SIST EN 14984:2017

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kalkdünger - Bestimmung des Produkteinflusses auf den Boden-pH-Wert - BodeninkubationsverfahrenAmendements minéraux basiques - Détermination de l'effet d'un produit sur le pH d'un sol - Méthode par incubation du solLiming materials - Determination of product effect on soil pH - Soil incubation method65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 14984:2016SIST EN 14984:2017en,fr,de01-april-2017SIST EN 14984:2017SLOVENSKI
STANDARDSIST EN 14984:20061DGRPHãþD



SIST EN 14984:2017



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 14984
July
t r s x ICS
x wä r z r Supersedes EN
s v { z vã t r r xEnglish Version
Liming materials æ Determination of product effect on soil pH æ Soil incubation method Amendements minéraux basiques æ Détermination de l 5effet d 5un produit sur le pH d 5un sol æ Méthode par incubation du sol
Kalkdünger æ Bestimmung des Produkteinflusses auf den BodenæpHæWert æ Bodeninkubationsverfahren This European Standard was approved by CEN on
s { May
t r s xä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
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t r s x CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s v { z vã t r s x ESIST EN 14984:2017



EN 14984:2016 (E) 2 Contents Page European foreword . 4 Introduction . 5 1 Scope . 6 2 Normative references . 6 3 Terms and definitions . 7 4 Principle . 9 4.1 General . 9 4.2 Method A. 9 4.3 Method B. 9 5 Method A. 10 5.1 Reagents and materials . 10 5.1.1 Reference soil, . 10 5.1.2 Reference liming material (RLM), . 10 5.1.3 Water, . 10 5.2 Apparatus . 10 5.2.1 Temperature-controlled room, . 10 5.2.2 pH meter, . 10 5.2.3 Beakers, . 10 5.2.4 Pots, . 10 5.2.5 Volumetric spoons, . 10 5.2.6 Magnetic stirrer . 10 5.2.7 Balance, . 10 5.2.8 Precision balance, . 10 5.2.9 Test sieves, . 11 5.3 Sampling of products and sample preparation . 11 5.4 Procedure. 11 5.4.1 Preparation of the standard soil . 11 5.4.2 Test portions . 11 5.4.3 Preparation of pots . 11 5.4.4 Incubation . 12 5.4.5 pH measurements . 12 5.5 Expression of results . 12 5.6 Precision . 14 5.6.1 General . 14 5.6.2 Repeatability . 14 5.6.3 Reproducibility . 15 6 Method B. 17 6.1 Reagents and materials . 17 6.1.1 Standard soil, . 17 6.1.2 Alternative standard soils, . 18 6.1.3 Reference liming material, . 18 6.1.4 Water, . 18 6.2 Apparatus . 18 6.2.1 Temperature-controlled room, . 18 SIST EN 14984:2017



EN 14984:2016 (E) 3 6.2.2 pH meter, . 18 6.2.3 Beakers, . 19 6.2.4 Pots, . 19 6.2.5 Volumetric spoons,. 19 6.2.6 Magnetic stirrer . 19 6.2.7 Balance, . 19 6.2.8 Precision balance, . 19 6.2.9 Test sieves, . 19 6.3 Sampling of products and sample preparation . 19 6.4 Procedure . 19 6.4.1 Preparation of the standard soil . 19 6.4.2 Test portions . 20 6.4.3 Preparation of pots . 20 6.4.4 Incubation . 21 6.4.5 pH measurements. 21 6.5 Expression of results . 21 6.5.1 pH measurements. 21 6.5.2 Soil-lime efficiency data . 21 6.6 Precision . 22 6.6.1 General . 22 6.6.2 Repeatability . 22 6.6.3 Reproducibility . 23 7 Test report . 26 Annex A (informative)
Variations to the test methods . 27 A.1 General . 27 A.2 Variations . 27 A.2.1 Different measurement periods . 27 A.2.2 Supply of different amounts . 27 A.2.3 Soil different from the standard soil. 27 A.2.4 Different incubation temperature . 28 A.2.5 Additional measurements . 28 Annex B (normative)
Determination of moisture at full soil water holding capacity . 29 Bibliography . 31
SIST EN 14984:2017



