SIST EN 14429:2015

Characterisation of waste - Leaching behaviour test - Influence of pH on leaching with initial acid/base addition

This European Standard specifies a method for the determination of the influence of pH on the leachability of inorganic constituents from a waste material. The equilibrium condition as defined in the standard is established by addition of pre-determined amounts of acid or base to reach desired end pH values. This test method produces eluates, which are subsequently characterized physically and chemically.
This European Standard is a parameter specific test as specified in EN 12920. The application of this test method alone is not sufficient for the determination of the detailed leaching behaviour of a waste under specified conditions.

Charakterisierung von Abfällen - Untersuchung des Auslaugungsverhaltens - Einfluss des pH-Wertes unter vorheriger Säure/Base Zugabe

Diese Europäische Norm legt ein Verfahren für die Bestimmung des Einflusses des pH-Wertes auf die Eluierbarkeit von anorganischen Bestandteilen aus Abfall fest. Der Gleichgewichtszustand, wie er in dieser Norm definiert ist, wird durch Zugabe einer vorher bestimmten Menge an Säure oder Base hergestellt, um die gewünschten endgültigen pH-Werte zu erreichen. Dieses Prüfverfahren führt zu Eluaten, die anschließend physikalisch und chemisch charakterisiert werden.
Diese Europäische Norm ist eine parameterspezifische Prüfung, wie in EN 12920 festgelegt. Die Anwendung nur dieses Prüfverfahrens ist für die Bestimmung des genauen Elutionsverhaltens eines Abfalls unter festgelegten Bedingungen nicht ausreichend.

Caractérisation des déchets - Essais de comportement à la lixiviation - Influence du pH sur la lixiviation avec ajout initial d'acide/base

La présente Norme européenne définit une méthode de détermination de l’influence du pH sur la lixiviabilité des constituants inorganiques d’un déchet. L’état d’équilibre tel que défini dans la présente norme s’obtient en ajoutant des quantités prédéfinies d’acide ou de base pour atteindre les valeurs de pH souhaitées. Cette méthode d’essai produit des éluats qui sont ensuite caractérisés du point de vue physico-chimique.
La présente Norme européenne est un essai paramétrique, tel que spécifié dans l’EN 12920. Cette méthode d’essai n’est pas suffisante, à elle seule, pour déterminer le comportement à la lixiviation d’un déchet dans des conditions spécifiées.

Karakterizacija odpadkov - Izluževalni preskus - Vpliv pH na izluževanje z začetnim dodatkom kisline/baze

General Information

• Status: Published
• Public Enquiry End Date: 19-Nov-2013
• Publication Date: 07-May-2015
• ICS: 13.030.01 - Wastes in general
• Technical Committee: KAT - Soil quality
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 16-Apr-2015
• Due Date: 21-Jun-2015
• Completion Date: 08-May-2015
• Directive: 99/31/EC - Landfill of waste
• Directive: TP131 - Uredba o odlagališčih odpadkov
• Mandate: M/326 - Standardization mandate to CEN for the development of standardized methods for the characterization of waste
• Ref Project: EN 14429:2015 - Characterization of waste - Leaching behaviour test - Influence of pH on leaching with initial acid/base addition

Relations

• Replaces: SIST-TS CEN/TS 14429:2006 - Characterization of waste - Leaching behaviour tests - Influence of pH on leaching with initial acid/base addition
• Effective Date: 01-Jun-2015

Overview

EN 14429:2015 - Characterization of waste: Leaching behaviour test - Influence of pH on leaching with initial acid/base addition (CEN) - defines a laboratory method to determine how pH affects the leachability of inorganic constituents from waste materials. The method establishes an equilibrium condition by adding pre-determined amounts of acid or base to reach a set of end pH values and produces eluates that are subsequently characterized physically and chemically. EN 14429:2015 is a parameter-specific test (per EN 12920) and is intended for basic characterization rather than a complete leaching assessment on its own.

Key topics and technical requirements

• Test principle: pH dependence is assessed by initial acid/base addition to test portions to reach target end-pH values; eluates are collected after a defined contact time and analyzed.
• Sample preparation: guidance on laboratory sample reduction, preparation of test portions and determination of dry residue to ensure representative testing.
• Reagents and equipment: specified laboratory-grade acids/bases and standard laboratory apparatus; water quality and preservation requirements are referenced.
• Procedure elements:
  • Selection of pH range and target end-pH values
  • Preparation of leachant and controlled addition of acid/base
  • Contact time, agitation and approaches to approach equilibrium
  • Eluate treatment, storage and analytical characterization
• Supporting tests and checks: blank tests, preliminary titration for acid/base neutralization capacity (ANC/BNC), and guidance on dividing acid/base consumption for extreme pH values.
• Performance and quality: inclusion of repeatability and reproducibility data (Annex E) and a required test report with standardized metadata.
• Scope and limitations: clear statement that this method alone is not sufficient to fully characterize leaching under all environmental conditions; distinguishes this initial-addition test from pH-static tests with continuous control (e.g., EN 14997).

