1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 16166:2012Sludge, treated biowaste and soil Determination of adsorbable organically bound halogens (AOX)BS EN 16166:2012 BRITISH STANDARDNational forewordThis British Stand
2、ard is the UK implementation of EN 16166:2012. The UK participation in its preparation was entrusted to T e c h n i c a l Committee H/-/4, Environmental testing programmes.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purp
3、ort to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2012Published by BSI Standards Limited 2012ISBN 978 0 580 56586 1 ICS 13.030.01; 13.080.10 Compliance with a British Standard cannot confer immunity from le
4、gal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 September 2012.Amendments issued since publicationDate T e x t a f f e c t e dBS EN 16166:2012EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16166 August 2012 ICS 13.030
5、.01; 13.080.10 English Version Sludge, treated biowaste and soil - Determination of adsorbable organically bound halogens (AOX) Boues, biodchets traits et sols - Dtermination des composs organiques halogns adsorbables (AOX) Schlamm, behandelter Bioabfall und Boden - Bestimmung von adsorbierbaren org
6、anisch gebundenen Halogenen (AOX) This European Standard was approved by CEN on 24 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 a national standard without any alteration. Up-to-date
7、 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 u
8、nder 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, Forme
9、r 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 COMIT E
10、UROPEN 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 16166:2012: EBS EN 16166:2012EN 16166:2012 (E) 2 Contents Page Forewor
11、d 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Principle 55 Interferences 56 Reagents .67 Apparatus .77.1 Apparatus for combustion and detection .77.2 Equipment for adsorption .77.3 Equipment for sample preparation 78 Sample storage and pretreatment78.1 Sample storage
12、 78.2 Sample pretreatment .89 Procedure .89.1 General 89.2 Adsorption and inorganic halide removal .89.3 Combustion 89.4 Initial calibration 99.4.1 General 99.4.2 Calibration of the entire system .99.4.3 Check of argentometric measuring device 109.5 Recalibration . 109.6 Blank determination . 1010 C
13、alculation . 1110.1 Method of calculation . 1110.1.1 Entire system calibration (according to 9.4.2) . 1110.1.2 Direct argentometric measurement device calibration (according to 9.4.3) 1110.2 Expression of results . 1211 Precision 1212 Test report . 12Annex A (informative) Repeatability and reproduci
14、bility data . 13A.1 Materials used in the interlaboratory comparison study . 13A.2 Interlaboratory comparison results 14Annex B (informative) Storage of activated carbon 15Annex C (informative) Schematic diagram of an AOX apparatus . 16Bibliography . 17BS EN 16166:2012EN 16166:2012 (E) 3 Foreword Th
15、is document (EN 16166:2012) has been prepared by Technical Committee CEN/TC 400 “Project Committee - Horizontal standards in the fields of sludge, biowaste and soil”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publicati
16、on of an identical text or by endorsement, at the latest by February 2013, and conflicting national standards shall be withdrawn at the latest by February 2013. 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 sh
17、all not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. The preparation of this document by CEN is based on a mandate by the European Commission (Mandat
18、e M/330), which assigned the development of standards on sampling and analytical methods for hygienic and biological parameters as well as inorganic and organic determinants, aiming to make these standards applicable to sludge, treated biowaste and soil as far as this is technically feasible. Accord
19、ing 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, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany,
20、Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16166:2012EN 16166:2012 (E) 4 Introduction This document is the result of a desk study
