SIST EN 16198:2013
(Main)Fertilizers - Determination of magnesium by complexometry
Fertilizers - Determination of magnesium by complexometry
This European Standard specifies a method for the determination of magnesium in fertilizer extracts by complexometry. The method is applicable to the following EC fertilizer extracts for which the determination of total magnesium and/or water-soluble magnesium is provided for according to the Regulation (EC) No 2003/2003, Annex I: - fertilizers listed in, Annex I: straight nitrogenous fertilizers, type 1b + 1c (calcium magnesium nitrate), type 7 (magnesium sulfonitrate), type 8 (nitrogenous fertilizers with magnesium) and straight potassic fertilizers, type 2 (enriched kainite), type 4 (potassium chloride containing magnesium), type 6 (potassium sulfate containing magnesium salt); - fertilizers listed in, Annex I D relating to secondary nutrients.
Düngemittel - Komplexometrische Bestimmung von Magnesium
Diese Europäische Norm legt ein Verfahren zur Bestimmung von Magnesium in Düngemittelextrakten fest.
Das Verfahren gilt für die folgenden EG-Düngemittelextrakte, für die die Angabe des Gesamtmagnesiums und/oder des wasserlöslichen Magnesiums entsprechend der Verordnung (EG) Nr. 2003/2003, Anhang I, [3], vorgeschrieben ist:
in [3], Anhang I, aufgeführte Düngemittel: Einnährstoff-Stickstoffdünger vom Typ 1b 1c (Calcium-Magnesiumnitrat), Typ 7 (Stickstoff-Magnesiumsulfat), Typ 8 (Stickstoffdünger mit Magnesium) und Einnährstoff-Kalidünger vom Typ 2 (angereichertes Kainit), Typ 4 (Kaliumchlorid mit Magnesium), Typ 6 (Kaliumsulfat mit Magnesium);
in [3], Anhang I D, aufgeführte Düngemittel mit Bezug auf Sekundärnährstoffe.
Engrais - Dosage du magnésium par complexométrie
La présente norme européenne spécifie une méthode de dosage du magnésium, par complexométrie, dans les extraits d’échantillons d’engrais.
Cette méthode est applicable aux extraits d’échantillons d’engrais CE pour lesquels le dosage du magnésium total et/ou soluble eau est prévu, conformément au Règlement (CE) n° 2003/2003, Annexe I de la référence bibliographique [3] :
engrais répertoriés dans l’Annexe I de la référence bibliographique [3] ; engrais azotés simples, type 1b + 1c (nitrate de calcium et de magnésium), type 7 (sulfonitrate de magnésium), type 8 (engrais azotés contenant du magnésium) et engrais potassiques simples, type 2 (kaïnite enrichie), type 4 (chlorure de potassium contenant du magnésium), type 6 (sulfate de potassium contenant du sel de magnésium) ;
engrais répertoriés dans l’Annexe I D de la référence bibliographique [3] relative aux éléments nutritifs secondaires.
Gnojila - Kompleksometrijsko določevanje magnezija
Ta evropski standard določa metodo za določevanje magnezija v ekstraktih gnojil s kompleksometrijo. Metoda se uporablja za naslednje ekstrakte gnojil ES, za katere je predvideno določanje količine skupnega magnezija in/ali v vodi topnega magnezija v skladu s Prilogo I k Uredbi (ES) št. 2003/2003: – gnojila, uvrščena na seznam v Prilogi I: enostavna dušična gnojila vrste 1b + 1c (kalcij-magnezijev nitrat), vrste 7 (magnezijev sulfonitrat), vrste 8 (dušična gnojila z magnezijem) in enostavna kalijeva gnojila vrste 2 (obogateni kajnit), vrste 4 (kalijev klorid, ki vsebuje magnezij), vrste 6 (kalijev sulfat, ki vsebuje magnezijevo sol); – gnojila, uvrščena na seznam v Prilogi I D v zvezi s sekundarnimi hranili.
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel - Komplexometrische Bestimmung von MagnesiumEngrais - Dosage du magnésium par complexométrieFertilizers - Determination of magnesium by complexometry65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 16198:2012SIST EN 16198:2013en,fr,de01-maj-2013SIST EN 16198:2013SLOVENSKI
STANDARDSIST-TS CEN/TS 16198:20111DGRPHãþD
SIST EN 16198:2013
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16198
November 2012 ICS 65.080 Supersedes CEN/TS 16198:2011English Version
Fertilizers - Determination of magnesium by complexometry
Engrais - Dosage du magnésium par complexométrie
Düngemittel - Komplexometrische Bestimmung von Magnesium This European Standard was approved by CEN on 6 October 2012.
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 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 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-CENELEC Management Centre has the same status as the official versions.
