DIN EN 15875-2012 Characterization of waste - Static test for determination of acid potential and neutralisation potential of sulfidic waste German version EN 15875 2011《废料特性描述 硫化物.pdf

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1、November 2012 Translation by DIN-Sprachendienst.English price group 13No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).I

2、CS 13.030.10!$Jg“1923968www.din.deDDIN EN 15875Characterization of waste Static test for determination of acid potential and neutralisationpotential of sulfidic waste;English version EN 15875:2011 + AC:2012,English translation of DIN EN 15875:2012-11Charakterisierung von Abfllen Statische Prfung zur

3、 Bestimmung des Surebildungspotenzials und desNeutralisationspotenzials von sulfidhaltigen Abfllen;Englische Fassung EN 15875:2011 + AC:2012,Englische bersetzung von DIN EN 15875:2012-11Caractrisation des dchets Essai statique pour la dtermination du potentiel de gnration dacide et du potentiel dene

4、utralisation des dchets sulfurs;Version anglaise EN 15875:2011 + AC:2012,Traduction anglaise de DIN EN 15875:2012-11SupersedesDIN EN 15875:2012-01www.beuth.deDocument comprises In case of doubt, the German-language original shall be considered authoritative.27 pages10.12- DIN EN 15875:2012-11 2 A co

5、mma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 292 “Characterization of waste” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Co

6、mmittee), Working Committee NA 119-01-02-02 UA Chemische und physikalische Verfahren. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 3310-1 DIN ISO 3310-1 ISO 15178 DIN ISO 15178 ISO 16720 DIN EN ISO 16720 Amendments This standard diff

7、ers from DIN EN 15875:2012-01 as follows: a) modification to 8.2.3: in Table 1, in the heading of the last column, “c(HCI) = 0,1 mol/l” has been replaced with “c(HCI) = 1 mol/l”. Previous editions DIN EN 15875: 2012-01 National Annex NA (informative) Bibliography DIN ISO 3310-1, Test sieves Technica

8、l requirements and testing Part 1: Test sieves of metal wire cloth DIN ISO 15178, Soil quality Determination of total sulfur by dry combustion DIN EN ISO 16720, Soil quality Pretreatment of samples by freeze-drying for subsequent analysis EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15875 Oc

9、tober 2011 ICS 13.030.10 English Version Characterization of waste - Static test for determination of acid potential 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 dc

10、hets sulfurs Charakterisierung von Abfllen - Statische Prfung zur Bestimmung des Surebildungspotenzials und des Neutralisationspotenzials 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 Regulati

11、ons 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.

12、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 m

13、embers are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spa

14、in, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES 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 M

15、embers. Ref. No. EN 15875:2011: E2 Contents Page 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

16、sample .77.2 Test sample 87.3 Determination of 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 Calculatio

17、n 98.2 Determination of neutralisation potential 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 (inf

18、ormative) Example of a data sheet for the recording 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

19、 18Annex C (informative) Speciation of sulfur compounds 20Annex D (informative) Explanation of formulas used . 23D.1 Acid potential 23D.2 Carbonate rating . 23Bibliography . 25DIN EN 15875:2012-11 EN 15875:2011 + AC:2012 (E) 3 Foreword This document (EN 15875:2011 has been prepared by Technical Comm

20、ittee CEN/TC 292 “Characterization of waste”, the secretariat 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 withd

21、rawn at the latest by April 2012. 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. The preparation of this document by CEN is based on

22、a mandate by the European Commission (Mandate M/395), which 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 thi

23、s European Standard: Austria, Belgium, Bulgaria, Croatia, 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

24、 and the United Kingdom. + AC:2012)DIN EN 15875:2012-11 EN 15875:2011 + AC:2012 (E) 4 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 industr

25、ies, especially relating to technical requirements for waste characterization as sulfide 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 rel

26、atively fast to perform, but gives only indicative information based on total composition 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 me

27、thod alone may not be sufficient to determine the actual potential in the field for the 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

28、buffering capacity mineralogical information is required. A number of special cases can 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 infor

29、mation in circumstances of uncertainty. DIN EN 15875:2012-11 EN 15875:2011 + AC:2012 (E) 5 1 Scope This 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)

30、 and the neutralisation potential (NP) of the material. From these results the net neutralisation potential (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

31、 have pH 6,0 20Measure and record the pH of the slurry after 22 h 15 min. If the pH is above 2,5 add 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

32、 volume added (VA, t=22h) and the pH after the acid addition. If the pH at t = 22 h before acid addition 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

33、) in table 1 one line above the one used in the discarded test. EXAMPLE 1 In the test the added HCl 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

34、of the test due to problems described in examples above it is allowed to use an initial volume of acid 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 correspon

35、ding 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 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 trie

36、d. DIN EN 15875:2012-11 EN 15875:2011 + AC:2012 (E) 12 NOTE 2 Materials 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 hydroxid

37、e solution (6.1.3). Record the exact volume of NaOH consumed in titration. 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 t

38、he most dominant weak acid. NOTE 4 An example of a data sheet for 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/

39、kg (Equation (5) dBA(NaOH)(NaOH)(HCl)(HCl)NPMVcVc = (5) where c(HCl) 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

40、the test portion expressed in grams (g). b) expressed as carbonate 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 c

41、alculated in H+content in mol/kg. The resulting neutralisation potential 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 betwee

42、n AP minerals and NP minerals. Different mineralogy and crystalline 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

43、+in mol/kg, these figures differ by a factor of 4. Consequently, 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 deter

44、mination of neutralisation potential (NP) is dependent on a number 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 exi

45、sting international method descriptions (Lawrence and Wang 3), with 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 cal

46、cite in acidic conditions CaCO3+ 2H+ Ca2+ H2CO30 (B.4) Fe and Mn 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 sul

47、fidic soils (clays) organic matter may contribute significantly to 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 g

48、ive an indication of reactivity of some carbonate minerals the following sequence may be used: monohydrocalcite aragonite calcite dolomite magnesite siderite rhodochrosite In Table B.1, a more detailed list of carbonate minerals is shown. DIN EN 15875:2012-11 EN 15875:2011 + AC:2012 (E) 19 Table B.1

49、 Mineralized environment, carbonate minerals. Mineral group Mineral Chemical Formula 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(CO3)2(OH)2 Malachite Cu2CO3(OH)2 If slowly reacting carbonat