1、November 2012 Translation by DIN-Sprachendienst.English price group 8No 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 13.030.01!$L“1922541www.din.deDDIN EN 15933Sludge, treated biowaste and soil Determination of pH;English version EN 15933:2012,English translation of DIN EN 15933:2012-11Schlamm, behandelter Bioabfall und Boden Bestimmung des pH-Werts;Englische Fassung EN 15933:2012,Englische bersetzung von DIN EN
3、 15933:2012-11Boues, bio-dchets traits et sols Dtermination du pH;Version anglaise EN 15933:2012,Traduction anglaise de DIN EN 15933:2012-11www.beuth.deDocument comprises 15 pagesIn case of doubt, the German-language original shall be considered authoritative.10.12 DIN EN 15933:2012-11 2 A comma is
4、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). The responsible German body involved in its preparation was the Normenaussc
5、huss Wasserwesen (Water Practice Standards Committee), Working Committee NA 119-01-02 Abfall- und Bodenuntersuchung119-01-02-02 AA Chemische und physikalische Verfahren. , NAThe DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 5725-2 DIN ISO
6、 5725-2 ISO 10390 DIN ISO 10390 DIN EN 15933:2012-11 3 National Annex NA (informative) Bibliography DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DI
7、N ISO 10390, Soil quality Determination of pH DIN EN 15933:2012-11 4 Leerseite EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15933 August 2012 ICS 13.030.01 English Version Sludge, treated biowaste and soil Determination of pH Boues, bio-dchets traits et sols Dtermination du pH Schlamm, behan
8、delter Bioabfall und Boden Bestimmung des pH-Werts 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 alter
9、ation. Up-to-date 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
10、 by translation 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, Estoni
11、a, Finland, Former 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 STANDA
12、RDIZATION COMIT 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 15933:2012: E EN 15933:2012 (E) 2 Contents Page Forew
13、ord 3Introduction . 41 Scope 52 Normative references 53 Principle 54 Interferences 55 Reagents . 56 Apparatus . 67 Sample pretreatment . 68 Procedure . 78.1 Preparation of a suspension 78.2 Calibration of the pH-meter 78.3 Measurement of the pH . 79 Expression of results 710 Precision . 711 Test rep
14、ort 8Annex A (informative) Repeatability and reproducibility data 9A.1 Materials used in the interlaboratory comparison study 9A.2 Interlaboratory comparison results . 10Bibliography 11DIN EN 15933:2012-11EN 15933:2012 (E) 3 Foreword This document (EN 15933:2012) has been prepared by Technical Commi
15、ttee 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 endorsement, at the latest by Febr
16、uary 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 identifying any or all such pate
17、nt 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 development of standards on samplin
18、g 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 Regulations, the national standa
19、rds 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, Italy, Latvia, Lithuania, Lux
20、embourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 15933:2012-11EN 15933:2012 (E) 4 Introduction This European Standard is applicable and validated for several types of matrices as indicated in Table 1
21、 (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 Compost Soil Arable soil Forest soilWARNING Persons using this European Standard should be famili
22、ar 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 regulatory condition
23、s. IMPORTANT It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. DIN EN 15933:2012-11EN 15933:2012 (E) 5 1 Scope This European Standard specifies a method for the determination of pH within the range pH 2 to pH 12 in a suspens
24、ion of sludge, treated biowaste or soil in either water (pH-H2O), or a 0,01 mol/l calcium chloride solution (pH-CaCl2). This European Standard is applicable to sludge, treated biowaste and fresh or air-dry soil samples. 2 Normative references The following documents, in whole or in part, are normati
25、vely 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 biowaste and soil Guidance for sample
26、pretreatment EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) 3 Principle The pH is measured in a suspension of a test portion which is made up in 5 times its volume of either water or a 0,01-mol/l-solution of calcium chloride. NOTE To make the procedure gen
27、erally applicable to all types of sludge, treated biowaste and soil samples, a volume fraction ratio is chosen because then all types of samples can be treated in the same way. For the purpose of this standard, taking the required volume of test portion with a measuring spoon is sufficiently accurat
28、e. 4 Interferences In samples with a high content of charged particles (e.g. organic matter, clay) the suspension effect can modify the potential difference between the electrodes, and thereby have an influence on the recorded pH value. This problem is minimized by gentle stirring of the suspension.
