EN 16179-2012 en Sludge treated biowaste and soil - Guidance for sample pretreatment《污泥 处理的生物废弃物和土壤 试样预处理指南》.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 16179:2012Sludge, treated biowaste andsoil Guidance for samplepretreatmentBS EN 16179:2012 BRITISH STANDARDNational forewordThis British Standard is the UK implementation o

2、f EN 16179:2012. The UK participation in its preparation was entrusted to TechnicalCommittee 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 purport to include all the necessary provis

3、ions of a contract. Users are responsible for its correct application. The British Standards Institution 2012. Published by BSI Standards Limited 2012ISBN 978 0 580 72670 5 ICS 13.030.01; 13.080.05 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard

4、 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 16179:2012EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16179 August 2012 ICS 13.080.05; 13.030.01 English Version Sludge

5、, treated biowaste and soil - Guidance for sample pretreatment Boues, bio-dchets traits et sols - Lignes directrices pour le prtraitement des chantillons Schlamm, behandelter Bioabfall und Boden - Anleitung zur Probenvorbehandlung This European Standard was approved by CEN on 23 June 2012. CEN membe

6、rs 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 national standards may be obtained on applicatio

7、n 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 language and notified to the CEN-CENELEC Manageme

8、nt 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, Hungary, Iceland, Ireland, Italy, Latvia, L

9、ithuania, 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 Management Centre: Avenue Marnix 17, B-1000 Bru

10、ssels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16179:2012: EBS EN 16179:2012EN 16179:2012 (E) 2 Contents Page Foreword 4Introduction .51 Scope 62 Normative references 63 Terms and definitions .74 Safety remarks .95 Prin

11、ciple 95.1 General 95.2 Preservation and storage of samples . 135.3 Pretreatment in the field . 135.4 Pretreatment in the laboratory for determination of inorganic and physico-chemical parameters . 195.5 Pretreatment in the laboratory for determination of organic volatile compounds 195.6 Pretreatmen

12、t in the laboratory for determination of moderately volatile organic compounds 196 Reagents 207 Apparatus 207.1 General . 208 Sampling and pretreatment procedures in the field (from field sample to laboratory sample) 228.1 General . 228.2 Selection of workplace . 238.3 Estimation of minimum subsampl

13、e mass 238.4 Pretreatment methods 258.4.1 Procedure for macro aggregate reduction by hand 258.4.2 Subsampling methods . 258.4.3 Liquid sludge handling 269 Storing and preservation . 269.1 General . 269.2 Appropriate sample container . 269.3 Preservation 2710 Pretreatment procedures in the laboratory

14、 (from laboratory sample to test sample) . 2710.1 General . 2710.2 Pretreatment for determination of chemical and physico-chemical parameters . 2710.2.1 General . 2710.2.2 Laboratory sample description . 2810.2.3 Drying of solid samples . 2810.2.4 Removal of extraneous materials and crushing 2910.2.

15、5 Subsampling . 2910.2.6 Milling . 3010.2.7 Liquid sludge samples . 3110.3 Pretreatment for determination of organic compounds . 3210.3.1 General . 3210.3.2 Volatile compounds 3210.3.3 Moderately volatile organic compounds Grinding necessary 3310.3.4 Moderately volatile organic compounds Grinding no

16、t possible or not necessary 35BS EN 16179:2012EN 16179:2012 (E) 3 11 Test report 36Annex A (informative) Subsampling methods . 37A.1 Long pile and alternate shovel method . 37A.2 Coning and quartering 38A.3 Riffling 39A.4 Application of Tyler divider 40A.5 Application of mechanised turntable (rotati

17、ng divider) 40Annex B (informative) Information concerning vapour pressure, boiling and melting points of volatile organic compounds . 42Bibliography 45BS EN 16179:2012EN 16179:2012 (E) 4 Foreword This document (EN 16179:2012) has been prepared by Technical Committee CEN/TC 400 “Project Committee -

18、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 2013, and conflicting national s

19、tandards 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 rights. This document has been pre

