Thermogravimetry Thermogravimetry was born out of problems encountered in gravimetric analysis .

for example , a common a precipitating and weighing form for the determination of calcium oxalate was precipitated, filtered, and the filtrate dried and weighed. The drying step was difficult to reproduce . for example , a particular routine procedure might recommend dryng at 110oC for 20 min and cooling prior to weighing. The analyst could then obtain very reproducible result derived from his or her own work. second worker might recommend o drying at 12! C for 10 min, cooling , and these results might not agree with those of the first research worker . the thermogram of calcium oxalate is shown in "ig. 1#.1. this problem is more easily understood when we examine the thermogram and find that water is driven off at temperature up to 22!oC . the water that is driven off includes not only uncombined but absorbed water from the precipitating solution , but also water of crystalli$ation that is bound to the calcium oxalate.. it is only when both types of water are driven off the reproducible results are archievable. %f the sample were heated to 110 oC , the absorbed water would be driven off, but a small amount of combine water would also be lost . similarly, if the drying temperature were 12!oC , the absorbed water would be driven off and a different small amount of combined water would be lost. s long as a drying temperature was rigidly adhered to , the results would be reproducible , but the results using a different drying temperature would show defferences because the amount of water crystalli$ation obtained would vary from one set of conditions to another. The problem was solved when Claudia &uval, working at the 'orbonne in (aris. , produced thermogravimetry curves for manytypes of precipitates and deduced , in the their correct drying temperatures for gravimetry analisis. %n the case of calcium oxalate a temperature i excess of 200oC was necessary to ensure that all water was driven off. The system rapidly became more important when it was reali$ed thai it could also be used to characteri$e compounds in order to study chemical reactions and decompositions at elevated temperatures. 1. ) *uipment for themogravimetry Thermogravimetry +T, - is concerned with the change of weight of material as its temperature change. "irst , this determines the temperature at which the material loses weight. This loss indicates decomposition or evaporation of the sample. 'econd , the temperature at which no weght loss takes place in revealed .hich indicates stability of the material . these temperature ranges are physical properties of chemical compounds and can be used for their identification. /nowledge of the temperatures at which a sample is unstable and sub0ect to decomposition or chemical change is important to the engineer because it reveals the temperature range over which such materials as polimers , alloys, building materials , packing materials, and high1pressure valves may not be used , as well as the temperatures at which they may be used safely. %t is also important to the analytical chemist, because it helps distinguish samples such as two different polimers or differentiates between a polymer that would fail in service and one that would be satisfactory. nother important piece of information that can be obtained by T, is the weight lost by a sample heated to a given temperature. This helps the inorganic or analytical chemist determine the composition of a compound and follow the reactions involved in its

decomposition . it also enables the analytical chemist to identify crystals of unknown compositions or determine the percentage of a given compound in a mixture of compounds. "or example, if calcium carbonate +CaC2 3- is heated to 4!0oC , it loses ##5 of its weight +"ig 1#.1- . lso , the gas evolved can be collected and identified as C2 2 . This observation virtually confirms that the reactions 6 CaC23 Ca2 7 C22

Take place at this temperature . the loss of C2 2 would also lead to a loss in weight of ##5 , and the products of the reactions can be identified as Ca2 and C22 . The formation of C22 can be verified by in0ecting the offcoming gases into a mass spectrometer and confirming by the spectrum observed.