EN 16965-2018 Fertilizers - Determination of cobalt copper iron manganese and zinc using flame atomic absorption spectrometry (FAAS).pdf

1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Fertilizers Determination of cobalt, copper, iron, manganese and zinc using flame atomic absorption spectrometry (FAAS)BS EN 16965:2018EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16965 January 2018 ICS 65.080 E

2、nglish Version Fertilizers - Determination of cobalt, copper, iron, manganese and zinc using flame atomic absorption spectrometry (FAAS) Engrais - Dosage du cobalt, du cuivre, du fer, du manganse et du zinc par spectromtrie dabsorption atomique de flamme (FAAS) Dngemittel - Bestimmung von Cobalt, Ku

3、pfer, Eisen, Mangan und Zink mit Flammen-Atomabsorptionsspektrometrie (FAAS) This European Standard was approved by CEN on 15 October 2017. 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 natio

4、nal 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 vers

5、ion 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, C

6、zech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United

7、Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels 2018 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN

8、 16965:2018 ENational forewordThis British Standard is the UK implementation of EN 16965:2018.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

9、 secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0 580 91788 2ICS 65.080Compliance with a British Standard cann

10、ot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 February 2018.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN 16965:2018EUROPEAN STANDARD NORME EUROPENNE EUROP

11、ISCHE NORM EN 16965 January 2018 ICS 65.080 English Version Fertilizers - Determination of cobalt, copper, iron, manganese and zinc using flame atomic absorption spectrometry (FAAS) Engrais - Dosage du cobalt, du cuivre, du fer, du manganse et du zinc par spectromtrie dabsorption atomique de flamme

12、(FAAS) Dngemittel - Bestimmung von Cobalt, Kupfer, Eisen, Mangan und Zink mit Flammen-Atomabsorptionsspektrometrie (FAAS) This European Standard was approved by CEN on 15 October 2017. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving

13、 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 three offici

14、al 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 bodies of A

15、ustria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, S

16、pain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels 2018 CEN All rights of exploitation in any form and by any means reserved wo

17、rldwide for CEN national Members. Ref. No. EN 16965:2018 EBS EN 16965:2018EN 16965:2018 (E) 2 Contents Page European foreword . 3 Introduction 4 1 Scope 5 2 Normative references 5 3 Terms and definitions . 5 4 Principle . 5 5 Interferences 5 6 Reagents . 6 7 Apparatus . 7 8 Procedure. 7 8.1 Preparat

18、ion of test and blank solutions . 7 8.2 Preparation of the calibration solutions 7 8.3 Measurement 7 9 Calculation and expression of the results 8 10 Precision . 8 10.1 Inter-laboratory test 8 10.2 Repeatability . 9 10.3 Reproducibility 9 11 Test report 11 Annex A (informative) Statistical results o

19、f the inter-laboratory test . 12 Bibliography . 22 BS EN 16965:2018EN 16965:2018 (E) 3 European foreword This document (EN 16965:2018) 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 give

20、n the status of a national standard, either by publication of an identical text or by endorsement, at the latest by July 2018, and conflicting national standards shall be withdrawn at the latest by July 2018. Attention is drawn to the possibility that some of the elements of this document may be the

21、 subject of patent rights. CEN 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. According to the CEN-CENELEC Internal Regulations, the national

22、 standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuan

23、ia, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16965:2018EN 16965:2018 (E) 4 Introduction The preparation of this document is based on a mandate given to CEN by the European Commissio

24、n and the European Free Trade Association (Mandate M/335) concerning the modernization of methods of analysis of fertilizers in the framework of Regulation (EC) No 2003/2003 1. This document is part of a modular approach and concerns the analytical measurement step. “Modular” means that a test stand

25、ard concerns a specific step in assessing a property and not the whole chain of measurements. Flame atomic absorption spectrometry (FAAS) is widely used and well established in most laboratories. The European Standard can be used for the determination of cobalt, copper, iron, manganese and zinc in a

26、ll extracts prepared according to EN 16962 and EN 16964. The method can be applied to mineral fertilizers with micro-nutrient content of 10 % as well as of 10 %. The inter-laboratory study reflects the final properties of the method for determination of individual micro-nutrients in water and aqua r

27、egia extracts including extraction steps. WARNING Persons using this European Standard should be familiar with normal laboratory practice. This European Standard does not purport to address all of the safety issues, if any, associated with its use. It is the responsibility of the user to establish a

28、ppropriate health and safety practices and to ensure compliance with any national regulatory conditions. IMPORTANT It is absolutely essential that tests conducted according to this European Standard are carried out by suitably trained staff. BS EN 16965:2018EN 16965:2018 (E) 5 1 Scope This European

29、Standard specifies a method for the determination of cobalt, copper, iron, manganese and zinc in fertilizer extracts using flame atomic absorption spectrometry (FAAS). This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 16962 and/or EN 16964. NOTE In most c

30、ases, the presence of small quantities of organic matter will not affect determinations by FAAS and it is not necessary to apply organic matter removal. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its appl

31、ication. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 12944-1, Fertilizers and liming materials and soil improvers Vocabulary Part 1: General terms EN 12944-2, Fertilizers and liming

32、 materials and soil improvers Vocabulary Part 2: Terms relating to fertilizers EN 16962, Fertilizers Extraction of water soluble micro-nutrients in fertilizers and removal of organic compounds from fertilizer extracts EN 16964, Fertilizers Extraction of total micro-nutrients in fertilizers using aqu

