1、November 2012 Translation by DIN-Sprachendienst.English price group 19No 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 13.080.05; 13.030.01!$QI“1924638www.din.deDDIN EN 16179Sludge, treated biowaste and soil Guidance for sample pretreatment;English version EN 16179:2012,English translation of DIN EN 16179:2012-11Schlamm, behandelter Bioabfall und Boden Anleitung zur Probenvorbehandlung;Englische Fassung EN 16179:
3、2012,Englische bersetzung von DIN EN 16179:2012-11Boues, bio-dchets traits et sols Lignes directrices pour le prtraitement des chantillons;Version anglaise EN 16179:2012,Traduction anglaise de DIN EN 16179:2012-11www.beuth.deDocument comprises 49 pagesIn case of doubt, the German-language original s
4、hall be considered authoritative.10.12 DIN EN 16179:2012-11 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 fields of sludge, biowaste and soil” (Secretariat: DIN, Germany). Th
5、e responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee), Working Committees NA 119-01-02 Abfall- und Bodenuntersuchung and NA 119-01-02-01 UA Probenahme. DIN EN 16179 was developed at European level over a number of years and in
6、its present version is essentially a consolidation of the two International Standards ISO 11464:2006 and ISO 14507:2004. In its comments rejecting the adoption of the European draft version of this standard, the German mirror committee formerly responsible for this work, NA 119-01-02-02 UA Chemische
7、 und physikalische Verfahren, had tried to incorporate into EN 16179 content and structural elements from DIN 19747:2009 “Investigation of solids Pretreatment, preparation and processing of samples for chemical, biological and physical investigations”, including elements particularly important for t
8、he biological investigation of solids. Most of the German comments were not taken into consideration. Therefore, the present version of DIN EN 16179:2012 does not reflect modern laboratory practice in terms of the pretreatment of samples; it also does not conform with the horizontal cross-matrix app
9、roach favoured in Germany, which is effectively standardized in DIN 19747:2009. According to the rules for standards work laid down in DIN 820-2, DIN EN 16179 only partially replaces DIN 19747:2009. However, the elements of DIN 19747:2009 which have not been replaced cannot be identified as longer,
10、contiguous text passages, but as individual passages and sentences, and as individual elements of figures and tables. It would therefore be very difficult to take those elements of DIN 19747:2009 which are not covered by DIN EN 16179 and present them in a residual standard. In laboratory practice, t
11、his would also mean that the same sample would have to be prepared on the basis of two different standards. On the other hand, DIN ISO 14507:2004 is fully replaced by the present standard. For the time being the method laid down in DIN 19747:2009 will have to be used in German laboratories because i
12、t is cited in various German regulations (e.g. the German Landfill Regulation (DepV), the planned German regulation on substitute building materials (Ersatzbaustoffverordnung), and the amended German Federal Soil Protection and Contaminated Sites Ordinance (Novelle BBodSchV) and also because it is c
13、losely connected with LAGA PN 98, the “Guideline for procedures for physical, chemical and biological testing in connection with the recovery/disposal of waste”. Thus, most waste, soil and sludge samples to be investigated in Germany will be covered. Practice has shown that even for applications not
14、 governed by such regulations the methods laid down in DIN 19747:2009 and LAGA PN 98 are used. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 565 DIN ISO 565 ISO 10381-4 DIN ISO 10381-4 ISO 14507 DIN ISO 14507 ISO 18512 DIN ISO 18512 D
15、IN EN 16179:2012-11 3 National Annex NA (informative) Bibliography DIN ISO 565, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openings DIN ISO 10381-4, Soil quality Sampling Part 4: Guidance on the procedure for investigation of natural, near-natural a
16、nd cultivated sites DIN ISO 14507, Soil quality Pretreatment of samples for determination of organic contaminants DIN ISO 18512, Soil quality Guidance on long and short term storage of soil samples DIN EN 16179:2012-11 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE N
17、ORM EN 16179 August 2012 ICS 13.080.05; 13.030.01 English Version Sludge, 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 Probenvorbehandlu
18、ng This European Standard was approved by CEN on 23 June 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 ref
19、erences 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 under the responsibility of a C
20、EN 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, Former Yugoslav Republic of Macedon
21、ia, 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 EUROPEN DE NORMALISATION EUROPI
22、SCHES 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 16179:2012: EEN 16179:2012 (E) 2 Contents Page Foreword 4Introduction .51 Scope 62 Normative referen
23、ces 63 Terms and definitions .74 Safety remarks .95 Principle 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 deter
24、mination of organic volatile compounds 195.6 Pretreatment 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 Selec
25、tion of workplace . 238.3 Estimation of minimum subsample 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 Pre
26、servation 2710 Pretreatment procedures in the laboratory (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.
27、2.4 Removal of extraneous materials and crushing 2910.2.5 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 33
28、10.3.4 Moderately volatile organic compounds Grinding not possible or not necessary 35DIN EN 16179:2012-11 EN 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 Ty
29、ler divider 40A.5 Application of mechanised turntable (rotating divider) 40Annex B (informative) Information concerning vapour pressure, boiling and melting points of volatile organic compounds . 42Bibliography 45DIN EN 16179:2012-11 EN 16179:2012 (E) 4 Foreword This document (EN 16179:2012) has bee
30、n 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 publication of an identical text or by endor
31、sement, 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 shall not be held responsible for ide
32、ntifying 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 (Mandate M/330), which assigned the develo
33、pment 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. According to the CEN/CENELEC Internal Reg
34、ulations, 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, Greece, Hungary, Iceland, Ireland,
35、Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16179:2012-11 EN 16179:2012 (E) 5 Introduction This document has been developed upon existing International Standards for
36、 the pretreatment of soils of specified particle fractions. Historically 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 th
37、e samples into fractions 2 mm where the fraction 2 mm and the extraneous 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. DIN EN 16179:2012-11 EN 16179:2012 (E) 10 Beside
38、 the requirements given in this European Standard, the subsequently applied 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 s
39、everal parameters are being investigated, the sample pretreatment shall be designed 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
40、 group of parameters. Whenever volatile compounds are to be determined, the 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 s
41、hall be pretreated in accordance with the appropriate analytical standard and 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.
42、Figure 1, Figure 2 and Figure 3 show flow charts for: pretreatment for inorganic 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-chemi
43、cal and organic parameters in liquid sludge (Figure 3). Aside from the parameter 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 1038
44、1-8 is used (see Table 2 in 8.3). Grinding of the sample depends on the mass 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
45、obtain adequate results for those parameters. EXAMPLES dry matter, total organic compounds (TOC), pH, EC. DIN EN 16179:2012-11 EN 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 D95r
46、equired, remarksProcedurebAmmonium- and nitrate-nitrogen Solid 15 g No D95requirements, 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 D95requirement
47、s, sample as receive Fig. 1, Route A Sludge No D95requirements, direct measurement 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 D95requireme
48、nts, direct measurement in the liquid phase Fig. 3 Dry matter fraction Solid 30 g 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) at 550 C All 2 g No D95
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