SIST EN 13971:2008
Carbonate liming materials - Determination of reactivity - Potentiometric titration method with hydrochloric acid
Carbonate liming materials - Determination of reactivity - Potentiometric titration method with hydrochloric acid
This document specifies a method for the determination of the speed and effectiveness of the neutralizing potential of calcium carbonate and calcium magnesium carbonate liming materials by potentiometric titration with hydrochloric acid.This method is applicable only to liming materials with a maximum particle size of 6,3 mm.
Carbonatische Kalke - Bestimmung der Reaktivität - Potentiometrisches Titrationsverfahren mit Salzsäure
Diese Europäische Norm legt ein Verfahren für die Bestimmung der Geschwindigkeit und Wirksamkeit des
Neutralisationspotentials von Calciumcarbonat und carbonatischen Calcium-Magnesiumkalken durch
potentiometrische Titration mit Salzsäure fest.
Dieses Verfahren gilt nur für Calcium-/Magnesium-Bodenverbesserungsmittel mit einer Korngröße von
höchstens 6,3 mm. Deshalb muss die Korngröße nach EN 12948 bestimmt werden.
ANMERKUNG Zusätzlich sollte der Typ des Calcium-/Magnesium-Bodenverbesserungsmittels nach EN 14069
identifiziert werden.
Hinsichtlich der Präzision des Verfahrens werden die Ergebnisse nicht dazu verwendet, einen Wert zu
bestätigen, sondern um die unterschiedlichen Produktgruppen einzuteilen.
Amendements minéraux basiques carbonatés - Détermination de la réactivité - Méthode par titration potentiométrique a l'acide chlorhydrique
La présente norme spécifie une méthode pour déterminer la vitesse et l'efficacité du potentiel de
neutralisation des carbonates de calcium et carbonates de calcium et de magnésium, utilisés comme
amendements minéraux basiques, par titration potentiométrique a l’acide chlorhydrique.
La présente méthode s'applique seulement aux amendements minéraux basiques dont les particules ne
dépassent pas 6,3 mm. Par conséquent, la taille des particules doit etre mesurée selon la norme EN 12948.
NOTE Par ailleurs, il conviendrait d’identifier le type d’amendement minéral basique, selon la norme EN 14069.
En ce qui concerne l’étude relative a la fidélité de la méthode, il faut signaler que les résultats obtenus ne sont
pas utilisés pour déclarer des valeurs, mais pour classer les différents groupes de produits.
Karbonatna sredstva za apnjenje - Določevanje reaktivnosti - Potenciometrijska titracijska metoda s klorovodikovo kislino
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Carbonate liming materials - Determination of reactivity - Potentiometric titration method with hydrochloric acidQFLRPHWULMVNDAmendements minéraux basiques carbonatés - Détermination de la réactivité - Méthode par titration potentiométrique a l'acide chlorhydriqueCarbonatische Kalke - Bestimmung der Reaktivität - Potentiometrisches Titrationsverfahren mit SalzsäureTa slovenski standard je istoveten z:EN 13971:2008SIST EN 13971:2008en,fr,de65.080ICS:SIST EN 13971:20031DGRPHãþDSLOVENSKI
STANDARDSIST EN 13971:200801-april-2008
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13971February 2008ICS 65.080; 91.100.10Supersedes EN 13971:2002
English VersionCarbonate liming materials - Determination of reactivity -Potentiometric titration method with hydrochloric acidAmendements minéraux basiques carbonatés -Détermination de la réactivité - Méthode par titrationpotentiométrique à l'acide chlorhydriqueCarbonatische Kalke - Bestimmung der Reaktivität -Potentiometrisches Titrationsverfahren mit SalzsäureThis European Standard was approved by CEN on 28 December 2007.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 CEN 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 CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2008 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13971:2008: E
EN 13971:2008 (E) 2 Contents page Foreword.3 Introduction.4 1 Scope.4 2 Normative references.4 3 Principle.4 4 Apparatus.4 5 Reagents.5 6 Preparation of the test sample.5 7 Procedure.6 8 Expression of results.8 9 Precision.9 10 Test report.9 Annex A (normative)
Preparation of the test portion of liming materials coarser than 1 mm.10 Annex B (normative)
Arrangement of the test apparatus.11 Bibliography.13
EN 13971:2008 (E) 3 Foreword This document (EN 13971:2008) 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 August 2008, and conflicting national standards shall be withdrawn at the latest by August 2008. 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 EN 13971:2002. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom.
