Fertilizers - Determination of cobalt, copper, iron, manganese and zinc using flame atomic absorption spectrometry (FAAS)

This European 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 prEN 16962 and/or prEN 16964.
NOTE   In most cases, the presence of small quantities of organic matter will not affect determinations by FAAS and it is not necessary to apply organic matter removal.

Düngemittel - Bestimmung von Cobalt, Kupfer, Eisen, Mangan und Zink mit Flammen-Atomabsorptionsspektrometrie (FAAS)

Diese Europäische Norm legt ein Verfahren zur Bestimmung von Cobalt, Kupfer, Eisen, Mangan und Zink in Düngemittelextrakten mit Flammen Atomabsorptionsspektrometrie (FAAS) fest.
Dieses Verfahren ist auf Wasser  und Königswasserextrakte von Düngemitteln anwendbar, die nach EN 16962 und/oder EN 16964 erhalten wurden.
ANMERKUNG   In den meisten Fällen wird das Vorhandensein geringer Mengen organischer Bestandteile die Bestimmung mit FAAS nicht beeinträchtigen, und es ist daher nicht notwendig, die Beseitigung organischer Bestandteile anzuwenden.

Engrais - Dosage du cobalt, du cuivre, du fer, du manganèse et du zinc par spectrométrie d'absorption atomique de flamme (FAAS)

La présente norme européenne spécifie une méthode pour le dosage du cobalt, du cuivre, du fer, du manganèse et du zinc dans les extraits d’engrais par spectrométrie d’absorption atomique de flamme (FAAS).
Cette méthode est applicable aux extraits d’engrais aqueux et à l’eau régale obtenus conformément à l’EN 16962 et/ou à l’EN 16964.
NOTE   Dans la plupart des cas, la présence de petites quantités de matière organique n’a aucune incidence sur les dosages par FAAS et il n’est pas nécessaire d’appliquer l’élimination de la matière organique.

Gnojila - Določevanje kobalta, bakra, železa, mangana in cinka s plamensko atomsko absorpcijsko spektrometrijo (FAAS)

Ta evropski standard določa metodo za določevanje kobalta, bakra, železa, mangana in cinka v ekstraktih gnojila s plamensko atomsko absorpcijsko spektrometrijo (FAAS).
Ta metoda se uporablja za ekstrakte gnojil v vodi in zlatotopki, pridobljene v skladu s standardom prEN 16962 in/ali prEN 16964.
OPOMBA:   V večini primerov prisotnost majhnih količin organske snovi ne bo vplivala na določitve FAAS in odstranjevanje organske snovi ni nujno.

General Information

Status
Published
Public Enquiry End Date
05-Apr-2016
Publication Date
17-May-2018
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
04-May-2018
Due Date
09-Jul-2018
Completion Date
18-May-2018

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.SODPHQVNRDüngemittel - Bestimmung von Cobalt, Kupfer, Eisen, Mangan und Zink mit Flammen-Atomabsorptionsspektrometrie (FAAS)Engrais - Dosage du cobalt, du cuivre, du fer, du manganèse et du zinc par spectrométrie d'absorption atomique de flamme (FAAS)Fertilizers - Determination of cobalt, copper, iron, manganese and zinc using flame atomic absorption spectrometry (FAAS)65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 16965:2018SIST EN 16965:2018en,fr,de01-junij-2018SIST EN 16965:2018SLOVENSKI

STANDARD
SIST EN 16965:2018
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16965
January
t r s z ICS
x wä r z r English Version

Fertilizers æ Determination of cobaltá copperá ironá manganese and zinc using flame atomic absorption Engrais æ Dosage du cobaltá du cuivreá du ferá du manganèse et du zinc par spectrométrie d 5absorption

Düngemittel æ Bestimmung von Cobaltá Kupferá Eisená Mangan und Zink mit FlammenæThis European Standard was approved by CEN on

s w October
t r s yä

egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä

translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä

CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä

EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre:
Rue de la Science 23,
B-1040 Brussels

t r s z CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN

s x { x wã t r s z ESIST EN 16965:2018

EN 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 Preparation 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 of the inter-laboratory test ..................................................... 12 Bibliography ................................................................................................................................................................. 22

SIST EN 16965:2018

EN 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 given 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 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 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, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16965:2018

EN 16965:2018 (E) 4 Introduction The preparation of this document is based on a mandate given to CEN by the European Commission 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 standard 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 all 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 regia 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 appropriate 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. SIST EN 16965:2018

EN 16965:2018 (E) 5 1 Scope This European 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 cases, 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 application. 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 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 aqua 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 concentration 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 matching 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 flame may be neglected. The formation of refractory compounds is prevented or reduced by adding a releasing agent (lanthanum). SIST EN 16965:2018

EN 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 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 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) and 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 used 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 of 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 solutions 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 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 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 thoroughly. The substance concentration of this solution amounts to approximately 0,5 mol/l nitric acid. SIST EN 16965:2018

EN 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 for an air-acetylene flame. WARNING — It is essential that the manufacturer’s 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 16964 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 lanthanum 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 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 element in the calibration solutions are: 0 mg/l; 0,5 mg/l; 1 mg/l; 2 mg/l and 5 mg/l. Mixed calibration solutions for all elements or individual sets of calibration solutions for each element may be used. If necessary, higher or lower concentrations of calibration solutions may be prepared in the same way. NOTE Small differences in acid concentration between sample extracts and calibration solutions do not usually affect the measurement. The calibration range may be extended for Fe and Mn up to 10 mg/l. Although it has been demonstrated that lanthanum addition and background correction is not necessary for some elements and/or matrices, it is strongly recommended to apply background correction and lanthanum addition for all elements and matrices. 8.3 Measurement Set up the atomic absorption spectrometer (7.1) according to the manufacturer's instructions at the appropriate wavelength (see Table 1). Aspirate a calibration solution (8.2) and optimize the aspiration conditions, burner height and flame conditions. Aspirate the set of calibration solutions in ascending order. Set the delay and the integration time according to the manufacturer's instructions (usually 3 s of delay and 3 s to 5 s of integration are sufficient). Care shall be taken to ensure that, when using more concentrated standards, the absorbance is < 1, and preferably not more than 0,7. The software of the instrument is used to plot the calibration graph and to calculate concentrations of the elements in the individual test solutions. All test solutions, blanks and calibration solutions are measured under the SIST EN 16965:2018

EN 16965:2018 (E) 8 same conditions using backgroun
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