SIST EN 14984:2006
(Main)Liming materials - Determination of product effect on soil pH - Soil incubation method
Liming materials - Determination of product effect on soil pH - Soil incubation method
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.
NOTE These methods allow comparison of products under controlled climatic conditions but do not replace field experiments. The methods are not applicable to mineral products coarser than 6,3 mm for method A or 20 mm for method B.
Calcium-/Magnesium-Bodenverbesserungsmittel - Bestimmung des Produkteinflusses auf den Boden-pH-Wert - Bodeninkubationsverfahren
Diese Europäische Norm legt zwei Verfahren (Verfahren A und Verfahren B) zur Messung der Auswirkungen fest, die sich ergeben, wenn Materialien, für die eine Calcium-/Magnesium-Bodenverbesserungswirkung beansprucht wird, in Böden eingebracht werden, wobei für beide Verfahren dieselben Grundprinzipien angewendet werden.
Mit Verfahren A werden die Veränderungen des Boden-pH-Wertes gemessen, die sich ergeben, wenn Materialien, für die eine Calcium-/Magnesium-Bodenverbesserungswirkung beansprucht wird, in einen Standardboden eingebracht werden, wobei die Messdauer einen Monat beträgt.
Mit Verfahren B wird der Wirkungsgrad der Materialien bewertet, für die eine Calcium-/Magnesium-Bodenverbesserungswirkung beansprucht wird, wobei eine Reihe festgelegter Böden über einen Zeitraum von bis zu 2,5 Jahren gemessen wird.
ANMERKUNG Diese Verfahren gestatten einen Vergleich von Produkten unter kontrollierten Klimabedingungen, ersetzen jedoch nicht die Feldversuche. Die Verfahren sind nicht auf mineralische Produkte anwendbar, deren Korngröße über 6,3 mm (Verfahren A) oder 20 mm (Verfahren B) liegt.
Amendements minéraux basiques - Détermination de l'effet d'un produit sur le pH d'un sol - Méthode par incubation du sol
Ce document spécifie deux méthodes (méthode A et méthode B) pour mesurer l’effet de l’ajout de tout matériau revendiquant un effet basique sur le sol, en utilisant les memes principes de base.
La méthode A mesure les changements du pH du sol suite a l’ajout d’un matériau revendiquant un effet basique sur un sol type, mesuré sur une période d’un mois.
La méthode B évalue l’efficience d’un matériau revendiquant un effet basique en utilisant un sol pris dans une série de sols définis et des mesures faites sur une période allant jusqu’a 2,5 ans.
NOTE Ces méthodes permettent de comparer des produits dans des conditions climatiques contrôlées mais ne remplacent pas les expériences au champ. Les méthodes ne sont pas applicables a des produits minéraux ayant une granulométrie supérieure a 6,3 mm pour la méthode A ou 20 mm pour la méthode B.
Sredstva za apnjenje – Določanje vpliva sredstva za apnjenje na pH tal – Inkubacijska metoda
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Liming materials - Determination of product effect on soil pH - Soil incubation methodAmendements minéraux basiques - Détermination de l'effet d'un produit sur le pH d'un sol - Méthode par incubation du solCalcium-/Magnesium-Bodenverbesserungsmittel - Bestimmung des Produkteinflusses auf den Boden-pH-Wert - BodeninkubationsverfahrenTa slovenski standard je istoveten z:EN 14984:2006SIST EN 14984:2006en,fr,de65.080ICS:SLOVENSKI
STANDARDSIST EN 14984:200601-september-2006
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14984April 2006ICS 65.080 English VersionLiming materials - Determination of product effect on soil pH -Soil incubation methodAmendements minéraux basiques - Détermination de l'effetd'un produit sur le pH d'un sol - Méthode par incubation dusolCalcium-/Magnesium-Bodenverbesserungsmittel -Bestimmung des Produkteinflusses auf den Boden-pH-Wert - BodeninkubationsverfahrenThis European Standard was approved by CEN on 2 March 2006.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 Central Secretariat 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 Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, 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© 2006 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14984:2006: E
EN 14984:2006 (E) 2 Contents Page Foreword.3 Introduction.4 1 Scope.5 2 Normative references.5 3 Terms and definitions.6 4 Principle.7 5 Method A.8 6 Method B.15 7 Test report.24 Annex A (informative)
Variations to the test methods.25 Annex B (normative)
Determination of moisture at full soil water holding capacity.27 Bibliography.28
EN 14984:2006 (E) 3 Foreword This document (EN 14984:2006) 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 October 2006, and conflicting national standards shall be withdrawn at the latest by October 2006. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, 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.
