1、BRITISH STANDARDBS EN14672:2005Characterization of sludges Determination of total phosphorusThe European Standard EN 14672:2005 has the status of a British StandardICS 13.030.20g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54
2、g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 14672:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 July 2006 BSI 2006ISBN 0 580 46288 9National forewordThis British Standard is the official English
3、 language version of EN 14672:2005.The UK participation in its preparation was entrusted to Technical Committee EH/5, Sludge characteristics, which has the responsibility to:A list of organizations represented on this committee can be obtained on request to its secretary.BSI Technical Committee EH/5
4、 considers that this method has been superseded long ago by advances in analytical techniques. It has not been used in the UK for 20 years or more.This method has also been validated using one sludge only, and this sludge is inadequately defined, such that it would be impossible for a user of the st
5、andard to assess whether its characteristics are similar to the sample for which the method is to be used.However, this method for total phosphorus has been used successfully elsewhere for over 40 years. Although only one inadequately defined sludge has been used in this method, the method itself is
6、 thought to be robust and fit for purpose. The user is therefore urged to use relevant certified reference materials when undertaking this method.EH/5 considers the publication of this method as a European Standard to be inconsistent with CEN/TC 308s Business Plan (Clause 4.2) which states:“The TC w
7、ill subject all of its test methods to international interlaboratory trials in order to ensure that they give reliable results. This is considered an essential feature of any standard method of test and therefore each test method will include a chapter reporting its precision, repeatability and repr
8、oducibility and how this was assessed.”as the information provided in Annex A is limited. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related in
9、ternational and European developments and promulgate them in the UK.Summary of pagesThis document comprises a front cover, an inside front cover, page i, a blank page, the EN title page, pages 2 to 9 and a back cover.The BSI copyright notice displayed in this document indicates when the document was
10、 last issued.Amendments issued since publicationAmd. No. Date CommentsBS EN 14672:2005iCross-referencesThe British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Corre
11、spondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not o
12、f itself confer immunity from legal obligations.blankEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14672August 2005ICS 13.030.20English versionCharacterization of sludges - Determination of total phosphorusCaractrisation des boues - Dosage du phosphore total Charakterisierung von Schlmmen - Best
13、immung vonGesamtphosphorThis European Standard was approved by CEN on 27 June 2005.CEN members are bound to comply with the CEN/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
14、bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility
15、of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, La
16、tvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CE
17、N All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14672:2005: EEN 14672:2005 (E) 2 Contents Page Foreword 3 1 Scope .4 2 Normative references .4 3 Terms and definitions.4 4 Principle.5 5 Limitations and interferences 5 6 Hazards5 7 Appar
18、atus 5 8 Reagents6 9 Sample pre-treatment .6 10 Procedure 6 11 Expression of results7 12 Test report .8 Annex A (informative) Performance data of interlaboratory comparison 9 EN 14672:2005 (E) 3 Foreword This European Standard (EN 14672:2005) has been prepared by Technical Committee CEN/TC 308 “Char
19、acterization of sludges”, the secretariat of which is held by AFNOR. 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 2006, and conflicting national standards shall be withdrawn at the lat
20、est by February 2006. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Irel
21、and, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EN 14672:2005 (E) 4 1 Scope This European Standard specifies a procedure for complete digestion of raw/digested sludge, suitable for the subsequ
22、ent determination of phosphorus. NOTE Phosphorus in environmental samples can be present in many forms. This method of pre-treatment enables the analyst to determine all forms - i.e. total phosphorus, by quantitative oxidation yielding an aqueous solution of orthophosphate which should be analysed f
23、or phosphate according to method EN ISO 6878, EN ISO 10304-2 or an equivalent validated method. The range of the method is up to 50 g/kg P assuming appropriate dilution of the digest in the final measurement step. 2 Normative references The following referenced documents are indispensable for the ap
24、plication 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 residue and water content EN ISO 3696, Water for
25、 analytical laboratory use Specification and test methods (ISO 3696:1987) EN ISO 6878, Water quality Determination of phosphorus Ammonium molybdat spectrometric method (ISO 6878:2004) EN ISO 10304-2, Water quality Determination of dissolved anions by liquid chromatography of ions Part 2: Determinati
26、on of bromide, chloride, nitrate, nitrite, orthophosphate and sulfate in waste water (ISO 10304-2:1995) 3 Terms and definitions For the purposes of this European Standard, the following terms and definitions apply. 3.1 total phosphorus phosphorus converted to orthophosphate by oxidation. NOTE This i
27、ncludes condensed phosphates (e.g. pyro and polyphosphates), organophosphorus (e.g. phosphate esters and aminophosphonic acids) and free phosphates 3.2 dry residue dry mass portion of the sludge obtained after the specified drying process. It is expressed as percent EN 12880:2000, 3.1 3.3 dry mass (
28、dry matter) mass of solid obtained after the specified drying process. It is expressed as grams or kilograms EN 12880:2000, 3.3 EN 14672:2005 (E) 5 4 Principle A boiling mixture of sulfuric and nitric acids oxidises organic matter, releasing any phosphorus present and converting it to orthophosphate
29、. As the mixture boils, nitric acid is lost due to the oxidation process and due to distillation. As the proportion of nitric acid decreases, the boiling temperature rises and any organic matter still unoxidised reacts with the sulfuric acid, causing the mixture to char. Small additions of nitric ac
30、id are used to complete the oxidation, at which point, no further charring occurs resulting in white fumes and a clear solution. This solution, when diluted and neutralised with sodium hydroxide, is used for phosphate analysis by method EN ISO 10304-2, EN ISO 6878 or an equivalent validated method.