29、 For calcareous material, carbon dioxide may be absorbed by the suspension, which makes it difficult to reach an equilibrium value. Other sources of error are associated with materials containing sulfidic minerals or volatile acids. 5 Reagents Use only reagents of recognized analytical grade, unless
30、 otherwise specified. 5.1 Water, grade 2 as specified in EN ISO 3696. The water shall have a specific electric conductivity 0,2 mS/m at 25 C, and pH 5,6. 5.2 Calcium chloride solution, c(CaCl2) = 0,01 mol/l. Dissolve 1,47 g calcium chloride dihydrate (CaCl2 2 H2O) in water (5.1) and dilute to 1 000
31、ml. This solution may be stored for several months in a refrigerator in a closed volumetric flask or other type of closed glass vessel. DIN EN 15933:2012-11EN 15933:2012 (E) 6 5.3 Buffer solution, for calibration of the pH-meter. Use at least two of the following buffer solutions for calibration. Co
32、mmercially available buffer solutions of similar or equivalent pH may also be used. Freshly prepared, the buffer solutions 5.3.1, 5.3.2 and 5.3.3 are stable for one month when stored in polyethylene bottles. 5.3.1 Buffer solution pH = 4,00, at 20 C. Dissolve 10,21 g potassium hydrogen phthalate (C8H
33、5O4K) in water (5.1) and dilute to 1 000 ml. Potassium hydrogen phthalate shall be dried before use for 2 h at (120 5) C. 5.3.2 Buffer solution pH = 6,88, at 20 C. Dissolve 3,39 g potassium dihydrogen phosphate (KH2PO4) and 3,53 g disodium hydrogen phosphate (Na2HPO4) in water (5.1) and dilute to 1
34、000 ml. Potassium dihydrogen phosphate shall be dried before use for 2 h at (120 5) C. 5.3.3 Buffer solution pH = 9,22, at 20 C Dissolve 3,80 g disodium tetraborate decahydrate (Na2B4O7 10 H2O) in water (5.1) and dilute to 1 000 ml. NOTE Disodium tetraborate decahydrate may lose water of crystalliza
35、tion when stored for a long time. 6 Apparatus 6.1 pH-meter, readable to two decimal points. The device shall allow calibration of the pH-electrode for zero and the slope of the function. A normalisation to the standard temperature (25 C) shall be applied. 6.2 Combined glass electrode, pH/temperature
36、 combination electrode consisting of a measurement sensor and a temperature sensor. 6.3 Shaking device 6.4 Measuring spoon 6.5 Bottle, polyethylene (PE) or glass with tightly fitting cap or stopper. 7 Sample pretreatment Pretreat the samples according to EN 16179, if not otherwise specified. For tre
37、ated biowaste particle sizes can be between 10 mm and 40 mm. Therefore, treated biowaste samples are measured without pretreatment. Liquid sludge is measured directly without pretreatment. DIN EN 15933:2012-11EN 15933:2012 (E) 7 8 Procedure 8.1 Preparation of a suspension For solid samples take a te
38、st portion of at least 5 ml from the test sample using a measuring spoon (6.4). Place the test portion in a bottle (6.5). Add water (5.1) or calcium chloride solution (5.2) to a volume which is 5 times the volume of the test portion. For treated biowaste the procedure and volume ratio (1:5) is the s
39、ame, except that at least 60 ml sample volume is added to 300 ml of either water or calcium chloride solution. For liquid sludge the suspension is prepared without the addition of water. Measurements in liquid sludge shall be made directly in the liquid suspension. Shake or mix the suspension for (6
40、0 10) min using a shaking device. Allow the suspension to settle for at least 1 h, but not longer than 3 h. NOTE For soils with high contents of calcium carbonate and/or magnesium carbonate the equilibration time can be longer than 3 h. Ingress of air during standing after shaking should be avoided.
41、 8.2 Calibration of the pH-meter Adjust and calibrate the pH-meter (6.1) as specified in the manufacturers instructions, using the buffer solutions (5.3) at (20 2) C. NOTE Temperature compensation can be used when measuring the sample. Depending on the expected pH-range start the calibration of the
42、pH-meter with buffer solution pH 6,88 (5.3.2) and use then either buffer solution pH 4,00 (5.3.1) for acidic suspensions or buffer solution pH 9,22 (5.3.3) for alkaline suspensions. Commercially available standards within the same pH range may also be used. 8.3 Measurement of the pH Measure the pH i
43、n the suspension at (20 2) C immediately after or whilst being stirred. The stirring should be at such a rate to achieve a reasonably homogenous suspension of the particles, but entrainment of air should be avoided. 9 Expression of results The results of the pH determinations should be reported to o
44、ne decimal place. 10 Precision The performance characteristics of the method have been evaluated, see A.2. DIN EN 15933:2012-11EN 15933:2012 (E) 8 11 Test report The test report shall contain at least the following information: a) a reference to this European Standard (EN 15933); b) complete identif
45、ication of the sample; c) sample preparation (e.g. fresh or air-dried); d) the solution used to make the suspension: water or CaCl2solution; e) expression of results, according to Clause 9; f) any details not specified in this European Standard or which are optional, as well as any factor which may
46、have affected the results. DIN EN 15933:2012-11EN 15933:2012 (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 pH in sludge, treated biowaste and soil was carried out wi
47、th 14 to 16 European laboratories on six materials. Detailed information can be found in the final report on the interlaboratory comparison study mentioned in 8. Table A.1 lists the types of materials tested. Table A.1 Materials tested in the interlaboratory comparison for the determination of pH in
48、 sludge, treated biowaste and soil Grain size Sample Material Sludge ( 0,5 mm) Sludge 1 Mix 1 of municipal waste water treatment plant sludges from North Rhine Westphalia, Germany Sludge 2 Mix 2 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 soil from Hohenheim, Germany Soil 5 Agricultural soil from
