EN 13475:2001

Liming materials - Determination of calcium content - Oxalate method

This European Standard specifies a method for the determination of the calcium content of silicate liming materials including slags.
NOTE 1   The method has been shown to be suitable for other liming materials too, but there are no precision data available yet.
NOTE 2   The method is also applicable for the determination of the calcium content of mineral fertilizers.

Calcium-/Magnesium-Bodenverbesserungsmittel - Bestimmung des Calciumgehaltes - Oxalatverfahren

Diese Europäische Norm legt ein Verfahren zur Bestimmung des Calciumgehaltes von Kalken aus Eisenhütten-schlacken sowie anderer silikatischer Schlacken fest.
ANMERKUNG 1   Das Verfahren hat sich auch für andere Calcium-/Magnesium-Bodenverbesserungsmittel als geeignet erwiesen, jedoch liegen derzeit diesbezüglich keine Präzisionsdaten vor.
ANMERKUNG 2   Das Verfahren gilt auch für die Bestimmung des Calciumgehaltes von mineralischen Düngemitteln.

Amendements minéraux basiques - Détermination de la teneur en calcium - Méthode à l'oxalate

Le présent projet de Norme européenne spécifie une méthode de détermination de la teneur en calcium des amendements minéraux basiques contenant des silicates de calcium, y compris les amendements basiques sidérurgiques
NOTE 1   La méthode a été reconnue comme utilisable pour l'analyse des autres amendements minéraux basiques, mais on ne dispose pas encore  dans ce cas, de données de fidélité.
NOTE 2   La méthode est également applicable à la détermination de la teneur en calcium des engrais minéraux.

Sredstva za apnjenje - Določevanje kalcija - Oksalatna metoda

General Information

• Status: Published
• Publication Date: 13-Nov-2001
• Withdrawal Date: 30-May-2002
• ICS: 65.080 - Fertilizers
• Technical Committee: CEN/TC 260 - Fertilizers and liming materials
• Drafting Committee: CEN/TC 260/WG 3 - Liming materials
• Current Stage: 9093 - Decision to confirm - Review Enquiry
• Start Date: 08-Jul-2022
• Completion Date: 14-Apr-2025
• Ref Project: SIST EN 13475:2002 - Liming materials - Determination of calcium content - Oxalate method

Overview

EN 13475:2001 is a European Standard developed by the European Committee for Standardization (CEN) that specifies a precise and reliable method for determining the calcium content in silicate liming materials, including slags, using the oxalate method. This standard is also applicable to other liming materials and mineral fertilizers, ensuring versatile use across agricultural and industrial sectors. The oxalate method described in EN 13475:2001 is essential for quality control, material characterization, and compliance with regulatory requirements in fertilizer and soil amendment industries.

Key Topics

• Scope and Application

  • Specifies determination of calcium content in silicate liming materials and slags.
  • Applicable for other liming materials and mineral fertilizers although precision data for these are pending.

• Principle of the Method

  • Sample dissolution in hydrochloric and nitric acids.
  • Calcium precipitated as calcium oxalate at pH 4.4-4.6.
  • Separation of precipitate using immersion filters.
  • Dissolution of precipitate in sulfuric acid.
  • Titration with potassium permanganate to quantify calcium content.

• Reagents and Apparatus

  • Includes detailed preparation of reagents such as hydrochloric acid, nitric acid, ammonium oxalate, and potassium permanganate solutions.
  • Standard laboratory equipment required, including water bath, immersion filters, titration apparatus, and test sieves according to ISO 3310-1.

• Sampling and Preparation

  • Sampling in accordance with EN 1482 to ensure representative and consistent samples.
  • Sample drying at 105 ± 2 °C, grinding to pass a 250 µm sieve, and homogenization for accurate testing.

• Analytical Procedure

  • Precise steps from sample digestion to titration.
  • Use of color indicators and pH adjustment for optimal calcium oxalate precipitation.
  • Filtration and washing of precipitate followed by dissolution and endpoint titration under controlled conditions.

