1、BRITISH STANDARDBS EN 14671:2006Characterization of sludges Pre-treatment for the determination of extractable ammonia using 2 mol/l potassium chlorideThe European Standard EN 14671:2006 has the status of a British StandardICS 13.030.20g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g
2、3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Licensed Copy: Wang Bin, na, Tue Aug 21 00:57:46 GMT+00:00 2007, Uncontrolled Copy, (c) BSIBS EN 14671:2006This British Standard was published under the authority o
3、f the Standards Policy and Strategy Committee on 30 April 2007 BSI 2007ISBN 978 0 580 50513 3National forewordThis British Standard was published by BSI. It is the UK implementation of EN 14671:2006.The UK participation in its preparation was entrusted to Technical Committee EH/5, Sludge characteriz
4、ation.A list of organizations represented on EH/5 can be obtained on request to its secretary.The UK committee has never seen the need to standardize this method at a European level and, as a consequence, has not been actively involved in the development of this standard. However, the UK committee i
5、s pleased that a classic British method was selected. The method has long been used as a valuable operational-control method and is available in existing technical literature (see reference 1 in the bibliography of this standard). Due to the difficulty and cost of sending liquid sludge samples (in s
6、uch a manner that their properties do not change) to laboratories for international interlaboratory trials of the performance of this method, interested parties convened at a workshop to assess the test. Their conclusion was that the results are operationally defined (e.g. by the filter paper used)
7、and, as the document does not specify all such operational details, the performance data are not really applicable outside the context of the workshop. As a result, the members of EH/5 have no information to offer on the reproducibility of the results.This publication does not purport to include all
8、 the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations. Amendments issued since publicationAmd. No. Date CommentsLicensed Copy: Wang Bin, na, Tue Aug 21 00:57:46 GMT+00:00 2007, Uncon
9、trolled Copy, (c) BSIEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14671June 2006ICS 13.030.20English VersionCharacterization of sludges - Pre-treatment for the determinationof extractable ammonia using 2 mol/l potassium chlorideCaractrisation des boues - Prtraitement pour ladtermination de lAzo
10、te ammoniacal extractible utilisant2mol/l de chlorure de potassiumCharakterisierung von Schlmmen - Vorbehandlung zurBestimmung des extrahierbaren Ammoniums unterVerwendung von 2 mol/l KaliumchloridThis European Standard was approved by CEN on 24 May 2006.CEN members are bound to comply with the CEN/
11、CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any
12、 CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN me
13、mbers are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerlan
14、d and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14671:
15、2006: ELicensed Copy: Wang Bin, na, Tue Aug 21 00:57:46 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14671:2006 (E) 2 Contents Page Foreword3 Introduction .4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Principle5 5 Limitations and interferences.5 6 Hazards .6 7 Reagents.6 8 Appar
16、atus .6 9 Sample pre-treatment7 10 Procedure .7 11 Expression of results 8 12 Test report 8 Annex A (informative) Performance data of the interlaboratory comparison Summary of sludge exchangeable ammonia results.9 Bibliography. 11 Licensed Copy: Wang Bin, na, Tue Aug 21 00:57:46 GMT+00:00 2007, Unco
17、ntrolled Copy, (c) BSIEN 14671:2006 (E) 3 Foreword This document (EN 14671:2006) has been prepared by Technical Committee CEN/TC 308 “Characterization of sludges”, the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publicatio
18、n of an identical text or by endorsement, at the latest by December 2006, and conflicting national standards shall be withdrawn at the latest by December 2006. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement th
19、is European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdo
20、m. Licensed Copy: Wang Bin, na, Tue Aug 21 00:57:46 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14671:2006 (E) 4 Introduction Because sludge may be applied to land as manure or as a disposal, there is a need to monitor extractable ammonia. Licensed Copy: Wang Bin, na, Tue Aug 21 00:57:46 GMT+00:00
