SVENSK STANDARD SS-EN 1302

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1 SENSK STANDARD SS-EN 30 Handläggande organ Fastställd Utgåva Sida Standardiseringsgruppen STG (+5) Copyright SIS. Reproduction in any for without perission is prohibited. Cheicals used for treatent of water intended for huan consuption Aluiniu-based coagulants Analytical ethods Processkeikalier för beredning av dricksvatten Aluiniubaserade koaguleringsedel Analysetoder The European Standard EN 30:999 has the status of a Swedish Standard. This docuent contains the official English version of EN 30:999, Cheicals used for treatent of water intended for huan consuption Aluiniu-based coagulants Analytical ethods. The Standard specifies analytical ethods to be used for products described in EN 878, EN 88, EN 88, EN 883, pren 885, pren 886, pren 887 and pren 935. The following technical corrigendu to page 9 has been requested by the responsible Working Group within CEN/TC 64 Drinking Water Treatent: Europastandarden EN 30:999 gäller so svensk standard. Detta dokuent innehåller den officiella engelska versionen av EN 30:999, Cheicals used for treatent of water intended for huan consuption Aluiniu-based coagulants Analytical ethods. Standarden specificerar analysetoder att använda för produkter beskrivna i SS-EN 878, SS-EN 88, SS-EN 88, SS-EN 883 sat i standardförslagen pren 885, pren 886, pren 887 och pren 935. Den ansvariga arbetsgruppen ino CEN/TC 64 Drinking Water Treatent har begärt att följande tekniska rättelser införs i EN 30, sidan 9: Clause A.4.6.: Replace: Punkt A.4.6.: Står: X 4. =0, x c x x 000 = 55,85 x c x X 4. =0, x c x x 000 = 55,85 x c x with: skall vara: X 4. = 6 x 55,85 x c x X 4. = 6 x 55,85 x c x Replace: 0, is the ass, in gras, of Fe corresponding to l of the potassiu dichroate solution c (K Cr O 7 ) = 0,067 ol/l with: 55,85 is the ass, in gras, of one ole of iron Står: 0, is the ass, in gras, of Fe corresponding to l of the potassiu dichroate solution c (K Cr O 7 ) = 0,067 ol/l skall vara: 55,85 is the ass, in gras, of one ole of iron ICS Standarder kan beställas hos SIS so även länar allänna upplysningar o svensk och utländsk standard. Postadress: SIS, Box 6455, 3 8 STOCKHOLM Telefon: Telefax: Upplysningar o sakinnehållet i standarden länas av STG. Telefon: Telefax: E-post: info@stg.se Prisgrupp S Tryckt i oktober 999

2 Sida SS-EN 30:999 Clause A.4.6.: Replace: Punkt A.4.6.: Står: X 4. = 0, x c x x 000 = 55,85 x c x X 4. = 0, x c x x 000 = 55,85 x c x with: skall vara: X 4. = 6 55,85 c x X 4. = 6 55,85 c x Replace: 0, is the ass, in gras, of Fe corresponding to l of the potassiu dichroate solution c (K Cr O 7 ) = 0,067 ol/l with: 55,85 is the ass, in gras, of one ole of iron Står: 0, is the ass, in gras, of Fe corresponding to l of the potassiu dichroate solution c (K Cr O 7 ) = 0,067 ol/l skall vara: 55,85 is the ass, in gras, of one ole of iron Swedish Standards corresponding to docuents referred to in this Standard are listed in Catalogue of Swedish Standards, issued by SIS. The Catalogue lists, with reference nuber and year of Swedish approval, International and European Standards approved as Swedish Standards as well as other Swedish Standards. Motsvarigheten och aktualiteten i svensk standard till de publikationer so onäns i denna standard fragår av Katalog över svensk standard, so ges ut av SIS. I katalogen redovisas internationella och europeiska standarder so fastställts so svenska standarder och övriga gällande svenska standarder.