21、“Horizontal European standard for determination of AOX in sewage sludge and comparable matrices“ in the project “Horizontal“ and aims at evaluating the latest developments in assessing AOX in sludge, soil, treated biowaste and neighbouring fields. After an evaluation study, in which the ruggedness o
22、f the method was studied, a European wide validation of the draft standard has taken place. The results of the desk studies as well as the evaluation and validation studies have been subject to discussions with all parties involved in the evaluation. This European Standard is applicable and validate
23、d for several types of matrices as indicated in Table 1 (see also Annex A for the results of the validation). Table 1 Matrices for which this European Standard is applicable and validated Matrix Materials used for validation Sludge Municipal sludge Compost Fresh compost Compost Soil Sludge amended s
24、oil Agricultural soil WARNING Persons using this European Standard should be familiar with usual laboratory practice. This European Standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety a
25、nd health practices and to ensure compliance with any national regulatory conditions. IMPORTANT It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. BS EN 16166:2012EN 16166:2012 (E) 5 1 Scope This European Standard specifies a
26、n empirical method for the direct determination of organically bound chlorine, bromine and iodine (but not fluorine) adsorbed and occluded to the sample matrix. Non-volatile organically bound halogens adsorbable on activated carbon present in the aqueous phase of the sample prior to drying or adsorb
27、ed to sample surface are included in the determination. This European Standard is intended for analysis of sludge, treated biowaste or soil in concentrations ranging from 5 mg/kg dry matter to approximately 6 g/kg dry matter. The exact concentration range covered depends on the instrument used for d
28、etermination. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (inclu
29、ding any amendments) applies. EN 16179, Sludge, treated biowaste and soil Guidance for sample pretreatment EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) EN ISO 5667-15, Water quality Sampling Part 15: Guidance on the preservation and handling of sludge an
30、d sediment samples (ISO 5667-15) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 adsorbable organically bound halogens AOX equivalent amount of chlorine, bromine, and iodine contained in organic compounds, expressed as chloride when determine
31、d according to this European Standard 4 Principle Activated carbon is added to a dried, homogenised solid sample. Inorganic halides are eluted and at the same time water soluble organic compounds are adsorbed onto the activated carbon by shaking with acidified nitrate solution. The loaded carbon/sam
32、ple mixture is combusted in an oxygen stream. The hydrogen halides produced are absorbed followed by determination of the halide ions by an argentometric titration, such as microcoulometry. The result is expressed as the mass concentration of chloride. 5 Interferences Sparingly soluble or occluded i
33、norganic halides are included in the determination and may, if present, give a significant positive bias. Adequate washing is essential to remove inorganic interference. NOTE Halogenated substances that volatilise at 105 C are lost. Organic bromine and iodine compounds may, during combustion, lead t
34、o the formation of elemental bromine or iodine respectively or to the formation of halogen oxides. The determination of these AOX fractions may be incomplete, thus leading to negative bias. BS EN 16166:2012EN 16166:2012 (E) 6 6 Reagents Use only reagents of recognised analytical grade and water grad
35、e 1 in accordance with EN ISO 3696. The AOX contribution from water, reagents and gases should be significantly lower than the lowest AOX content to be determined. The overall AOX content of water, chemicals, and gases shall be checked by measuring the total blank (see 9.6). 6.1 Activated carbon, gr
36、ain size approximately 10 m to 50 m. For the storage of activated carbon, see Annex B. The blank value of the washed activated carbon shall be less than 15 g of chloride equivalent per gram of activated carbon. 6.2 Nitric acid, HNO3, = 1,4 g/ml, 65 % (mass fraction) solution. 6.3 Hydrochloric acid,
