SIST EN 13466-1:2002

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 à toutes les engrais solides. Le résultat (eau KFM) englobe l'eau "libre" et l'eau de cristallisation des éléments suivants des matières 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 être 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
• ICS: 65.080 - Fertilizers
• Technical Committee: KAT - Soil quality
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-Nov-2002
• Due Date: 01-Nov-2002
• Completion Date: 01-Nov-2002
• Ref Project: EN 13466-1:2001 - Fertilizers - Determination of water content (Karl Fischer methods) - Part 1: Methanol as extracting medium

Overview

EN 13466-1:2001 (CEN) specifies a Karl Fischer titrimetric method using methanol as the extracting medium to determine the water content of solid mineral fertilizers. The method measures a combined result (KFM water) that includes free water plus water of crystallization extracted by methanol from a range of commonly encountered hydrated fertilizer components. This standard is intended for routine quality control, formulation verification and storage/handling assessment.

Key Topics

• Scope and applicability: Method is applicable to all solid mineral fertilizers and reports KFM water as a mass fraction (%).
• Forms of water measured: The test result includes free water and water of crystallization from compounds such as:
  • calcium nitrate tetrahydrate (Ca(NO3)2·4H2O)
  • calcium hydrogen phosphate dihydrate (CaHPO4·2H2O)
  • calcium sulfate dihydrate/hemihydrate (gypsum CaSO4·2H2O, CaSO4·0.5H2O)
  • magnesium sulfate heptahydrate (MgSO4·7H2O)
  • various potassium/magnesium salts (kainite, schoenite, leonite, syngenite, carnallite)
  • magnesium nitrate hexahydrate (Mg(NO3)2·6H2O)
• Interferences and corrections: Metal oxides and hydroxides soluble in methanol and pyridine can affect results and may be corrected for when their content is known.
• Procedure variants: Two extraction paths depending on dispersibility in methanol:
  • Direct dispersion/titration in the titration vessel for methanol-dispersible fertilizers.
  • Separate centrifuge extraction and transfer of supernatant when dispersion is incomplete.
• Calibration & quality assurance: Karl Fischer reagent is standardized by titration against a known mass of water or sodium tartrate dihydrate. Drift correction and blank tests are required.

Applications

• Quality control (QC): Monitor moisture levels that affect nutrient stability and product specifications.
• Storage and handling: Determine water levels relevant to caking, flowability and shelf life.
• Formulation analysis: Identify contributions of hydrated salts to total water content when selecting drying or blending strategies.

Practical notes: typical apparatus includes a Karl Fischer titrator, balance (0.0001 g), centrifuge, dispersing turbine (eg. Ultra Turrax), and methanol with low water content. The standard provides guidance on test portion mass, extraction volumes, centrifugation and titration practice.

Related Standards

• EN 13466-2: Karl Fischer methods - 2-propanol as extracting medium (complements Part 1)
• EN 12048 and EN 12049: Gravimetric moisture determination methods for solid fertilizers

This standard delivers a reproducible, industry-recognized Karl Fischer titrimetric procedure for accurate water determination in solid mineral fertilizers, supporting regulatory compliance and reliable product handling.

Standards Content (Sample)

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
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

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
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