• Calculation and Expression of Results

  • Calcium oxide content expressed as a mass fraction (% CaO).
  • Conversion formulas provided for results on dry material basis and for calcium content (% Ca).
  • Clear instructions for adjusting results based on sample moisture content.

• Accuracy and Precision

  • Repeatability and reproducibility limits defined through interlaboratory tests.
  • Ensures confidence in test results across different laboratories and operators.

• Test Reporting

  • Standardized reporting format with sample identification, reference to EN 13475:2001, results, units, observations, and deviations from the method.

Applications

• Agriculture

  • Determining calcium content in liming materials used to improve soil properties, pH adjustment, and enhance crop yields.
  • Testing mineral fertilizers for compliance with nutrient content specifications.

• Industrial

  • Quality control of silicate slags and other by-products used as liming agents or soil conditioners.
  • Monitoring calcium levels in raw materials to ensure suitability for specific applications.

• Environmental

  • Assessing amendments used for soil remediation projects where calcium availability influences soil chemistry and contaminant fate.

Related Standards

• EN 1482: Sampling of solid fertilizers and liming materials – pivotal for correct sampling prior to calcium analysis.
• ISO 3310-1: Test sieves – technical requirements for sieve sizes used in sample preparation.
• Other CEN standards covering fertilizer and liming material testing and classification, contributing to a comprehensive regulatory framework.

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Keywords: EN 13475:2001, calcium content determination, liming materials, oxalate method, silicate slags, mineral fertilizers, CEN standard, fertilizer testing, calcium analysis, soil amendments, potassium permanganate titration, European Standard, laboratory method.

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Calcium-/Magnesium-Bodenverbesserungsmittel - Bestimmung des Calciumgehaltes - OxalatverfahrenAmendements minéraux basiques - Détermination de la teneur en calcium - Méthode a l'oxalateLiming materials - Determination of calcium content - Oxalate method65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 13475:2001SIST EN 13475:2002en01-november-2002SIST EN 13475:2002SLOVENSKI
STANDARD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13475November 2001ICS 65.080English versionLiming materials - Determination of calcium content - OxalatemethodAmendements minéraux basiques - Détermination de lateneur en calcium - Méthode à l'oxalateCalcium-/Magnesium-Bodenverbesserungsmittel -Bestimmung des Calciumgehaltes - OxalatverfahrenThis European Standard was approved by CEN on 29 September 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 13475:2001 ESIST EN 13475:2002

ScopeThis European Standard specifies a method for the determination of the calcium content of silicate liming materialsincluding slags.NOTE 1The method has been shown to be suitable for other liming materials too, but there are no precision data available yet.NOTE 2The method is also applicable for the determination of the calcium content of mineral fertilizers.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.ISO 3310-1, Test sieves – Technical requirements and testing – Part 1: Test sieves of metal wire cloth.3 PrincipleAfter dissolution of the sample in a mixture of hydrochloric acid and nitric acid, calcium is precipitated in the form ofcalcium oxalate at a pH between 4,4 and 4,6. The supernatant solution is removed by means of an immersion filter.The calcium oxalate precipitate is dissolved in sulfuric acid and the calcium content is determined by titration withpotassium permanganate.4 Reagents4.1 GeneralCommercially available standard solutions may be used instead of standard solutions produced in the laboratory.Variations in concentration shall be taken into account for the calculation of the results.4.2Hydrochloric acid, 20(HCl) = 1,19 g/ml, c(HCl) = 12,5 mol/l.4.3Nitric acid, 20(HNO3) = 1,40 g/ml, c(HNO3) = 14,9 mol/l.4.4Citric acid solutionDissolve 300 g of citric acid monohydrate in water and make up to 1 l.4.5Ammonium chloride solutionDissolve 100 g of ammonium chloride in water and make up to 1 l. Mix well.4.6Bromocresol greenDissolve 5 g of bromocresol green in ethanol with a volume concentration of ethanol of 96% and make up to 1 l.4.7Ammonium oxalate solution, saturatedDissolve sufficient ammonium oxalate monohydrate (approximately 70 g) in 1 l of water to produce a saturatedsolution. After reaching saturation, filter the solution.SIST EN 13475:2002
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