1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 16168:2012Sludge, treated biowaste and soil Determination of total nitrogen using dry combustion methodBS EN 16168:2012 BRITISH STANDARDNational forewordThis British Standa
2、rd is the UK implementation of EN 16168:2012. 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 purpo
3、rt 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 56694 3 ICS 13.030.01; 13.080.10 Compliance with a British Standard cannot confer immunity from leg
4、al 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 16168:2012EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16168 August 2012 ICS 13.030.
5、01; 13.080.10 English Version Sludge, treated biowaste and soil - Determination of total nitrogen using dry combustion method Boues, biodchets traits et sols - Dtermination de la teneur totale en azote par combustion sche Schlamm, behandelter Bioabfall und Boden - Bestimmung des Gesamt-Stickstoffgeh
6、alts mittels trockener Verbrennung 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-dat
7、e 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
8、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 versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Form
9、er 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
10、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 worldwide for CEN national Members. Ref. No. EN 16168:2012: EBS EN 16168:2012EN 16168:2012 (E) 2 Contents Page Forewo
11、rd 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Principle 55 Interferences and sources of errors 56 Reagents .67 Apparatus .68 Sample storage and sample pretreatment 69 Procedure .69.1 General 69.2 Confirmation of calibration .79.3 Blank test 79.4 Determination of tot
12、al nitrogen content 710 Calculation 711 Expression of results 812 Precision .813 Test report 8Annex A (informative) Repeatability and reproducibility data 9A.1 Materials used in the interlaboratory comparison study 9A.2 Interlaboratory comparison results 10Bibliography . 11BS EN 16168:2012EN 16168:2
13、012 (E) 3 Foreword This document (EN 16168:2012) 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
14、, either by publication 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.
15、CEN and/or CENELEC shall 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 Europe
16、an Commission (Mandate 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 technic
17、ally feasible. According 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 Macedon
18、ia, France, Germany, 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 16168:2012EN 16168:2012 (E) 4 Introduction This European Standard
19、is applicable and validated 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 Biowaste Fresh compostCom
20、post Soil Sludge amended soil 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 esta
21、blish appropriate safety and 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 16168:2012EN 16168:2012 (E) 5 1 Scope This Eur
22、opean Standard specifies the determination of total nitrogen (organic and inorganic) according to the procedure of Dumas in sludge, treated biowaste and soil. A typical limit of detection is 0,02 % nitrogen, and a typical limit of quantification is 0,08 % nitrogen. 2 Normative references The followi
23、ng 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 (including any amendments) applies. EN 15934, Sludge,
24、treated biowaste, soil and waste Calculation of dry matter fraction after determination of dry residue or water content 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-
25、15, Water quality Sampling Part 15: Guidance on the preservation and handling of sludge and sediment samples (ISO 5667-15) ISO 18512, Soil quality Guidance on long and short term storage of soil samples 3 Terms and definitions For the purposes of this document, the following terms and definitions ap
26、ply. 3.1 total nitrogen amount of nitrogen that is released after Dumas combustion of the sample 4 Principle The total nitrogen content of the material is determined by heating it to a temperature of at least 850 C in the presence of oxygen. Mineral (inorganic) and organic nitrogen compounds are oxi
27、dized and/or volatilized. The combustion products are oxides of nitrogen (NOx) and molecular nitrogen (N2). After transforming all nitrogen into molecular nitrogen, the content of the nitrogen gas is measured using thermal conductometry or other device specific detectors. 5 Interferences and sources
28、 of errors Pores in the material to be analysed are filled with air and therefore with nitrogen. Nitrogen also enters the combustion cell when it is opened to exchange the sample. Purging of the cell and the material to be analysed by inert gas is sufficient in leaving no nitrogen gas behind. Moist
29、samples shall be used only in special cases and handled with care, as they can leach out of sample vials during the process or contaminate the device by spattering. Fluctuations of total nitrogen may be caused by differences in nitrogen content of carrier gases used. Therefore a blank determination
30、shall be performed after changing gas bottles and each day before starting the analytical series. BS EN 16168:2012EN 16168:2012 (E) 6 6 Reagents Use only reagents of recognized analytical grade, unless otherwise specified. 6.1 Water, grade 2 as specified in EN ISO 3696. 6.2 Combustion gas (oxygen),
31、free of nitrogen. 6.3 Inert gas, carrier gas, free of nitrogen, e.g. helium. 6.4 Ethylenediaminetetraacetic acid (EDTA), or other calibration substances with known content of nitrogen, e.g. acetanilide (C8H9NO), L-aspartic acid (C4H7NO4), sulfanilic acid or other amino acids or reference standards (
