1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 12782-5:2012Soil quality Parametersfor geochemical modellingof leaching and speciationof constituents in soils andmaterialsPart 5: Extraction of humic substances fromaq
2、ueous samples (ISO 12782-5:2012)BS EN ISO 12782-5:2012 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO12782-5:2012.The UK participation in its preparation was entrusted to TechnicalCommittee EH/4, Soil quality.A list of organizations represented on this comm
3、ittee can beobtained 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 2012ISBN 978 0 580 66915 6ICS 13.080.05
4、Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 30 June 2012.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM
5、 EN ISO 12782-5 June 2012 ICS 13.080.05 English Version Soil quality - Parameters for geochemical modelling of leaching and speciation of constituents in soils and materials - Part 5: Extraction of humic substances from aqueous samples (ISO 12782-5:2012) Qualit du sol - Paramtres pour la modlisation
6、 gochimique de la lixiviation et de la spciation des constituants des sols et des matriaux - Partie 5: Extraction des substances humiques des chantillons aqueux (ISO 12782-5:2012) Bodenbeschaffenheit - Parameter zur geochemischen Modellierung der Elution und Speziation von Bestandteilen in Bden und
7、Materialien - Teil 5: Extraktion von Huminstoffen aus wssrigen Proben (ISO 12782-5:2012) This European Standard was approved by CEN on 31 May 2012. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of
8、 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)
9、. 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, C
10、yprus, 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, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDAR
11、DIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 12782-5:2012: EBS EN ISO 12782-5:2012EN ISO 12782-
12、5:2012 (E) 3 Foreword This document (EN ISO 12782-5:2012) has been prepared by Technical Committee ISO/TC 190 “Soil quality“ in collaboration with Technical Committee CEN/TC 345 “Characterization of soils” the secretariat of which is held by NEN. This European Standard shall be given the status of a
13、 national standard, either by publication of an identical text or by endorsement, at the latest by December 2012, and conflicting national standards shall be withdrawn at the latest by December 2012. Attention is drawn to the possibility that some of the elements of this document may be the subject
14、of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgar
15、ia, 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, Turkey and the United Kingdom. Endorsement
16、notice The text of ISO 12782-5:2012 has been approved by CEN as a EN ISO 12782-5:2012 without any modification. BS EN ISO 12782-5:2012ISO 12782-5:2012(E) ISO 2012 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope 12 Normative references . 13 Terms and definitions . 14 Principle .
17、35 Apparatus 36 Reagents 37 Sampling 47.1 Laboratory sample 47.2 Test sample . 47.3 Test portion . 48 Procedure 48.1 Preparation of DAX-8 resin . 48.2 Determination of total humic acid (HA), fulvic acid (FA) and hydrophilic organic carbon (Hy) content in aqueous samples 59 Eluate treatment and stora
18、ge . 510 Analytical determination . 511 Blank test . 512 Calculation 612.1 General correction factors for the calculation of humic acid (HA), fulvic acid (FA), hydrophilic organic carbon (Hy) and hydrophobic neutral organic carbon (HON) in aqueous samples 612.2 Concentration of total humic acid (HA)
19、, fulvic acid (FA), hydrophilic organic carbon (Hy) and hydrophobic neutral organic carbon (HON) concentrations in aqueous samples . 713 Expression of results . 814 Test report . 815 Performance characteristics 8Annex A (informative) Schematic representation of the fractionation procedure 9Annex B (
20、informative) Validation of procedure 11Annex C (informative) Conditions regarding centrifugation .16Bibliography .19BS EN ISO 12782-5:2012ISO 12782-5:2012(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). Th
21、e work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-gov
22、ernmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.Th
23、e main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote
24、.Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights.ISO 12782-5 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 7, Soil and
25、 site assessment.ISO 12782 consists of the following parts, under the general title Soil quality Parameters for geochemical modelling of leaching and speciation of constituents in soils and materials: Part 1: Extraction of amorphous iron oxides and hydroxides with ascorbic acid Part 2: Extraction of
26、 crystalline iron oxides and hydroxides with dithionite Part 3: Extraction of aluminium oxides and hydroxides with ammonium oxalate/oxalic acid Part 4: Extraction of humic substances from solid samples Part 5: Extraction of humic substances from aqueous samplesiv ISO 2012 All rights reservedBS EN IS
27、O 12782-5:2012ISO 12782-5:2012(E)IntroductionIn addition to leaching procedures for subsequent chemical and ecotoxicological testing of soil and other materials including waste, predictive models are becoming indispensable tools in the environmental risk assessment of these materials. Models are par
28、ticularly required when the results of laboratory leaching tests are to be translated to specific scenarios in the field, with regard to assessing the risks of both contaminant migration and bioavailability.In the past few years, geochemical models have been shown to be valuable tools to be combined
29、 with the data obtained from characterization leaching standards, such as pH-dependence and percolation tests. These models have the advantage of being based on fundamental thermodynamic parameters that have a general validity. In order to enable extrapolation of laboratory leaching data to the mobi
30、lity and/or bioavailability of a constituent in a specific field scenario, these models require additional input parameters for specific soil properties (see Figure 1).Key1 experiment2 geochemical speciation modelling3 available metal concentration4 dissolved humic substances5 reactive (solid) surfa
