1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 12782-3:2012Soil quality Parametersfor geochemical modellingof leaching and speciationof constituents in soils andmaterialsPart 3: Extraction of aluminium oxides andhyd
2、roxides with ammonium oxalate/oxalicacidBS EN ISO 12782-3:2012 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO12782-3:2012.The UK participation in its preparation was entrusted to TechnicalCommittee EH/4, Soil quality.A list of organizations represented on t
3、his committee 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 66913 2ICS 1
4、3.080.05Compliance 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 EUROPIS
5、CHE NORM EN ISO 12782-3 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 3: Extraction of aluminium oxides and hydroxides with ammonium oxalate/oxalic acid (ISO 12782-3:2012) Qualit du
6、 sol - Paramtres pour la modlisation gochimique de la lixiviation et de la spciation des constituants des sols et des matriaux - Partie 3: Extraction des oxydes et hydroxydes daluminium lacide oxalique et loxalate dammonium (ISO 12782-3:2012) Bodenbeschaffenheit - Parameter zur geochemischen Modelli
7、erung der Elution und Speziation von Bestandteilen in Bden und Materialien - Teil 3: Extraktion von Aluminiumoxiden und -hydroxiden mittels Ammoniumoxalat/Oxalsure (ISO 12782-3:2012) This European Standard was approved by CEN on 31 May 2012. CEN members are bound to comply with the CEN/CENELEC Inter
8、nal 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
9、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 ver
10、sions. CEN members 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, S
11、lovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION 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 worldwid
12、e for CEN national Members. Ref. No. EN ISO 12782-3:2012: EBS EN ISO 12782-3:2012EN ISO 12782-3:2012 (E) 3 Foreword This document (EN ISO 12782-3:2012) has been prepared by Technical Committee ISO/TC 190 “Soil quality“ in collaboration with Technical Committee CEN/TC 345 “Characterization of soils”
13、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 December 2012, and conflicting national standards shall be withdrawn at the latest by December 2012. Attent
14、ion 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. According to the CEN/CENELEC Internal Regulations, the national standards organisations of t
15、he following countries are bound to implement this 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, Romani
16、a, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 12782-3:2012 has been approved by CEN as a EN ISO 12782-3:2012 without any modification. BS EN ISO 12782-3:2012ISO 12782-3:2012(E) ISO 2012 All rights reserved iiiContents PageForewor
17、d ivIntroduction v1 Scope 12 Normative references . 13 Terms and definitions . 14 Principle . 25 Apparatus 26 Reagents 37 Sample pretreatment 37.1 Sample size . 37.2 Particle size reduction . 47.3 Determination of the water content 58 Procedure 58.1 Preparation of the extraction solution . 58.2 Extr
18、action 58.3 Analytical determination . 59 Calculation 510 Expression of results . 611 Test report . 6Annex A (informative) Conditions regarding centrifugation . 7Bibliography .10BS EN ISO 12782-3:2012ISO 12782-3:2012(E)ForewordISO (the International Organization for Standardization) is a worldwide f
19、ederation of national standards bodies (ISO member bodies). The 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 co
20、mmittee. International organizations, governmental and non-governmental, 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 accord
21、ance with the rules given in the ISO/IEC Directives, Part 2.The 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
22、 approval by at least 75 % of the member bodies casting a vote.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 12782-3 was prepared by Technical C
23、ommittee ISO/TC 190, Soil quality, Subcommittee SC 7, Soil and 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
24、oxides and hydroxides with ascorbic acid Part 2: Extraction of 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 substanc
25、es from aqueous samplesiv ISO 2012 All rights reservedBS EN ISO 12782-3:2012ISO 12782-3:2012(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 en
26、vironmental risk assessment of these materials. Models are particularly 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, geochemi
27、cal models have been shown to be valuable tools to be combined 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 t
28、o enable extrapolation of laboratory leaching data to the mobility 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 con
29、centration4 dissolved humic substances5 reactive (solid) surfaces6 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
30、the environment (modified after M. Gfeller this portion of material, resulting from the laboratory sample by means of an appropriate method of sample pre-treatment, and having the size (volume/mass) necessary for the desired testing or analysisNOTE Adapted from ISO 11074:2005.3.4test portionanalytic
31、al portionquantity of material, of proper size, for measurement of the concentration or other property of interest, removed from the test sampleNOTE 1 The test portion may be taken from the primary sample or from the laboratory sample directly if no preparation of sample is required (e.g. with liqui
