SIST EN 13971:2013
(Main)Carbonate and silicate liming materials - Determination of reactivity - Potentiometric titration method with hydrochloric acid
Carbonate and silicate liming materials - Determination of reactivity - Potentiometric titration method with hydrochloric acid
This European Standard specifies a method for the determination of the speed and effectiveness of the neutralising potential of calcium carbonate, calcium magnesium carbonate and calcium magnesium silicate 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. The type of liming material should be identified according to EN 14069 and the particle size should be determined according to EN 12948.
Carbonatische und silikatische 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 sowie carbonatischen und silikatischen Calcium /Magnesium-Bodenverbesserungsmitteln (Kalkdüngern) durch potentiometrische Titration mit Salzsäure fest.
Dieses Verfahren gilt nur für Calcium-/Magnesium-Bodenverbesserungsmittel mit einer Korngröße von höchstens 6,3 mm.
ANMERKUNG Der Typ des Calcium-/Magnesium-Bodenverbesserungsmittels sollte nach EN 14069 identifiziert und die Korngröße nach EN 12948 bestimmt werden.
Amendements minéraux basiques carbonatés et silicatés - Détermination de la réactivité - Méthode par titrage potentiométrique à l'acide chlorhydrique
La présente Norme européenne spécifie une méthode pour déterminer la vitesse et l'efficacité du potentiel de neutralisation des carbonates de calcium, carbonates de calcium et de magnésium et silicates de calcium et de magnésium utilisés comme amendements minéraux basiques, par titrage potentiométrique à l’acide chlorhydrique.
La présente méthode s'applique seulement aux amendements minéraux basiques dont la taille des particules ne dépasse pas 6,3 mm.
NOTE Le type d’amendement minéral basique doit être identifié conformément à l’EN 14069 et la taille des particules doit être déterminée conformément à l’EN 12948.
Karbonatna in silikatna sredstva za apnjenje - Določevanje reaktivnosti - Potenciometrijska titracijska metoda s klorovodikovo kislino
Ta evropski standard določa metodo za ugotavljanje hitrosti in učinkovitosti nevtralizacijskega potenciala sredstev za apnenje s kalcijevim karbonatom, kalcijevim magnezijevim karbonatom in kalcijevim magnezijevim silikatom s potenciometrijsko titracijo s klorovodikovo kislino. Ta metoda se uporablja le za sredstva za apnenje z največjo velikostjo delcev 6,3 mm. Vrsta sredstva za apnenje naj bi se opredelila v skladu s standardom EN 14069, velikost delcev pa v skladu s standardom EN 12948.
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Carbonatische und silikatische Kalke - Bestimmung der Reaktivität - Potentiometrisches Titrationsverfahren mit SalzsäureAmendements minéraux basiques carbonatés et silicatés - Détermination de la réactivité - Méthode par titrage potentiométrique à l'acide chlorhydriqueCarbonate and silicate liming materials - Determination of reactivity - Potentiometric titration method with hydrochloric acid65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 13971:2012SIST EN 13971:2013en,fr,de01-maj-2013SIST EN 13971:2013SLOVENSKI
STANDARDSIST EN 13971:20081DGRPHãþD
SIST EN 13971:2013
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 13971
December 2012 ICS 65.080 Supersedes EN 13971:2008English Version
Carbonate and silicate liming materials - Determination of reactivity - Potentiometric titration method with hydrochloric acid Amendements minéraux basiques carbonatés et silicatés -Détermination de la réactivité - Méthode par titrage potentiométrique à l'acide chlorhydrique
Carbonatische und silikatische Kalke - Bestimmung der Reaktivität - Potentiometrisches Titrationsverfahren mit Salzsäure This European Standard was approved by CEN on 3 November 2012.
