EN 12485:2010

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kemikalije, ki se uporabljajo za pripravo pitne vode - Kalcijev karbonat, visoko kalcijevo apno in polžgan dolomit, magnezijev oksid in kalcij-magnezijev karbonat - Preskusne metodeProdukte zur Aufbereitung von Wasser für den menschlichen Gebrauch - Calciumcarbonat, Weißkalk und halbgebrannter Dolomit - Analytische VerfahrenProduits chimiques utilisés pour le traitement de l'eau destinée à la consommation humaine - Carbonate de calcium, chaux et dolomie semi calcinée - Méthodes d'analyseChemicals used for treatment of water intended for human consumption - Calcium carbonate, high-calcium lime and half-burnt dolomite, magnesium oxide and calcium magnesium carbonate - Test methods71.100.80Chemicals for purification of water13.060.20Pitna vodaDrinking waterICS:Ta slovenski standard je istoveten z:EN 12485:2010SIST EN 12485:2011en,fr,de01-november-2011SIST EN 12485:2011SLOVENSKI
STANDARDSIST EN 12485:20011DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 12485
April 2010 ICS 71.100.80 Supersedes EN 12485:2001English Version
Chemicals used for treatment of water intended for human consumption - Calcium carbonate, high-calcium lime, half-burnt dolomite, magnesium oxide and calcium magnesium carbonate -Test methods
Produits chimiques utilisés pour le traitement de l'eau destinée à la consommation humaine - Carbonate de calcium, chaux et dolomie semi calcinée - Méthodes d'analyse
Produkte zur Aufbereitung von Wasser für den menschlichen Gebrauch - Calciumcarbonat, Weißkalk, halbgebrannter Dolomit, Magnesiumoxid und Calciummagnesiumcarbonat - Analytische Verfahren This European Standard was approved by CEN on 18 March 2010.
CEN members are bound to comply 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 may be obtained on application to the CEN Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official versions.
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Analytical scheme . 60Annex B (informative)
Table B.1: Precision data for the test methods . 66Bibliography . 67 SIST EN 12485:2011

The requirement values for free MgO and free Mg(OH)2 in half-burnt dolomite shall be expressed as free MgO in accordance with EN 1017. The same requirement is related to free CaO. The requirement value for MgO in magnesium oxide shall be expressed as MgO in dry substance in accordance with prEN 16004. Therefore, SIST EN 12485:2011

For the determination of the water-soluble content of high-calcium lime, the method in 6.5 is considered as the reference method. The sugar method described in 6.6 can be used as an alternative method if it is demonstrated that the results obtained with this method are equivalent to those of the reference method.
Table 1 — Methods for analysis Determination Method Principle Standard Screen oversize 4.1 Air-jet sieving EN 12518
4.2 Wet sieving EN 12518 Free water 6.1 Gravimetry EN 1018, EN 12518, prEN 16003 Loss on ignition at 450 °C 6.2 Gravimetry EN 1017, EN 12518, prEN 16004 Carbon dioxide 6.3 Gravimetry EN 1017, EN 12518, prEN 16004 Residue insoluble in hydrochloric acid 6.4 Acidimetry, Gravimetry EN 1018, prEN 16004 Water-soluble calcium oxide or calcium hydroxide 6.5 Acidimetric titration EN 12518 Sugar-soluble calcium oxide or calcium hydroxide 6.6 Acidimetric titration EN 12518 Water-insoluble constituents 6.7 Gravimetry EN 12518 Free calcium oxide 6.8 Extraction, acidimetric titration EN 1017, prEN 16004 Calcium oxide and magnesium oxide 6.9 Complexometric titration EN 1017, EN 1018, prEN 16003,
prEN 16004 Sulfate 6.10 Gravimetry EN 1017 Solubility index 6.11 Conductivity EN 12518 Magnesium 7.1 or 7.2 AAS (flame) or ICP-OES EN 1017, EN 1018, prEN 16003,
prEN 16004 Silicium, Aluminium, Iron, 7.1 or 7.2 AAS (flame) or ICP-OES EN 1017, EN 12518, prEN 16003,
prEN 16004 SIST EN 12485:2011
prEN 16003,
prEN 16004 Arsenic, Antimony, Selenium 8.3 AAS (hydride) EN 1017, EN 1018, EN 12518,
prEN 16003,
prEN 16004 Mercury 8.4 AAS (cold-vapour technique) EN 1017, EN 1018, EN 12518,
prEN 16003,
prEN 16004 3.3 Sample preparation The general recommendations specified in ISO 3165 shall be observed when sampling. Sampling shall be performed in accordance with EN 459-2. For products less than 6 mm grain size, the size of the sample shall be 1 l.
Before performing the chemical analyses, the size of the sample shall be reduced by using a sample divider and/or by dividing it into four parts in order to obtain a suitable subsample. The coarse-grain material in this sample shall be reduced to a size of less than 0,2 mm before performing the chemical analysis. When sampling milk of lime, the material from which the sample is to be taken shall be thoroughly mixed with an electrically driven stirrer of adequate power. The milk of lime shall be dried at (105 ± 5) °C (see 6.1) before being analysed chemically. Since the subsamples under examination are altered by the absorption of moisture and carbon dioxide, their exposure to air shall be minimized. They shall therefore be transported and stored in air-tight containers and all the handling shall be carried out as quickly as possible. 3.4 Reagents All reagents shall be of a recognized analytical grade appropriate for the method being used. The water used shall conform to grade 3 in accordance with EN ISO 3696:1995 unless otherwise specified in the method. The concentration of the analytes in the water and reagents shall be negligible compared with the lowest concentration to be determined.
The concentrated liquids used for the reagents in this standard have the following densities (ρ) (in grams per millilitre at 20 °C):  hydrochloric acid
1,16 to 1,19;  nitric acid
1,40 to 1,42;  ammonium hydroxide solution 0,88 to 0,91;  triethanolamine
1,12. Dilutions are specified as the sum of the volumes. Thus, (1 + 2) dilute hydrochloric acid means 1 part by volume of concentrated hydrochloric acid mixed with 2 parts by volume of water. SIST EN 12485:2011