33、a regia EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 12944-1 and EN 12944-2 apply. 4 Principle The method is based on the FAAS measurement of the concentrati

34、on of the elements in fertilizer extracts prepared according to EN 16962 and/or EN 16964. The elements are determined after appropriate dilution of the extracts. Background correction, matrix matching and lanthanum addition are applied to remove possible interferences. 5 Interferences Matrix matchin

35、g can avoid interferences from different physical behaviour of the standards and samples (in particular, different viscosity can influence aspiration of the solution). Light scattering is eliminated by background correction. Ionization of cobalt, copper, iron, manganese and zinc in air-acetylene fla

36、me may be neglected. The formation of refractory compounds is prevented or reduced by adding a releasing agent (lanthanum). BS EN 16965:2018EN 16965:2018 (E) 6 6 Reagents All reagents shall be of recognized analytical grade and they shall have negligible concentration of the element to be determined

37、 if compared to the lowest concentration of that element in the sample solution. 6.1 Water, grade 2 according to EN ISO 3696, free from micro-nutrients. 6.2 Nitric acid, c(HNO3) = 14,3 mol/l; = 1,4 g/ml. 6.2.1 Diluted nitric acid solution, c(HNO3) = 5 mol/l. Add 350 ml of nitric acid (6.2) to 650 ml

38、 of water (6.1). 6.2.2 Diluted nitric acid solution, c(HNO3) = 0,5 mol/l. Dilute 35 ml nitric acid (6.2.) to 1 l with water (6.1). 6.3 Hydrochloric acid, c(HCl) = 12 mol/l; = 1,18 g/ml. 6.4 Mixed solution, 0,8 mol/l nitric acid and 1,8 mol/l hydrochloric acid. Add 150 ml of hydrochloric acid (6.3) a

39、nd 56 ml nitric acid (6.2) to 800 ml of water (6.1). 6.5 Standard stock solutions, cobalt, copper, iron, manganese and zinc standard stock solutions, = 1 000 mg/l for each element. Both single-element stock solutions and multi-element stock solutions with adequate specification, stating the acid use

40、d and the preparation technique, are commercially available. These solutions are considered to be stable for more than one year, but in reference to guaranteed stability, the recommendations of the manufacturer should be considered. Alternatively, the stock solutions may be prepared by dissolution o

41、f high purity metals. 6.5.1 Standard solution, = 100 mg/l of element. Pipette 10 ml of the appropriate standard stock solution (6.5) into a 100 ml volumetric flask. Add 10 ml of diluted nitric acid (6.2.1), fill to the mark with water and mix well. This solution is used to prepare spiked test soluti

42、ons and calibration solutions. 6.6 Lanthanum solution, = 10 g/l lanthanum. Place 11,73 g of lanthanum oxide (La2O3) in a 500 ml beaker, add 150 ml of water and slowly add 140 ml of diluted nitric acid (6.2.1). After complete dissolution transfer the solution quantitatively into a 1 000 ml volumetric

43、 flask and then make up to 1 l with water (6.1) and mix thoroughly. The substance concentration of this solution amounts to approximately 0,5 mol/l nitric acid. Alternatively, lanthanum chloride, lanthanum sulfate or lanthanum nitrate may be used. Alternative procedures: Dissolve 26,7 g of lanthanum

44、 chloride heptahydrate (LaCl3.7 H2O) or 31,2 g of lanthanum nitrate hexahydrate La(NO3)3.6 H2O or 26,2 g of lanthanum sulfate nonahydrate La2(SO4)3.9 H2O in 150 ml of water (6.1), then add 100 ml of diluted nitric acid (6.2.1). Allow to dissolve and then make up to 1 l with water (6.1). Mix thorough

45、ly. The substance concentration of this solution amounts to approximately 0,5 mol/l nitric acid. BS EN 16965:2018EN 16965:2018 (E) 7 7 Apparatus 7.1 Atomic absorption spectrometer, equipped with: a hollow cathode lamp or other suitable light emission source; background correction; a burner, suitable

46、 for an air-acetylene flame. WARNING It is essential that the manufacturers safety instructions are strictly observed when using this apparatus. 8 Procedure 8.1 Preparation of test and blank solutions Dilute an aliquot portion of the water or aqua regia extract obtained according to EN 16962 or EN 1

47、6964 in one or more steps so that a final concentration of the element to be determined is in the given calibration range (8.2). In the final diluting step add a suitable volume of the extract or diluted extract to a 100 ml volumetric flask, add 10 ml of diluted nitric acid (6.2.1), 10 ml of lanthan

48、um solution (6.6), fill to the mark with water and mix well. Prepare a blank solution by pipetting only extracting solution diluted in the same way as the test solution. For extracts where further dilution is not suitable pipette 20 ml of the sample extract into a 25 ml volumetric flask, add 2,5 ml

49、of lanthanum solution (6.6) and fill to the mark with water (6.1). Mix well and use for the measurement. 8.2 Preparation of the calibration solutions Pipette volumes of: 0 ml; 0,5 ml; 1 ml; 2 ml and 5 ml of the standard solution (6.5.1) into 100 ml volumetric flasks and add 10 ml of lanthanum solution (6.6). Add acid solution (6.2.1, 6.2.2 or 6.4) in a volume necessary to reach the same final acid concentration in the test (8.1) and calibration solutions, and fill to the mark with water. The mass concentrations of each e