Carbonate liming materials - Determination of reactivity - Automatic titration method with citric acid

This European Standard specifies a method for the determination of the reactivity of calcium carbonate and calcium magnesium carbonate liming materials. It assesses the speed and effectiveness of their neutralising potential by automatic titration with citric acid.
This method is applicable only to liming materials with a maximum particle size of 6,3 mm determined according to EN 12948.
NOTE   For marble dolomite (BET procedure according to ISO 9277 below 500 m2/kg), see EN 14984.

Carbonatische Kalke - Bestimmung der Reaktivität - Automatisches Titrationsverfahren mit Citronensäure

Diese Europäische Norm legt ein Verfahren für die Bestimmung der Reaktivität von Calciumcarbonat sowie carbonatischen Calcium-/Magnesium-Bodenverbesserungsmitteln fest. Die Geschwindigkeit und Wirksamkeit deren Neutralisationspotentials werden durch automatische Titration mit Citronensäure beurteilt.
Dieses Verfahren ist nur für Calcium-/Magnesium-Bodenverbesserungsmittel mit einer Korngröße von höchstens 6,3 mm, bestimmt nach EN 12948, anwendbar.
ANMERKUNG   Für Marmordolomit (BET-Verfahren nach ISO 9277 unter 500 m2/kg), siehe EN 14984.

Amendements minéraux basiques carbonatés - Détermination de la réactivité - Méthode par titration automatique à l'acide citrique

La présente norme européenne spécifie une méthode de détermination de la réactivité des amendements minéraux basiques à base de carbonate de calcium ou à base de carbonate de calcium et de magnésium. Il évalue la rapidité et l'efficacité de leur potentiel de neutralisation par titration automatique à l'acide citrique.
Cette méthode s'applique uniquement aux amendements minéraux basiques ayant une taille de particules maximale de 6,3 mm déterminée selon l'EN 12948.
NOTE   Pour les dolomies d’origine métamorphique (de type marbre) (Procédure BET selon l’ISO 9277 en-dessous de 500 m²/kg), voir EN 14984.

Karbonatna sredstva za apnjenje - Določevanje reaktivnosti - Metoda avtomatske titracije s citronsko kislino

Ta evropski standard določa metodo za določevanje reaktivnosti sredstev za apnenje s kalcijevim karbonatom in kalcijevim magnezijevim karbonatom. Ugotavlja hitrost in učinkovitost njihovega nevtralizacijskega potenciala z avtomatsko titracijo s citronsko kislino. Ta metoda se uporablja samo za sredstva za apnenje z največjo velikostjo delcev 6,3 mm, ki je v skladu s standardom EN 12948.

General Information

Status
Published
Publication Date
06-Aug-2013
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
05-Jun-2025
Completion Date
23-Sep-2025
Ref Project
SIST EN 16357:2013 - Carbonate liming materials - Determination of reactivity - Automatic titration method with citric acid

Overview - EN 16357:2013 (CEN)

EN 16357:2013 specifies a laboratory method for determining the reactivity of carbonate liming materials (calcium carbonate and calcium–magnesium carbonate) by an automatic titration method with citric acid. The procedure assesses the speed and effectiveness of a liming material’s neutralising potential by measuring citric acid consumption under controlled pH conditions. The method applies to samples with a maximum particle size of 6.3 mm (EN 12948) and uses a partial reaction over a fixed time (15 minutes) at pH 4.5 (pH stat).

Key topics and technical requirements

  • Principle: Limited decomposition of carbonate by citric acid; titration under stable pH (pH stat) and measurement of citric acid consumed in a set time.
  • Apparatus: automatic motor-driven burette/titrator with pH electrode, pH stat programme, propeller or magnetic stirring, suitable beakers and balance. Burette must deliver small accurate steps (modern titrators meet this).
  • Reagents: mono-hydrated citric acid (solution ca. 457.17 g/L prepared and used within specified storage limits), analytical-grade water, defoamer, pH buffers (pH 4 and pH 7).
  • Sample size & preparation:
    • Typical test portion: 5.0 g (±0.2 g) “as received”.
    • For coarser or heterogeneous materials (>1 mm or non-representative), prepare fraction-wise and use 10 g test portion (Annex A).
    • Moisture should be recorded (EN 12048) and sample preparation per EN 1482-2.
  • Calibration & quality control: pH electrode calibration with pH 4 and pH 7 buffers, electrode response time check, verification with a reference precipitated calcium carbonate (PCC) where applicable.
  • Outputs: citric-acid based reactivity value, neutralising value correction, and MgO content determination; precision and reproducibility data are provided in Clause 9.

