EN 15875-2011 en Characterization of waste - Static test for determination of acid potential and neutralisation potential of sulfidic waste (Incorporating corrigendum August 2012)《.pdf

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1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 15875:2011Characterization of waste Static test for determinationof acid potential andneutralisation potential ofsulfidic wasteBS EN 15875:2011Incorporating corrigendum Aug

2、ust 2012BS EN 15875:2011 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 15875:2011.The UK participation in its preparation was entrusted to TechnicalCommittee B/508/3, Characterization of waste.A list of organizations represented on this committee can beobtaine

3、d on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2012. Published by BSI StandardsLimited 2012 ISBN 978 0 580 64440 5ICS 13.030.10 Compliance with a

4、 British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 30 April 2012.Amendments issued since publicationDate Text affectedBS EN 15875:2011 BRITISH STANDARDNational forewordThis British St

5、andard is the UK implementation of EN 15875:2011, incorporating corrigendum August 2012.The UK participation in its preparation was entrusted by Technical Committee B/508, Waste Management, to Subcommit ee B/508/3, harac erization of waste.subcommittee can be /corrigenda iss ed since publicationDate

6、 Text affected30 April 2013 Implementation of CEN corrigendum August 2012: Modification to Table 13 380587BS EN 15875:2011EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15875 October 2011 ICS 13.030.10 English Version Characterization of waste - Static test for determination of acid potential

7、and neutralisation potential of sulfidic waste Caractrisation des dchets - Essai statique pour la dtermination du potentiel de gnration dacide et du potentiel de neutralisation des dchets sulfurs Charakterisierung von Abfllen - Statische Prfung zur Bestimmung des Surebildungspotenzials und des Neutr

8、alisationspotenzials von sulfidhaltigen Abfllen This European Standard was approved by CEN on 17 September 2011. 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 al

9、teration. 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 m

10、ade 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, Est

11、onia, 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 STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUR

12、OPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15875:2011: EIncorporating corrigendum August 2012BS EN 15875:2011EN 15875:2011 (E) 2 Contents Pa

13、ge Foreword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Symbols and abbreviations 65 Principle 76 Reagents and laboratory devices 76.1 Reagents .76.2 Laboratory devices 77 Sampling and sample preparation .77.1 Laboratory sample .77.2 Test sample 87.3 Determination of

14、 dry residue of the sample .87.4 Test portion for the determination of neutralisation potential 88 Test procedures .98.1 Determination of acid potential 98.1.1 General 98.1.2 Total sulfur content .98.1.3 Determination of sulfur species .98.1.4 Calculation 98.2 Determination of neutralisation potenti

15、al 108.2.1 General . 108.2.2 Carbonate rating . 108.2.3 Neutralisation potential 108.2.4 Calculation . 129 Calculation of neutralisation potential ratio and net neutralisation potential 1210 Performance characteristics . 1311 Test report . 13Annex A (informative) Example of a data sheet for the reco

16、rding of test results according to 8.2.3 . 15Annex B (informative) Operation and uses of the test: influence of parameters 16B.1 Sulfur determination . 16B.2 Particle size . 16B.3 Mineralogy . 16B.3.1 Sources of acidity . 16B.3.2 Neutralisation potential 18Annex C (informative) Speciation of sulfur

17、compounds 20Annex D (informative) Explanation of formulas used . 23D.1 Acid potential 23D.2 Carbonate rating . 23Bibliography . 25BS EN 15875:2011EN 15875:2011 (E) 3 Foreword This document (EN 15875:2011) has been prepared by Technical Committee CEN/TC 292 “Characterization of waste”, the secretaria

18、t of which is held by NEN. 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 April 2012, and conflicting national standards shall be withdrawn at the latest by April 2012. Attention is drawn to the

19、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. The preparation of this document by CEN is based on a mandate by the European Commission (Mandate M/395), which

20、assigned the development of standards on the characterization of waste from extractive industries. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cy

21、prus, 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 the United Kingdom. BS EN 15875:2011EN 15875:2011 (E) 4