21、2007, Uncontrolled Copy, (c) BSIEN 14671:2006 (E) 5 1 Scope This European standard specifies a procedure for the determination of extractable ammonia using a 2 mol/l potassium chloride solution in raw and digested sewage sludges. The range of the method is up to 100 g/kg N assuming appropriate dilut
22、ion of the potassium chloride extract in the final measurement step. NOTE The above wording will be modified once the round robin results are available. It may be suitable for other types of sludges, but the user should validate the method using these sludges. 2 Normative references The following re
23、ferenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 12880:2000, Characterization of sludges Determination of dry r
24、esidue and water content EN ISO 3696:1995, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) 3 Terms and definitions For the purposes of this European Standard, the following terms and definitions apply. 3.1 extractable ammonia ammonia that is released when the homog
25、enised sludge is shaken with 2 mol/l potassium chloride for 1 h at room temperature 3.2 dry residue dry mass portion of the sludge obtained after the specified drying process, expressed as a percentage EN 12880:2000, 3.1 4 Principle An aliquot of the homogenised sludge is shaken for 1 h with 2 mol/l
26、 potassium chloride at room temperature. The sample is then filtered and the ammonia determined by a suitable method. Potassium chloride (2 mol/l) is used rather than water to ensure that both soluble and ion exchangeable forms of the determinand are determined. It also minimises biological activity
27、 in the extracted sample. All results are expressed as nitrogen. Although undried samples are taken for analysis, it is recognised practice to report results on a dry weight basis. Consequently the dry residue content of the homogenised sample used for analysis should also be determined using a sepa
28、rate test portion (see EN 12880). 5 Limitations and interferences Substances present at their normal concentration in these types of samples should not cause significant interference in the pre-extraction step. For the vast majority of sewage sludges, the relatively high concentration of ammonia com
29、pared with potential interferences should not result in any significant Licensed Copy: Wang Bin, na, Tue Aug 21 00:57:46 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14671:2006 (E) 6 interferences in the final measurement stage. The user should carry out suitable recovery checks to confirm this. 6 H
30、azards 6.1 General Waste and sludge samples may contain hazardous and inflammable substances. They may contain pathogens and be liable for biological action. Consequently it is recommended that these samples should be handled with special care. The gases, which may be produced by microbiological act
31、ivity are potentially inflammable and will pressurise sealed bottles. Exploding bottles are likely to result in infectious shrapnel and/or pathogenic aerosols. Glass bottles should be avoided whenever possible. National regulations should be followed with respect to microbiological hazards associate
32、d with this method. NOTE All equipment used in the vicinity should be flame proof to avoid any risk of ignition. 6.2 Storage It is not advisable to store samples in an open laboratory. If samples are to be stored, store them between 0 C and 4 C. Sample containers that enable the escape of any genera
33、ted gas should be used. 7 Reagents 7.1 Water complying with purity grade 2 of EN ISO 3696:1995 7.2 Potassium chloride c(KCl) = 2,5 mol/l Dissolve (931,9 1) g of potassium chloride (dried at (105 2) C for 1 h) in approximately 3 l of water and dilute to 5 l with water in a volumetric flask. 8 Apparat
34、us Ordinary laboratory apparatus and the following: 8.1 Extraction bottles Wide-necked glass or plastics bottles with secure stoppers or caps, for example 250 ml nominal capacity. 8.2 Mechanical shaking apparatus Any suitable horizontal or inversion shaker shall be used (e. g. horizontal shaker (20
35、rpm to 40 rpm with 20 mm throw); roller table rotating at about 10 rpm; end-over-end tumbler (5 rpm to 10 rpm). NOTE Other shaking devices may be used provided that they can be shown to provide equivalent results. The material being leached should not settle or be agitated too vigorously so that par