3 EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN 30 April 999 ICS English version Cheicals used for treatent of water intended for huan consuption - Aluiniu-based coagulants - Analytical ethods Produits chiiques utilisés pour le traiteent de l'eau destinée à la consoation huaine - Coagulants à base d'aluiniu - Méthodes d'analyse Produkte zur Aufbereitung von Wasser für den enschlichen Gebrauch - Flockungsittel auf Aluiniubasis - Analytische Methoden This European Standard was approved by CEN on April 999. CEN ebers are bound to coply 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 ay be obtained on application to the Central Secretariat or to any CEN eber. This European Standard exists in three official versions (English, French, Geran). A version in any other language ade by translation under the responsibility of a CEN eber into its own language and notified to the Central Secretariat has the sae status as the official versions. CEN ebers are the national standards bodies of Austria, Belgiu, Czech Republic, Denark, Finland, France, Gerany, Greece, Iceland, Ireland, Italy, Luxebourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdo. EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG Central Secretariat: rue de Stassart, 36 B-050 Brussels 999 CEN All rights of exploitation in any for and by any eans reserved worldwide for CEN national Mebers. Ref. No. EN 30:999 E

4 Page EN 30:999 Contents Scope...4 Norative references Preparation of the test saple Methods of analysis Expression of results...7 Annexe A (norative) Reference ethods of analysis...8 Annexe B (inforative) Routine ethods...49 Annex C (inforative) Bibliography...5

5 Page 3 EN 30:999 Foreword This European Standard has been prepared by Technical Coittee CEN/TC 64 "Water supply", 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 endorseent, at the latest by October 999, and conflicting national standards shall be withdrawn at the latest by October 999. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to ipleent this European Standard: Austria, Belgiu, Czech Republic, Denark, Finland, France, Gerany, Greece, Iceland, Ireland, Italy, Luxebourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdo.

6 Page 4 EN 30:999 Scope This European standard is applicable to aluiniu-based coagulants used for treatent of water intended for huan consuption. It specifies analytical ethods to be used for products described in EN 878, EN 88, EN 88, EN 883, pren 885, pren 886, pren 887 and pren 935. Norative references This European Standard incorporates by dated or undated reference, provisions fro other publications. These norative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent aendents to or revisions of any of these publications apply to this European Standard only when incorporated in it by aendent or revision. For undated references the latest edition of the publication referred to applies. EN 878, Cheicals used for treatent of water intended for huan consuption - Aluiniu sulfate EN 88, Cheicals used for treatent of water intended for huan consuption - Aluiniu chloride, aluiniu chloride hydroxide and aluiniu chloride hydroxide sulfate (onoeric). EN 88, Cheicals used for treatent of water intended for huan consuption - Sodiu aluinate. EN 883, Cheicals used for treatent of water intended for huan consuption - Polyaluiniu chloride hydroxide and Polyaluiniu chloride hydroxide sulfate. pren 885, Cheicals used for treatent of water intended for huan consuption - Polyaluiniu chloride hydroxide silicate. pren 886, Cheicals used for treatent of water intended for huan consuption - Polyaluiniu hydroxide silicate sulfate. pren 887, Cheicals used for treatent of water intended for huan consuption - Aluiniu-iron (III) sulfate. pren 935, Cheicals used for treatent of water intended for huan consuption - Aluiniu-iron (III) chloride and aluiniu-iron (III) chloride hydroxide (onoeric). EN ISO 3696, Water for analytical use - Specification and test ethods (ISO 3696:987). ISO 5666-:983, Water quality - Deterination of total ercury by flaeless atoic absorption spectroetry - Part : Method after digestion with peranganate-peroxodisulfate.

