SIST EN 12678:2016

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kemikalije, ki se uporabljajo za pripravo pitne vode - Kalijev peroksomonosulfatProdukte zur Aufbereitung von Wasser für den menschlichen Gebrauch - KaliumperoxomonosulfatProduits chimiques utilisés pour le traitement de l'eau destinée à la consommation humaine - Peroxomonosulfate de potassiumChemical used for treatment of water intended for human consumption - Potassium peroxomonosulfate71.100.80Chemicals for purification of water13.060.20Pitna vodaDrinking waterICS:Ta slovenski standard je istoveten z:EN 12678:2016SIST EN 12678:2016en,fr,de01-julij-2016SIST EN 12678:2016SLOVENSKI
STANDARDSIST EN 12678:20081DGRPHãþD



SIST EN 12678:2016



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 12678
May
t r s x ICS
y sä s r rä z r Supersedes EN
s t x y zã t r r zEnglish Version
Chemical used for treatment of water intended for human consumption æ Potassium peroxomonosulfate Produits chimiques utilisés pour le traitement de l 5eau destinée à la consommation humaine æ Peroxomonosulfate de potassium
Produkte zur Aufbereitung von Wasser für den menschlichen Gebrauch æ Kaliumperoxomonosulfat This European Standard was approved by CEN on
s z March
t r s xä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey andUnited Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
9
t r s x CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s t x y zã t r s x ESIST EN 12678:2016



EN 12678:2016 (E) 2 Contents Page European foreword . 4 Introduction . 5 1 Scope . 6 2 Normative references . 6 3 Description . 6 3.1 Identification . 6 3.1.1 Chemical name . 6 3.1.2 Synonym or common name . 6 3.1.3 Relative molecular mass . 6 3.1.4 Empirical formula of triple salt . 6 3.1.5 CAS Registry Number . 7 3.1.6 EINECS reference . 7 3.2 Commercial form . 7 3.3 Physical properties of triple salt . 7 3.3.1 Appearance and odour . 7 3.3.2 Density . 7 3.3.3 Solubility in water . 7 3.3.4 Vapour pressure . 7 3.3.5 Boiling point at 100 kPa . 7 3.3.6 Melting point . 7 3.3.7 Specific heat . 7 3.3.8 Viscosity (dynamic) . 7 3.3.9 Critical temperature . 7 3.3.10 Critical pressure . 8 3.3.11 Physical hardness . 8 3.4 Chemical properties . 8 4 Purity criteria . 8 4.1 General . 8 4.2 Composition of commercial product . 8 4.3 Impurities and main by-products . 8 4.4 Chemical parameters . 8 5 Test methods . 9 5.1 Sampling . 9 5.2 Analysis . 9 5.2.1 Determination of potassium peroxomonosulfate (KHSO5) (active ingredient) . 9 5.2.2 Chemical parameters . 12 6 Labelling - Transportation - Storage . 14 6.1 Means of delivery . 14 6.2 Labelling according to the EU Legislation
.......................................................................................... 15 6.3 Transportation regulations and labelling ........................................................................................... 15 6.4 Marking ............................................................................................................................................................ 15 6.5 Storage ............................................................................................................................................................. 15 6.5.1 Generals ........................................................................................................................................................... 15 6.5.2 Long term stability ....................................................................................................................................... 15 SIST EN 12678:2016



EN 12678:2016 (E) 3 6.5.3 Storage incompatibilities . 16 Annex A (informative)
General information on potassium peroxomonosulfate . 17 A.1 Origin . 17 A.1.1 Raw materials . 17 A.1.2 Manufacturing process . 17 A.2 Use . 17 A.2.1 Function . 17 A.2.2 Form in which it is used. 17 A.2.3 Treatment dose . 17 A.2.4 Means of application . 17 A.2.5 Secondary effects . 17 A.2.6 Removal of excess product . 18 Annex B (normative)
General rules relating to safety . 19 B.1 Rules for safe handling and use . 19 B.2 Emergency procedures . 19 B.2.1 First aid . 19 B.2.2 Spillage . 19 B.2.3 Fire . 19 Annex C (normative)
Determination of arsenic, antimony and selenium (atomic absorption spectrometry hydride technique) . 20 C.1 Safety precautions . 20 C.2 General principle . 20 C.3 Interferences . 20 C.4 Reagents . 20 C.5 Apparatus . 22 C.6 Procedure . 24 C.6.1 Preparation of the apparatus . 24 C.6.2 Preparation of calibration solutions . 24 C.6.3 Preparation of test solutions and standard solutions . 24 C.6.4 Determination of arsenic with sodium borohydride . 24 C.6.5 Determination of selenium with sodium borohydride . 25 C.6.6 Determination of antimony with sodium borohydride . 25 C.7 Calculation. 25 Bibliography . 26
SIST EN 12678:2016