36、ticle abrasion occurs. 8.3 Balance with on accuracy 0,05 g. 8.4 Drying oven, capable of maintained at (105 5) C 8.5 Suitable apparatus for the determination of ammonia in diluted sludge filtrates (See 10.4). Licensed Copy: Wang Bin, na, Tue Aug 21 00:57:46 GMT+00:00 2007, Uncontrolled Copy, (c) BSIE
37、N 14671:2006 (E) 7 8.6 Filter papers Cellulose filter papers with a pore size of 20 to 25 . (For example Whatman 5411). 9 Sample pre-treatment 9.1 Sample preservation Sludge samples can change composition through biological and/or chemical activity. They shall be kept in cool boxes at less than 4 C
38、in transit to the laboratory. They shall be analysed as soon as possible (within 24 h) after sampling. If prolonged storage is unavoidable, then store the samples at or below a temperature of 18 C in a freezer for a maximum period of 4 weeks and note this on the test report. 9.2 Preparation of sampl
39、e The purpose of pre-treatment is to obtain a representative and homogeneous sample. Samples shall not be subject to any drying prior to homogenisation because this will result in a loss of ammonia. For frozen samples see NOTE below. NOTE For frozen sludges, it is recommended that a suitable aliquot
40、 (equivalent to 0,25 g to 1 g of dry matter) of the frozen homogenised sample is directly transferred to the potassium chloride solution, as transformation of nitrogen compounds can occur during the thawing process. 10 Procedure 10.1 Transfer a known weight (m gram) of suitably homogenised (as sampl
41、ed) sludge (equivalent to (0,25 to 1) g 2 mg of dry matter, see NOTES 1 and 2) to an extraction bottle (8.1). Add (80 1) ml 2,5 mol/l potassium chloride (7.2) and (20 m) 1 ml of water (7.1) (See also 9.2, NOTE). NOTE 1 If a dry solids result is not available and an immediate analysis is required, th
42、en visually estimate the dry solids content. NOTE 2 The maximum “as received” weight of sludge taken should not exceed 20 g. 10.2 Replace the bottle cap and place on a shaker for (60 5) min at room temperature (see 8.2). 10.3 Owing to the difficulty in filtering many types of sludge samples, it is r
43、ecommended that a suitable aliquot of the leached sample is centrifuged. Then filter a suitable volume aliquot through a fluted filter paper (8.6) discarding at least the first 10 ml. In some cases paper filtration is too slow or even impossible. In such cases a validated alternative procedures for
44、obtaining a clear supernatant are acceptable and the technique used shall be reported. The filtrate is stable for some hours in a hermetically closed polyethylene bottle if stored in a refrigerator at (0 to 4) C. The filtrate can be stored for longer periods in a deep freezer at less than -18 C. NOT
45、E Vacuum filtration should not be used as it can result in loss of ammonia. In most instances the ammonia concentration will be sufficiently high to dilute the leached sample extract 10 times prior to this filtration step. This will greatly aid the speed of the filtration step. This dilution must be
46、 1) This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of the product named. Equivalent products may be used if they can be shown to lead to the same results. Licensed Copy: Wang Bin, na, Tue Aug 21 00:57:46 GMT+00:00 2007,
47、Uncontrolled Copy, (c) BSIEN 14671:2006 (E) 8 accounted for in the final calculation and the calibration standards need to be made up in 0,2 mol/l KCl rather than 2 mol/l KCl. 10.4 Analyse the ammonia according to ISO 5664, EN ISO 11732 or EN ISO 14911 or equivalent validated method within one day u
48、nless stored at less than 18 C (4 weeks). 10.5 A reagent blank without the addition of any sludge shall be taken throughout the whole procedure. 10.6 It is important to ensure that the calibration standards and blank shall be prepared in 2 mol/l potassium chloride (Add 80 ml of reagent 7.2, (2,5 mol
49、/l KCl) per 100 ml). 11 Expression of results 11.1 Calculation The extractable ammonia content, EAis expressed in g of nitrogen, N per kg dry mass and is given by equation (1): ()drbA10 wmVCCE= (1) where C is the ammonium nitrogen concentration in the extract, in mg/l ; Cbis the ammonium nitrogen concentration in the reagent blank, in mg/l ; m is the wet mass of sample taken for extraction, in g; wdris the dry residue of the sludge determined by method EN 12880, in %; V is the total volume of the extractant used, in ml (100 ml) 1