37、c(HCl) = 0,100 mol/l. The molarity shall be precisely known, since the acid is used for checking the micro-titration (see 9.4.3). 6.4 Sulfuric acid, H2SO4, = 1,84 g/ml. 6.5 Gases for combustion, e.g. oxygen (O2), or a mixture of oxygen and an inert gas. 6.6 Sodium nitrate, NaNO3, for the preparation
38、 of stock solution. 6.7 Nitrate stock solution, acidified, c(NaNO3) = 0,2 mol/l. Dissolve 17 g of sodium nitrate (6.6) in water in a 1 000 ml volumetric flask, add 15 ml of nitric acid (6.2), and make up to volume with water. 6.8 Nitrate washing solution, c(NaNO3) = 0,01 mol/l. Pipette 50 ml of the
39、nitrate stock solution (6.7) in a 1 000 ml volumetric flask, and make up to volume with water. 6.9 Methanol, CH3OH. 6.10 4-Chlorophenol stock solution, C6H5ClO, equivalent to AOX = 2,0 g/l. Dissolve 0,725 g of 4-chlorophenol in methanol (6.9) in a 100 ml calibrated flask and make up to volume with m
40、ethanol (6.9). 6.11 4-Chlorophenol working solutions, equivalent to AOX = 0,1 g/l and 0,5 g/l AOX, respectively. Pipette 5 ml and 25 ml of 4-chlorophenol stock solution (6.10) into two separate 100 ml calibrated flasks, and make up to volume with methanol (6.9). The stock solution (6.10) may be stor
41、ed for at least one month and the working solutions (6.11) for one week in a refrigerator in glass bottles. BS EN 16166:2012EN 16166:2012 (E) 7 7 Apparatus 7.1 Apparatus for combustion and detection 7.1.1 Combustion apparatus, a furnace capable of being heated to at least 950 C, equipped with a quar
42、tz tube approximately 30 cm long with an internal diameter of between 2 cm and 4 cm (see Annex C). NOTE It is essential that the combustion temperature is sufficient. Temperatures below 950 C are likely to result in poor recovery and increased variability. 7.1.2 Quartz sample boat, to fit in the qua
43、rtz tube. 7.1.3 Argentometric measuring device for determining halide concentrations, e.g. a microcoulometer, capable of determining at least 0,03 mol/l chloride with a repeatability variation coefficient of less than 10 %, or an equivalent device to determine chloride ions. 7.1.4 Absorber, filled w
44、ith sulfuric acid (6.4), to dry the gas stream and designed so that the acid does not backflush into the furnace. 7.1.5 Syringe, to pipette volumes of 1 l to 10 l of hydrochloric acid (6.3) or 4-chlorophenol solutions (6.10 and 6.11). 7.2 Equipment for adsorption 7.2.1 Filtration apparatus, e.g. wit
45、h a funnel capacity of 0,15 l and a filter diameter of 25 mm. 7.2.2 Low-halide polycarbonate membrane filter, to fit the filtration apparatus (7.2.1), with a pore size of 0,45 m, or any equivalent filtration material, such as a dedicated quartz filter for AOX determination. 7.2.3 Conical flask (Erle
46、nmeyer flask) of 25 ml capacity with ground glass stopper or 12 ml to 20 ml screw cap vial with polytetrafluoroethene (PTFE) lined cap. 7.2.4 Mechanical shaker. 7.3 Equipment for sample preparation 7.3.1 Porcelain evaporating dish. 7.3.2 Oven with forced ventilation or natural ventilation through ad
47、justable vents adjustable to (105 5) C. 7.3.3 Desiccator, provided with a suitable desiccant. 7.3.4 Analytical mill or porcelain mortar. 7.3.5 Precision balance. 8 Sample storage and pretreatment 8.1 Sample storage For the sampling and storage of sludge samples refer to EN ISO 5667-15. Samples shall
48、 be stored in suitable containers with an appropriate closure material such as PTFE. Samples to be frozen may be stored in aluminium containers pre-cleaned by heating to 450 C for minimum 4 h or by rinsing with a non-chlorinated solvent. BS EN 16166:2012EN 16166:2012 (E) 8 Samples shall be kept cold
49、 at a temperature 8 C and in the dark. The sample pretreatment should take place within 24 h of sampling. Alternatively, samples may be frozen (18 C) directly after sampling and kept frozen for a maximum of one month before sample pretreatment. 8.2 Sample pretreatment Pretreat the samples according to EN 16179, if not otherwise specified. Cool the dried test sample in a desiccator, comminute and homogenize in an analytical mill or porcelain mortar (7.3.4) to a part
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