EN 17043:2018

Fertilizers - Determination of molybdenum in concentrations ≤ 10 % using spectrometry of a complex with ammonium thiocyanate

This European Standard specifies a method for determination of total and water extractable molybdenum in mineral fertilizers containing less than or equal to 10 % molybdenum.
This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 16962 and/or EN 16964.

Düngemittel - Bestimmung von Molybdän in Konzentrationen ≤ 10 % durch Spektrometrie eines Komplexes mit Ammoniumthiocyanat

Diese Europäische Norm legt ein Verfahren zur Bestimmung von Gesamtmolybdän und von wasserextrahierbarem Molybdän in mineralischen Düngemitteln, die weniger als oder gleich 10 % Molybdän enthalten, fest.
Dieses Verfahren ist auf Wasser  und Königswasser Extrakte von Düngemitteln anwendbar, die nach EN 16962 und/oder EN 16964 erhalten wurden.

Engrais - Dosage du molybdène dans des concentrations ≤ 10 % par spectrométrie d'un complexe avec du thiocyanate d'ammonium

La présente Norme européenne spécifie une méthode pour le dosage du molybdène total et du molybdène extractible à l’eau dans des engrais minéraux contenant au plus 10 % de molybdène.
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.

Gnojila - Določevanje molibdena v koncentracijah, manjših ali enakih 10 %, s spektrometrijo kompleksa z amonijevim tiocianatom

Ta dokument določa postopek za določevanje skupne vsebnosti molibdena in molibdena, ki ga je mogoče ekstrahirati z vodo, v mineralnih gnojilih, ki vsebujejo manj kot oziroma 10 % molibdena. Metode ekstrahiranja so določene v standardu EN 260172 in/ali EN 260176.

General Information

• Status: Published
• Publication Date: 12-Jun-2018
• Withdrawal Date: 30-Dec-2018
• ICS: 65.080 - Fertilizers
• Technical Committee: CEN/TC 260 - Fertilizers and liming materials
• Drafting Committee: CEN/TC 260/WG 7 - Chemical analysis
• Directive: 2003/2003 - Regulation (EC) N° 2003/2003 of the European Parlament and of the council of 13 October 2003 relating to fertilisers
• Directive: 2019/1009 - Regulation (EU) 2019/1009 of the European Parliament and of the Council of 5 June 2019 laying down rules on the making available on the market of EU fertilising products and amending Regulations (EC) No 1069/2009 and (EC) No 1107/2009 and repealing Regulation (EC) No 2003/2003
• Mandate: M/335 - Standardization Mandate assigned to the CEN concerning the modernisation of the methods of anylysis of Fertilizers
• Ref Project: SIST EN 17043:2018 - Fertilizers - Determination of molybdenum in concentrations ≤ 10 % using spectrometry of a complex with ammonium thiocyanate

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.XUFK65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 17043:2018SIST EN 17043:2018en,fr,de01-september-2018SIST EN 17043:2018SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 17043
June
t r s z ICS
x wä r z r English Version
Fertilizers æ Determination of molybdenum in concentrations ≤
s r
¨ using spectrometry of a complex with ammonium thiocyanate Engrais æ Dosage du molybdène dans des concentrations ≤
s r
¨ par spectrométrie d 5un complexe avec du thiocyanate d 5ammonium
Düngemittel æ Bestimmung von Molybdän in Konzentrationen ≤
s r
¨ durch Spektrometrie eines Komplexes mit Ammoniumthiocyanat This European Standard was approved by CEN on
t x February
t r s zä
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 y r v uã t r s z ESIST EN 17043:2018