3.5 Glassware Glass containers and pipettes shall be cleaned with hot dilute nitric acid immediately before use and then rinse with water. If determining trace elements rinse with grade 2 water. 3.6 Expression of results The analytical results for the major and minor constituents shall be reported as mass fraction in %, while those for trace elements shall be reported as mass fraction in milligrams per kilogram, as the mean of two determinations. In general, analytical values shall be reported to three significant figures. EXAMPLE (CaO) = 91,2 %; (SiO2) = 3,70 %; (MnO2) = 0,15 %; (Cr) = 0,32 mg/kg; (Hg) = 0,05 mg/kg. If the results of a duplicate determination differ from one another by more than twice the repeatability standard deviation, the determination shall be repeated. The result shall then be deemed to be the mean of the two results with the lowest difference. To assess whether the analytical results meet the requirements laid down in EN 12518 for high-calcium lime, in EN 1018 for calcium carbonate products and in EN 1017 for half-burnt dolomites, in prEN 16003 for calcium magnesium carbonate and in prEN 16004 for magnesium oxide, the results have to be converted to the form in which the requirements are stated in the above standards. Subclauses of this standard are given in Table 2 and contain the relevant calculation methods.
d) sample pretreatment, e.g. method of digestion (see Clause 5); e) any deviation from this standard and an indication of any circumstances which can have affected the results. 4 Determination of screen oversize of high-calcium lime 4.1 Air-jet sieving method 4.1.1 General The method is used to determine the retention on sieving of high-calcium quicklime and hydrated lime as specified in EN 12518. The particle size distribution of high-calcium quicklime and hydrated lime can be determined using airjet sieving apparatus. For quicklime, the method is suitable for particles which substantially pass a 2,0 mm test sieve. For hydrated lime, the method can be used to determine the particle size distribution of the agglomerates of very fine particles produced by the manufacturing process. This method uses test sieves with aperture sizes of 0,60 mm and 0,09 mm. SIST EN 12485:2011

Key 1 housing 7 test sample 2 dish 8 oversize material 3 sieve drum 9 undersize material 4 lid 10 air jet 5 slit-nozzle 11 air discharge 6 sieve 12 pressure gauge socket, with dust hood Figure 1 — Air-jet sieving apparatus 4.1.2.2 Test sieves, 200 mm diameter, aperture sizes 0,60 mm and 0,09 mm. NOTE The effective operation of some makes of air-jet apparatus can require non-standard sieve frames and additional gaskets. This is permissible, provided the sieving medium and general method of construction comply with the requirements of this standard. 4.1.2.3 Trays or other suitable containers of sufficient size to contain the test portion. 4.1.2.4 Balance, accurate to 0,1 mg. 4.1.2.5 Soft brush.
4.1.2.6 Ultrasonic cleaning bath for cleaning the mesh of the sieves.
4.1.2.7 Mallet, if there is a tendancy for material to adhere to the lid of the apparatus. A rubber or plastics tipped mallet is preferred. 4.1.2.8 Drying oven (optional), thermostatically controlled to maintain a temperature of (105 ± 5) °C. SIST EN 12485:2011

