EG FORTISCHEM ENERGOCHEMICA COMPANY STANDARD Revision: 0 SODIUM HYPOCHLORITE TECHNICAL PN 10-017-14 KP 24.13.22 This company standard is valid for the production, testing and delivery of Sodium hypochlorite technical. 1. IN GENERAL 1.1 CAS number: 7681-52-9 EINECS number: 231-668-3 1.2. Sodium hypochlorite technical (thereinafter Sodium hypochlorite) is water solution of sodium hypochlorite and sodium chloride with the content of sodium carbonate, sodium hydroxide and sodium chlorate. Chemical formula: Naocl Relative molecular weight: 74,5 g.mol™ 1.3. Sodium hypochlorite is produced by chlorine absorption in diluted sodium hydroxide solution, 1.4 Sodium hypochlorite is yellow-green, clear or slightly cloudy liquid, decomposes spontaneously during transport and storage during which time reducing the active chlorine content. The decomposition accelerates heat, light and catalytic activity of the metals (nickel, copper, iron, etc). 1.5 Sodium hypochlorite is widely used in various industries, in consumers and in widely community as an oxidizer and bleaching agent, dyeing and textile treatment, cleaning and washing, disinfection and water treatment, etc. 2. TECHNICAL PARAMETERS Sodium hypochlorite must comply with the following technical requirements: Parameter Unit Value Test method Content of active chlorine, min. in winter g/l 150__| FCH-PP-7-21-2014 Content of active chlorine, min. in summer” 7 140__| FCH-PP-7-21-2014 Content of sodium hydroxide, max. g/l 12 FCH-PP-7-21-2014 ‘Supply: PND 10-017-12 from 01.08.2012 Approved: Ing. Tibor Ziak Ing. Jaroslav Horak Head of Qualty Management and Cgntroling | Head of Technology ca aa ee | A Lio € pater EG. oL019 putes 2: 6 OKE( FORTISCHEM QE ENERGOCHEMICA em SGSSGS_ “en SOS Page: 2/7 Content of sodium carbonate, max. g/l 4 FCH-PP-7-21-2014 Content of iron, max. ell 0,008 | FCH-PP-7-21-2014 “For the summer period is the period from 01/05 to 30/09 of calendar year. 3. SAMPLING AND TESTING 3.1 Sampling ‘The sampling is performed according to STN 65 0512. Only 500 ml of fractional sample is taken from each tank. 3.2 Testing 3.2.1 Determination of active chlorine content 3.2.1.1 Principle of determination Active chlorine will release iodine from potassium iodide solution. The released iodine is titrated with a standard solution of sodium thiosulphate. 3.2.1.2 Chemicals and materials . acetic acid 99 % (p = 1,0525 g.cm-3), diluted 1:3, or HCl p. a. diluted 1:1 . potassium iodide, 10 % solution, new prepared . sodium thiosulfate, the volumetric solution c(NazS203) = 0,1 mol/I starch solution volumetric flasks capacity 500 ml titration flasks capacity 250 ml pipettes capacity 10 mi, 20 ml, 25 ml automatic burette capacity 50 ml, graduated at 0,1 ml intervals 3.2.1.3 Procedure for determination 25 ml of the sample is pipetted into 500 ml volumetric flask and filled up to the line with destilled water. After mixing, 20 ml from this solution is pipetted into 250 mI titration flask, 20 ml of potassium iodide and 10 ml of acetic acid are added. The released iodine is titrated with sodium thiosulfate to a bright-yellow color. 2 mi of starch solution is added and titrated till the solution becomes colorless. 3.2.1.4 Calculation The content of active chlorine (X) in g/l is given by the formula: z 500 = fx bx 01x 35,453 x zxV 25x20 fxbeqxMxE( FORTISCHEM Qn ENERGOCHEMICA S68 “mm SOS Page: 3/7 X = 3,545 x fx b where f is factor of Na,S,0; volumetric solution consumption of Na;S;0; volumetric solution in ml concentration of Na,S.Os volumetric solution (c = 0,1 mol.) chlorine molecular weight (M = 35,453 g.mol*) stock solution volume in ml sample volume in ml stock solution volume pipetted for determination in ml < Nzoo 3.2.2 Determination of sodium hydroxide content 3.2.2.1 Principle of determination The sample is decomposed by hydrogen peroxide and sodium hydroxide is determined by titration with volumetric solution of hydrochloric acid. 3.2.2.2 Chemicals and materials hydrochloric acid, volumetric solution e(HCl) = 0,1 mol/|, hydrogen peroxide, 30 % solution (p = 1,11 g.cm-3), neutral, barium chloride p. a., phenolphthalein solution, destilled water, denatured alcohol, titration flasks capacity 250 ml, pipettes capacity 10 ml, 20 ml, 25 ml, automatic burette 50 mi * analytical balance capable of weighing to 0,0001 g 3.2.2.3 Procedure for determination 10 ml of the sample is pipetted into 250 ml of titration vessel and diluted with 40 ml of water. During mixing hydrogen peroxide solution is added as long as the sample is decomposed during effervescence. 5 ~ 10 g of barium chloride and 5 drops of phenolphthalein are added and during constant mixing the solution is dropwise titrated with HCI volumetric solution till the solution becomes colorless. 