SIST EN 12485:2011
(Main)Chemicals 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 methods
Chemicals 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 methods
This European Standard specifies the methods used for the chemical analyses and the determination of physical properties of calcium carbonate, high-calcium lime and half-burnt dolomite used to treat water for human consumption.
This document describes the reference methods and, in certain cases, an alternative method which can be considered to be equivalent. In the case of a dispute, only the reference methods are used.
Any other methods may be used provided they are calibrated, either against the reference methods or against internationally accepted reference materials, in order to demonstrate their equivalence.
NOTE Schematic diagrams of the analyses are given in Annex A (Figures A.1 to A.4).
Produkte zur Aufbereitung von Wasser für den menschlichen Gebrauch - Calciumcarbonat, Weißkalk und halbgebrannter Dolomit - Analytische Verfahren
Diese Europäische Norm legt die Verfahren zur chemischen Analyse und zur Bestimmung von physikalischen Eigenschaften von Calciumcarbonat, Weißkalk, halb¬gebranntem Dolomit, Magnesiumoxid und Calcium¬magnesiumcarbonat fest. Diese Stoffe werden zur Aufbereitung von Wasser für den menschlichen Gebrauch eingesetzt.
Diese Europäische Norm beschreibt Referenzprüfverfahren und in einigen Fällen Alternativprüfverfahren, die als gleichwertig angesehen werden können. Im Streitfall ist nur das Referenzverfahren maßgebend.
Werden andere Verfahren angewendet, so sind diese gegen die Referenzverfahren oder gegen international anerkannte Referenzmaterialien zu kalibrieren, um ihre Eignung nachzuweisen.
ANMERKUNG Der Analysengang ist schematisch im Anhang A dargestellt (siehe Bilder A.1 bis A.6).
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
La présente Norme européenne décrit les méthodes utilisées pour réaliser les analyses chimiques et
déterminer les propriétés physiques du carbonate de calcium, de la chaux et de la dolomie semi-calcinée, de
l’oxyde de magnésium et du carbonate de calcium et de magnésium utilisés pour le traitement de l’eau
destinée à la consommation humaine.
Le présent document décrit les méthodes de référence et, dans certains cas, une méthode alternative qui
peut être considérée comme étant équivalente. En cas de conflit, seules les méthodes de référence sont à
utiliser.
D’autres méthodes peuvent être utilisées, dans la mesure où elles sont étalonnées, soit par rapport aux
méthodes de référence, soit par rapport aux matériaux de référence internationalement reconnus, de manière
à démontrer leur équivalence.
NOTE Les représentations schématiques des analyses sont données à l’Annexe A (Figures A.1 à A.6).
Kemikalije, ki se uporabljajo za pripravo pitne vode - Kalcijev karbonat, visoko kalcijevo apno in polžgan dolomit, magnezijev oksid in kalcij-magnezijev karbonat - Preskusne metode
Ta evropski standard določa metode, ki se uporabljajo za kemične analize in določanje fizikalnih lastnosti kalcijevega karbonata, visokega kalcijevega apna in polžganega dolomita, ki se uporabljajo za pripravo pitne vode.
Ta dokument opisuje referenčne metode in v nekaterih primerih alternativno metodo, ki velja za enakovredno. V primeru spora se uporabljajo samo referenčne metode.
Druge metode se lahko uporabljajo, če so kalibrirane glede na referenčne metode ali glede na mednarodno sprejete referenčne materiale, kar je dokaz njihove enakovrednosti.
OPOMBA: Shematski diagrami analiz so podani v dodatku 1 (slike od A.1 do A.4).