EN 14984:2006 (E) 4 Introduction The chemical methods for determining the neutralizing value (NV) (see EN 12945) and the reactivity (see EN 13971) 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. Method A characterizes products through their effect on the pH of a soil under controlled, standard conditions, which are close to those in the field. Method B establishes the efficiency of products when applied to a standard soil. However, attention is drawn to the limitations of these methods. They are laboratory methods carried out in 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.
EN 14984:2006 (E) 5 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. NOTE These methods allow comparison of products under controlled climatic conditions but do not replace field experiments. The methods are not applicable to mineral products coarser than 6,3 mm for method A or 20 mm for method B. 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. prEN 1482-1, Fertilizers and liming materials — Sampling and sample preparation — Part 1: Sampling
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 3696:1987) 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 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
EN 14984:2006 (E) 6 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 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 This efficiency is maintained even if pH later drops due to soil microbial counteraction (acidification). NOTE 2 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.
EN 14984:2006 (E) 7
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 The liming index, LIx is an indicator given by the following formula: pH4) - (pH3pH2) - pH1(x=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 time x is the length of time of the incubation test 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.
EN 14984:2006 (E) 8 4.2 Method A Monitoring after 24 h, 2 week and 4 week the changes in soil pH under controlled temperature and moisture conditions. 4.3 Method B Monitoring after 24 h, 1 week, 3 week, 6 week, 12 week, 24 week and 48 week, and 1 year, 1,5 year, 2 year and 2,5 year 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 day. The test may be stopped at any time after 3 week, 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. 5 Method A 5.1 Reagents and materials 5.1.1 Reference soilwith 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 Note in Clause 2); c) mass fraction of organic carbon 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, (72,1.×=COMO); 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, 20 ml
EN 14984:2006 (E) 9 5.2.6 Magnetic stirrer 5.2.7 Balance, capable of weighing to the nearest 1 g 5.2.8 Precision balance, capable of weighing to the nearest 1 mg 5.2.9 Test sieves, wire sieves (ISO 3310-1), 1 mm, 2 mm, 4 mm and 6,3 mm nominal aperture size 5.3 Sampling of products and sample preparation Take a sample in accordance with prEN 1482-1. 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 (4.1.2) 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.
EN 14984:2006 (E) 10
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 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). Continue the incubation process until the next measurement. Add 100 ml water (5.1.3) to the contents of each beaker, measure the pH of each settling suspension after 16 h in accordance with ISO 10390:2005, 7.1.3, 7.2 and 7.3 and record each result (see Table 2). 5.5 Expression of results For each set of six results from a pair of pots (i.e. pot A1 and pot A2, pot B1 and pot B2 and pot C1 and pot C2), after each time interval, calculate the mean values of the pH and the deviation and report them in Table 2.
EN 14984:2006 (E) 11 Table 2 — Presentation of results for method A Test Measurement or calculation pH after 24 h pH after 2 weeks pH after 4 weeks Initial pH
Soil alone
pot C1 n° 1
n° 2
n° 3
Mean value pot C1 (1 + 2 + 3) / 3
pot C2 n° 1
n° 2
n° 3
Mean value pot C2 (1 + 2 + 3) / 3
General mean
(C1 + C2) / 2
Deviation
Abs (C2 - C1)
Soil + calcium hydroxide (RLM)a
pot B1 n° 1
n° 2
n° 3
Mean value pot B1 (1 + 2 + 3) / 3
pot B2 n° 1
n° 2
n° 3
Mean value pot B2 (1 + 2 + 3) / 3
General mean
(B1 + B2) / 2
Deviation
Abs (B2 - B1)
Soil + tested product
pot A1 n° 1
n° 2
n° 3
Mean value pot A1 (1 + 2 + 3) / 3
pot A2 n° 1
n° 2
n° 3
Mean value pot A2 (1 + 2 + 3) / 3
General mean
(A1 + A2) / 2
Deviation
Abs (A2 - A1)
NOTE Additionally, it is possible to express the results as a ratio between the tested product performance and the reference liming material performance regarding the soil without any product. This ratio is called ‘Liming Index’ LI (see 3.4). It always refers to a period of time (24 h, 2 weeks, 4 weeks).
a Reference Liming Material
5.6 Precision 5.6.1 General Precision data have been established by an inter-laboratory trial, carried out in accordance with ISO 5725-1 and ISO 5725-2.
