1、November 2012 Translation by DIN-Sprachendienst.English price group 9No 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).IC
2、S 13.080.10; 13.030.01!$J“1922539www.din.deDDIN EN 16168Sludge, treated biowaste and soil Determination of total nitrogen using dry combustion method;English version EN 16168:2012,English translation of DIN EN 16168:2012-11Schlamm, behandelter Bioabfall und Boden Bestimmung des Gesamt-Stickstoffgeha
3、lts mittels trockener Verbrennung;Englische Fassung EN 16168:2012,Englische bersetzung von DIN EN 16168:2012-11Boues, bio-dchets traits et sols Dtermination de la teneur totale en azote par combustion sche;Version anglaise EN 16168:2012,Traduction anglaise de DIN EN 16168:2012-11www.beuth.deDocument
4、 comprises 15 pagesIn case of doubt, the German-language original shall be considered authoritative.10.12 DIN EN 16168:2012-11 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 f
5、ields 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 BodenuntersuchungNA119-01-02-02 AA Chemische und physikalische
6、Verfahren. ,The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 5725-2 DIN ISO 5725-2 ISO 13878 DIN ISO 13878 ISO 18512 DIN ISO 18512 DIN EN 16168:2012-11 3 National Annex NA (informative) Bibliography DIN ISO 5725-2, Accuracy (trueness and
7、 precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN ISO 13878, Soil quality Determination of total nitrogen content by dry combustion (“elemental analysis”) DIN ISO 18512, Soil quality Gui
8、dance on long and short term storage of soil samples DIN EN 16168:2012-11 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16168 August 2012 ICS 13.030.01; 13.080.10 English Version Sludge, treated biowaste and soil Determination of total nitrogen using dry com
9、bustion method Boues, bio-dchets traits et sols Dtermination de la teneur totale en azote par combustion sche Schlamm, behandelter Bioabfall und Boden Bestimmung des Gesamt-Stickstoffgehalts mittels trockener Verbrennung This European Standard was approved by CEN on 24 May 2012. CEN members are boun
10、d 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 application to the CE
11、N-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 Management Centre h
12、as 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, Lithuania, L
13、uxembourg, 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 Brussels 2012
14、CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16168:2012: E EN 16168:2012 (E) 2 Contents PageForeword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Principle 55 Interferences and sources of errors 5
15、6 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 total nitrogen content 710 Calculation 711 Expression of results 812 Precision .813 Test report 8Annex A (informative) Repeatability
16、and reproducibility data 9A.1 Materials used in the interlaboratory comparison study 9A.2 Interlaboratory comparison results 10Bibliography . 11DIN EN 16168:2012-11EN 16168:2012 (E) 3 Foreword This document (EN 16168:2012) has been prepared by Technical Committee CEN/TC 400 “Project Committee - Hori
17、zontal 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 stand
18、ards 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 prepare
19、d 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 and
20、 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 countr
21、ies 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, Pola
22、nd, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16168:2012-11EN 16168:2012 (E) 4 Introduction This European Standard is applicable and validated for several types of matrices as indicated in Table 1 (see also Annex A for the results of the
23、 validation). Table 1 Matrices for which this European Standard is applicable and validated Matrix Materials used for validation Sludge Municipal sludge Biowaste Fresh compostCompost Soil Sludge amended soil Agricultural soil WARNING Persons using this European Standard should be familiar with usual
24、 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 regulatory conditions. IMPORTANT
25、It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. DIN EN 16168:2012-11EN 16168:2012 (E) 5 1 Scope This European Standard specifies the determination of total nitrogen (organic and inorganic) according to the procedure of Dum
26、as 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 following documents, in whole or in part, are normatively referenced in this document and are indispensable for its applicati
27、on. 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, treated biowaste, soil and waste Calculation of dry matter fraction after determination of dry residue or water conten
28、t 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 and sediment samples (ISO 5667
29、-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 apply. 3.1 total nitrogen amount of nitrogen that is released after Dumas combustion of the sample 4 Principle The total
30、 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 oxidized and/or volatilized. The combustion products are oxides of nitrogen (NOx) and molecular nitrogen (N2). After tran
31、sforming 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 of errors Pores in the material to be analysed are filled with air and therefore with nitrogen. Nitrogen also enters
32、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 samples shall be used only in special cases and handled with care, as they can leach out of sample vials during the pr
33、ocess 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 shall be performed after changing gas bottles and each day before starting the analytical series. DIN EN 16168:2012-11
34、EN 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), free of nitrogen. 6.3 Inert gas, carrier gas, free of nitrogen, e.g. helium. 6.4 Ethylenediaminetetraacetic acid (
35、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 (e.g. NIST) which contain the matrix materials of investigations. 7 Apparatus Usual laboratory apparatus, and in pa
36、rticular 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 a detection device for measurement of nitrogen gas. 7.2 Crucibles, adapted to the Dumas apparatus (7.1) of variab
37、le 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 5667-15. For the purpose of this European Standard biowaste may be stored like soil. Pretreat the sample according
38、 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 or at room temperature may cause losses of nitrogen due to microbial activity within the sample. Therefore rapid dr
39、ying 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 the dry mass of the sample according to EN 15934. 9 Procedure 9.1 General The total nitrogen contribution from wate
40、r (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 and gases (6.2, 6.3) shall be checked by performing a blank test (see 9.3). Ascertain homogeneity of the laboratory
41、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 in the Dumas apparatus. DIN EN 16168:2012-11EN 16168:2012 (E) 7 The Dumas apparatus (7.1) is used to combust the m
42、aterial 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 gas formed. 9.2 Confirmation of calibration Confirm the calibration of the apparatus by analyzing calibration s
43、ubstances (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 nitrogen. If necessary, check the linearity of the analyser with different amounts of EDTA (6.4) or the calibrating
44、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 reproducible blank value is measured, it shall be considered during calibration. Otherwise, the reason shall be
45、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 analyzed to the nearest of 0,1 % accuracy into the crucible (7.2). The amount depends on the expected total nitrogen
46、 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/or fixing of combustion gases that interfere with the analysis, refer to the manufacturers instructions. 10 Ca
47、lculation 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 milligrams per kilogram (mg/kg); X is the primary result in milligram (mg) nitrogen; m is the mass of the test sa
48、mple in the crucible, expressed in kilograms (kg); wdmis the dry matter fraction, expressed in percent (%), determined according to EN 15934. DIN EN 16168:2012-11EN 16168:2012 (E) 8 11 Expression 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
