient content in the sample by AAS or by ICP. The AAS determination may be carried out in accordance with the appropriate EC methods, referred to in 1. If flame AAS is used, removal of the organic compounds is requ

44、ired and should be made in accordance with method 9.3 (1) using H2O2(6.2) and HCl 0,5 mol/l for the digestion of the samples and 0,5 % La as La(NO3)3, 0,2 % Cs as CsCl and 5 % HCl as matrix modifier. Let S(i)be the water-soluble micro-nutrient content in the sample, expressed as mass fraction in per

45、cent. DIN EN 15962:2011-04 EN 15962:2011 (E) 7 9 Expression of results 9.1 Complexed micro-nutrient content in the fertilizer The content of a complexed micro-nutrient (i) in the fertilizer, C(i), expressed as mass fraction in percent, is given by the following equation: WVdC=0002(i)(i)(1) where d(i

46、)is the micro-nutrient (i) concentration of the filtrate solution, in milligrams per litre; W is the mass of the test portion, in grams; V is the volume of the extract in millilitres. 9.2 Complexed fraction of a micro-nutrient in the fertilizer The complexed fraction F(i)of a micro-nutrient (i) is t

47、he ratio of the complexed micro-nutrient content C(i)to the water-soluble micro-nutrient content S(i)in the fertilizer, expressed as a percentage, and is given by the following equation: (i)(i)(i)100SCF = (2) where C(i)is the complexed micro-nutrient (i) content in percent (mass fraction); S(i)is th

48、e water-soluble micro-nutrient (i) content in percent (mass fraction). 10 Precision 10.1 Inter-laboratory test An inter-laboratory test has been carried out in 2008 with twelve participating laboratories and four different commercial samples. The results of this inter-laboratory test are summarized

49、in Annex A. The results of one of the samples (LS-2) were not statistically analyzed because soluble element content was very low and few laboratories were able to measure it. Repeatability and reproducibility were calculated according to ISO 5725-2. A second inter laboratory test was performed later in 2008 with ten participating laboratories and three different samples. In this test the method was modified, but it did