If material adheres to the lid of the apparatus, gently tap the centre of the lid with the mallet.
If the material agglomerates under the action of the air-jet, interrupt the sieving process, and break up the agglomerates with the soft brush. After (5 ± 0,2) min, switch off the apparatus and carefully remove the sieve. Transfer the material retained on the sieve into a tray or other suitable container. Carefully clean the mesh of the sieve over the tray using a soft brush.
Determine the mass of the residue, including the material brushed from the sieve mesh, and record the mass to the nearest 1 mg. Refit the sieve into the apparatus and transfer all of the residue back to the sieve mesh. Repeat the weighing and sieving stages until the sieving end-point has been achieved, and record the end-point mass to the nearest 1 mg. The sieving end-point is defined as being when not more than 0,2 % of the mass of the original test portion passes through the sieve in 1 min. Fit the 0,60 mm test sieve into the apparatus, and repeat the weighing and sieving stages until the mass of the residue confirms that the sieving end-point has been reached. Record the end-point mass to the nearest 1 mg. 4.1.4 Expression of results The mass retained on each sieve expressed as m (P0,60 or 0,09) in mass fraction in %, is given by the following equation: ()mmm100
P 10,09or
0,60×= (1) where m is the mass of the dry substance in the test portion, in grams; m1 is the mass of the residue retained on the test sieves, in grams. 4.2 Wet sieving method 4.2.1 General The method is used for the determination of the retentions on sieving of milk of lime as specified in EN 12518. 4.2.2 Apparatus 4.2.2.1 Balance, accurate to 0,1 mg. 4.2.2.2 500 ml wide-mouthed bottle, or other suitable vessel which can be sealed with a stopper. SIST EN 12485:2011

P 10,09or
0,60×= (2) where m is the mass of the dry substance in the test portion, in grams; m1 is the mass of the residue retained on the test sieves, in grams. SIST EN 12485:2011

 calcium carbonate as specified in EN 1018 in order to determine calcium and magnesium;  magnesium oxide as specified in prEN 16004 in order to determine magnesium, silicon, aluminium and iron;  calcium magnesium carbonate as specified in prEN 16003 in order to determine calcium and magnesium. 5.1.2 Principle After fusing the sparingly soluble oxide constituents of the lime sample with lithium tetraborate, the fusion cake is dissolved in hydrochloric acid and the solution made up to 250 ml in a volumetric flask. Magnesium, silicon, aluminium, iron and manganese are determined in aliquot parts of this solution by flame-AAS (7.1) or ICP-OES (7.2). 5.1.3 Reagents 5.1.3.1 Lithium tetraborate, Li2B4O7.
5.1.3.2 Hydrochloric acid, ρ = 1,16 g/ml. 5.1.3.3 Hydrochloric acid, diluted, (1 + 5). 5.1.4 Apparatus Ordinary laboratory apparatus and the following: 5.1.4.1 Platinum-gold crucible. 5.1.4.2 Hot plate. 5.1.5 Procedure Weigh (0,25 ± 0,02) g to the nearest 0,1 mg of the sample into a platinum-gold crucible and add 1,5 g of lithium tetraborate (5.1.3.1). Roast at (1 000 ± 25) °C until the melt is clear. Remove from the heat, cover the crucible with a watch glass and stand the crucible in water for a few seconds, remove and allow it to stand until it has cooled completely. Transfer the cold melt to a beaker using approximately 50 ml of hydrochloric acid (5.1.3.3) and dissolve while stirring and heating at 100 °C. Then transfer the solution to a 250 ml volumetric flask with water (3.4) and, after cooling to room temperature, add each 10 ml of the appropriate reagent solutions (7.1.2.6 and 7.1.2.7 for the AAS measurement) or 1 ml of scandium solution (7.2.2.2, internal standard solution for the ICP measurement) and make up to the mark with water (digestion solution (I) for AAS and (II) for ICP). SIST EN 12485:2011

Continue boiling for 3 min and, after the precipitate has settled, filter the solution immediately through a fluted filter paper (particle retention size 2,5 µm) into a 500 ml volumetric flask. Wash the filter residue three times with ammonium hydroxide solution (5.2.3.5) and three times with water. After the solution has cooled to room temperature, make the solution up to the mark with water and shake the contents of the flask thoroughly (digestion solution III). SIST EN 12485:2011