EN 13971:2008 (E) 4 Introduction The results obtained by this method can be used to estimate the behaviour of the liming material in the soil. The results show a good correlation with the results obtained by a soil incubation method (see [1] to [5]). Regarding the precision of the method, the results are not used to declare a value, but to classify the different product groups. 1 Scope This European Standard specifies a method for the determination of the speed and effectiveness of the neutralizing potential of calcium carbonate and calcium magnesium carbonate liming materials by potentiometric titration with hydrochloric acid. This method is applicable only to liming materials with a maximum particle size of 6,3 mm. NOTE The type of liming material should be identified according to EN 14069 and the particle size should be determined according to EN 12948. 2 Normative references The following referenced documents are indispensable for the application of this document. 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 12048, Solid fertilizers and liming materials — Determination of moisture content — Gravimetric method by drying at (105 ± 2) °C (ISO 8190:1992 modified) EN 12945, Liming materials — Determination of neutralizing value — Titrimetric methods EN 12948, Liming materials — Determination of size distribution by dry and wet sieving 3 Principle Decomposition of carbonates with acids according to the following reaction: MeCO3 + 2 H+ → Me2+ + H2O + CO2 Titration under stable pH conditions either with an automatic titration apparatus or a manual method. The acid consumption during a given time is a direct measure of the reaction rate of the liming materials being tested. 4 Apparatus Usual laboratory apparatus and, in particular, the following: 4.1 pH meter, with electrode. 4.2 Burette NOTE Used only for 5,0 mol/l hydrochloric acid solution (5.3).
EN 13971:2008 (E) 5 4.2.1 50 ml motor driven burette (for automatic titration), for example Metrohm 716 DMS Titrino® 1) 4.2.2 50 ml burette (for manual titration) 4.3 250 ml glass beaker, with an inner diameter of 65 mm. 4.4 Magnetic stirrer, with centring mark for the 250 ml glass beaker. 4.5 Magnetic stirrer rod, (9 ± 1) mm diameter times (50 ± 1) mm length, with central ring. 4.6 Stop-watch 5 Reagents 5.1 General All reagents shall be of recognized analytical grade. 5.2 Hydrochloric acid solution, mass fraction, w(HCl) = 25 %. 5.3 Hydrochloric acid, standard volumetric solution, c(HCl) = 5,0 mol/l. 5.4 Calcium carbonate, precipitated, mass fraction, w(CaCO3) = of at least 99 %. 5.5 Silicone defoamer 5.6 Standard buffer solution, pH 2,0 (commercial solution). NOTE This has a limited life. 5.7 Standard buffer solution, pH 4,0 (commercial solution). NOTE This has a limited life. 6 Preparation of the test sample 6.1 Prepare the sample of the liming material in accordance with EN 1482-2. 6.2 Dry the test sample in accordance with EN 12048. Record the result for information only. 6.3 Use the dried test sample without further preparation, e.g. grinding. 6.4 Weigh out a 5,0 g test portion of the dried sample to the nearest 0,01 g. For liming materials coarser than 1 mm, the test portion shall be prepared in accordance with Annex A.
1) Metrohm 716 DMS Titrino® 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. Equivalent products may be used if they can be shown to lead to the same results.
EN 13971:2008 (E) 6 7 Procedure 7.1 Automatic titration 7.1.1 Calibration 7.1.1.1 Calibrate the pH meter (4.1) with two standard buffer solutions, pH 2,0 (5.6) and pH 4,0 (5.7) to exactly the indicated values. The pH electrode shall react quickly. Check the sluggishness of the electrode and if necessary, clean it carefully with hydrochloric acid with a mass fraction of 25 % (5.2) and re-calibrate with the standard buffer solutions. NOTE Checking and cleaning is more frequently required for liming materials containing clay. 7.1.1.2 Adjust the motor driven burette (4.2.1) to the position “continuous working” and a standard flow rate of 35 ml/min to 38 ml/min. NOTE Wide deviations in the flow rate adversely affect the results obtained. 7.1.1.3 Place the glass beaker (4.3) centrally on the magnetic stirrer (4.4). Add 100 ml water and the magnetic stirrer rod (4.5). The test apparatus shall be arranged according to Figure B.1. 7.1.1.4 Set the magnetic stirrer speed control to between 500 min-1 and 600 min-1. Fill the burette (4.2.1) with 5,0 mol/l hydrochloric acid (5.3). 7.1.1.5 Adjust the titration control so that the stepwise run of the titrati
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