Applications and who uses it

  • Practical uses:
    • Quality control of liming materials and fertilizers.
    • Comparative evaluation of neutralising speed (reactivity) for agronomic performance.
    • Regulatory compliance testing and product labelling.
  • Primary users:
    • Fertilizer and liming material manufacturers.
    • Independent testing laboratories and conformity assessment bodies.
    • Agricultural extension services, soil scientists, agronomists and regulatory agencies.

Related standards

  • EN 12948 - Liming materials: determination of size distribution (max particle size reference).
  • EN 1482-2 - Sampling and sample preparation for fertilizers and liming materials.
  • EN 12048 - Moisture determination for fertilizers/liming materials.
  • EN 14984 - Specific guidance for marble dolomite (BET < 500 m2/kg).
  • EN ISO 3696 - Water for analytical laboratory use.

Keywords: EN 16357:2013, carbonate liming materials, reactivity, automatic titration, citric acid, pH stat, neutralising value, liming materials testing.

Frequently Asked Questions

EN 16357:2013 is a standard published by the European Committee for Standardization (CEN). Its full title is "Carbonate liming materials - Determination of reactivity - Automatic titration method with citric acid". This standard covers: This European Standard specifies a method for the determination of the reactivity of calcium carbonate and calcium magnesium carbonate liming materials. It assesses the speed and effectiveness of their neutralising potential by automatic titration with citric acid. This method is applicable only to liming materials with a maximum particle size of 6,3 mm determined according to EN 12948. NOTE For marble dolomite (BET procedure according to ISO 9277 below 500 m2/kg), see EN 14984.

This European Standard specifies a method for the determination of the reactivity of calcium carbonate and calcium magnesium carbonate liming materials. It assesses the speed and effectiveness of their neutralising potential by automatic titration with citric acid. This method is applicable only to liming materials with a maximum particle size of 6,3 mm determined according to EN 12948. NOTE For marble dolomite (BET procedure according to ISO 9277 below 500 m2/kg), see EN 14984.

EN 16357:2013 is classified under the following ICS (International Classification for Standards) categories: 65.080 - Fertilizers. The ICS classification helps identify the subject area and facilitates finding related standards.

You can purchase EN 16357:2013 directly from iTeh Standards. The document is available in PDF format and is delivered instantly after payment. Add the standard to your cart and complete the secure checkout process. iTeh Standards is an authorized distributor of CEN standards.

Standards Content (Sample)


2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Carbonatische Kalke - Bestimmung der Reaktivität - Automatisches Titrationsverfahren mit CitronensäureAmendements minéraux basiques carbonatés - Détermination de la réactivité - Méthode par titration automatique à l'acide citriqueCarbonate liming materials - Determination of reactivity - Automatic titration method with citric acid65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 16357:2013SIST EN 16357:2013en,fr,de01-oktober-2013SIST EN 16357:2013SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16357
August 2013 ICS 65.080 English Version
Carbonate liming materials - Determination of reactivity - Automatic titration method with citric acid
Amendements minéraux basiques carbonatés - Détermination de la réactivité - Méthode par titration automatique à l'acide citrique
Carbonatische Kalke - Bestimmung der Reaktivität - Automatisches Titrationsverfahren mit Citronensäure This European Standard was approved by CEN on 29 June 2013.
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 © 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16357:2013: ESIST EN 16357:2013

Preparation of the test portion of liming materials coarser than 1 mm . 14 A.1 General . 14 A.2 Calculation of mass fractions retained on the test sieves . 14 A.3 Calculation of the test portion to be weighed . 14 Annex B (normative)
Arrangement of the test apparatus . 15 Bibliography. 16
= 457,17 g/l. Preferably, use a fresh home-made solution as described below. Under these conditions, the solution concentration is conventionally supposed to be equal to the necessary one, ca = 457,17 g pure citric acid per litre. SIST EN 16357:2013

