Heat of Hydration of Cement

Step 1: Preparation of zinc oxide and calorimeter

• Inspect the wax lining of the calorimeter carefully by clicking on it and ensure it is free from faults.
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• Click on the dropper and measure 9.6 ± 0.1 ml of hydrofluoric acid and add it to the calorimeter .
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• Place the crucible containing zinc oxide inside the muffle furnace.

• Click on the bottle and measure 388.0 ± 0.1 ml of 2.0 N nitric acid and add it into the calorimeter using a standard flask.
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• Close the muffle furnace door securely.

• Click on the bottle of zinc oxide and weigh a sufficient quantity for about six determinations into a clean crucible.
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• Click on the muffle furnace door to open it .
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• Click on the crucible to place zinc oxide in the muffle furnace.
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• Set the temperature to 900–950 °C and ignite zinc oxide for one hour by clicking in the green button.
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• After ignition, remove the crucible with zinc oxide from the furnace by clicking on the furnance door.
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• Click on the crucible to cool the ignited zinc oxide in a desiccator containing anhydrous calcium chloride.
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• Click on NEXT to proceed.

Step 2: Heating zinc oxide sample for each determination

• Click on the tare button of the balance to adjust and ensure exactly about 7.0 g of ignited zinc oxide is measured.
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• Click on the trowel or spatula to add ignited zinc oxide into the crucible until the desired amount is obtained.
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• Click on the furnace door handle to open it .
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• Click on the crucible to place it inside the muffle furnace.
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• Click on the furnace door handle again to close it and heat the crucible at 900–950 °C for 5 minutes.
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• Remove the crucible from the furnace and click on the crucible to place it in the desiccator containing anhydrous calcium chloride to cool the reheated zinc oxide for 2.5–5 hours.
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• Click on NEXT to proceed.

Step 3: Operation of calorimeter and addition of zinc oxide

• Click on the power switch of the calorimeter unit to start the stirrer and run it for at least 5 minutes to obtain a uniform temperature. Record the temperature (to 0.001°C) at one-minute intervals for 5 minutes to determine the initial heating or cooling correction.
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• Click on the crucible containing zinc oxide and pour the powder steadily through the funnel into the calorimeter over 1–2 minutes, then brush the funnel clean with a camel-hair brush.
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• Click on NEXT to proceed

Step 4: Preparation and weighing of cement samples

• Click on the tare button of the balance to zero it.
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• Click on the trowel to add cement onto the pan and accurately weigh 60 g of cement.
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• Click on the measuring cylinder to measure 24 ml of distilled water and add it to the weighed cement, then mix thoroughly to a uniform paste.
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• Click on the tare button of the larger balance to zero it before weighing the main cement batch.
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• Click on the trowel to transfer cement from the bag into the dish until about 3.0 g is obtained for the heat of solution test.
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• Click on the trowel again to collect and place an additional cement portion of approximately 7.0 g in another dish for loss-on-ignition determination.
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• Click on the dish containing the cement sample to place it near the calorimeter for carrying out the temperature-rise determination exactly as in Step 3 using the same calorimeter and correction procedure.
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• Click on the crucible containing the cement sample and place it inside the muffle furnace, then heat it at 900 °C for 3–4 hours.
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• Click on the furnance door to remove the heated cement sample from the furnace.
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• Click on the crucible again and place the hot cement sample in a desiccator containing anhydrous calcium chloride to cool it.
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• Click on the tare button of the balance to zero it before weighing the cooled cement sample.
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• Click on the crucible with cooled cement and place it on the balance pan to weigh the sample accurately to the nearest milligram.

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• Click on NEXT to proceed.