General Information
Relations
Standards Content (Sample)
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
SIST EN 12485:2011
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.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 12485:2010: ESIST EN 12485:2011
EN 12485:2010 (E) 2 Contents Page Foreword .31Scope .42Normative references .43General requirements .43.1Number of determinations .43.2Methods for analysis .43.3Sample preparation .63.4Reagents .63.5Glassware .73.6Expression of results .73.7Repeatability and reproducibility limits .83.8Test report .84Determination of screen oversize of high-calcium lime .84.1Air-jet sieving method .84.2Wet sieving method . 105Preparation of test solutions . 125.1Fusion with lithium tetraborate . 125.2Extraction with hydrochloric acid . 135.3Microwave digestion with nitric acid . 145.4Pressurized digestion with nitric acid . 146Conventional methods of determining major and minor constituents . 156.1Determination of free water . 156.2Loss on ignition at 450 °C . 166.3Determination of carbon dioxide . 176.4Determination of residue insoluble in hydrochloric acid . 186.5Determination of content of water soluble calcium oxide or calcium hydroxide (reference method) . 196.6Determination of sugar soluble calcium oxide or calcium hydroxide (alternative method) . 216.7Water-insoluble matter . 236.8Determination of free CaO . 246.9Determination of calcium oxide and magnesium oxide . 256.10Determination of sulfate . 286.11Determination of solubility index by conductivity . 296.12Calculation of the composition of a commercial product . 327Determination of constituents by modern techniques . 347.1Determination of minor constituents by AAS flame technique . 347.2Determination of major and minor constituents by ICP-OES . 388Determination of trace elements . 438.1Determination of lead, cadmium, chromium and nickel by AAS graphite tube technique . 438.2Determination of lead, cadmium, chromium and nickel by ICP-OES . 498.3Determination of arsenic, antimony and selenium by AAS hydride technique . 538.4Determination of mercury by cold-vapour technique . 56Annex A (informative)
Analytical scheme . 60Annex B (informative)
Table B.1: Precision data for the test methods . 66Bibliography . 67 SIST EN 12485:2011
EN 12485:2010 (E) 3 Foreword This document (EN 12485:2010) 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 October 2010, and conflicting national standards shall be withdrawn at the latest by October 2010. 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 12485:2001. Annexes A and B are informative. Significant technical differences between this edition and EN 12485:2001 are as follows: a) addition of a method for determination of sugar-soluble calcium oxide or calcium hydroxide (see 6.6); b) addition of a method for determination of solubility index (see 6.11). 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom.
SIST EN 12485:2011
EN 12485:2010 (E) 4 1 Scope This European Standard specifies the methods used for the chemical analyses and the determination of physical properties of calcium carbonate, high-calcium lime, half-burnt dolomite, magnesium oxide and calcium magnesium carbonate used to treat water for human consumption. This document describes the reference methods and, in certain cases, an alternative method which can be considered to be equivalent. In the case of a dispute, only the reference methods are used. Any other methods may be used provided they are calibrated, either against the reference methods or against internationally accepted reference materials, in order to demonstrate their equivalence. NOTE Schematic diagrams of the analyses are given in Annex A (Figures A.1 to A.6). 2 Normative references The following referenced documents are indispensable for the application 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 459-2, Building lime — Part 2: Test methods EN 1017, Chemicals used for treatment of water intended for human consumption — Half-burnt dolomite EN 1018, Chemicals used for treatment of water intended for human consumption — Calcium carbonate EN 12518, Chemicals used for treatment of water intended for human consumption — High-calcium lime prEN 16003, Chemicals used for treatment of water intended for human consumption — Calcium magnesium carbonate prEN 16004, Chemicals used for treatment of water intended for human consumption — Magnesium oxide EN ISO 3696:1995, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987) ISO 3165, Sampling of chemical products for industrial use — Safety in sampling ISO 4793:1980, Laboratory sintered (fritted) filters — Porosity grading, classification and designation 3 General requirements 3.1 Number of determinations Two analyses shall be carried out to determine the various constituents (see Clause 5 to Clause 8, see also 3.6). 3.2 Methods for analysis The methods to be used for the analysis of half-burnt dolomite, calcium carbonate, high calcium lime, magnesium oxide and calcium magnesium carbonate and the principle of each method are listed in Table 1.
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
EN 12485:2010 (E) 5 the analysis of half-burnt dolomite and magnesium oxide shall be performed on a sample which is bound-water free. Before starting the chemical analysis, the loss on ignition at 450 °C shall be determined as described in 6.2. The analysis itself shall be performed on the material obtained after the determination of the loss on ignition. The requirement values for calcium carbonate, hydrated lime and calcium magnesium carbonate shall be expressed in dry substance in accordance with EN 1018, EN 12518 and prEN 16003. Therefore, the analysis of these products shall be performed on a sample which has been dried in accordance with the procedure described in 6.1.
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
EN 12485:2010 (E) 6 Table 1 (continued) Determination Method Principle Standard Manganese 7.2 ICP-OES EN 12518 Sulfur 7.2 ICP-OES EN 1017 Lead, Cadmium, Chromium, Nickel 8.1 or 8.2 AAS (flameless) or ICP-OES EN 1017, EN 1018, EN 12518,
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
EN 12485:2010 (E) 7 The concentrations of reference and standard volumetric solutions are specified as amount-of-substance concentrations, c (mol/l), while those of stock and standard solutions are specified as concentrations by mass, c (g/l or mg/l). Suitable element solutions for atomic absorption spectroscopy (AAS) and for optical emission spectroscopy by inductively coupled plasma (ICP-OES) are commercially available and can be used as stock solutions. They shall be prepared for the purposes of analysis in accordance with the manufacturer´s instructions. The appropriate element standard solutions are prepared in accordance with the instructions given in this European Standard. This European Standard makes no stipulations relating to the shelf life of stock, standard and reference solutions. In the case of stock solutions having an element concentration of 1 g/l, the manufacturer generally specifies a shelf life of one year. It is advisable to check the calibration solutions regularly.