22、 Introduction This document has been developed primarily to support the implementation of the Directive 2006/21/EC of the European Parliament and of the council on the management of waste from the extractive industries, especially relating to technical requirements for waste characterization as sulf

23、ide bearing materials may generate sulfuric acid when subjected to weathering. Test methods for the determination of acid generation behaviour can be divided in static and kinetic tests. A static test is usually relatively fast to perform, but gives only indicative information based on total composi

24、tion of the waste material. The kinetic test gives more detailed information on behaviour based on reaction rates under specified conditions. This standard only covers static testing. The application of this test method alone may not be sufficient to determine the actual potential in the field for t

25、he formation of acidic drainage as site specific conditions will affect the behaviour in the field and require a more detailed assessment. To carry out a more precise assessment of the acid generation potential and buffering capacity mineralogical information is required. A number of special cases c

26、an be identified: e.g. presence of sulfate (e.g. gypsum), non-acid producing sulfides or carbonates with no buffering capacity. Acid neutralisation behaviour as obtained by other methods can provide additional information in circumstances of uncertainty. BS EN 15875:2011EN 15875:2011 (E) 5 1 Scope T

27、his European standard specifies methods to determine the potential of sulfide bearing materials for the formation of acidic drainage. Specified are methods for determining both the acid potential (AP) and the neutralisation potential (NP) of the material. From these results the net neutralisation po

28、tential (NNP) and the neutralisation potential ratio (NPR) are calculated. This European standard is applicable to all sulfide bearing wastes from the extractive industries excluding wastes which will have pH 6,0 20 Measure and record the pH of the slurry after 22 h 15 min. If the pH is above 2,5 ad

29、d HCl (6.1.2) to adjust the pH between 2,0 and 2,5. It is strongly recommended to adjust the pH as close as possible to 2,0 to ensure being in the range of pH = 2,0 to 2,5 at t = 24 h. Record the exact volume added (VA, t=22h) and the pH after the acid addition. If the pH at t = 22 h before acid add

30、ition is below pH = 2,0, too much acid was added in the beginning of the test and the test shall be repeated adding a smaller volume of acid. For the repeated test use the acid addition at start (t = 0) in table 1 one line above the one used in the discarded test. EXAMPLE 1 In the test the added HCl

31、 was VA, t=0= 1,5 ml which corresponds to line 2 in table 1. At t = 22 h the measured pH was pH 2,5). If neither a smaller nor a bigger volume of initial acid addition from Table 1 leads to completion of the test due to problems described in examples above it is allowed to use an initial volume of a

32、cid deviating from Table 1. This deviation should be documented in the test report together with information of the acid volumes used in the preceding trials. EXAMPLE 3 VA, t=0= 10 ml is used corresponding to line 7 in Table 1. At t = 22 h pH is adjusted to 2,0. Still, pH of the slurry is above 2,5

33、at t = 24 h. In the next trial VA, t=0= 14 ml is used corresponding to line 8 in table 1 leading to pH of the slurry being below 2,0 at t = 22 h. For the following trial e.g. VA, t=0= 12 ml may be tried. Volume c(HCI) = 1 mol/l (6.1.2) to be added in mlBS EN 15875:2011EN 15875:2011 (E) 12 NOTE 2 Mat

34、erials usually contain other neutralizing compounds than calcium carbonate, which may react slower than calcium carbonate and thus leads to underestimation of NP. (See Annex B). Titrate the slurry to a pH of 8,3 using a sodium hydroxide solution (6.1.3). Record the exact volume of NaOH consumed in t

35、itration. NOTE 3 The end point of the back-titration is 8,3, being the usual endpoint for acidity titrations, corresponding to the stoichiometric equivalence point for carbonate/bicarbonate in natural waters in which carbonic acid is the most dominant weak acid. NOTE 4 An example of a data sheet for

36、 the recording of test results is given in Annex A, Table A.1. 8.2.4 Calculation Calculate the NP of the sample expressed as H+content in mol/kg and as carbonate equivalents (CaCO3) in kg/t as follows: a) expressed as H+content in mol/kg (Equation (5) dBA(NaOH)(NaOH)(HCl)(HCl)NPMVcVc = (5) where c(H

