1、November 2012 Translation by DIN-Sprachendienst.English price group 11No 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 13.080.10; 13.030.01!$E“1923427www.din.deDDIN EN 16166Sludge, treated biowaste and soil Determination of adsorbable organically bound halogens (AOX);English version EN 16166:2012,English translation of DIN EN 16166:2012-11Schlamm, behandelter Bioabfall und Boden Bestimmung von adsorbierbaren orga
3、nisch gebundenen Halogenen (AOX);Englische Fassung EN 16166:2012,Englische bersetzung von DIN EN 16166:2012-11Boues, bio-dchets traits et sols Dtermination des composs organiques halogns adsorbables (AOX);Version anglaise EN 16166:2012,Traduction anglaise de DIN EN 16166:2012-11www.beuth.deDocument
4、comprises 21 pagesIn case of doubt, the German-language original shall be considered authoritative.10.12 DIN EN 16166:2012-11 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 400 “Project Committee Horizontal standards in the fi
5、elds of sludge, biowaste and soil” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (WaterPractice Standards Committee), Working Committee NA 119-01-02 Abfall- und Bodenuntersuchung,119-01-02-02 AA Chemische und physikalische Ve
6、rfahren. NA The DIN Standard corresponding to the International Standard referred to in this document is as follows: ISO 5725-2 DIN ISO 5725-2 DIN EN 16166:2012-11 3 National Annex NA (informative) Bibliography DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part
7、 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN EN 16166:2012-11 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16166 August 2012 ICS 13.030.01; 13.080.10 English Version Sludge, treated biowast
8、e and soil Determination of adsorbable organically bound halogens (AOX) Boues, bio-dchets traits et sols Dtermination des composs organiques halogns adsorbables (AOX) Schlamm, behandelter Bioabfall und Boden Bestimmung von adsorbierbaren organisch gebundenen Halogenen (AOX) This European Standard wa
9、s 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 lists and bibliographical references concerning such natio
10、nal 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 under the responsibility of a CEN member into its own langua
11、ge 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece,
12、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 EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Mana
13、gement 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: E EN 16166:2012 (E) 2 Contents PageForeword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions
14、.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 78.2 Sample pretreatment .89 Procedure .89.1 General 89.2 Adsorption and i
15、norganic 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 Calculation . 1110.1 Method of calculation . 1110.1.1 Entire system calibrat
16、ion (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 reproducibility data . 13A.1 Materials used in the interlaboratory comparison study
17、. 13A.2 Interlaboratory comparison results 14Annex B (informative) Storage of activated carbon 15Annex C (informative) Schematic diagram of an AOX apparatus . 16Bibliography . 17DIN EN 16166:2012-11EN 16166:2012 (E) 3 Foreword This document (EN 16166:2012) has been prepared by Technical Committee CE
18、N/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 publication of an identical text or by endorsement, at the latest by February 20
19、13, 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 shall not be held responsible for identifying any or all such patent righ
20、ts. 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 (Mandate M/330), which assigned the development of standards on sampling and a
21、nalytical 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. According to the CEN/CENELEC Internal Regulations, the national standards org
22、anizations 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, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg
23、, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16166:2012-11EN 16166:2012 (E) 4 Introduction This document is the result of a desk study “Horizontal European standard for determination of AOX in sewage sl
24、udge 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 of the method was studied, a European wide validation of the draft s
25、tandard 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 validated for several types of matrices as indicated in Table 1 (see also A
26、nnex 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 soil Agricultural soil WARNING Persons using this European Standard
27、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 and health practices and to ensure compliance with any national regu
28、latory conditions. IMPORTANT It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. DIN EN 16166:2012-11EN 16166:2012 (E) 5 1 Scope This European Standard specifies an empirical method for the direct determination of organically
29、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 adsorbed to sample surface are included in the determination. This Eu
30、ropean 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 determination. 2 Normative references The following documents, i
31、n 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 (including any amendments) applies. EN 16179, Sludge, treated biowast
32、e 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 and sediment samples (ISO 5667-15) 3 Terms and definitions For th
33、e 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 determined according to this European Standard 4 Principle Activated car
34、bon 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/sample mixture is combusted in an oxygen stream. The hydrogen hali
35、des 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 inorganic halides are included in the determination and may, if
36、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 to the formation of elemental bromine or iodine respectively or
37、to the formation of halogen oxides. The determination of these AOX fractions may be incomplete, thus leading to negative bias. DIN EN 16166:2012-11EN 16166:2012 (E) 6 6 Reagents Use only reagents of recognised analytical grade and water grade 1 in accordance with EN ISO 3696. The AOX contribution fr
38、om 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, grain size approximately 10 m to 50 m. For the storage of act
39、ivated 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, c(HCl) = 0,100 mol/l. The molarity shall be precisely known
40、, 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 of stock solution. 6.7 Nitrate stock solution, acidified,
41、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 nitrate stock solution (6.7) in a 1 000 ml volumetric flask
42、, 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 methanol (6.9). 6.11 4-Chlorophenol working solutions, equiv
43、alent 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 stored for at least one month and the working solutions (6.11)
44、for one week in a refrigerator in glass bottles. DIN EN 16166:2012-11EN 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 quartz tube approximately 30 cm long with an internal diame
45、ter 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 quartz tube. 7.1.3 Argentometric measuring device for dete
46、rmining 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 with sulfuric acid (6.4), to dry the gas stream and desi
47、gned 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. with a funnel capacity of 0,15 l and a filter diameter of
48、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 (Erlenmeyer 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 pr