7 Page 5 EN 30:999 ISO 575-, Accuracy (trueness and precision) of easureent ethods and results Part : Basic ethod for the deterination of repeatability and reproducibility of a standard easureent ethod. ISO 606:979, Cheical products for industrial use Sapling ocabulary. ISO 67:98, Cheical products for industrial use - General ethod for deterination of chloride ions - Potentioetric ethod. ISO 638:98, General ethod for deterination of silicon content - Reduced olybdosilicate spectrophotoetric ethod. 3 Preparation of the test saple 3. Definitions For the purposes of this European Standard, the following definitions apply : 3.. laboratory saple a saple as prepared for sending to the laboratory and intended for inspection or testing [ISO 606:979]. 3.. test saple a saple prepared fro the laboratory saple and fro which test portions will be taken [ISO 606:979] test portion the quantity of aterial drawn fro the test saple (or fro the laboratory saple if both are the sae) and on which the test or observation is actually carried out [ISO 606:979] 3. Procedure Fro the laboratory saple, prepare the test saple by grinding the solid saples until particle size is below,5 and hoogenizing, and hoogenize the liquid saples. 4 Methods of analysis The ethods to be used for analysis of aluiniu-based coagulants and the principles of each ethod are listed in table and described in full in annex A for reference ethods and in annex B for routine ethods. The ethods which are applicable to only soe of the products described in EN 878, EN 879, EN 88, EN 88, pren 885, pren 886, pren 887 and pren 935 are listed in table.

8 Page 6 EN 30:999 Table - Methods of analysis Deterination Method Principle Aluiniu A. a) EDTA coplexoetric titration with EDTA Aluiniu A. Separation of iron, CDTA coplexoetric titration Iron A.3 Atoic absorption spectroetry (flae) Iron A.4 Potentioetric titration Sodiu A.5 Atoic absorption spectroetry (flae) Calciu A.6 Atoic absorption spectroetry (flae) Chloride A.7 Potentioetric titration Sulfate A.8 Bariu sulfate gravietry Silicate A.9 Reduced olybdosilicate spectrophotoetry Free acidity A.0 Acidietric titration Basicity A. Acidietric titration, oxalate ethod Basicity A. Acidietric titration, KF ethod Insoluble atter A.3 Gravietry Arsenic A.5 Inductively coupled plasa optical eission spectroetry (ICP/OES) (hydride) Cadiu A.4 Inductively coupled plasa optical eission spectroetry (ICP/OES) Chroiu A.4 Inductively coupled plasa optical eission spectroetry (ICP/OES) Mercury A.6 Atoic absorption spectroetry (flaeless) Nickel A.4 Inductive coupled plasa optical eission spectroetry (ICP/OES) Lead A.4 Inductive coupled plasa optical eission spectroetry (ICP/OES) Antiony A.5 Inductively coupled plasa optical eission spectroetry (ICP/OES) (hydride) Seleniu A.5 Inductive coupled plasa optical eission spectroetry(icp/oes) (hydride) a) Only applicable for deterination of aluiniu in EN 88 for low iron grades or other grades. Table - Applicability ethods of analysis EN/prEN Aluiniu A./A. A. A. A. A. A. A. A. Aluiniu Fe/Al < 0,0 % (/) A. A. A. A. A. Iron A.3/A.4 A.3 A.3 A.3 A.3 A.3 A.4 A.4 Sodiu A5 A.5 Calciu A.6 A.6 A.6 Chloride A.7 A.7 A.7 A.7 Sulfate A.8 A.8 A.8 A.8 A.8 Silicate A.9 A.9 Free acidity A.0 A.0 A.0 A.0 Basicity Oxalate ethod. A. A. A. A. A. A. Basicity A. A. KF ethod. NOTE : The ethod given in B. should only be used for deterination of basicity by calculation ethod in EN 883, pren 885 and pren 886.

9 Page 7 EN 30:999 5 Expression of results 5. Aluiniu content The aluiniu content shall be expressed as Al. The following equation gives the aluiniu content expressed as aluina (Al O 3 ) : 0 AlO3 (Al) Repeatability Each laboratory shall calculate the repeatability of the ethod under their laboratory conditions according to the procedure defined in ISO 575-.