EN 14984:2016 (E) 4 European foreword This document (EN 14984:2016) 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 January 2017, and conflicting national standards shall be withdrawn at the latest by January 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 14984:2006. The following changes have been made to the former edition: a) effective neutralizing value by incubation (ENVI) added as alternative way for the expression of results; b) Formula for calculation of ENVI for method A added; c) Formula for calculation of ENVI for method B added; d) editorially 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 14984:2017



EN 14984:2016 (E) 5 Introduction The chemical methods for determining the neutralizing value (NV) (see EN 12945) and the reactivity (see EN 13971 and EN 16357) of liming materials are not always appropriate indicators for any material claimed to have a liming effect in the soil, particularly materials with a high organic matter content. The biological mineralization of organic matter contained in some products can, in the field, have an effect on pH, which cannot be quantified by the chemical methods. The two methods described in this document overcome these problems. Both methods characterize products through their effect on the pH of a soil under controlled, standard conditions, and establish the efficiency of products when applied to a standard soil. Method A specifies a reference soil with tight characteristics with respect to pH range before incubation, cation exchange capacity (CEC), mass fraction of organic carbon, and mass fraction of particles finer than 0,002 mm (clay). Method B can apply the same reference soil as Method A, but also allows alternative standard soils with a wider content of particles finer than 0,002 mm (clay), and a wider range of mass fraction of organic matter. Clay and organic matter are the decisive reactants to a liming material However, attention is drawn to the limitations of these methods. They are laboratory methods carried out under controlled conditions and care should be taken when applying the results to field conditions. The quality of incorporation of the liming material into the soil and the eventual need to break down the product agglomerates, together with the soil and climate conditions, can affect the results. Nevertheless, these methods allow a comparison of the potential neutralizing effect of liming products under optimum and reproducible conditions. SIST EN 14984:2017



EN 14984:2016 (E) 6 1 Scope This document specifies two methods (method A and method B) of measuring the effect of the addition of any material claimed to have a liming effect on the soil, using the same basic principles. Method A measures the changes to the soil pH resulting from the addition of any material claimed to have a liming effect on a standard soil, measured over a period of one month. Method B assesses the efficiency of any material claimed to have a liming effect, using a range of defined soils and measured over a period of up to 2,5 years. The methods are not applicable to mineral products coarser than 6,3 mm for method A or 20 mm for method B, determined according to EN 12948. NOTE These methods allow comparison of products under controlled climatic conditions but do not replace field experiments. 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 1482-1, Fertilizers and liming materials - Sampling and sample preparation - Part 1: Sampling EN 1482-3, Fertilizers and liming materials — Sampling and sample preparation — Part 3: Sampling of static heaps EN 12048, Solid fertilizers and liming materials - Determination of moisture content - Gravimetric method by drying at (105 +/- 2)°C (ISO 8190:1992 modified) EN 12049, Solid fertilizers and liming materials - Determination of moisture content - Gravimetric method by drying under reduced pressure (ISO 8189:1992 modified) EN 12945, Liming materials - Determination of neutralizing value - Titrimetric methods EN 12948, Liming materials - Determination of size distribution by dry and wet sieving EN 13040, Soil improvers and growing media - Sample preparation for chemical and physical tests, determination of dry matter content, moisture content and laboratory compacted bulk density EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696) ISO 3310-1, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire cloth ISO 3310-2, Test sieves — Technical requirements and testing — Part 2: Test sieves of perforated metal plate ISO 10390:2005, Soil quality — Determination of pH ISO 11272, Soil quality — Determination of dry bulk density ISO 11277, Soil quality — Determination of particle size distribution in mineral soil material — Method by sieving and sedimentation SIST EN 14984:2017