EN 14984:2006 (E) 12 5.6.2 Repeatability The absolute difference between two independent single test results, obtained using the same method on identical test material in the same laboratory by the same operator using the same equipment within the shortest feasible time interval will exceed the repeatability limit (r) on average not more than once in 20 cases in the normal and correct operation of the method. The values of r are given by Table 3 and Table 4: Table 3 — Repeatability limit r Repeatability of the measurement of the pH of treated soil and untreated soil after 24 h Number of laboratories Mean r Reference liming material (Ca(OH)2), 75 % CaO 7 1,056 0,180 Calcium carbonate (CaCO3), 53 % CaO, 80 % ≤ 140 µm 7 0,604 0,174 Burnt lime (CaO), 96 % CaO 6 1,168 0,241 Cow manure, 88,6 % DM 7 0,148 0,177 Limed sludge, 92,6 % DM, 39,8 % OM/DM 7 0,511 0,136 Green waste compost, 88,6 % DM, 58,4 % OM/DM 7 0,172 0,176 Repeatability of the measurement of the pH of treated soil and untreated soil after 2 weeks Number of laboratories Mean r Reference liming material (Ca(OH)2), 75 % CaO 7 1,011 0,136 Calcium carbonate (CaCO3), 53 % CaO, 80 % ≤ 140 µm 6 0,683 0,070 Burnt lime (CaO), 96 % CaO 4 1,270 0,204 Cow manure, 88,6 % DM 7 0,039 0,133 Limed sludge, 92,6 % DM, 39,8 % OM/DM 7 0,454 0,126 Green waste compost, 88,6 % DM, 58,4 % OM/DM 7 0,056 0,117 Repeatability of the measurement of the pH of treated soil and untreated soil after 4 weeks Number of laboratories Mean r Reference liming material (Ca(OH)2), 75 % CaO 4 1,285 0,073 Calcium carbonate (CaCO3), 53 % CaO, 80 % ≤ 140 µm 4 0,756 0,075 Burnt lime (CaO), 96 % CaO 4 1,359 0,215 Cow manure, 88,6 % DM 5 0,043 0,023 Limed sludge, 92,6 % DM, 39,8 % OM/DM 3 0,507 0,063 Green waste compost, 88,6 % DM, 58,4 % OM/DM 5 0,089 0,039
EN 14984:2006 (E) 13
Table 4 — Liming Index - repeatability limit r Repeatability of the determination of the Liming Index after 24 h
Number of laboratories Mean r Calcium carbonate (CaCO3), 53 % CaO, 80 % ≤ 140 µm 7 57,219 13,00 Burnt lime (CaO), 96 % CaO 6 121,053 24,403 Cow manure, 88,6 % DM 7 14,735 20,649 Limed sludge, 92,6 % DM, 39,8 % OM/DM 5 48,234 11,993 Green waste compost, 88,6 % DM, 58,4 % OM/DM 7 15,831 22,353 Repeatability of the determination of the liming index after 2 weeks Number of laboratories Mean r Calcium carbonate (CaCO3), 53 % CaO, 80 % ≤ 140 µm 7 61,592 6,890 Burnt lime (CaO), 96 % CaO 5 118,973 16,288 Cow manure, 88,6 % DM 5 5,180 8,047 Limed sludge, 92,6 % DM, 39,8 % OM/DM 6 49,669 18,252 Green waste compost, 88,6 % DM, 58,4 % OM/DM 6 8,958 10,303 Repeatability of the determination of the liming index after 4 weeks Number of laboratories Mean r Calcium carbonate (CaCO3), 53 % CaO, 80 % ≤ 140 µm 7 66,369 10,688 Burnt lime (CaO), 96 % CaO 5 124,879 21,573 Cow manure, 88,6 % DM 5 6,350 4,566 Limed sludge, 92,6 % DM, 39,8 % OM/DM 6 48,316 14,333 Green waste compost, 88,6 % DM, 58,4 % OM/DM 6 12,765 27,582
EN 14984:2006 (E) 14 5.6.3 Reproducibility
The absolute difference between two independent single test results, obtained using the same method on identical test material in different laboratories with different operators using different equipment will exceed the reproducibility limit (R) on average no
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