EN 13971:2002
(Main)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 standard specifies a rapid method for the determination of the speed and effectiveness of the neutralizing potential of calcium carbonate and calcium/magnesium carbonate liming materials for fertilization and soil conditioning by potentiometric titration with hydrochloric acid. This method is applicable to liming materials with a maximum particle size of 6,3 mm.
Carbonatische Kalke - Bestimmung der Reaktivität - Potentiometrisches Titrationsverfahren mit Salzsäure
Amendements minéraux basiques carbonatés - Détermination de la réactivité - Méthode par titration potentiométrique à 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 à 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 être mesurée selon la norme EN 12948.
NOTE Par ailleurs, il conviendrait d'identifier le type d'amendement minéral basique, selon le projet prEN 14069.
En ce qui concerne l'étude relative à 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.
Karbonatni materiali za apnjenje – Ugotavljanje reaktivnosti – Potenciometrijska titracijska metoda s solno kislino
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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 acidKarbonatni materiali za apnjenje – Ugotavljanje reaktivnosti – Potenciometrijska titracijska metoda s solno kislinoAmendements 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 13971:2002SIST EN 13971:2003en65.080ICS:SLOVENSKI
STANDARDSIST EN 13971:200301-oktober-2003
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13971December 2002ICS 65.080English 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 23 October 2002.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, Malta, 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© 2002 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13971:2002 E
EN 13971:2002 (E)2ContentspageForeword.3Introduction.41Scope.42Normative references.43Principle.44Apparatus.55Reagents.56Preparation of the test sample.67Procedure.68Expression of results.89Precision.810Test report.9Annex A (normative)
Preparation of the test portion of liming materials coarser than 1 mm.10Annex B (normative)
Arrangement of the test apparatus.11Bibliography.12
EN 13971:2002 (E)3ForewordThis document (EN 13971:2002) 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 June 2003, and conflicting national standards shall be withdrawn at the latest byJune 2003.Annexes A and B are normative.This document contains a Bibliography.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, Malta, Netherlands, Norway, Portugal, Spain,Sweden, Switzerland and the United Kingdom.
EN 13971:2002 (E)4IntroductionThe 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]).1 ScopeThis European Standard specifies a method for the determination of the speed and effectiveness of theneutralizing potential of calcium carbonate and calcium magnesium carbonate liming materials bypotentiometric titration with hydrochloric acid.This method is applicable only to liming materials with a maximum particle size of 6,3 mm. Therefore, theparticle size shall be determined according to EN 12948.NOTEIn addition, the type of liming material should be identified according to prEN 14069.Regarding the precision of the method, the results are not used to declare a value but to classify the differentproducts groups.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.EN 12048, Solid fertilizers and liming materials — Determination of moisture content — Gravimetric method bydrying 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.ISO 5725:19861), Precision of test methods — Determination of repeatability and reproducibility for a standard testmethod by inter-laboratory tests.3 PrincipleDecomposition of carbonates with acids according to the following reaction:MeCO3 + 2 H+ ® Me2+ + H2O + CO2
1)ISO 5725:1986 (now withdrawn) was used to obtain the precision data.
EN 13971:2002 (E)5Titration under stable pH conditions either with an automatic titration apparatus or a manual method. Theacid consumption during a given time is a direct measure for the reaction rate of the liming materials beingtested.4 ApparatusUsual laboratory apparatus and, in particular, the following.4.1 pH meterwith electrode.4.2 BuretteNOTEUse only for 5,0 mol/l hydrochloric acid solution (5.3).4.2.1 50 ml motor driven burette (for automatic titration), for example Metrohm 716 DMS Titrino® 2)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-watch5 Reagents5.1 GeneralAll 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 defoamer5.6 Standard buffer solution, pH 2,0 (commercial solution).NOTEThis has a limited life.5.7 Standard buffer solution, pH 4,0 (commercial solution).NOTEThis has a limited life.
2)Metrohm 716 DMS Titrino® is an example of a suitable product available commercially. This information is given for theconvenience of users of this European Standard and does not constitute an endorsement by CEN of this product. Equivalentproducts may be used if they can be shown to lead to the same results.
EN 13971:2002 (E)66 Preparation of the test sample6.1Sample the liming material in accordance with EN 1482.6.2Dry test sample in accordance with EN 12048. Record the result.6.3Use test sample without further preparation, e.g. grinding.6.4Weigh out a 5,0 g test portion to the nearest 0,01 g. For liming materials coarser than 1 mm, the test portionshould be prepared in accordance with annex A.7 Procedure7.1 Automatic titration7.1.1 Calibration7.1.1.1Calibrate the pH meter (4.1) with two standard buffer solutions, pH 2,0 (5.6) and pH 4,0 (5.7) to exactlythe 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 massfraction of 25 % (5.2) and re-calibrate with the standard buffer solutions.NOTEChecking and cleaning is more frequently required for liming materials containing clay.7.1.1.2Adjust the motor driven burette (4.2.1) to the position “continuous working” and a standard flow rate of35 ml/min to 38 ml/min.NOTEWide deviations in the flow rate adversely affect the results obtained.7.1.1.3Place the glass beaker (4.3) centrally on the magnetic stirrer (4.4). Add 100 ml water and the magneticstirrer rod (4.5).7.1.1.4Set the magnetic stirrer speed control to between 500 min-1 and 600 min-1. Fill the burette (4.2.1) with5,0 mol/l hydrochloric acid (5.3).7.1.1.5Adjust the titration contr
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