METTLER TOLEDO

Cement determination
1. Titration of Calcium oxide (CaO)
10 mL sample are diluted with 25 mL deion. water. Add 10 mL Triethanole amine solution (1:4). (to mask the Fe & Al) Adjust pH to 12.5 with conc. NaOH. Titrate with EDTA 0,03 mol/L. Indicator: 0,1 g murexide 0.1 %; Indication: DP660 Murexide: 0.1% in water

2. Magnesium oxide (MgO)

10 mL sample are diluted with 25 mL deion. water. Add 10 mL Triethanole amine solution (1:4). (to mask the Fe & Al) Add ~ 17 mL EDTA 0,03 mol/L (excess to CaO, to mask Ca.) Adjust pH to 10.5 with conc. NH4OH. Titrate with DCTA 0,01 mol/L. Indicator: 0.1 g Methylthymol blue 1 %, Indication: DP660 Methylthymol blue 1 % in water

3. Iron (III) oxide (Fe2O3)

Method 1: 20 mL of sample are diluted with 30 mL deion. water. Adjust pH to 2.0 with sodium acetat solution. Add 4 mL Tiron as Indicator Titrate with EDTA 0,02 mol/L. Indication: DP660

Method 2: 20 mL of sample are diluted with 30 mL deion. water. Add 0.5 g amino acetic acid and 0.3 - 0.4 g sulfo salcylic acid indicator Adjust the pH to 1.5 with NH4OH 10 % Heat to 47 C, the temperature should not above 50 C. Titrate with EDTA 0,02 mol/L. Indication: DP550

Cement

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METTLER TOLEDO
sulfo salcylic acid: 1 2 % in water

Cement

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METTLER TOLEDO

4. Aluminum oxide (Al2O3)

Method 1: 20 mL of sample are diluted with 25 mL deion. water. Add NH4OH to adjust the pH to 2.0. Adjust pH to 3.0 with ammonium/acetat buffer. Add 4 mL EDTA 0,02 mol/L. (excess!!) Boil 3 minutes. The complexation of Al is very slow, which is why boiling and addition of an excess of EDTA is necessary) Cool to 30 C. Add 10 drops PAN and 4 drops Cu-EDTA. Titrate with CuSO4 0.02mol/L. Indication DP550 PAN = 1-Pyridin(2)azo-naphtol-2 0.025 % in ethanole

Cu-EDTA 0.05 mol/L: 1:1 mixture of CuSO4 0.05 mol/L and EDTA 0.05 mol/L

Method 2: 20 mL of sample are diluted with 25 mL deion. water. Adjust pH to 4.6 with acetat buffer. Add 10 mL EDTA 0.1 mol/L. (excess!!) Boil 3 minutes. The complexation of Al is very slow, which is why boiling and addition of an excess of EDTA is necessary) Cool to 30 C. Add 4 drops of xylene orange 0.1 % Titrate with ZnSO4 0.1 mol/L. Indication DP550 Color change: yellow to red.

Remarks: xylene orange 0.1 %, prepared in deion. water with some NaOH or in ethanole It is important to add the indicator after the excess of EDTA. If the indicator is added before the EDTA, the color is red instead yellow. There is no color change at the EQP.

Cement

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