3.2.2.4 Calculation The content of sodium hydroxide (X) in g/| is given by the formul fxaxcxM fx ax 01x 40 X= > — sc oaxaxt v 10EG FORTISCHEM ENERGOCHEMICA where f is factor of HCl volumetric solution 2 consumption of HCI volumetric solution in ml 1 _concetration of HCl volumetric solution (c; = M NaOH molecular weight (M = 40,0 g.mo!'') V_ sample volume in mi 1 mol), 3.2.3. Determination of sodium carbonate content 3.2.3.1 Principle of determination Sodium carbonate content is determined by titration with HCl volumetric solution. 3.2.3.2 Chemicals and materials hydrochloric acid, volumetric solution c(HCl) = 0,1 mol/l hydrogen peroxide, 30 % solution (p = 1,11 g.cm’), neutral methyl orange solution destilled water denatured alcohol titration flasks capacity 250 ml pipettes capacity 10 ml, 20 ml, 25 ml automatic burette capacity 50 ml 3.2.3.3 Procedure for determination 10 ml of the sample is pipetted into 250 ml of titration vessel and diluted with 40 ml of water. During mixing hydrogen peroxide solution is added as long as the sample is decomposed during effervescence. 5 ml of methyl orange is added and titrated dropwise with HCI volumetric solution till the first orange-coloured. 3.2.4.4 Calculation The content of sodium carbonate (X) in g/I is given by the formula: fx(b-a)xaxM f x (b - a) x01 x 53 X= $$ = ——____________ = 053 x f x (b - a) v 10 where f is factor of HCl volumetric solution b HCI volumetric solution consumption to methyl orange in ml 2 HCI volumetric solution consumption to phenolphthalein in ml (in NaOH determination) concentration of entry HCI volumetric solution (c; = 0,1 mol.) M —_Na2CO3 molecular weight (M (NazCOs) = 53 g.mol"], V___ sample volume (V = 10 ml)E( FORTISCHEM © ENERGOCHEMICA on SCS Page: 5/7 3.2.4 Determination of iron content 3.2.4.1 Principle of determination Fe” is formed by oxidation Fe” with hydrogen peroxide. Fe” with potassium thiocyanate formed red coloration and the color intensity is measured spectrophotometrically. 3.2.4.2 Chemicals and materials * hydrochloric acid, diluted (1:1) hydrogen peroxide, 30 % solution potassium thiocyanate, 20 % solution iron reference solution with concentration of 1 g.!* destilled water volumetric flask capacity 100 ml beaker capacity 250 ml spectrophotometer with accessories * analytical balance capable of weighing to 0,0001 mg * pipette capacity 10 ml © measuring cylinder cap: ry 50 mI 3.2.4.3 Procedure for determination 10 ml of the sample is pipetted into a beaker of 250 ml. 40 ml of destilled water is added During mixing, hydrogen peroxide solution (3 ml to 5 ml) is added dropwise as long as the sample decomposes with effervescence. 10 ml of HCI is added, boiled for about 5 minutes and after cooling, the solution is quantitatively transferred into a volumetric flask of 100 ml. Next, 10 ml of Potassium thiocyanate solution is added, filled up to the line with water and mixed well. After 10 min. the color intensity is measured by spectrophotometer at a wavelength of 470 nm against the blank (thiocyanate, peroxide, destilled water). The iron content in mg is read from the measured absorbance from the calibration graph. NOTE: Spectrophotometer is regularly (at least 1 per year) calibrated to the required concentration range. At the same time, a calibration curve is constructed, where the Fe content is on the x-axis in 100 ml volumetric flasks and absorbance on the y-axis 3.2.4.4 Calculation The content of iron (X) in % is given by the formula a = O1lxa vE( FORTISCHEM ENERGOCHEMICA Page: 6/7 where A is measured absorbance v sample volume in ml a the Fe** amount which is read from calibration curve in mg k slope of a straight line (concentration of Fe” in dependence on absorbance) 4. PACKAGING, TRANSPORT, LABELLING AND STORAGE 4.1 Sodium hypochlorite is delivered in rubberized tanks, polyethylene or polypropylene IBC containers or other, in advance agreed wrapping materials resistant to effects of sodium hypochlorite. Used tanks are assigned only for transport of goods and not for its storage. The due- time emptying and returning of FORTISCHEM’s railway wagons is at most 4 days after the arrival of ‘the wagon on the delivery track of the buyer. 4.2 Each pack unit must be labelled with the following informations: a) producer name b) product name c) net weight d) production date e) number of standard 4.3. During transport and storage, there is a decrease in the content of active chlorine. Authoritative is the sample analysis, which was collected by the manufacturer on the day of expedition 4.4 Sodium hypochlorite technical is stored in rubberized iron tanks or titanous, polyethylene, polypropylene resistant to effects of sodium hypochlorite. The recommended storage temperature is max. 20°C. At higher temperatures the decomposition is accelerated. 5, SAFETY STATEMENT Detailed data are mentioned in Safety Data Sheet. 6. STANDARDS QUOTED STN 650512 Sampling of liquids Designed: URKK - Ing. Jana Sevcova, Specialist for Standardization