EN 14984:2016 (E) 7 ISO 11465, Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric method ISO 14235, Soil quality — Determination of organic carbon by sulfochromic oxidation NF X31-130, Soil quality — Chemical methods — Determination of the cationic exchange capacity (CEC) and extractible cations (buffered at pH = 7, Metson method)1) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 efficiency ability of a liming material to react in soil or solution within a specified time Note 1 to entry: In this document, efficiency is calculated as mentioned in 6.5.2. 3.2 internal peak values approach crediting fine fractions of a product or other highly reactive materials for 100 % efficiency in soil when reaching maximum pH value Note 1 to entry: This efficiency is maintained even if pH later drops due to soil microbial counteraction (acidification). Note 2 to entry: For further clarification see Figure 1 and Figure 2.
Key
no liming material
different products X weeks of incubation Y soil pH Figure 1 — Soil pH versus weeks of soil incubation
1) No international buffered method is available at pH = 7. As soon as an International Standard is available for cation exchange capacity buffered at pH = 7, it will replace the NF X 31-130. SIST EN 14984:2017



EN 14984:2016 (E) 8
Key
no liming material
different products X weeks of incubation Y efficiency in percent Figure 2 — Efficiency versus weeks of soil incubation 3.3 liming index ratio of the improvement in soil pH due to the product under test to that achieved using the reference liming material Note 1 to entry: The liming index, LIx is an indicator given by the following =x(pH1 - pH2)(pH3 - pH4)LI where LI is the liming index; pH1 is the pH of the soil with tested product after time x; pH2 is the pH of the soil alone after time x; pH3 is the pH of the soil with the reference liming material after time x; pH4 is the pH of the soil alone after time x; x is the length of time of the incubation test. Default value is four weeks. SIST EN 14984:2017



EN 14984:2016 (E) 9 3.4 effective neutralising value by incubation
ENVI alternative expression of results, expressed as NV equivalent Note 1 to entry: The effective neutralizing value by incubation, ENVI, is an indicator given by the following Formula: =×4weeksENVILIRLMNV (for method A, see 5.5, Table 2) =×iweeksiweeks/100ENVIERLMNV (for method B, see 6.5.2) where ENVI is the effective neutralizing value by incubation; LI4weeks is the liming index at 4 weeks in method A; Ei weeks is the efficiency at i weeks in method B; RLMNV is the neutralizing value of the reference liming material (5.1.2); if the conventional NV unit is CaO, RLMNV = 75,6 if the conventional NV unit is HO-, RLMNV = 45,8. 4 Principle 4.1 General Incorporation of a standardized amount of liming material or material claimed to have a liming effect into a reference soil or range of defined soils. Incubation of these soils under controlled climatic conditions for a defined period. Checking the buffer capacity of the soil with a reference liming material and measuring the changes in soil pH. 4.2 Method A Monitoring after 24 h, 2 weeks and 4 weeks the changes in soil pH under controlled temperature and moisture conditions. 4.3 Method B Monitoring after 24 h, 1 week, 3 weeks, 6 weeks, 12 weeks, 24 weeks and 48 weeks, and 1 year, 1,5 years, 2 years and 2,5 years of the changes in soil pH under controlled temperature and moisture conditions. When testing calcined products (burnt products and slaked products), add monitoring at 1 h, 3 h and 6 h and 3 days. The test may be stopped at any time after 3 weeks, according to information required. The tests should be performed within the pH range of 4,6 to 7,0, subject to there being a linearity response. SIST EN 14984:2017



EN 14984:2016 (E) 10 5 Method A 5.1 Reagents and materials 5.1.1 Reference soil, with the following characteristics: a) pH 5,6 to pH 6,4 in water, when determined in settling suspension after 16 h in accordance with ISO 10390:2005, 7.1.3, 7.2 and 7.3; b) cation exchange capacity of 9 cmol+/kg to 11 cmol+/kg, when determined in accordance with NF X 31-130 (see footnote in Clause 2); c) mass fraction of organic carbon (OC)of 0,50 % to 2,00 % on a dry basis, when determined in accordance with ISO 14235 (this is equivalent to 0,86 % to 3,44 % expressed as organic matter, (OM)(×OM=OC1,72)); d) mass fraction of particles of equivalent spherical diameter less than 0,002 mm (clay) shall be less than 20 %, when determined in accordance with ISO 11277. 5.1.2 Reference liming material (RLM), calcium hydroxide of recognized analytical grade. 5.1.3 Water, conforming to EN ISO 3696, grade 3. 5.2 Apparatus 5.2.1 Temperature-controlled room, capable of being maintained at (20 ± 2) °C. 5.2.2 pH meter, capable of being read to the nearest 0,01 unit. 5.2.3 Beakers, capacity 200 ml. 5.2.4 Pots, of inert material with respect to soil, 50 mm to 200 mm diameter, capacity according to Table 1. 5.2.5 Volumetric spoons, capacity 20 ml. 5.2.6 Magnetic stirrer 5.2.7 Balance, with an accuracy of ± 1 g. 5.2.8 Precision balance, with an accuracy of ± 1 mg. SIST EN 14984:2017