Applications

• Identifying pH-sensitive release of inorganic contaminants (metals, major ions) from wastes, soils, sediments and construction materials.
• Supporting basic characterization for waste management, landfill acceptance, material recycling and environmental risk screening.
• Providing data to select targeted follow-up tests or compliance procedures as part of a larger leaching test program.

Who uses this standard

• Environmental laboratories and accredited testing facilities
• Waste producers, recyclers and construction material manufacturers
• Landfill operators, consultants and environmental risk assessors
• Regulators and permitting authorities implementing EU/EFTA waste characterization frameworks

Related standards

• EN 12920 (parameter specific tests framework)
• EN 14997 (pH-static / continuous pH control leaching test)
• EN 14346, EN 15002, EN 16192, EN 14899 (sampling, sample prep, eluate analysis)
• EN ISO 3696, EN ISO 5667-3 (water for analytical use; sample preservation)

EN 14429:2015 is a practical, standardized method for assessing pH-driven leaching behaviour and should be used within a broader testing strategy for robust waste characterization.

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Charakterisierung von Abfällen - Untersuchung des Auslaugungsverhaltens - Einfluss des pH-Wertes unter vorheriger Säure/Base ZugabeCaractérisation des déchets - Essais de comportement à la lixiviation - Influence du pH sur la lixiviation avec ajout initial d'acide/baseCharacterisation of waste - Leaching behaviour test - Influence of pH on leaching with initial acid/base addition13.030.01Odpadki na splošnoWastes in generalICS:Ta slovenski standard je istoveten z:EN 14429:2015SIST EN 14429:2015en,fr,de01-junij-2015SIST EN 14429:2015SLOVENSKI
STANDARDSIST-TS CEN/TS 14429:20061DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 14429
March 2015 ICS 13.030.01 Supersedes CEN/TS 14429:2005English Version
Characterization of waste - Leaching behaviour test - Influence of pH on leaching with initial acid/base addition
Caractérisation des déchets - Essais de comportement à la lixiviation - Influence du pH sur la lixiviation avec ajout initial d'acide/base
Charakterisierung von Abfällen - Untersuchung des Elutionsverhaltens - Einfluss des pH-Wertes auf die Elution unter vorheriger Säure/Base-Zugabe This European Standard was approved by CEN on 26 December 2014.
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
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 14429:2015 ESIST EN 14429:2015

Example of a data sheet . 19 Annex B (informative)
Operation and uses of the test — Influence of pH on the leaching behaviour . 20 B.1 Clarification of the two modes of operation of the test: influence of pH on the leaching behaviour . 20 B.2 Expression of results . 22 B.3 Scope and limits of the application field of the test . 22 B.3.1 Remarks on the use of pH dependence test results to assess the effects of ageing . 22 B.3.2 Examples of test result use and considerations on scope . 23 B.4 Example: Identification of the sensitivity of leaching to pH over the environmentally relevant pH range. 24 Annex C (informative)
Preliminary determination of the acid/base consumption . 25 C.1 General . 25 SIST EN 14429:2015

Examples of acid and base neutralization capacities for waste, soil, sediment and construction materials . 30 D.1 Examples of acid and base neutralization capacities . 30 D.2 Use of acid and base neutralization capacity data . 32 Annex E (informative)
Repeatability and reproducibility data . 33 E.1 Materials used in the interlaboratory comparison study . 33 E.2 Interlaboratory comparison results . 33 Bibliography . 51
1) Council Directive 1999/31/EC of 26 April 1999 on the landfill of waste. 2) Council Decision 2003/33/EC of 19 December 2002. SIST EN 14429:2015

is the undried mass of the test portion, in grams (g); Md
is the dried mass of the test portion, in grams (g); wdr is the dry residue of the waste, expressed as a percentage (%). 9 Procedure 9.1 Contact time The leaching procedure consists of three defined stages: — Period A (acid/base addition)
from t0 up t0 + 4 h for acid/base addition in three steps; — Period B (equilibration period) from t0 + 4 h up to t0 + 44 h equilibration period; — Period C (verification period) from t0 + 44 h up to t0 + 48 h for verification of equilibrium condition. Measure the pH in the liquid after each of these periods. The total contact period (A+B+C) is 48 h. 9.2 pH range The test shall cover the range pH 2 to pH 12 (both included i.e. the lowest value ≤ 2 and the highest value ≥ 12) with at least 8 pH values tested including the natural pH (without acid or base addition). The maximum difference between two consecutive pH values shall not exceed 1,5 pH units. NOTE To ensure that the appropriate pH values can be obtained in one run additional bottles can be prepared of which only the ones with the desired final pH values are retained for analysis. The pH range covered by the test may be restricted to a pH range relevant for the specific material and the considered problem. The pH range to be covered can also depend on the specific properties of the waste material, the available information on this material and the questions to be answered by performing the test. The number of pH levels considered can be reduced or increased in a specific pH domain as needed. Release measured at low pH (pH = 2) can be used to estimate the potential availability for leaching, which is a relevant property for geochemical modelling. SIST EN 14429:2015