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 © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13971:2012: ESIST EN 13971:2013
EN 13971:2012 (E) 2 Contents Page Foreword .3Introduction .41Scope .52Normative references .53Principle .54Apparatus .55Reagents .66Preparation of the test sample .67Procedure .78Expression of results .99Precision . 1010Test report . 12Annex A (normative)
Preparation of the test portion of liming materials coarser than 1 mm . 13Annex B (normative)
Arrangement of the test apparatus . 14Bibliography . 16 SIST EN 13971:2013
EN 13971:2012 (E) 3 Foreword This document (EN 13971:2012) 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 June 2013, and conflicting national standards shall be withdrawn at the latest by June 2013. 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 13971:2008. The following has been added to the former edition of the European Standard: a) silicate liming materials added to the scope and to the title; b) EN 12947 and EN 13475 added to the normative references; c) Clause 3 reaction formula for silicates added; d) subclauses 7.1.2 and 7.2.2 enlarged concerning determination of silicate liming materials; e) subclause 8.2 and formulas (2), (3) and (4) on expression of results for silicate liming materials added; f) subclause 9.2 and Table 2 on the precision data for silicate liming materials added; g) Bibliography revised. According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: 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 the United Kingdom.
SIST EN 13971:2013
EN 13971:2012 (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. SIST EN 13971:2013
EN 13971:2012 (E) 5 1 Scope This European Standard specifies a method for the determination of the speed and effectiveness of the neutralising potential of calcium carbonate, calcium magnesium carbonate and calcium magnesium silicate 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. 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 documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. 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 12947, Liming materials — Determination of magnesium content — Atomic absorption spectrometric method EN 12948, Liming materials — Determination of size distribution by dry and wet sieving EN 13475, Liming materials — Determination of calcium content — Oxalate method 3 Principle Decomposition of carbonates and silicates with acids according to the following reactions: MeCO3 + 2 H+ → Me2+ + H2O + CO2 MeSiO4 + 2 H+ → Me(OH)2 + SiO2 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. SIST EN 13971:2013
EN 13971:2012 (E) 6 4.2 Burette. NOTE Used only for 5,0 mol/l hydrochloric acid solution (5.2). 4.2.1 50 ml motor driven burette (for automatic titration),a pH stat function is recommended, 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. 4.7 Filter paper, acid-proof, medium filtration speed, average retention capacity about 5 µm to 12 µm. 5 Reagents All reagents shall be of recognised analytical grade. 5.1 Hydrochloric acid solution, mass fraction, w(HCl) = 25 %. 5.2 Hydrochloric acid, standard volumetric solution, c(HCl) = 5,0 mol/l. 5.3 Calcium carbonate, precipitated, mass fraction, w(CaCO3) = of at least 99 %. Precipitated calcium carbonate is from crystalline origin. Commercial PCC for analysis is granted for its chemical characteristics. However, physical characteristics are not granted. The use of a highly reactive PCC, such as commercial PCC from VWR / Prolabo / BDH, reference GPR, Rectapur, Ref 22296.294, Molar mass 100,092) which will consume 15 ml after 15 min, is recommended.
5.4 Silicone defoamer. 5.5 Standard buffer solution, pH = 2,0 (commercial solution). NOTE This has a limited life. 5.6 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.
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. 2) This substance is an example of a suitable product available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by CEN of this product. SIST EN 13971:2013
EN 13971:2012 (E) 7 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 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. 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 (5.5) and pH 4,0 (5.6). The pH electrode shall react quickly. Check the sluggishness of the electrode and if necessary, clean it carefully with hydrochloric acid (5.1) and re-calibrate with the standard buffer solutions. Checking and cleaning is more frequently required for liming materials containing clay. It is recommended to flush the acid introduction pipe between each sample for slow reacting samples. 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 (5.2). 7.1.1.5 Adjust the titration control so that the stepwise run of the titration only starts below pH 2,5. For apparatus with a step length adjustment, set the adjustment at the middle position. 7.1.1.6 Set up the electrode (4.1) and the burette (4.2.1) in the glass beaker (4.3) according to Figure B.1. This is to ensure that the added hydrochloric acid (5.2) is mixed with the contents of the glass beaker before reaching the electrode (4.1). Avoid contact with the walls of the glass beaker. 7.1.1.7 For the exact adjustment of the o
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