32、e.g. NIST) which contain the matrix materials of investigations. 7 Apparatus Usual laboratory apparatus, and in particular the following: 7.1 Dumas apparatus, suitable and calibrated for determination of total nitrogen by combustion of the sample at a temperature of at least 850 C, and equipped with
33、 a detection device for measurement of nitrogen gas. 7.2 Crucibles, adapted to the Dumas apparatus (7.1) of variable sizes, e.g. 1 ml to 20 ml of nominal volume or special foil. 8 Sample storage and sample pretreatment Store soil samples according to ISO 18512 and sludge samples according to EN ISO
34、5667-15. For the purpose of this European Standard biowaste may be stored like soil. Pretreat the sample according to EN 16179, if not otherwise specified. During the drying procedure or a milling process, care shall be taken to avoid losses of ammonium-N and/or nitrate-N. Prolonged drying at 40 C o
35、r at room temperature may cause losses of nitrogen due to microbial activity within the sample. Therefore rapid drying methods should be used. If necessary, moist samples can be used. In this case determine the dry mass on a special sample, so that the result can be referred to dry mass. Determine t
36、he dry mass of the sample according to EN 15934. 9 Procedure 9.1 General The total nitrogen contribution from water (6.1), reagents and gases (6.2, 6.3) shall be significantly less than the lowest total nitrogen content to be determined. The overall total nitrogen content of water (6.1), reagents an
37、d gases (6.2, 6.3) shall be checked by performing a blank test (see 9.3). Ascertain homogeneity of the laboratory sample and the air-dried test sample. In special cases the use of moist samples is necessary. Take care that the sample is homogeneous and avoid spattering during the combustion process
38、in the Dumas apparatus. BS EN 16168:2012EN 16168:2012 (E) 7 The Dumas apparatus (7.1) is used to combust the material at a minimum temperature of 850 C in the presence of oxygen (6.2), to reduce the nitrogen oxides, to eliminate the interfering gases and to detect the content of molecular nitrogen g
39、as formed. 9.2 Confirmation of calibration Confirm the calibration of the apparatus by analyzing calibration substances (6.4) to control the combustion and the apparatus on the day of use as follows: Weigh an adequate amount of EDTA (6.4) or any calibrating substance and measure the amount of nitrog
40、en. If necessary, check the linearity of the analyser with different amounts of EDTA (6.4) or the calibrating substance used. If the confirmation value derives by more than 3 %, the calibration should be updated. 9.3 Blank test Carry out blank determinations (empty crucibles) in each series. If a re
41、producible blank value is measured, it shall be considered during calibration. Otherwise, the reason shall be determined and removed. NOTE Fingerprints on sample containers may lead to blank values. 9.4 Determination of total nitrogen content Weigh a portion of the dried or moist sample to be analyz
42、ed to the nearest of 0,1 % accuracy into the crucible (7.2). The amount depends on the expected total nitrogen content and on the size of the crucible. Carry out the analysis in accordance with the manufacturers instructions. Use oxygen (6.2) as combustion gas. For reduction, oxidation, removal and/
43、or fixing of combustion gases that interfere with the analysis, refer to the manufacturers instructions. 10 Calculation Calculate the content of nitrogen wN, in milligrams per kilogram, using Formula (1): dmN100wmXw= (1) where wNis the content of nitrogen on the basis of dry matter, expressed in mil
44、ligrams per kilogram (mg/kg); X is the primary result in milligram (mg) nitrogen; m is the mass of the test sample in the crucible, expressed in kilograms (kg); wdmis the dry matter fraction, expressed in percent (%), determined according to EN 15934. BS EN 16168:2012EN 16168:2012 (E) 8 11 Expressio
45、n of results The result shall be expressed in milligrams per kilogram (mg/kg) dry matter or in percent (%) on the basis of dry matter and reported to two significant figures. 12 Precision The performance characteristics of the method have been evaluated (see Annex A). 13 Test report The test report
46、shall contain at least the following information: a) a reference to this European Standard (EN 16168); b) complete identification of the sample; c) the results calculated according to Clause 10 and expressed according to Clause 11; d) any details not specified in this European Standard or which are
47、optional, as well as any factor which may have affected the results. BS EN 16168:2012EN 16168:2012 (E) 9 Annex A (informative) Repeatability and reproducibility data A.1 Materials used in the interlaboratory comparison study The interlaboratory comparison of the determination of total nitrogen dry c
48、ombustion method in sludge, treated biowaste and soil was carried out with 12 to 13 European laboratories on six materials. Detailed information can be found in the final report on the interlaboratory comparison study mentioned in 6. Table A.1 lists the types of materials tested. Table A.1 Materials
49、 tested in the interlaboratory comparison of the determination of total nitrogen dry combustion method in sludge, treated biowaste and soil Grain size Sample Material Sludge ( 0,5 mm) Sludge 1 Mix of municipal waste water treatment plant sludges from North Rhine Westphalia, Germany Sludge 2 Mix of municipal waste water treatment plant sludges from North Rhine Westphalia, Germany Fine grained ( 2,0 mm) Compost 1 Fresh compost from Vienna, Austria Compost 2 Compost from Germany Soil 4 Sludge amended