20、pared 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 analytical methods for hygienic

21、 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 organizations of the following co

22、untries 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, Malta, Netherlands, Norway,

23、Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16179:2012EN 16179:2012 (E) 5 Introduction This document has been developed upon existing International Standards for the pretreatment of soils of specified particle fractions. Historicall

24、y this has been the case for analysing organic compounds after pretreatment according to e.g. ISO 14507. Standards describing pretreatment for chemical and physico-chemical parameters, e.g. ISO 11464, historically have divided the samples into fractions 2 mm where the fraction 2 mm and the extraneou

25、s material removed from the sample the results also can be calculated referring to the mass of the whole sample. The report shall clearly state to which fraction the results refer. BS EN 16179:2012EN 16179:2012 (E) 10 Beside the requirements given in this European Standard, the subsequently applied

26、analytical standards shall be regarded for particular requirements to be observed. The determination of some parameters requires sample pretreatment soon after sampling as specified in the respective analytical methods. If several parameters are being investigated, the sample pretreatment shall be d

27、esigned so that the parameters of major importance are determining the pretreatment. If this is not possible, e.g. the required precision for each parameter can not be achieved, separate pretreatment shall be set up for each group of parameters. Whenever volatile compounds are to be determined, the

28、process of sample pretreatment can result in a substantial loss of these compounds. Sample pretreatment shall be omitted in these cases by taking specific samples for the determination of volatile components. These samples shall be pretreated in accordance with the appropriate analytical standard an

29、d analysed as soon as possible after sampling. When preparing composite samples the analytical requirements shall be considered. For example, composite samples are not appropriate if volatile compounds are to be determined. Figure 1, Figure 2 and Figure 3 show flow charts for: pretreatment for inorg

30、anic and physico-chemical parameters in solid sludge, treated biowaste and soil (Figure 1), pretreatment for organic parameters in solid sludge, treated biowaste and soil (Figure 2), pretreatment for inorganic, physico-chemical and organic parameters in liquid sludge (Figure 3). Aside from the param

31、eter to be determined, the procedure to be applied also depends on the required minimum mass of the sample to be used in relation to the maximum particle size D95of the sample. For this the relationship described in ISO 10381-8 is used (see Table 2 in 8.3). Grinding of the sample depends on the mass

32、 of the subsample being taken. Table 1 gives the requirements for a wide group of parameters. For some parameters the requirements stated in 8.3 need not to be followed exactly as the homogeneity of the samples is enough to obtain adequate results for those parameters. EXAMPLES dry matter, total org

33、anic compounds (TOC), pH, EC. BS EN 16179:2012EN 16179:2012 (E) 11 Table 1 Required maximum particle size (D95) for the determination of several parameters.(1 of 2) Parameter MatrixaTest portion on dry matter basis D95required, remarksProcedurebAmmonium- and nitrate-nitrogen Solid 15 g No D95require

34、ments, sample as received, no heating and no freeze drying allowed Fig. 1, Route A Sludge No D95requirements, direct measurement in the liquid phase Fig. 3 Anions (Cl , F ,Br , 34PO , 24SO ) Solid 15 g No D95requirements, sample as receive Fig. 1, Route A Sludge No D95requirements, direct measuremen

35、t in the liquid phase Fig. 3 Adsorbable organic halogens (AOX) All 5 mg to 100 mg 250 m Fig. 3 Cyanide Solid 10 g to 40 g No D95requirements, sample as received, no heating allowed Fig. 1, Route A Sludge No D95requirements, direct measurement in the liquid phase Fig. 3 Dry matter fraction Solid 30 g

36、 to 50 g No D95requirements Fig. 1, Route A Solid, air dried 10 g to 15 g No D95requirements Sludge 0,5 g No D95requirements Fig. 3 Electrical conductivity Solid 20 g No D95requirements, drying (optional) Fig. 1, Route C Sludge No grinding, direct measurement in liquid phase Loss on ignition (LOI) a