EN 12678:2016 (E) 4 European foreword This document (EN 12678:2016) has been prepared by Technical Committee CEN/TC 164 “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 endorsement, at the latest by November 2016, and conflicting national standards shall be withdrawn at the latest by November 2016. 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 patent rights. This document supersedes EN 12678:2008. Significant technical difference between this edition and EN 12678:2008 is as follows: — deletion of reference to EU Directive 67/548/EEC of June 27, 1967 in order to take into account the latest Regulation in force (see [3]). According to the CEN/CENELEC Internal Regulations, the national standards 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, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 12678:2016



EN 12678:2016 (E) 5 Introduction In respect of potential adverse effects on the quality of water intended for human consumption, caused by the product covered by this European Standard: a) this European Standard provides no information as to whether the product may be used without restriction in any of the Member States of the EU or EFTA; b) it should be noted that, while awaiting the adoption of verifiable European criteria, existing national regulations concerning the use and/or the characteristics of this product remain in force. NOTE 1 Conformity with this European Standard does not confer or imply acceptance or approval of the product in any of the Member States of the EU or EFTA. The use of the product covered by this European Standard is subject to regulation or control by National Authorities. NOTE 2 This product is a biocide and needs to comply with the relevant legislation in force. In the European Union, at the time of publication, this legislation is REGULATION (EU) No 528/2012 [1]). SIST EN 12678:2016



EN 12678:2016 (E) 6 1 Scope This European Standard is applicable to potassium peroxomonosulfate used for treatment of water intended for human consumption. It describes the characteristics of potassium peroxomonosulfate and specifies the requirements and the corresponding test methods for potassium peroxomonosulfate. It gives information on its use in water treatment. 2 Normative references The following documents, in whole or in part, are normatively 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 1233, Water quality — Determination of chromium — Atomic absorption spectrometric methods EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696) EN ISO 12846, Water quality — Determination of mercury — Method using atomic absorption spectrometry (AAS) with and without enrichment (ISO 12846) ISO 3165, Sampling of chemical products for industrial use — Safety in sampling ISO 6206, Chemical products for industrial use — Sampling — Vocabulary ISO 8213, Chemical products for industrial use — Sampling techniques — Solid chemical products in the form of particles varying from powders to coarse lumps ISO 8288, Water quality — Determination of cobalt, nickel, copper, zinc, cadmium and lead — Flame atomic absorption spectrometric methods 3 Description 3.1 Identification 3.1.1 Chemical name Potassium peroxomonosulfate triple salt. 3.1.2 Synonym or common name Potassium peroxomonosulfate, Potassium monopersulfate, Potassium hydrogenperoxomonosulfate, Pentapotassium-bis(peroxomonosulfate)bis(sulfate). 3.1.3 Relative molecular mass Triple salt: 614,76. (Active ingredient KHSO5: 152,17). 3.1.4 Empirical formula of triple salt K5H3S4O18 (2 KHSO5. KHSO4. K2SO4). Active ingredient KHSO5. SIST EN 12678:2016



EN 12678:2016 (E) 7 3.1.5 CAS Registry Number1) 70693-62-8. 3.1.6 EINECS reference2) 274-778-7. 3.2 Commercial form Potassium peroxomonosulfate as commercial product exists as a triple salt comprising potassium peroxomonosulfate (2KHSO5) potassium hydrogen sulfate (KHSO4) and potassium sulfate (K2SO4). 3.3 Physical properties of triple salt 3.3.1 Appearance and odour The product is white, odourless, granular, free-flowing salt. 3.3.2 Density The bulk density of the product is approximately between 1 g/cm3 and 1,2 g/cm3. 3.3.3 Solubility in water The solubility of the product is: — approximately 250 g/l at 20 °C; — approximately 300 g/l at 50 °C; — approximately 330 g/l at 70 °C. 3.3.4 Vapour pressure Not applicable. 3.3.5 Boiling point at 100 kPa3) Not applicable. 3.3.6 Melting point The product decomposes above 60 °C. 3.3.7 Specific heat Not applicable. 3.3.8 Viscosity (dynamic) Not applicable. 3.3.9 Critical temperature Not applicable.
1) Chemical Abtracts Service Registry Number. 2) European Inventory of Existing Commercial Chemical Substances. 3) 100 kPa = 1 bar SIST EN 12678:2016



