Fertilizers - Determination of water content (Karl Fischer methods) - Part 1: Methanol as extracting medium

This European Standard specifies a Karl Fischer titrimetric method for the determination of the water content of fertilizers based on the use of methanol as extracting medium.
The method is applicable to all solid mineral fertilizers. The result (KFM water) includes "free" water and extracted water of crystallization from the following components of fertilizers: calcium nitrate tetrahydrate (Ca(NO3)2·4H2O); calcium hydrogen phosphate dihydrate (CaHPO4·2H2O); calcium sulfate dihydrate (gypsum, CaSO4·2H2O), calcium sulfate hemihydrate (CaSO4·0,5H2O); magnesium sulfate heptahydrate (MgSO4·7H2O) ; potassium chloride magnesium sulfate water (1/1/2,75, Kainite, KCl·MgSO4·2,75H2O); potassium magnesium sulfate hexahydrate (Schoenite, K2SO4·MgSO4·6H2O); potassium magnesium sulfate tetrahydrate (Leonite, K2SO4·MgSO4·4H2O); potassium sulfate calcium sulfate monohydrate (Syngenite, K2SO4·CaSO4·H2O); potassium chloride magnesium chloride hexahydrate (Carnallite, KCl·MgCl2·6H2O); magnesium nitrate hexahydrate (Mg(NO3)2·6H2O).
Metal oxides and hydroxides soluble in methanol and pyridine will have an effect which can be corrected for, if their content is known.

Düngemittel - Bestimmung des Wassergehaltes (Karl-Fischer-Verfahren) - Teil 1: Methanol als Extraktionsmittel

Diese Europäische Norm legt ein titrimetrisches Karl-Fischer-Verfahren für die maßanalytische Bestimmung des Wasser-gehaltes von Düngemitteln fest, das auf der Verwendung von Methanol als Extraktionsmittel basiert.
Das Verfahren gilt für alle festen mineralischen Düngemittel. Das Ergebnis (KFM-Wasser) umfasst ?freies" Wasser sowie extrahiertes Kristallwasser der folgenden Düngemittelbestandteile: Calciumnitrattetrahydrat (Ca(NO3)2 · 4H2O); Calciumhydrogenphosphatdihydrat (CaHPO4 · 2H2O); Calciumsulfatdihydrat (Gips, CaSO4 · 2H2O), Calciumsulfa-themihy-drat (CaSO4 · 0,5H2O); Magnesiumsulfatheptahydrat (MgSO4 · 7H2O); Kaliumchlorid-Magnesiumsulfathydrat-wasser (1/1/2,75, Kainit, KCl · MgSO4 · 2,75H2O); Kalium-Magnesium-sulfat-hexahydrat (Schoenit, K2SO4 · MgSO4 · 6H-2O); Kalium-Magnesiumsulfattetrahydrat (Leonit, K2SO4 · MgSO4 · 4H2O); Kaliumsulfat-Calciumsulf-atmonohydrat (Syngenit, K2SO4 · CaSO4 · H2O); Kaliumchlorid-Magnesiumchloridhexahydrat (Carnallit, KCl · MgCl2 · 6H2O); Magnesiumnitrathexahy-drat (Mg(NO3)2 · 6H2O).
In Methanol und Pyridin lösliche Metalloxide und Hydroxide haben Auswirkungen, die jedoch korrigiert werden können, falls deren Anteil bekannt ist.

Engrais - Détermination de la teneur en eau (Méthodes Karl Fischer) - Partie 1: Le méthanol comme milieu d'extraction

La présente norme spécifie une méthode Karl Fischer de titrage de la teneur en eau des engrais, reposant sur l'utilisation de méthanol comme milieu d'extraction.
La méthode est applicable a toutes les engrais solides. Le résultat (eau KFM) englobe l'eau "libre" et l'eau de cristallisation des éléments suivants des matieres fertilisantes : nitrate de calcium tétrahydraté (Ca(NO3)2.4H2O), hydrogénophosphate de calcium dihydraté (CaHPO4).2H2O), sulfate de calcium dihydraté (gypse, (CaSO4.2H2O), sulfate de calcium hémihydraté (CaSO4.0,5 H2O), sulfate de magnésium heptahydraté (MgSO4.7H2O), eau au sulfate de magnésium/chlorure de potassium (1°1/2,75, Kainite, KCl MgSO4.2,75H2O), sulfate de magnésium-potassium hexahydraté (Schoenite, K2SO4 MgSO4.6H2O), sulfate de magnésium-potassium tétrahydraté (Léonite, K2SO4 MgSO4 . 4H2O), sulfate de potassium - sulfate de calcium monohydraté (Syngénite, K2SO4 CaSO4.H2O), chlorure de potassium - chlorure de magnésium hexahydraté (carnallite, KCl MgCl2.6H2O), nitrate de magnésium hexahydraté (Mg(NO3)2.6H2O).
Les oxydes et les hydroxydes de métaux solubles dans le méthanol et la pyridine ont un effet qui peut etre corrigé si leur teneur est connue.