European foreword . 3 Introduction . 4 1 Scope . 5 2 Normative references . 5 3 Terms and definitions . 5 4 Principle . 5 5 Sampling and sample preparation . 5 6 Reagents . 5 7 Apparatus . 7 8 Procedure. 7 8.1 Preparation of calibration solutions . 7 8.2 Preparation of the test solutions . 7 8.3 Development and separation of the complex . 7 8.4 Measurement . 8 9 Calculation and expression of the result . 8 10 Test report . 8 Annex A (informative)
Verification data – Comparison of ICP-AES method and spectrophotometric method with ammonium thiocyanate . 10 A.1 Introduction . 10 A.2 Validation based on water extraction. 10 A.2.1 Test materials used in the validation study . 10 A.2.2 Results of the validation study . 11 A.2.3 Conclusions . 12 A.3 Validation based on aqua regia extraction . 12 A.3.1 Test materials used in the validation study . 12 A.3.2 Comparison of ICP-AES and spectrophotometry . 14 A.3.3 Comparison of HCl- and aqua regia extraction . 15 A.3.4 Conclusions . 16 Bibliography . 17
= 1,18 g/ml. 6.2.1 Diluted hydrochloric acid solution, with a concentration of about 6 mol/l. Mix one volume of hydrochloric acid (6.2) with one volume of water (6.1). 6.2.2 Diluted hydrochloric acid solution, with a concentration of about 0,5 mol/l. Add 42 ml of hydrochloric acid (6.2) to approximately 600 ml of water (6.1) in a 1 000 ml volumetric flask (7.4). Fill to the mark with water (6.1) after cooling. 6.3 Copper solution,
= 70 mg/l in 1,5 mol/l hydrochloric acid. Dissolve 275 mg of copper sulfate (CuSO4 5H2O) weighed to within 0,1 mg in 250 ml of the 6 mol/l hydrochloric acid solution (6.2.1) in a 1 000 ml volumetric flask (7.4). Make up to volume with water (6.1) and mix thoroughly. 6.4 Ascorbic acid solution,
= 50 g/l. Dissolve 50 g of ascorbic acid (C6H8O6) in water (6.1) in a 1 000 ml volumetric flask (7.4). Make up to volume with water (6.1), mix thoroughly and keep in a refrigerator. 6.5 n-butyl acetate. 6.6 Ammonium thiocyanate solution, c = 0,2 mol/l. Dissolve 15,224 g of ammonium thiocyanate (NH4SCN) in water (6.1) in a 1 000 ml volumetric flask (7.4). Make up to volume with water (6.1), mix thoroughly and store in a dark-coloured bottle. 6.7 Stannous chloride solution,
= 50 g/l in 2 mol/l hydrochloric acid. This solution shall be perfectly clear and prepared immediately before use. Very pure stannous chloride shall be used otherwise the solution will not be clear. For the preparation of 100 ml of solution, dissolve 5 g of (SnCl2 2H2O) in 35 ml of 6 mol/l hydrochloric acid solution (6.2.1). Add 10 ml of the copper solution (6.3). Make up to volume with water (6.1) and mix thoroughly. 6.7.1 Molybdenum stock solution,
= 1 000 mg/l. Dissolve 1,840 g of ammonium molybdate [(NH4)6Mo7O24 4H2O] weighed to within 0,1 mg in the 0,5 mol/l hydrochloric acid (6.2.2) in a 1 000 ml volumetric flask (7.4). Make up to volume with that solution and mix thoroughly. Commercially available stock solutions with adequate specification may be used. The solution is considered to be stable for more than one year, but in reference to guaranteed stability, the recommendations of the manufacturer shall be considered. 6.7.2 Molybdenum intermediate solution,
= 100 mg/l. Place 10 ml of the stock solution (6.7.1) in a 100 ml volumetric flask (7.3). Make up to volume with 0,5 mol/l hydrochloric acid (6.2.2) and mix thoroughly. 6.7.3 Molybdenum working solution,
= 10 mg/l. Place 10 ml of the intermediate solution (6.7.2) in a 100 ml volumetric flask (7.3). Make up to volume with 0,5 mol/l hydrochloric acid (6.2.2) and mix thoroughly. SIST EN 17043:2018
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