EN 12678:2016 (E) 8 3.3.10 Critical pressure Not applicable. 3.3.11 Physical hardness Not applicable. 3.4 Chemical properties Potassium peroxomonosulfate is a powerful oxidizing agent. Aqueous solutions of the product exhibit a strongly acid reaction; a mass fraction solution of 3 % has a pH value of 2 at 20 °C. The standard reduction potential E0 of potassium peroxomonosulfate for the reaction: HSO5- + 2H+ + 2e-  HSO4- + H2O
(1) is: + 1,82 V at 25°C 4 Purity criteria 4.1 General This European Standard specifies the minimum purity requirements for potassium peroxomonosulfate used for the treatment of water intended for human consumption. Limits are given for impurities commonly present in the product. Depending on the raw material and the manufacturing process other impurities may be present and, if so, this shall be notified to the user and when necessary to the relevant authorities. Users of this product should check the national regulations in order to clarify whether it is of appropriate purity for treatment of water intended for human consumption, taking into account raw water quality, required dosage, contents of other impurities and additives used in the product not stated in the product standard. Limits have been given for impurities and chemicals parameters where these are likely to be present in significant quantities from the current production process and raw materials. If the production process or raw materials leads to significant quantities of impurities, by-products or additives being present, this shall be notified to the user. 4.2 Composition of commercial product The commercial product shall contain KHSO5 (potassium peroxomonosulfate) at a mass fraction greater than 45 percent or the manufacturer’s declared values. Typical composition in mass fraction should be approximately: 45 % potassium peroxsomonosulfate (KHSO5), 25 % potassium hydrogen sulfate (KHSO4), and 30 % potassium sulfate (K2SO4). 4.3 Impurities and main by-products See 4.1. 4.4 Chemical parameters NOTE For the purpose of this European Standard, “chemical parameters” are those defined in the EU Directive 98/83/EC of 3 November 1998 (see [2]). The content of chemical parameters shall conform to the requirements specified in Table 1. SIST EN 12678:2016



EN 12678:2016 (E) 9 Table 1 — Chemical parameters Parameter Limit (mg/kg of dry product) Type 1 Type 2 Arsenic (As) max. 2 10 Cadmium (Cd) max. 1 10 Chromium (Cr) max. 0,4 10 Mercury (Hg) max. 4 8 Nickel (Ni) max. 1 10 Lead (Pb) max. 2 10 Antimony (Sb) max. 10 10 Selenium (Se) max. 10 10 NOTE Cyanide is usually not relevant in a strong oxidizing medium. Pesticides and polycyclic aromatic hydrocarbons are not by-products of the manufacturing process. 5 Test methods 5.1 Sampling Observe the general recommendations of ISO 3165 and take ISO 6206 into account. Prepare the laboratory sample(s) required by the relevant procedure described in ISO 8213. 5.2 Analysis 5.2.1 Determination of potassium peroxomonosulfate (KHSO5) (active ingredient) 5.2.1.1 Principle Iodometric titration with sodium thiosulfate standard volumetric solution in sulfuric acid medium. The method depends on the oxidizing action of the peroxomonosulfate ion (HSO5-) on iodide ions, Formula (2) and the subsequent determination of iodine formed, through the reducing agent sodium thiosulfate, Formula (3). The inflection point of the potentiometric titration is located around 250 mV (reference to Ag/AgCl-Electrode). HSO5- + 3 Kl + H2SO4 \ HSO4- + Kl3 + K2SO4 + H2O (2) Kl3 + 2 Na2S2O3 \ Kl
ª
t Nal
ª Na2S4O6 (3) 5.2.1.2 Reagents All reagents shall be of a recognized analytical grade and the water used shall conform to grade 3 in accordance with EN ISO 3696. SIST EN 12678:2016