is the added mass of mono hydrated citric acid (5.2), in grams; 192,14 is the molar mass of anhydrous citric acid, in grams; 210,14 is the molar mass of mono hydrated citric acid, in grams. 5.4 Calcium carbonate, precipitated (or PCC), mass fraction, w(CaCO3) at least 99 %. Commercial PCC for analysis is granted for its chemical characteristics. However, physical characteristics are not granted. As reactivity depends on fineness, even for PCC, it is essential to take as a reference a highly reactive PCC, such as commercial PCC from VWR / Prolabo / BDH, reference GPR, Rectapur, Ref 22296.294, Molar mass 100,09 1), which will consume 15 ml after 15 min. This PCC was used in the ring test before launching measurements. By experience, some PCC do not meet this requirement. See also the note in 7.2.6. 5.5 Silicone defoamer. 5.6 Standard buffer solution, pH 4 (commercial solution, pH 4,01). NOTE This solution has a limited lifetime. 5.7 Standard buffer solution, pH 7 (commercial solution, pH 6,98). NOTE This solution has a limited lifetime. 6 Sampling and sample preparation 6.1 General Sampling is not part of the methods 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.
1) This substance is an example of a suitable product available commercially. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of this product. SIST EN 16357:2013
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Die Norm EN 16357:2013 bietet eine klar definierte Methode zur Bestimmung der Reaktivität von carbonathaltigen Kalkungsmaterialien, insbesondere von Calciumcarbonat und Calcium-Magnesiumcarbonat. Ihr Anwendungsbereich konzentriert sich auf die Bewertung der Neutralisationsgeschwindigkeit und -effektivität durch ein automatisches Titrationsverfahren mit Zitronensäure. Diese Methodik ist entscheidend für Branchen, die stark auf die Qualität von Kalkungsmaterialien angewiesen sind, wie beispielsweise die Landwirtschaft und die Bauindustrie. Ein wesentlicher Vorteil dieser Norm ist die Präzision, die durch das automatisierte Verfahren erzielt wird, da es eine objektive Messung der Reaktivität ermöglicht. Diese Standardisierung sorgt dafür, dass die Ergebnisse reproduzierbar und vergleichbar sind, was für die Beurteilung von Kalkungsmaterialien von großer Bedeutung ist. Zudem legt die Norm fest, dass nur solche Kalkungsmaterialien mit einer maximalen Partikelgröße von 6,3 mm untersucht werden dürfen, was die Qualitätssicherung in der Anwendung weiter erhöht. Die Relevanz der EN 16357:2013 liegt auch in ihrer kompatiblen Anwendung mit anderen Normen, was eine umfassende Bewertung der Materialeigenschaften ermöglicht. Diese Norm trägt somit zur Schaffung einer soliden Basis für die Standards in der Branche bei, indem sie sicherstellt, dass alle Bewertungen nach einheitlichen Kriterien durchgeführt werden. Insgesamt stellt die EN 16357:2013 nicht nur einen wichtigen Leitfaden für die Bestimmung der Reaktivität von Kalkungsmaterialien dar, sondern ist auch ein wesentliches Instrument zur Gewährleistung der Qualität und Leistungsfähigkeit von Produkten in Bereichen, in denen calciumhaltige Materialien angewendet werden.

SIST EN 16357:2013은 탄산칼슘 및 탄산칼슘 마그네슘 석회 자재의 반응성을 결정하기 위한 방법을 규정한 유럽 표준으로, 이 문서의 범위는 특히 자동 적정법을 활용한 구연산을 통한 중화 잠재력의 속도와 효과성을 평가하는 데 중점을 두고 있습니다. 이 표준의 주요 강점은 자동 적정법을 통해 정확하고 신뢰할 수 있는 결과를 제공한다는 점입니다. 이는 사용자가 수동으로 실험을 진행하는 데서 발생할 수 있는 인적 오류를 최소화하면서, 다양한 석회 자재의 반응성을 비교 분석하는 데 유리합니다. 또한, 최대 입자 크기가 6.3mm로 정해져 있어 표준화된 샘플에 대해 일관성 있는 분석을 제공함으로써, 칼슘 탄산염 및 칼슘 마그네슘 탄산염 자재의 품질을 더욱 명확하게 평가할 수 있게 됩니다. 이 표준은 환경 친화성을 고려한 농업 및 토양 관리 분야에서 매우 중요한 역할을 하며, 석회 자재의 효과적인 사용을 통해 토양의 pH 조절 및 비옥도 증진에 기여할 수 있습니다. 따라서, SIST EN 16357:2013은 농업 기술자, 연구자 및 관련 산업 전문가들에게 매우 유용한 기준이 될 수 있습니다. 이 문서는 특히 석회 자재의 반응성을 과학적으로 측정하고 이해하는 데 필수적인 자료로, 관련 분야의 발전과 함께 지속 가능한 농업 관행을 촉진하는 데 중요한 의미를 가집니다.