31、ces6 database with stability constants7 computer program8 assumptionsFigure 1 Relationships between experimental data, as obtained from laboratory leaching/extraction tests, and geochemical modelling of the speciation of a heavy metal in the environment (modified after M. Gfeller V2is the added volu
32、me of hydrochloric acid for precipitation of HA, in millilitres (ml);mDAX,iis the wet mass of DAX-8 applied for the adsorption of FA or used in the blank experiment, in grams (g) (see the last paragraph of this subclause);wm,DAXis the moisture content of the cleaned DAX-8, as a percentage (%);V4,iis
33、 the sample volume taken into account for the DAX-8 adsorption experiment, in millilitres (ml), after removal of HA, or the amount of 0,1 mol/l hydrochloric acid used in the blank experiment (see the last paragraph of this subclause). i = Lfor aqueous samples and i = BLin the blank experiments;DOCBL
34、1is the DOC concentration in the 0,1 mol/l hydrochloric acid solution used in the blank experiment (mg C/l); when DOCBL10.HADOC VVVV DOC f=()HAFAHyHON5113 11000(4)Concentration of Hy in solution, in milligrams of carbon per litre (mg C/l):Hy DOCfBl=Hy 2,LDAX(5)Concentration of FA + HON in solution,
35、in milligrams of carbon per litre (mg C/l):FA HON DOC fHy+=()FAHyHON1(6)Concentration of DOCFAafter correction of blank DAX-8 contribution, in milligrams of carbon per litre (mg C/l).Only apply if DOCFA,measured,i DOCBL,DAX 0, otherwise 0 is used.DOC DOC DOCFA,i FA,measured,iBL,DAX= (7)Concentration
36、 of FA in solution, in milligrams of carbon per litre (mg C/l):FADOC VV= FA,i 11,ii144,L(8)Concentration of HON in solution, in milligrams of carbon per litre (mg C/l):HON FA HONFA=+ (9)whereDOCHAis the measured DOC concentration of HA, in milligrams of carbon per litre (mg C/l);V5is the added volum
37、e of potassium hydroxide to dissolve the HA fraction, in millilitres (ml);V3is the volume of supernatant after acid precipitation and centrifugation, in millilitres (ml);V11,iis the added volume(s) of potassium hydroxide to dissolve FA from DAX-8 in aqueous samples; volumes are registered separately
38、 (i = 1 to 4);DOCFAHyHONis the measured DOC concentration of the sample after removal of HA, in milligrams of carbon per litre (mg C/l);DOCHyis the measured DOC concentration of the sample after equilibration with DAX-8, in milligrams of carbon per litre (mg C/l);DOCFA,measured,iis the DOC concentra
39、tion(s) in 0,1 mol/l potassium hydroxide after dissolution of FA from DAX-8 in aqueous samples, in milligrams of carbon per litre (mg C/l). DOC concentrations are registered separately (i = 1 to 4). ISO 2012 All rights reserved 7BS EN ISO 12782-5:2012ISO 12782-5:2012(E)13 Expression of resultsReport
40、 the concentration of HA, FA, Hy and HON in the sample, in milligrams of carbon per litre (mg C/l).14 Test reportThe test report shall include at least the following details:a) a reference to this part of ISO 12782;b) any information necessary for the complete identification of the sample;c) a refer
41、ence to the method used for the analytical determination, i.e. ISO 8245;d) the result of the determination;e) any details that are optional or deviations from the specifications of this part of ISO 12782, and any effects which may have affected the results.15 Performance characteristicsThe performan
42、ce characteristics of the method are described in Reference 15.8 ISO 2012 All rights reservedBS EN ISO 12782-5:2012ISO 12782-5:2012(E)Annex A (informative) Schematic representation of the fractionation procedure ISO 2012 All rights reserved 9BS EN ISO 12782-5:2012ISO 12782-5:2012(E)Key1 centrifugati
43、on2 filtration3 starting point for solid samples (see ISO 12782-4)4 starting point for liquid samples5 HA dissolution 0,1 M KOH6 TOC analysis7 DAX-8 addition, 1 h equilibration8 FA dissolution 0,1 M KOH, 1 h9 5 min settlingFigure A.1 Schematic representation of the fractionation procedure10 ISO 2012
44、 All rights reservedBS EN ISO 12782-5:2012ISO 12782-5:2012(E)Annex B (informative) Validation of procedureB.1 GeneralThe validation of the procedure specified in this part of ISO 12782 is also described in Reference 15. Several choices made in the development of the procedure are described in this a
45、nnex.B.2 Notes on the use of cleaned DAX-8The average moisture content (wm,DAX) of the cleaned moist resin was (60,3 3,4) % (n = 5). Small changes in moisture content have a limited effect on the final results, so this average value was used to correct the measured FA and Hy concentrations for the r
46、esins water content.After severe cleaning of DAX-8, a blank DOC concentration of about 2 mg C/l was found in the procedure. The molecular size of the residual DOC in cleaned DAX-8 was 100 u (atomic mass units), based on high-performance size-exclusion chromatography. Therefore, it is assumed that th
47、e residual DOC originates from resin bleeding rather than from residual FA.B.3 Preliminary investigations of DAX-8 and XAD-8 performanceThe adsorption of FA on XAD-8 and DAX-8 was studied at different resin additions and the adsorption time was measured. Moreover, the reversibility of the adsorption
48、 process was measured because FA are generally identified on the basis of their adsorption and subsequent desorption from XAD-812161718. The results of these preliminary investigations are given in B.2 and this subclause. It should be noted that the DAX-8 resin tends to adsorb slightly greater amoun
49、ts (up to 5 %) of FA as compared to XAD-8. These results are consistent with Reference 19. These studies concluded that the XAD-8 and DAX-8 resins isolate mixtures of components with generally similar structural compositions, although the content of aliphatics within the extracted HS is slightly greater for DAX-8. It should be noted thatthe results in Reference 19 were based on mixtures of HA and FA, whereas this annex only focuses on the equivalence for FA sorption and desorption. It is concluded