EN 14984:2016 (E) 11 5.2.9 Test sieves, wire sieves, 1 mm, 2 mm, 4 mm and 6,3 mm nominal aperture size, according to ISO 3310-1. 5.3 Sampling of products and sample preparation Take a sample in accordance with EN 1482-1 or EN 1482-3. Determine the dry matter content of the sample in accordance with EN 12048 or EN 12049. Determine the dry matter content of the soil in accordance with ISO 11465. It shall be used to adjust the mass fraction of soil in Table 1 to determine field water capacity in 5.4.3. Determine the smallest aperture size sieve from the range 1 mm, 2 mm, 4 mm and 6,3 mm that all the sample will pass. For mineral products use the sample as received. For organic products use the sample as received, but after homogenization, unless it contains coarse particles (equivalent spherical diameter greater than 1 mm). If the sample contains coarse particles, prepare it in accordance with EN 13040 so that all the particles will pass a 1-mm aperture size sieve. Determine in that case the fineness of the product. 5.4 Procedure 5.4.1 Preparation of the standard soil Dry the soil to constant mass at a temperature below 40°C, sieve on a 2 mm aperture size sieve (5.2.9) and use the soil that passes the sieve. Measure the initial pH of the standard soil in a settling suspension of water after 16 h in accordance with ISO 10390:2005, 7.1.3, 7.2 and 7.3 and record it. 5.4.2 Test portions Weigh, to the nearest 0,001 g, two test portions each of the mass specified in Table 1. At the same time, weigh, to the nearest 0,001 g, two portions of reference liming material (4.1) of the same mass as the test portions. NOTE The portion of reference liming material is equivalent to 2 250 units of neutralizing value per hectare, on the basis of 3 000 t of dried soil per hectare, and in the standard soil it will raise the pH by approximately one unit. Table 1 — Mass of test portion and mass of standard soil Sieve size that test portion passes after preparation mm Mass of test portion, on a dry basis g Mass of standard soil per pot, on a dry basis (105 °C) g 1 0,5 ± 0,001 500 ± 1 2 1 ± 0,001 1 000 ± 1 4 2 ± 0,001 2 000 ± 1 6,3 3 ± 0,001 3 000 ± 1 5.4.3 Preparation of pots Into each of six or more pots, weigh, to the nearest 1 g, the mass of standard soil (5.1.1) specified in 5.4.2 and Table 1. To avoid lack or excess of air, height of soil in the pots shall be between 50 mm and SIST EN 14984:2017



EN 14984:2016 (E) 12 150 mm. Add a test portion to each of two pots (pots A1 and A2). Add a portion of reference liming material (5.1.2) to each of two further pots (pots B1 and B2), and possibly more pots and leave the remaining two pots (pots C1 and C2) with just the standard soil. Thoroughly mix the contents within each pot. Onto the soil in each pot, slowly add, by means of a drip, a mass of water (5.1.3) corresponding to 70 % of the water field capacity (see Annex B) considered at free drainage. Weigh each pot and its contents and record the masses. 5.4.4 Incubation Maintain the open pots at a constant temperature of (20 ± 2) °C in the temperature-controlled room (5.2.1). Regularly check the water losses in the pots by weighing and adjust using a drip as often as necessary. The water contents shall not fall below to 60 % of the water field capacity. Thoroughly mix the contents of each pot before watering to avoid soil compaction. 5.4.5 pH measurements Measure the pH after incubations of 24 h, 2 weeks and 4 weeks. Thoroughly mix the contents of each pot. Take three portions, each of 20 ml, from each pot, thoroughly mixing the contents after taking each portion. Place each of these portions in a separate beaker (5.2.3). Continu
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