10 Page 8 EN 30:999 Annexe A (norative) Reference ethods of analysis A. Deterination of aluiniu (EDTA coplexoetric ethod) A.. General This ethod is applicable for the deterination of aluiniu in aluiniu-based coagulants used for treatent of water intended for huan consuption, - as the reference ethod for products described in EN 878 (iron free grade) and EN 88 ; - as a routine ethod for products described in EN 878 (low iron grade), EN 88, EN 883, pren 885, pren 886 and pren 935 containing no ore than 0 g of Fe per kilogra of aluiniu. A.. Principle Dissolution in water, in the case of solid products, or dilution with water in the case of products in solution, of a test saple. Coplexation of aluiniu, in a hot acidic ediu with an excess of ethylenediainetetraacetic acid (EDTA) solution. Titration of the excess EDTA with a standard voluetric solution of zinc in the presence of xylenol orange as indicator. Al 3+ + EDTA 4- --> AlEDTA - Zn + + EDTA 4- --> ZnEDTA - A..3 Reagents All reagents shall be of a recognized analytical grade and the water used shall confor to grade 3 in accordance with EN ISO A..3. A..3. Sodiu acetate solution, 80 g/l. Sodiu hydroxide solution, 00 g/l. A..3.3 Hydrochloric acid : Dilute one volue of hydrochloric acid (p =,9 g/l) with one volue of water. A..3.4 Hydrochloric acid, 36,5 g/l, c(hcl) = ol/l. A..3.5 Disodiu ethylenediainetetraacetate dihydrate (NaEDTA), standard voluetric solution, c(c 0 H 4 N O 8 Na.H O) = 0,05 ol/l. Weigh to the nearest 0,000 g, 8,65 g of NaEDTA. Dissolve in water, transfer the solution quantitatively to a 000 l voluetric flask. Dilute to volue with water and hoogenize.

11 Page 9 EN 30:999 NOTE : Coercial standard voluetric solution could be used. A..3.6 Zinc, standard voluetric solution, c(zn) = 0,05 ol/l. Weigh to the nearest 0,000 g, 6,537 0 g( )of pure zinc (iniu content 99,9 % (/)). Dissolve in 60 l of hydrochloric acid solution (A..3.3). During the reaction, cover the beaker with a watch-glass. At the end of the reaction, boil the solution for 0 in, then cool to roo teperature. Dilute to about 500 l with water and add sodiu acetate solution (A..3.) until a ph of 5,5 ± 0, is obtained. Transfer the solution quantitatively to a 000 l voluetric flask. Dilute to volue with water and hoogenize. NOTE : if the ass of zinc is not exactly that stated above, the zinc concentration is given by the equation : c(zn) 65,37 where : is the ass in gras of zinc weighed ; 65,37 is the relative olecular ass of zinc ; c(zn) is the concentration of zinc solution, in oles per litre, calculated to the fourth significant figure. NOTE : Coercial standard solution could be used. A..3.7 Buffer solution, ph 5,5. Weigh 50 g of sodiu acetate trihydrate (CH 3 COONa.3H O). Dissolve in 500 l of water and add glacial acetic acid (CH 3 COOH) until a ph of 5,5 ± 0, is obtained. A..3.8 Xylenol orange. Grind,0 g of xylenol orange with 99 g of potassiu nitrate in a ortar until an hoogeneous ass is obtained. A..4 Apparatus Ordinary laboratory apparatus and glassware, and optionally : A..4. A..4. Autoatic titrator and photoeter with fibre optic probe. Microwave equipent. A..5 A..5. Procedure Preparation of the test solution Weigh, to the nearest 0,00 g, about 5 g of the test saple ( 0 ) into a 400 l beaker. Add approxiately 50 l of water at 80 C to 90 C. Stir until dissolved, using a glass stirrer. Transfer quantitatively to a 500 l voluetric flask. Dilute to volue with water and hoogenize. Filter if necessary through a filter paper (particle retention size,5 ) (test solution 0 ). Place l of this solution (see table A.) into a 00 l voluetric flask. Dilute to volue with water and hoogenize (diluted test solution ).

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