La norme EN 16357:2013, intitulée « Matériaux de chaux carbonate - Détermination de la réactivité - Méthode de titrage automatique avec acide citrique », est d'une grande pertinence pour l'évaluation des matériaux de chaux. Son champ d'application se concentre sur la détermination de la réactivité des matériaux de chaux contenant du carbonate de calcium et du carbonate de magnésium calcique. Un des points forts de cette norme réside dans sa capacité à évaluer la vitesse et l'efficacité du potentiel neutralisant de ces matériaux. En utilisant une méthode de titrage automatique à l'acide citrique, la norme permet une analyse précise et efficace. Cela garantit que les utilisateurs disposent d'une méthode transparente pour quantifier la réactivité des matériaux, ce qui est crucial pour leur utilisation appropriée dans le domaine de l'agriculture et de l'amendement des sols. De plus, la norme stipule que la méthode est applicable exclusivement aux matériaux de chaux dont la taille maximale des particules est de 6,3 mm, conformément à la norme EN 12948. Cela assure que la méthodologie est standardisée et que les résultats obtenus sont fiables. Pour les utilisateurs de dolomite marbrière, la norme fait référence à la procédure BET selon l'ISO 9277 pour les matériaux présentant des surfaces spécifiques inférieures à 500 m2/kg, renforçant ainsi la cohérence des méthodes de test. En résumé, la norme EN 16357:2013 est un outil essentiel pour la détermination de la réactivité des matériaux de chaux carbonate, offrant une méthode de titrage précise qui est à la fois applicable et standardisée. Sa pertinence dans le contexte de l'évaluation de la qualité des matériaux de chaux en fait un document incontournable pour les professionnels du secteur.

The standard EN 16357:2013 provides a crucial framework for assessing the reactivity of carbonate liming materials, specifically focusing on calcium carbonate and calcium magnesium carbonate. Its comprehensive scope reflects the necessity for an accurate evaluation of these materials, which are essential for soil amendment in agricultural practices. One of the notable strengths of this standard is its utilization of an automatic titration method with citric acid, which allows for a precise and reproducible determination of the reactivity of liming materials. This method enhances the reliability of results, ensuring that users can confidently assess the neutralising potential of their products. Moreover, EN 16357:2013 is relevant to various stakeholders in the agricultural and environmental sectors. It caters to producers of liming materials, agricultural engineers, and soil scientists, ensuring that they have a standardized method to evaluate the effectiveness of liming products. The specification for a maximum particle size of 6.3 mm further supports uniformity in testing and fosters comparability across different materials and studies. In conclusion, the EN 16357:2013 standard represents a significant advancement in the determination of reactivity in carbonate liming materials, providing both a scientifically robust methodology and a clear application pathway for industry stakeholders. Its meticulous approach underscores the importance of effective soil management and the role of liming materials in enhancing soil quality.

SIST EN 16357:2013は、炭酸塩の石灰材料の反応性を評価するための自動滴定法を定義したヨーロッパ規格です。この規格は、カルシウム炭酸塩およびカルシウムマグネシウム炭酸塩の石灰材料の中和能力の速さと効果を評価するために必要な手順を明確に示しています。特に、この規格は最大粒子サイズ6.3 mm以下の石灰材料に適用されるため、特定の材料特性を考慮に入れた標準化された方法論を提供しています。 主な利点は、自動滴定法がもたらす精度と再現性です。この方法により、使用される試薬の量や反応時間に関するヒューマンエラーを低減し、信頼性の高い結果を保証します。これにより、農業や土壌改良分野における石灰材料の効果的な利用を促進し、持続可能な農業実践の発展に寄与します。 加えて、EN 16357:2013は他の規格と容易に関連付けることができ、例えば、ISO 9277に基づくマーブルドロマイトに関する注意事項も含まれています。このように、異なる材料や方法との整合性を持つことで、業界全体での標準化が進められており、ユーザーにとっての利便性が向上しています。 全体として、SIST EN 16357:2013は、石灰材料の反応性を定義するための重要な基準を提供し、業界の標準化を進める上での基盤となるものです。その適用範囲は広く、科学的な裏付けを基にした信頼性の高い測定手法を求める専門家にとって、非常に価値のあるツールといえるでしょう。