is the dry mass of the test portion, in grams (g) (see 8.4). NOTE In relation to L/S-ratio, V in this equation is equivalent with the ”L” and Md is equivalent to the “S”. Calculate the amount of leachant to be added to the actual size of test portion and compensate for the moisture content in the test portion, as follows: 1001Lddr()VVMw=−−× (4) where VL is the volume of leachant to be added, in ml; V is the total volume of liquid in the test, in ml; Md
is the dry mass of the test portion, in grams (g) (see 8.4); wdr is the dry residue of the waste, expressed as percentage (%) (see 8.3). Prepare the leachant from demineralized water (see 6.1) and acid or base (see 6.2 or 6.3) according to the acid/base consumption for the relevant pH. Prepare the acid adjusted leachant as follows: LdeminAVVV=+ (5) dAAAMVC×= (6) where SIST EN 14429:2015

is the dry mass of the test portion, in grams (g) (see 8.4); CA is the concentration of the acid, in mole per litre (mol/l) (see 6.2). Prepare the base adjusted leachant as follows: LdeminBVVV=+ (7) dBBBMVC×= (8) where VL is the volume of prepared leachant, in ml; Vdemin is the volume of demineralized water used, in ml; VB is the volume of base needed, in ml; B is the base consumption for the pH, in mol OH-/kg DM; Md
is the dry mass of the test portion, in grams (g) (see 8.4); CB is the concentration of the base, in mole per litre (mol/l) (see 6.3). Split the volume VL of leachant into 3 equal fractions VL/3. 9.3.3 Leaching procedure Carry out the test at a temperature of 20 °C ± 5 °C. Select the appropriate bottle size according to the test portion size. For Md =15 g, 30 g and 60 g, this means respectively bottle sizes of 250 ml, 500 ml and 1 000 ml. Clean the bottle before use by filling it with 1 mol/l nitric acid (see 6.2), leaving it for at least 24 h and then flushing it out with demineralized water (see 6.1). Place one of the test portions in the rinsed bottle. Add the leachant volume VL/3 at three different times: — 1st fraction at t0; — 2nd fraction at t0 + 30 min; — 3rd fraction at t0 + 2 h. Close the bottle and agitate the suspension (see 7.2.1) between each leachant addition. Measure and record pH before addition of fractions 2 and 3, and prepare additional bottles with modified acid/base addition, if deviations are observed from the expected pH at that time. Continue to agitate after the last leachant addition until t = t0 + 48 h. SIST EN 14429:2015

NOTE The repeatability limit (r) and the reproducibility limit (R) as given in Tables E.2 and E.3 and in Table 1 are indicative values of the attainable precision, if the determination of the pH dependent leaching behaviour of substances from waste and stabilized waste is performed in accordance with this European Standard [EN 14429]. A limited number of materials and parameters were tested. Consequently, for other materials and parameters, performance characteristics may fall outside the limits as derived from the validation of the determination of the pH dependent leaching behaviour of substances from waste and stabilized waste. In particular for relatively heterogeneous materials, the repeatability and the reproducibility limits may be larger than the values given in Tables E.2 and E.3 and in Table 1. 13 Test report In order to conform to this European Standard include the following information in the test report: a) reference to this European Standard; b) date of receipt of the laboratory sample; c) sampling report according to 8.1; d) date of the test (beginning and end); e) complete identification of the laboratory sample (including dry residue); f) pretreatment (e.g. method of size-reduction, drying, sub-division) and storage conditions; g) temperature range during the performance of the test; h) selected pH interval and number of test portions tested (N) within this interval; i) dry mass of the test portion (g); j) acid volumes (ml) and concentrations (mol/l), base volumes (ml) and concentrations (mol/l) and the corresponding amounts of H+ or OH- (mol/kg DM); k) leachant volume (ml) and the resulting L/S (l/kg); SIST EN 14429:2015

h and t0 + 48 h, and difference in pH between t0 + 4 h and t0 + 44
h and between t0 + 44
h and t0 + 48 h; n) the method of preservation for the different elements in accordance with Clause 9; o) the analytical report in accordance with Clause 9; p) the date of the latest blank test. Blank results shall be available upon request; q) any deviation from the test method and the reason of this deviation together with all circumstances that have influenced the results; r) record the data for the test results on a data sheet. NOTE An example of the data sheet is given in Annex A. SIST EN 14429:2015

Example of a data sheet Table A.1 — An example of a data sheet for the recording of test results
Unit Bottle no.
1 2 3 4 5 6 7 8 Dry mass of the test portion g
Acid volume ml
Acid concentration mol/l
Base volume ml
Base concentration mol/l
H+ or OH- mol/kg DM
Leachant volume ml
Resulting L/S l/kg
pH at t0 + 4 h
pH at t0 + 44 h
pH at t0 + 48 h
ûpe (t0 + 4 h) - (t0 + 44 h)
ûpe (t0 + 44 h) - (t0 + 48 h)
Constituent 1 : mg/l
Constituent 2 : mg/l
Constituent 3 : mg/l
Constituent 4 : mg/l
Constituent 5 : mg/l
Constituent 6 : mg/l
etc.
Operation and uses of the test — Influence of pH on the leaching behaviour B.1 Clarification of the tw
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