37、Cl) is the concentration of HCl in mol/l; VA(HCl) is the volume of HCl added (VA, t=0 + VA, t=22h) in ml; c(NaOH) is the concentration of NaOH in mol/l; VB(NaOH) is the volume of NaOH used in back titration in ml; Mdis the dry mass of the test portion expressed in grams (g). b) expressed as carbonat

38、e equivalents (CaCO3) in kg/t (Equation (6) dBA(NaOH)(NaOH)(HCl)(HCl)50NPMVcVc = (6) 9 Calculation of neutralisation potential ratio and net neutralisation potential The acid potential (AP) and neutralisation potential (NP) are to be calculated in H+content in mol/kg. The resulting neutralisation po

39、tential ratio (NPR) (potential for neutralisation of acidic drainages) is assessed using the formula in Equation (7): APNPNPR = (7) NOTE 1 A NPR 1 should be enough to avoid acidic drainage. However, the reaction rates may differ between AP minerals and NP minerals. Different mineralogy and crystalli

40、ne structure may also lead to different availability. Thus, there is a range of NPR-values which will be interpreted as uncertain. (see Annex B). NOTE 2 In some countries the acid potential is expressed as pyrite in mol/kg instead of H+in mol/kg, these figures differ by a factor of 4. Consequently,

41、the value for insufficient neutralisation capacity would be NPR 2 provides an additional source of acidity. These minerals are therefore important as both sinks and potential sources of acidity. B.3.2 Neutralisation potential The determination of neutralisation potential (NP) is dependent on a numbe

42、r of parameters. Apart from sample mineralogy, the most important have been identified as being sample pre-treatment, temperature, testing time, particle size, end pH and back-titration pH. Some of them have already been defined in existing international method descriptions (Lawrence and Wang 3), wi

43、th levels set where results have been empirically proven to be appropriate. Other important parameters have been defined in this standard to increase the reproducibility and comparability of results. All NP is assumed to react like calcite in acidic conditions CaCO3+ 2H+ Ca2+ H2CO30 (B.4) Fe and Mn

44、carbonates are not neutralising under aerobic conditions (i.e. siderite, FeCO3, and rhodochrosite, MnCO3.); Silicates (and some other minerals) will contribute to the neutralisation to some extent (slower reaction than calcite); In sulfidic soils (clays) organic matter may contribute significantly t

45、o the neutralising capacity. When using the test described in this European standard it is assumed that all neutralisating capacity is determined within the testing time of 24 h. However, some minerals react faster, others slower. To give an indication of reactivity of some carbonate minerals the fo

46、llowing sequence may be used: monohydrocalcite aragonite calcite dolomite magnesite siderite rhodochrosite In Table B.1, a more detailed list of carbonate minerals is shown. BS EN 15875:2011EN 15875:2011 (E) 19 Table B.1 Mineralized environment, carbonate minerals. Mineral group Mineral Chemical For

47、mula Hydrated carbonates Monohydrocalcite CaCO3. H2O Aragonite group: Orthorhombic Aragonite CaCO3 Calcite group: Trigonal Calcite CaCO3 Magnesite MgCO3 Rhodochrosite MnCO3 Siderite FeCO3 Dolomite group: Trigonal Ankerite CaFe(CO3)2 Dolomite CaMg(CO3)2 Carbonates with hydroxyl or halogen Azurite Cu3

48、(CO3)2(OH)2 Malachite Cu2CO3(OH)2 If slowly reacting carbonates or silicates are present in higher concentrations the application of a dynamic test may be advisable to give a more realistic forecast of waste behaviour. CEN/TS 14429, CEN/TS 14497 and CEN-ISO/TS 21268-4 can provide more detailed acid

49、neutralisation behaviour of materials over wider pH ranges and assess the contributions of non-carbonate neutralisation and non-neutralising carbonates. Geochemical modelling of major elements analysed in sulfidic mining waste have also been shown to provide mineral and other phases contributing to ANC over pH ranges from pH 2 to 8. BS EN 15875:2011EN 15875:2011 (E) 20 Annex C (informative) Speciation of sulfur compounds For the analysis of sulfur species, no inter