37、t 550 C All 2 g No D95requirements, dried sample for determining dry matter is taken Metals: see trace elements Organic matter: see LOI Particle size distribution No pretreatment allowed pH Solid 5 ml No D95requirements, drying (optional) Fig. 1, Route A Sludge No D95requirements, direct measurement

38、 in liquid phase Fig. 3 BS EN 16179:2012BS EN 16179:2012EN 16179:2012 (E) 12 Table 1 (2 of 2) Parameter MatrixaTest portion on dry matter basis D95required, remarks ProcedurebPhosphorus (total): see trace elements Total organic carbon (TOC) All 2 g 2 mm Total Kjeldahl nitrogen Solid 2 g 2 mm Sludge

39、0,1 g to 1 g No grinding, sample as received Fig. 3 Total nitrogen (Dumas), All 2 g 2 mm Trace elements Extraction with aqua regia or nitric acid Solid 2 g 2 mm Sludge No D95requirements, homogenisation with high speed mixer or sonification, then direct digestion Fig. 3 Organic compounds, volatile (

40、e. g. volatile aromatic and halogenated compounds) All See analytical standard No D95requirements and no homogenisation allowed Fig. 2 Fig. 3 Organic compounds, moderately volatile Solid 10 g excluding drying agents 2 mm Sludge See analytical standard No D95requirements, sample as received Fig. 3 aM

41、atrix: “Solid” = solid sludge, treated biowaste, soil. “Sludge“ = liquid sludge bProcedure: figure number and option in that figure BS EN 16179:2012BS EN 16179:2012EN 16179:2012 (E) 13 5.2 Preservation and storage of samples The samples shall be kept cool and processed as soon as possible; see ISO 1

42、8512 for preservation and storage of soil samples, EN ISO 5667-13 for guidance on sampling of sludge samples and EN ISO 5667-15 for preservation and storage of sludge samples. Treat biowaste samples the same as soil samples regarding storage. 5.3 Pretreatment in the field When possible, the sample p

43、retreatment should take place in the laboratory, as sample integrity can be best guaranteed under laboratory conditions. Subsampling by the methods given in 8.4.2 can be performed in the field as well as in the laboratory. In the field, sample pretreatment is restricted to the process of subsampling

44、 by sample division. Pretreatment is necessary if field samples are too large to be transported to the laboratory, or if the amount of material sampled is larger than the amount of material necessary for the test or analysis. When subsampling is necessary, the relation between the minimum mass of th

45、e subsamples and the maximum size of the particles (D95) in the original field sample shall be taken into account (see 8.3). Samples are divided into subsamples either mechanically or manually. Subsampling methods are described in 8.4.2. In some cases the soil is strongly aggregated. Such macro aggr

46、egates can be reduced by hand (see 8.4.1) otherwise they should be seen as individual “particles“. BS EN 16179:2012EN 16179:2012 (E) 14 Figure 1 Flow chart for the pretreatment of solid sludge, treated biowaste and soil for the determination of inorganic and physico-chemical parameters (1 of 2) BS E

47、N 16179:2012EN 16179:2012 (E) 15 Figure 1 Flow chart for the pretreatment of solid sludge, treated biowaste and soil for the determination of inorganic and physico-chemical parameters (2 of 2) BS EN 16179:2012EN 16179:2012 (E) 16 Figure 2 Flow chart for the pretreatment of solid sludge, treated biow

48、aste and soil for the determination of organic parameters (1 of 2) BS EN 16179:2012EN 16179:2012 (E) 17 Figure 2 Flow chart for the pretreatment of solid sludge, treated biowaste and soil for the determination of organic parameters (2 of 2) BS EN 16179:2012EN 16179:2012 (E) 18 Figure 3 Flowchart for

49、 the pretreatment of liquid sludge samples for the determination of inorganic, organic and physico-chemical parameters Sample division in the field shall be carried out only if a sheltered area is available (see 8.2). Soon after sampling, and up until pretreatment in the laboratory, the samples should be stored in such a way that the characteristics of the samples are preserved (e.g. cool and light protected, see Clause