BS EN 14672-2005 Characterization of sludges - Determination of total phosphorous《淤泥的特性 磷总含量的测定》.pdf

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、g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Licensed Copy: Wang Bin, na, Thu Sep 14 08:49:11 BST 2006, Uncontrolled Copy, (c) BSIBS EN 14672:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 July 2006 BSI

3、 2006ISBN 0 580 46288 9National forewordThis British Standard is the official English 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 th

4、is committee can be obtained on request to its secretary.BSI Technical Committee EH/5 considers that this method has been superseded long ago by advances in analytical techniques.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

5、sludge is inadequately defined, such that it would be impossible for a user of the standard 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 on

6、ly one inadequately defined sludge has been used in this method, the method itself is 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

7、to be inconsistent with CEN/TC 308s Business Plan (Clause 4.2) which states:“The TC will 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 ea

8、ch test method will include a chapter reporting its precision, repeatability and reproducibility 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 interp

9、retation, or proposals for change, and keep UK interests informed; monitor related international 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 cove

10、r.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date CommentsLicensed Copy: Wang Bin, na, Thu Sep 14 08:49:11 BST 2006, Uncontrolled Copy, (c) BSIBS EN 14672:2005iCross-referencesThe British Standards which

11、 implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publicatio

12、n 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 of itself confer immunity from legal obligations.Licensed Copy: Wang Bin, na, Thu Sep 14 08:49:11 BST 2006, Uncontrolled Copy, (c)

13、BSIblankLicensed Copy: Wang Bin, na, Thu Sep 14 08:49:11 BST 2006, Uncontrolled Copy, (c) BSIEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14672August 2005ICS 13.030.20English versionCharacterization of sludges - Determination of total phosphorusCaractrisation des boues - Dosage du phosphore tot

14、al Charakterisierung von Schlmmen - Bestimmung 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 witho

15、ut any alteration. Up-to-date lists and 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

16、 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 members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Gree

17、ce, Hungary, Iceland, Ireland, Italy, Latvia, 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

18、 de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14672:2005: ELicensed Copy: Wang Bin, na, Thu Sep 14 08:49:11 BST 2006, Uncontrolled Copy, (c) BSIEN 14672:2005 (E) 2 Contents Page Foreword 3 1 Sc

19、ope .4 2 Normative references .4 3 Terms and definitions.4 4 Principle.5 5 Limitations and interferences 5 6 Hazards5 7 Apparatus 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

20、Licensed Copy: Wang Bin, na, Thu Sep 14 08:49:11 BST 2006, Uncontrolled Copy, (c) BSIEN 14672:2005 (E) 3 Foreword This European Standard (EN 14672:2005) has been prepared by Technical Committee CEN/TC 308 “Characterization of sludges”, the secretariat of which is held by AFNOR. This European Standar

21、d 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 latest by February 2006. According to the CEN/CENELEC Internal Regulations, the national stan

22、dards 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, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, S

23、lovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: Wang Bin, na, Thu Sep 14 08:49:11 BST 2006, Uncontrolled Copy, (c) BSIEN 14672:2005 (E) 4 1 Scope This European Standard specifies a procedure for complete digestion of raw/digested sludge, suitable for the subsequent d

24、etermination 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 for ph

25、osphate 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 applica

26、tion 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 anal

27、ytical 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: Determination of

28、 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 includ

29、es 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 (dry m

30、atter) mass of solid obtained after the specified drying process. It is expressed as grams or kilograms EN 12880:2000, 3.3 Licensed Copy: Wang Bin, na, Thu Sep 14 08:49:11 BST 2006, Uncontrolled Copy, (c) BSIEN 14672:2005 (E) 5 4 Principle A boiling mixture of sulfuric and nitric acids oxidises orga

31、nic matter, releasing any phosphorus present and converting it to orthophosphate. 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 w

32、ith the sulfuric acid, causing the mixture to char. Small additions of nitric acid 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 an

33、alysis by method EN ISO 10304-2, EN ISO 6878 or an equivalent validated method. 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

34、and sulfurusing ICP-OES after a suitable nitric acid based digestion, but it is 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 acc

35、ording to EN ISO 10304-2 by ion chromatography can be difficult when sulfate is 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 sl

36、udge samples may contain hazardous and inflammable substances. They shall contain 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 inflammab

37、le and will pressurise sealed bottles. Exploding bottles are likely to result in 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 equ

38、ipment used in the vicinity should be flame proof to avoid any source of ignition. 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.

39、3 Strong acids and alkalis The sulfuric and nitric acids and the sodium hydroxide, 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

40、 Ordinary laboratory apparatus and the following: 7.1 Kjeldahl flask, for example 200 ml nominal capacity or tube, for example 100 ml. 7.2 Heating device, Bunsen burner or heating mantle or suitable heating block. Licensed Copy: Wang Bin, na, Thu Sep 14 08:49:11 BST 2006, Uncontrolled Copy, (c) BSIE

41、N 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 (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 b

42、ottle. 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 preservation Sludge samples can change composition through biological and/or chemical activity. They shall be kept in cool boxes at less

43、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-treatment is to obtain a representative and homogeneous sample. NOTE 1 Sludge may be analysed dried and ground, or as a well-homogenised

44、 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 homogenised mechanically may be used directly. 10 Procedure Weigh sufficient sample (up to 2 g 2 mg dry mass), containing not more than 50

45、 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 flask or tube in a fume cupboard. Continue heating until brown fumes cease to be produced. If the mixture chars, carefully add approxima

46、tely 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 not 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

47、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 sodium hydroxide (8.3), in presence of phenolphthalein (8.4). Quantitatively transfer the solution to a 50 ml volumetric flask, with w

48、ater, make up to volume and mix well. Licensed Copy: Wang Bin, na, Thu Sep 14 08:49:11 BST 2006, Uncontrolled Copy, (c) BSIEN 14672:2005 (E) 7 Analyse the solution for phosphate phosphorus using method EN ISO 6878, EN ISO 10304-2 or equivalent validated method within 4 weeks. A reagent blank without

49、 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 total 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 millil