31、It is possible to analyse for phosphorus using ICP-OES, but the performance of this method shall be shown to be equivalent to the above standard method. NOTE 1 Many laboratories determine phosphorus together with metals and sulfurusing ICP-OES after a suitable nitric acid based digestion, but it is
32、felt that this nitric/sulfuric acid digestion method has been successfully used for many years for total phosphorus determinations and should still be available as an International Standard. NOTE 2 Determination of P according to EN ISO 10304-2 by ion chromatography can be difficult when sulfate is
33、present at relatively high concentrations in the sample. 5 Limitations and interferences If fluoride or fluorapatite is known to be present, a thick-walled Kjeldahl flask shall be used. 6 Hazards 6.1 General Waste and sludge samples may contain hazardous and inflammable substances. They shall contai
34、n pathogens and be liable to biological action. Consequently it is recommended that these samples should be handled with special care. The gases which may be produced by microbiological activity are potentially inflammable and will pressurise sealed bottles. Exploding bottles are likely to result in
35、 infectious shrapnel and/or pathogenic aerosols. Glass bottles shall be avoided wherever possible. National regulations should be followed with respect to microbiological hazards associated with this method. NOTE All equipment used in the vicinity should be flame proof to avoid any source of ignitio
36、n. 6.2 Storage It is not advisable to store samples in the open laboratory. If samples are to be stored, store them between 0 C and 4 C. Sample containers that allow for the escape of any generated gas should be used. 6.3 Strong acids and alkalis The sulfuric and nitric acids and the sodium hydroxid
37、e, as solid or in solution, are extremely corrosive and shall be handled with caution. Resistant gloves and eye protection shall be worn. Heating of acids shall be carried out under local exhaust ventilation. 7 Apparatus Ordinary laboratory apparatus and the following: 7.1 Kjeldahl flask, for exampl
38、e 200 ml nominal capacity or tube, for example 100 ml. 7.2 Heating device, Bunsen burner or heating mantle or suitable heating block. EN 14672:2005 (E) 6 8 Reagents 8.1 Sulfuric acid, = 1,84 g/ml (18 mol/l). 8.2 Nitric acid, = 1,42 g/ml (15 mol/l). 8.3 Sodium hydroxide c(NaOH) = (5 mol/l). Dissolve
39、(200 10) g of sodium hydroxide in approximately 800 ml of water, cool and dilute to (1 000 10) ml with water. Store in a polyethylene bottle. 8.4 Phenolphthalein indicator solution. 8.5 Water, distilled or deionised, complying with grade 3 defined in EN ISO 3696. 9 Sample pre-treatment 9.1 Sample pr
40、eservation Sludge samples can change composition through biological and/or chemical activity. They shall be kept in cool boxes at less than 4 C in transit to the laboratory. Total phosphorus is a conservative parameter. Analysis shall be within 4 weeks. 9.2 Preparation of sample The purpose of pre-t
41、reatment is to obtain a representative and homogeneous sample. NOTE 1 Sludge may be analysed dried and ground, or as a well-homogenised wet sample. NOTE 2 Dry residue obtained according to EN 12880 may be ground by suitable means (e.g. pestle and mortar) or wet sample which has been macerated or hom
42、ogenised mechanically may be used directly. 10 Procedure Weigh sufficient sample (up to 2 g 2 mg dry mass), containing not more than 50 mg of phosphorus into the Kjeldahl flask or tube. Add (2,0 0,1) ml sulfuric acid (8.1) and approximately 0,5 ml nitric acid (8.2). Swirl to mix. Heat the Kjeldahl f
43、lask or tube in a fume cupboard. Continue heating until brown fumes cease to be produced. If the mixture chars, carefully add approximately 0,5 ml of nitric acid (8.2), dropwise down the neck of the Kjeldahl flask and repeat 3 or 4 times the addition of 0,5 ml of nitric acid until the mixture does n
44、ot char when white fumes are produced. Allow the mixture to cool, add 10 ml of water (8.5) and heat to fuming and repeat one time this operation and allow to cool. Cautiously wash down the sides of the Kjeldahl flask or tube with (25 1) ml of water and allow to cool. Neutralise the solution with the
45、 sodium hydroxide (8.3), in presence of phenolphthalein (8.4). Quantitatively transfer the solution to a 50 ml volumetric flask, with water, make up to volume and mix well. EN 14672:2005 (E) 7 Analyse the solution for phosphate phosphorus using method EN ISO 6878, EN ISO 10304-2 or equivalent valida
46、ted method within 4 weeks. A reagent blank without the addition of any sludge shall be taken through the whole procedure. 11 Expression of results 11.1 Wet sludge sample The total phosphorus content (Ptot) of the original sample is given in equation (1): ()drwbtot10 wmVCCP= (1) where Ptotis the tota
47、l phosphorus content in grams per kilogram dry matter; C is the phosphorus concentration of the digestion solution in milligrams per litre; Cbis the phosphorus concentration in the reagent blank, in milligrams per litre; V is the volume of the digestion solution in the volumetric flask in millilitre
48、s; mwis the wet mass of sample taken for digest in grams; wdris the dry residue of the sludge determined by method EN 12880 in percent. 11.2 Dry sludge sample The total phosphorus content (Ptot) of the original sample is given in equation (2): ()1000 Dbtot=mVCCP (2) where Ptotis the total phosphorus
49、 content in grams per kilogram; C is the phosphorus concentration of the digest in milligrams per litre; Cbis the phosphorus concentration in the reagent blank, in milligrams per litre; V is the volume of solution in volumetric flask in millilitres; mDis the dry mass of sample taken for acid digestion in grams. 11.3 Precision See Annex A. EN 14672:2005 (E) 8 12 Test report The test report shall contain the following information: a) reference to this European Standard; b) all information necessary for complete identification of the sludge
