Metakaolin - measuring the total quantity of fixed Calcium Hydroxide...

http://metakaolin.info/quality-criteria/chapelle-test/index.html

Metakaolin - measuring the total quantity of fixed Calcium Hydroxide (Chapelle test modified) Referring to the French norm NF P 18-513, Annexe A
1. Principle The measure of the fixed quantity of calcium hydroxide on pozzolanic materials helps to define their pozzolanic activity. 1 g metakaolin is reacted with 2 g CaO in 250 ml of water. The non reacted lime is then measured and the result expressed in mg Ca(OH)2 fixed by the metakaolin. A blank experiment is done symmetrically without metakaolin

2. Equipment This consists of: - heated stirrer with a Teflon magnet - thermometer (scaled from 0 to 100C) - cooling column - Erlenmeyer in stainless steel with smooth inner surface (volume of 750 ml) - tap with 2 holes o one for the cooling column o one for the thermometer - balance e=0,1 mg

3. Reagents - calcium carbonate for analysis - distilled water without CO2. Prepare the water by passing it over an ion exchange resin. Use this water for all reactions. - Saccharose for analysis - Hydrochloric acid (decinormal) - Indicator solution: 0,1 % phenolphthalein in 50% alcohol solution

4. Working method - the apparatus id regulated to a temperature of 90C - weigh exactly 1 g of metakaolin in powder form into the dry clean Erlenmeyer - use a calibrated pipette to add 250 ml of the above water - add about 2 g of CaO exactly weighed - prepare the CaO the following way: o weigh 3,6 g of CaCO3 in a platinum crucible with known tare o calcine for about 30 minutes at 1000C o weigh and verify that the LOI (loss on ignition) be 44% - place the stirrer in the Erlenmeyer - place the tap with the thermometer and the cooling column and homogenise the content of the Erlenmeyer - place the apparatus on the heated stirrer and start heating - verify that the temperature gets to 85C5 - stir and heat for 16 hours - cool to room temperature - add to the Erlenmeyer 250 ml saccharose solution freshly prepared (60 g saccharose dissolved in exactly 250 ml water) - stir for 15 minutes on the magnetic stirrer. Filter about 200 ml take out 25 ml with a calibrated pipette.

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Metakaolin - measuring the total quantity of fixed Calcium Hydroxide...

http://metakaolin.info/quality-criteria/chapelle-test/index.html

- Make the same proceeding without metakaolin

4.2. Titrating the solution - titrate with a burette using the HCl 0,1N solution using the phenolphthalein as indicator

5. Calculations Definition: - V1 (ml) is the volume of 0,1N HCl necessary for the 25 ml of solution obtained by the blank sample - V2 (ml) is the volume of 0,1N HCl necessary for the 25 ml of solution obtained by the reaction of the metakaolin The titration reaction is: CaO + 2HCl CaCl + H O
2 2

Ca(OH) + 2 HCl CaCl + H2O

2 2

Check of the blank reaction 56 2 x V1 must be under 1000 Trial with metakaolin: Mg of Ca(OH)2 fixed = 2 x V1 - V2 x 74 x 1000 V1 56

6. Results The results are expressed in mg Ca(OH)2 fixed by the metakaolin

7. Precision The results should have a variation of 10%.

more info: Dr. Denis Bezard - questions@metakaolin.info - phone: +43 (0)2252 45970

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