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.
SIST EN 12485:2011
EN 12485:2010 (E) 8 Table 2 — Methods for calculation of the results Requirements from standard Parameter Required value for Calculation described in EN 1017 CaOfree, CaO CO2 MgO CaCO3 MgCO3 MgOfree 6.12.2.3 EN 1018 CaO MgO CaCO3 MgCO3 6.12.2.1 EN 12518 CO2 CaCO3 6.12.2.4 prEN 16004 MgO, loss on ignition at (1 000 ± 50) °C and (450 ± 25) °C (CO2 and H2O) 6.12.2.5 prEN 16003 MgO CaMg(CO3)2 6.12.2.2 3.7 Repeatability and reproducibility limits The repeatability and reproducibility limits were determined in an interlaboratory test (see Annex B) which was carried out in accordance with ISO 5725-2 and in which 28 laboratories took part. 3.8 Test report The report shall contain the following information: a) a reference to the method used; b) a complete identification of the sample; c) results obtained and the method of expression used (see 3.6)
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
EN 12485:2010 (E) 9 4.1.2 Apparatus 4.1.2.1 Air-jet sieving apparatus, of the general form shown in Figure 1. The apparatus shall be set to give a pressure difference of 2 kPa to 2,5 kPa across the sieves.
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
EN 12485:2010 (E) 10 4.1.3 Procedure Weigh to the nearest 1 mg (10 ± 0,5) g of quicklime (m) or (25 ± 0,5) g of hydrated lime (m). Fit the test sieve with the aperture size 0,09 mm into the apparatus and transfer all of the test portion onto the sieve mesh. Take care not to lose any of the test portion. Fit the lid and switch on the apparatus. Check that the vacuum created is above the minimum value stated in the manufacturer’s instructions, and that the slit nozzle is rotating properly.
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
EN 12485:2010 (E) 11 4.2.2.3 200 mm diameter 0,60 mm and 0,09 mm aperture size test sieves. 4.2.2.4 5 mm bore rubber or plastics tubing. 4.2.2.5 Ventilated drying oven (optional), thermostatically controlled to maintain a temperature of (105 ± 5) °C. 4.2.2.6 Two sintered glass filter crucibles, of porosity 2 (as specified in ISO 4793:1980) (maximum porosity diameter 40 µm to 100 µm) with filter flask and adapter funnel for crucibles. 4.2.2.7 Desiccator. 4.2.2.8 Wash bottle. 4.2.2.9 Filtration apparatus. 4.2.3 Procedure Superimpose the 0,60 mm mesh test sieve on the 0,09 mm mesh test sieve and wet the sieves with water. Place a volume of milk of lime containing (50 ± 0,5) g of dry substance in a 500 ml wide-mouthed bottle. Replace the stopper and shake the bottle for about 30 s. Remove the stopper immediately and pour the contents of the bottle onto the sieves. Wash any residue remaining in the bottle or on the stopper with a jet of water from the 5 mm bore tubing and at a pressure equal to a head of 1,2 m (approximately 10 kPa) on to the sieves. Then use the jet to wash the residue on the 0,60 mm mesh test sieve for (2 ± 0,1) min. Do not rub the residue through the sieve and take care not to flood the lower sieve during the operation. At the end of this period, wash the residue to one side of the sieve. Detach the 0,60 mm mesh test sieve and, using a wash bottle, transfer the residue from the sieve through a glass funnel into one of the tared, sintered glass filter crucibles connected to the filtration apparatus. When all the residue has been washed into the filter, and the water extracted, remove the filter containing the residue and dry it at (105 ± 5) °C for 1 h. Cool the dried filter in a desiccator and reweigh. Wash the residue on the 0,09 mm mesh test sieve for (5 ± 0,2) min. Transfer the residue to a tared filter crucible, dry at (105 ± 5) °C until constant mass is reached, cool and reweigh as described above. 4.2.4 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×= (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
EN 12485:2010 (E) 12 5 Preparation of test solutions 5.1 Fusion with lithium tetraborate 5.1.1 General Fusion with lithium tetraborate is used to dissolve: high-calcium lime as specified in EN 12518 in order to determine silicon, aluminium, iron and manganese; half-burnt dolomite as specified in EN 1017 in order to determine magnesium, silicon, aluminium and iron;
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
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