University Of Karachi

CHEMICAL PROCESS TECHNOLOGY
(Practical file)

Syed Saad Ahmed B-0933040 B.E 3rd Year Chemical Engineering

Submitted To: Ma’am Khehkashan

CHEMICAL PROCESS TECHNOLOGY 2012

Experiment no. 6
OBJECT:
Analysis of Portland cement

REAGENTS:
       Portland cement Ammonium chloride Concentrated HCl Bromine water Liquor ammonia Ammonium nitrate Oxalic acid

THEORY:
Portland cement is the essential bonding material in concrete, which is most widely used as a non-metallic material of construction. The properties of cement depend upon the relative proportion of the constitutional compounds present and each of them has different characteristics and properties. These constitutional compounds are also called microscopic constituents. Such as Tricalcium aluminates (C3A), Tricalcium silicate (C3S), Tetracalciumaluminoferrite (C4AF), Dicalcium silicates (C2S). Also some additives are also added in the cement such as accelerators (CaCl2), air entrainment agent (Vinsol resin and Darex), retarders (Carbohydrates derivative and calcium lignosulfonate), and water repelling agents (fatty acid compound such as calcium, ammonia, aluminum or sodium stearates). Also some workability reagents, gas forming agents and pozzolanic materials are also used.

REACTIONS:

2

Prepared By: Syed Saad Ahmed | B.E Chemical Engineering

CHEMICAL PROCESS TECHNOLOGY 2012
PROCEDURE:
a) Loss on ignition
Weight 1 gram of cement in a previously dried and weighted crucible and heat in a furnace for 15 minutes at 950 . Cool it in a desiccator and weigh to give constant weight. Calculate % of loss on ignition in weight.

b) Determination of total Silica in cement
Weight 1 gram of cement and 1 gram of NH4Cl in a 250 ml beaker and mix well. Cover with a watch glass and slowly run in 10 ml conc. HCl by the sides. When reaction subsides, stir and break the lump with a rod. Heat the covered beaker on a water bath for 30 min with frequent stirring. Dilute with 50 ml of hot water and filter through Whatman 41. Wash with dilute 10% HCl, then with distilled water until washings are free from chlorides, save the filtrate and washings. Place the precipitate and filter paper in the weighed crucible. Heat on a Bunsen flame to drive away water and slowly clear the filter paper till black smoke of carbon is eliminated. Ignite at 1000 for 45 min in a furnace. Cool and weight. The weight of the residue gives total silica.

c) Determination of SesquiOxide (Fe2O3+Al2O3)-M2O3
Take all the filtrate from silica determination. Add 1 ml of bromine water and 2 gram of NH 4Cl. Heat to oxidize all ferrous to ferric ions. Boil to expel any excess bromine. Add NH 4OH to the hot solution and heat to coagulate the flocculent precipitate formed. Filter through Whatman 41 and wash with 1 ml NH4NO3 and NH4OH mixture and hot water. Save the filtrate for determination of CaO and MgO. Ignite the ppt and filter paper on a Bunsen flame to drive off water and burn down carbon and filter paper in a previously weighed crucible. Then ignite for 15 min at 200 in a furnace. Cool and weight as M2O3.

d) Determination of CaO in cement
After determination of M2O3 evaporate the filtrate to 200ml.Add 2 grams of oxalic acid, heat to boiling and neutralize with dilute NH4OH (use a few drops). Heat and allow ppt. to settle for 30 min. Filter and wash with di-ammonium oxalate solution. Transfer filter paper with ppt. to a previously weighed crucible. Drive off water and burn the carbon over Bunsen flame, and ignite at 1100°C in furnace. Cool and weigh as CaO.

3

Prepared By: Syed Saad Ahmed | B.E Chemical Engineering

CHEMICAL PROCESS TECHNOLOGY 2012

CALCULATION:
a) Loss on ignition
Weight of empty crucible Initial weight of crucible + cement before ignition, A Final weight of crucible + cement after ignition, B = 14.20 grams = 15.20 grams = 15.05 grams

b) Determination of total Silica in cement
Weight of residue of silica = 0.22 grams

c) Determination of SesquiOxide (Fe2O3+Al2O3)-M2O3
Weight of M2O3 = 0.297 grams

d) Determination of CaO in cement
Weight of CaO = 0.333 grams

4

Prepared By: Syed Saad Ahmed | B.E Chemical Engineering

CHEMICAL PROCESS TECHNOLOGY 2012
RESULTS:
a) b) c) d) % loss in ignition is found to be 15 %. % total silicain cement is found to be 22%. % total sesqui oxide is found to be 29.7%. % total CaO is found to be 33.3%.

DISCUSSION:
Portland cement is a fine, typically gray powder comprised of four chief minerals  Dicalcium silicate (C2S)  Tricalcium silicate (C3S)  Tricalcium aluminate (C3A)  Tetracalcium aluminoferrite (C4AF) with the addition of forms of calcium sulfate. Portland cement has today found its way as being the basic ingredient for ready-mix concrete. It creates a strong bond as compared to the early techniques of concrete production.

5

Prepared By: Syed Saad Ahmed | B.E Chemical Engineering

Sign up to vote on this title
UsefulNot useful