CEN members are the national standards bodies of 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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16198:2012: ESIST EN 16198:2013
EN 16198:2012 (E) 2 Contents Page Foreword .31 Scope .42 Normative references .43 Terms and definitions .44 Principle .45 Sampling .46 Reagents .57 Apparatus .68 Preparation of the extraction solution .69 Procedure .69.1 Control test .69.2 Aliquot samples to be taken .79.3 Titration in the presence of Eriochrome black-T .79.4 Titration in the presence of calcein or of calcon carbonic acid .710 Calculation and expression of the result .711 Remarks .712 Precision .812.1 Inter-laboratory test .812.2 Repeatability .812.3 Reproducibility .813 Test report .9Annex A (informative)
Statistical results of the inter-laboratory test . 10Bibliography . 12 SIST EN 16198:2013
EN 16198:2012 (E) 3 Foreword This document (EN 16198:2012) 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 May 2013, and conflicting national standards shall be withdrawn at the latest by May 2013. Attention is drawn to the possibility that some 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 supersedes CEN/TS 16198:2011. The following changes have been made to the former edition: a) the CEN Technical Specification has been adopted as a European Standard; b) the document has been editorially revised. 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 organisations 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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
SIST EN 16198:2013
EN 16198:2012 (E) 4 1 Scope This European Standard specifies a method for the determination of magnesium in fertilizer extracts by complexometry. The method is applicable to the following EC fertilizer extracts for which the determination of total magnesium and/or water-soluble magnesium is provided for according to the Regulation (EC) No 2003/2003, Annex I [3]: fertilizers listed in [3], Annex I: straight nitrogenous fertilizers, type 1b + 1c (calcium magnesium nitrate), type 7 (magnesium sulfonitrate), type 8 (nitrogenous fertilizers with magnesium) and straight potassic fertilizers, type 2 (enriched kainite), type 4 (potassium chloride containing magnesium), type 6 (potassium sulfate containing magnesium salt); fertilizers listed in [3], Annex I D relating to secondary nutrients. 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 1482-2, Fertilizers and liming materials — Sampling and sample preparation — Part 2: Sample preparation EN 12944-1:1999, Fertilizers and liming materials and soil improvers — Vocabulary — Part 1: General terms EN 12944-2:1999, Fertilizers and liming materials and soil improvers — Vocabulary — Part 2: Terms relating to fertilizers EN 15960, Fertilizers — Extraction of total calcium, total magnesium, total sodium and total sulfur in the forms of sulfates EN 15961, Fertilizers — Extraction of water soluble calcium, magnesium, sodium and sulfur in the form of sulfates 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 12944-1:1999 and EN 12944-2:1999 apply. 4 Principle The magnesium is solubilised according to EN 15960 or EN 15961. First titration: with EDTA of Ca and Mg in the presence of Eriochrome black-T. Second titration: with EDTA of Ca in the presence of calcein or of calcone carbonic acid. Determination of magnesium by difference. 5 Sampling Sampling is not part of the method specified in this document. A recommended sampling method is given in EN 1482-1. Sample preparation shall be carried out in accordance with EN 1482-2. Grinding of the laboratory sample is recommended for homogeneity reasons. SIST EN 16198:2013
EN 16198:2012 (E) 5 6 Reagents 6.1 Magnesium standard solution, c = 0,05 mol/l. 6.1.1 Dissolve 1,232 g of magnesium sulfate (MgSO4 7H2O) in the hydrochloric acid solution (6.11) and make up to 100 ml with the same acid, or 6.1.2 Weigh 2,016 g of magnesium oxide, previously calcined to remove all traces of carbonation. Place it in a beaker with 100 ml of water. Stir in approximately 120 ml of hydrochloric acid (6.12). After dissolution, transfer quantitatively into a graduated 1 000 ml flask. Make up to volume and mix. 1 ml of these solutions should contain 1,216 mg of Mg (= 2,016 mg of MgO). The laboratory is responsible for testing the strength of this standard solution. 6.2 EDTA solution, c = 0,05 mol/l. Weigh 18,61 g of the dihydrated disodium salt of ethylenediaminetetraacetic (EDTA) (C10H14N2Na2O8,2H2O), place it in a beaker (7.4) and dissolve in 600 ml to 800 ml of water. Transfer the solution quantitatively into a graduated flask (7.3). Make up the volume and mix. Check this solution with the standard solution (6.1) by taking a sample of 20 ml of the latter and by titration according to the analytical procedure described in 9.2. 1 ml of the EDTA solution should correspond to 1,216 mg of Mg (= 2,016 mg of MgO) and to 2,004 mg of Ca (= 2,804 mg CaO) (see remarks 11.1 and 11.6). 6.3 Calcium standard solution, c = 0,05 mol/l. Weigh 5,004 g of dry calcium carbonate. Place it in a beaker with 100 ml of water. Progressively stir in 120 ml of hydrochloric acid (6.12). Bring to the boil in order to drive off the carbon dioxide, cool, transfer quantitatively into a graduated 1 l flask, make up the volume with water and mix. Check this solution against the EDTA solution (6.2) following analytical procedure (9.3). 1 ml of this solution should contain 2,004 mg of Ca (= 2,804 mg of CaO) and should correspond to 1 ml of the EDTA solution (6.2). 6.4 Calcein indicator. Carefully mix in a mortar 1 g of calcein with 100 g of sodium chloride. Use 10 mg of this mixture. The indicator changes from green to orange. Titration shall be carried out until an orange is obtained which is free from green tinges. 6.5 Calcon carbonic acid indicator. Dissolve 400 mg of calcon carbonic in 100 ml of methanol. This solution may only be kept for approximately four weeks. Use three drops of this solution. The indicator changes
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