EN 12678:2016 (E) 10 5.2.1.2.1 Sulfuric acid solution, mass fraction 25 %. Place 750 ml of water in a heat resistant beaker (volume 2 000 ml). Measure 135 ml of sulfuric acid, mass fraction 98 % , and dilute in the water by small additions and under gentle stirring. Cover the beaker with a watch glass and keep it for several hours in a safe place to cool. WARNING — During dilution the solution becomes very hot. 5.2.1.2.2 Hydrochloric acid solution, mass fraction 10 %. 5.2.1.2.3 Potassium iodide solution, mass fraction 30 %. Weigh, to the nearest 0,1 g, 60 g of potassium iodide, iodate-free grade, and dissolve it in 140 ml of water. Keep the solution in a dark place. 5.2.1.2.4 Starch solution, mass fraction 1 %. Weigh 1,00 g of soluble starch and make a slurry with 5 ml of water. Add 95 ml of water to the slurry and boil for several minutes to dissolve it. Cool the solution. This solution needs refrigeration to avoid decomposition of the starch which results in a vague end point. Keep the solution cool and use it within one week. Commercial starch solutions as indicators for iodine titration exist and may be used in place of the specified starch solution provided that their efficiency has been previously tested. 5.2.1.2.5 Potassium iodate (KIO3). 5.2.1.2.6 Sodium thiosulfate standard volumetric solution, c(Na2S2O3.5H2O) = 0,1 mol/l. Standard volumetric solutions of sodium thiosulfate are commercially available. Alternatively a standard volumetric solution may be prepared by the following procedure: Dissolve 24,8 g Na2S2O3 . Five H2O in a 1 000 ml one-mark volumetric flask in about 0,75 l water. After the temperature has equalized make up to the mark with water and mix thoroughly. To standardize: Weigh, to the nearest 0,1 mg, 3,600 g (m) of dry potassium iodate. Dissolve in water in a 1 000 ml one-mark volumetric flask, make up to the mark with water and mix (standard reference solution c(1/6 KIO3) = 0,1 mol/l). Place 200 ml of water in a 500 ml stoppered conical flask, add (2 ± 0,5) g of potassium iodide and stir to dissolve. Then introduce, by means of a pipette, 10,0 ml of sodium thiosulfate solution for standardization, add (15 ± 1) ml of hydrochloric acid solution (diluted 1 + 1 by volume) and (5 ± 1) ml of starch solution (5.2.1.2.4). Titrate immediately with the potassium iodate standard reference solution until the appearance of a blue coloration persisting for at least 30 s occurs. Record the volume (V1) of iodate used. The actual concentration, c, of the sodium thiosulfate standard volumetric solution (Na2S2O3.5H2O), expressed in moles per litre, is given by the following formula: ×=11VccV (4) where c1 is the concentration, expressed in moles per litre, of the potassium iodate standard reference solution [c(1/6 KIO3) = 0,1 mol/l ]; V is the volume, in millilitres, of the sodium thiosulfate standard volumetric solution used for the standardization (V = 10 ml); V1 is the volume, in millilitres, of potassium iodate standard reference solution used in the SIST EN 12678:2016



EN 12678:2016 (E) 11 titration. 5.2.1.3 Apparatus Ordinary laboratory apparatus and glassware together with the following: 5.2.1.3.1 Potentiometric titrimeter. 5.2.1.3.2 Automatic burette, volume 50 ml, equipped with an injection tip (made of brown glass). 5.2.1.3.3 Electromechanical stirrer. 5.2.1.3.4 Glass titration beaker, capacity 250 ml (made of brown glass). 5.2.1.3.5 Platinum-Ag/AgCl combination electrode with electrolytic junction with built-in diaphragm. 5.2.1.4 Procedure 5.2.1.4.1 Test solution Weigh, to the nearest 0,1 mg, a test portion of approximately 0,7 g (m) into a dry, clean beaker (5.2.1.3.4). Add 20 ml of potassium iodide solution (5.2.1.2.3) and 10 ml of sulfuric acid (5.2.1.2.1). After dissolution under gentle stirring cover the beaker with a watch glass and keep the solution in the dark for 30 min. Then add 100 ml of water. 5.2.1.4.2 Determination Input the calculation data in the titration microprocessor in accordance with the instruction manual. Place the electrodes in the titration beaker and titrate with the sodium thiosulfate solution (5.2.1.2.6). Record the titration curve and determine the inflection point as the equivalent point of the potentiometric titration. 5.2.1.5 Expression of results The potassium peroxomonosulfate (KHSO5) content, C1, expressed as a percentage by mass, is given by the following formula: ××=1761V
c
,C
m
(5) where V is the volume, expressed in millilitres, of the sodium thiosulfate standard volumetric solution (5.2.1.2.6) used for the titration; c is the concentration, in moles per litre, of the sodium thiosulfate solution (5.2.1.2.6) ; m is the mass of the test portion, expressed in grams. 76,1 is the mass in grams of KHSO5 corresponding to 1 000 ml of sodium thiosulfate c(Na2S2O3.5H2O) = 0,1mol/l. SIST EN 12678:2016



EN 12678:2016 (E) 12 5.2.1.6 Repeatability limit The absolute difference between two single test results, obtained under repeatability conditions, shall not be greater than the repeatability value, r, as calculated from the following formula: r = 0,001 z (6) where z is the mean of the two results, expressed in mass fraction %. NOTE Repeatibility conditions are conditions where mutually independant test results are obtained with the same method on identical test material in the same laboratory by the same operator using the same equipment within short intervals of time. 5.2.2 Chemical parameters 5.2.2.1 Determination of antimony (Sb), arsenic (As), cadmium (Cd), chromium (Cr), lead (Pb), nickel (Ni) and selenium (Se) 5.2.2.1.1 Principle The elements arsenic, antimony, cadmium, chromium, lead, nickel and selenium are determined b
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