Gnojila - Določevanje količine vode (Karl Fischerjeve metode) - 1. del: Ekstrakcija z metanolom

General Information

Status
Published
Publication Date
31-Oct-2002
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-Nov-2002
Due Date
01-Nov-2002
Completion Date
01-Nov-2002

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.PHWDQRORPDüngemittel - Bestimmung des Wassergehaltes (Karl-Fischer-Verfahren) - Teil 1: Methanol als ExtraktionsmittelEngrais - Détermination de la teneur en eau (Méthodes Karl Fischer) - Partie 1: Le méthanol comme milieu d'extractionFertilizers - Determination of water content (Karl Fischer methods) - Part 1: Methanol as extracting medium65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 13466-1:2001SIST EN 13466-1:2002en01-november-2002SIST EN 13466-1:2002SLOVENSKI
STANDARD



SIST EN 13466-1:2002



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13466-1October 2001ICS 65.080English versionFertilizers - Determination of water content - (Karl Fischermethods) - Part 1: Methanol as extracting mediumEngrais - Détermination de la teneur en eau (Méthodes KarlFischer) - Partie 1: Le méthanol comme milieu d'extractionDüngemittel - Bestimmung des Wassergehaltes (Karl-Fischer-Verfahren) - Teil 1: Methanol als ExtraktionsmittelThis European Standard was approved by CEN on 18 August 2001.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the 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 translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2001 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13466-1:2001 ESIST EN 13466-1:2002



EN 13466-1:2001 (E)2ContentspageForeword.3Introduction.41Scope.52Normative references.53Principle.54Reagents.55Apparatus.56Installation and test of the Karl Fischer titrator.67Sampling.68Procedure.69Calculation and expression of results.810Precision.911Test report.9Bibliography.10SIST EN 13466-1:2002



EN 13466-1:2001 (E)3ForewordThis European Standard has been prepared by Technical Committee CEN/TC 260 "Fertilizers and limingmaterials", 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 orby endorsement, at the latest by April 2002, and conflicting national standards shall be withdrawn at the latest byApril 2002.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden,Switzerland and the United Kingdom.SIST EN 13466-1:2002



EN 13466-1:2001 (E)4IntroductionThe water content of fertilizers has a significant effect on their quality and, especially, their storage and handlingproperties.Water can be present in a number of forms such as free water, bound water and water of crystallization. It is oftenimportant to be able to distinguish between these forms of water. The gravimetric methods for determination ofwater standardized in EN 12048 and EN 12049 have only limited applicability.The Karl Fischer method is applicable to a wide range of fertilizers. However, there are several variations to thebasic technique, different formulations of the Karl Fischer reagents are commercially available and a number ofdifferent solvents can be used. In this standard, methanol and 2-propanol are used as extracting media todistinguish between the different forms of water present in fertilizers.EN 13466 "Fertilizers – Determination of water content (Karl Fischer methods)" consists of two parts: Part 1 : Methanol as extracting medium Part 2 : 2-propanol as extracting mediumAs examples of the difference between methanol and 2-propanol as extracting media methanol gives a result whichis a combination of free water and extracted water of crystallization from the following components of fertilizers:calcium nitrate tetrahydrate (Ca(NO3)2·4H2O); calcium hydrogen phosphate dihydrate (CaHPO4·2H2O); calciumsulfate dihydrate (gypsum, CaSO4·2H2O)
calcium sulfate hemihydrate (CaSO4·0,5H2O); magnesium sulfateheptahydrate (MgSO4·7H2O); potassium chloride magnesium sulfate water (1/1/2,75, Kainite,KCl·MgSO4·2,75H2O); potassium magnesium sulfate hexahydrate (Schoenite, K2SO4·MgSO4·6H2O); potassiummagnesium sulfate tetrahydrate (Leonite, K2SO4·MgSO4·4H2O); potassium sulfate calcium sulfate monohydrate(Syngenite, K2SO4·CaSO4·H2O); potassium chloride magnesium chloride hexahydrate (Carnallite, KCl·MgCl2·6H2O); magnesium nitrate hexahydrate (Mg(NO3)2·6H2O).Extraction with 2-propanol gives a result which is a combination of free water and extracted water of crystallizationfrom the following components of fertilizers: calcium nitrate tetrahydrate (Ca(NO3)2·4H2O); magnesium sulfateheptahydrate (MgSO4·7H2O); potassium chloride magnesium chloride hexahydrate (Carnallite, KCl·MgCl2·6H2O);magnesium nitrate hexahydrate (Mg(NO3)2·6H2O).SIST EN 13466-1:2002



EN 13466-1:2001 (E)51 ScopeThis European Standard specifies a Karl Fischer titrimetric method for the determination of the water content offertilizers based on the use of methanol as extracting medium.The method is applicable to all solid mineral fertilizers. The result (KFM water) includes "free" water and extractedwater of crystallization from the following components of fertilizers: calcium nitrate tetrahydrate (Ca(NO3)2·4H2O);calcium hydrogen phosphate dihydrate (CaHPO4·2H2O); calcium sulfate dihydrate (gypsum, CaSO4·2H2O), calciumsulfate hemihydrate (CaSO4·0,5H2O); magnesium sulfate heptahydrate (MgSO4·7H2O) ; potassium chloridemagnesium sulfate water (1/1/2,75, Kainite, KCl·MgSO4·2,75H2O); potassium magnesium sulfate hexahydrate(Schoenite, K2SO4·MgSO4·6H2O); potassium magnesium sulfate tetrahydrate (Leonite, K2SO4·MgSO4·4H2O);potassium sulfate calcium sulfate monohydrate (Syngenite, K2SO4·CaSO4·H2O); potassium chloride magnesiumchloride hexahydrate (Carnallite, KCl·MgCl2·6H2O); magnesium nitrate hexahydrate (Mg(NO3)2·6H2O).Metal oxides and hydroxides soluble in methanol and pyridine will have an effect which can be corrected for, if theircontent is known.2 Normative referencesThis European Standard incorporates by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text, and the publications are listed hereafter. Fordated references, subsequent amendments to or revisions of any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision. For undated references the latest edition of thepublication referred to applies (including amendments).EN 1482, Sampling of solid fertilizers and liming materials.3 PrincipleExtraction of w
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