Seal the digestion vessel and place in the microwave apparatus. Before programming the apparatus, the heating conditions shall be determined, and a temperature and pressure versus time plot shall be prepared. Subject the test sample to a pressure of 500 kPa to 700 kPa and to a temperature of 90 °C for 10 min during a heating-up phase. Then subject the test sample to a pressure of 1 000 kPa and a temperature between 120 °C and 150 °C for 15 min to 20 min. Allow the digestion vessel to cool to room temperature. Open the digestion vessel, introduce the solution into a 100 ml volumetric flask rinse and make up to the mark with water. Filter and transfer the solution (digestion solution IV) to a polypropylene vessel in order to avoid adsorption on the glass. 5.4 Pressurized digestion with nitric acid 5.4.1 General The purpose of this method of digestion is to release trace elements from the accompanying matrix and determine the content of the various elements. The method is applied to high-calcium limes as specified in EN 12518, to calcium carbonate as specified in EN 1018, to calcium magnesium carbonate as specified in SIST EN 12485:2011

6.1.1 General The method is used to determine free water in high-calcium lime as specified in EN 12518, calcium carbonate as specified in EN 1018 and calcium magnesium carbonate as specified in prEN 16003. In the case of hydrated high-calcium lime, calcium carbonate or calcium magnesium carbonate, free water means the moisture attached to the product, in the case of milk of lime, it refers to the water content of the suspension. The method does not apply for high-calcium quicklime. The determination of the water content of milk of lime is required to calculate the water-soluble content of the suspended hydrated lime (see 6.5).
6.1.2 Principle When heating a sample of hydrated high-calcium lime, calcium carbonate or calcium magnesium carbonate to (105 ± 5) °C, in the drying oven the free water escapes. The loss of mass at this temperature is referred to as free water in the case of hydrated high-calcium lime, calcium carbonate and calcium magnesium carbonate and as the content of water in the milk of lime.
6.1.5 Expression of results The free water content of hydrated high-calcium lime, milk of lime, calcium carbonate or calcium magnesium carbonate expressed as
(H2O)
in mass fraction in % is given by the following equation: ()12()HO x 100mmm−= (3) where m is the mass of the test portion before heating, in grams; m1 is the mass of the test portion after heating, in grams. 6.2 Loss on ignition at 450 °C 6.2.1 General The method is used to determine the loss on ignition in high-calcium lime as specified in EN 12518, in half-burnt dolomite as specified in EN 1017 and in magnesium oxide as specified in prEN 16004. 6.2.2 Principle The loss on ignition at 450 °C is basically due the water of hydration.
6.2.4.2 Milk of lime The water content of the milk of lime shall be determined as specified in 6.1.4.2. After drying the sample this way, the determination shall be carried out as specified in 6.2.4.1. 6.2.5 Expression of results The loss on ignition at 450 °C expressed as LoI in mass fraction in % is given by the following equation: ()121()LoI100
−=×mmm (4) where m1 is the mass of the sample before ignition at (450 ± 25) °C, in grams; m2 is the mass of the sample after ignition at (450 ± 25) °C, in grams. 6.3 Determination of carbon dioxide 6.3.1 General The method is used to determine carbon dioxide in high-calcium lime as specified in EN 12518, in half-burnt dolomite as specified in EN 1017 and in magnesium oxide as specified in prEN 16004. 6.3.2 Principle The carbon dioxide content of the materials concerned is determined from the loss on ignition at 1 000 °C. The loss on ignition at 450 °C is basically due to free water and the water of hydration. The difference in mass between the loss on ignition at (1 000 ± 50) °C and the loss on ignition at (450 ± 25) °C is equal to the carbon dioxide content of the product. SIST EN 12485:2011

6.3.5 Expression of results The carbon dioxide content expressed as CO2 in mass fraction in % is given by the following equation: ()100
)(CO 1322×−=mmmc (5) where m1 is the mass of the sample before ignition at (450 ± 25) °C (6.2.5), in grams; m2 is the mass of the sample before ignition at (1 000 ± 50) °C, in grams; m3 is the mass of the sample after ignition at (1 000 ± 50) °C, in grams. 6.4 Determination of residue insoluble in hydrochloric acid 6.4.1 General The method is used to determine the residue in calcium carbonate as specified in EN 1018 and in calcium magnesium carbonate as specified in prEN 16003 which is insoluble in hydrochloric acid. 6.4.2 Principle After the sample has been dissolved in hydrochloric acid and filtered, the filtration residue is washed, dried and incinerated to constant mass to determine the insoluble component gravimetrically. 6.4.3 Reagents 6.4.3.1 Hydrochloric acid, ρ = 1,16 g/ml. 6.4.3.2 Hydrochloric acid, diluted, 1 + 1. 6.4.3.3 Hydrochloric acid, diluted, 1 + 3. SIST EN 12485:2011

×=mm (6) where m1 is the incineration residue, in grams; m is the mass of the sample, in grams. 6.5 Determination of content of water soluble calci
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