32、ds), but usually it is taken from the prepared test sample.NOTE 2 A unit or increment of proper homogeneity, size, and fineness, needing no further preparation, may be a test portion.ISO 11074:20053.5materialexcavated soil, dredged material, manufactured soil, treated soil and fill material and othe
33、r relevant materials, including soil amendments and waste materials4 PrincipleThe extraction principle is based mainly on the complexing affinity of acid oxalate to extract aluminium from short-range order materials5. The extracted concentrations of aluminium can be measured using inductively couple
34、d plasma/atomic emission spectroscopy (ICP-AES).5 ApparatusThe following apparatus shall be used. All materials that come into contact with the sample (material or reagents) should not contaminate the compounds to be determined or adsorb the compounds of interest.2 ISO 2012 All rights reservedBS EN
35、ISO 12782-3:2012ISO 12782-3:2012(E)5.1 Centrifuge tubes, e.g. polycarbonate, of appropriate size, rinsed in accordance with ISO 5667-3.5.2 Centrifuge, preferably at 3 000g. For other appropriate conditions, see Annex A.5.3 End-over-end shaking machine, operated in the dark at a constant temperature
36、of 20 C.NOTE Other shaking methods can be used provided they can be shown to provide equivalent results 5.4 Filter holders for syringes, 0,2 m, cellulose acetate, diameter 30 mm, cleaned with at least 10 ml of distilled water before use.5.5 Usual laboratory glass or plastic ware, rinsed in accordanc
37、e with ISO 5667-3.5.6 Plastic syringe, 50 ml, rinsed in accordance with ISO 5667-3.5.7 Balance, with an accuracy of at least 1 mg.5.8 Sieving equipment, with a nominal screen size of 2 mm or 4 mm.NOTE Due to sieving, contamination of the sample may occur to an extent which affects the leaching of so
38、me constituents of concern, e.g. cobalt and tungsten from tungsten carbide equipment or chromium, nickel and molybdenum from stainless-steel equipment.5.9 Sample splitter, for sub-sampling of laboratory samples (optional).5.10 Crushing equipment: jaw crusher or cutting device.NOTE Due to crushing, c
39、ontamination of the sample may occur to an extent which affects the leaching of some constituents of concern, e.g. cobalt and tungsten from tungsten carbide equipment or chromium, nickel and molybdenum from stainless-steel equipment.5.11 pH-meter, with a measurement accuracy of at least 0,05 pH unit
40、s.6 ReagentsThe reagents used shall be of analytical grade and the water used shall comply with grade 3 in accordance with ISO 3696.6.1 Water: use distilled and demineralized water with a specific conductivity of at most 0,2 mS/cm at 25 C and a pH 5,6.6.2 Di-ammonium oxalate monohydrate, M(NH4)2C2O4
41、 H2O = 142,11 g/mol.6.3 Oxalic acid dihydrate, M(C2H2O4 2H2O) = 126,07 g/mol.6.4 Nitric acid, c(HNO3) = 0,1 mol/l.7 Sample pretreatment7.1 Sample sizeSampling shall be performed in accordance with the guidelines for preparing a sampling plan for soil materials, as specified in ISO 10381-1 to ISO 103
42、81-6 and for waste in accordance with EN 14899, in order to obtain ISO 2012 All rights reserved 3BS EN ISO 12782-3:2012ISO 12782-3:2012(E)representative laboratory samples. Obtain a representative laboratory sample of at least 200 g (dry matter) for soil and soil materials and 2 kg (dry matter) for
43、waste material. Follow instructions for sample pretreatment: for soil and soil materials according to ISO 11464; for waste according to CEN/TR 15310-3 and EN 15002.Use a sample splitter (5.9) or apply coning and quartering to split the sample.NOTE The required size of the laboratory sample is depend
44、ent on the particle size distribution of the soil or material to be analysed (see ISO 11277). The specified sample size is generally adequate. In specific cases, a smaller sample size can be accepted for instance if, for specific reasons, less material is available provided that the test can be carr
45、ied out as specified in 7.2 and 7.3.Any deviation(s) to accommodate sample size or volume requirements shall be recorded in the test report.7.2 Particle size reduction7.2.1 GeneralThe tests shall be carried out preferably on material as received.7.2.2 Particle size reduction of soil and soil materia
46、lFor soil and soil material, the test portion to be prepared shall have a grain size 2 mm. If oversized material is not of natural origin and exceeds 5 % (mass fraction), the entire oversized fraction shall be separated by sieving (see 5.8) and crushed using suitable crushing equipment (5.10). On no
47、 account shall the material be finely ground. Oversized material of natural origin (e.g. stones, pebbles, twigs) in the sample shall be separated and discarded. Irrespective of any necessary size reduction, the separate fractions, with the exception of non-crushable and discarded material, shall be
48、mixed to constitute the test sample. If the laboratory sample cannot be crushed or sieved because of its water content, it is permitted, in this case only, to reduce the water content until the laboratory sample can be sieved. The drying temperature shall not exceed 25 C.7.2.3 Particle size reductio
49、n of wasteFor waste, the test shall be carried out on material with a grain size of at least 95 % (mass fraction) 4 mm. Therefore, the laboratory sample shall be sieved (see 5.8). If oversized material exceeds 5 % (mass fraction) the entire oversized fraction shall be crushed using crushing equipment (5.10). On no account shall the material be finely ground. Non-crushable material (e.g. metallic parts such as nuts, bolts, scrap) in the sample shall be separated and the mass and nature of the material shall be recorded.