Q1. Thermal stability and moisture contents of materials can be measured via Instrument A.

Suggest the name of instrument A and briefly describe its principle and applications. (3 marks) Q2. Thermal decomposition of Calcium Oxalate Monohydrate, CaC2O4H2O occurs as can be seen in Figure 1. The theoretical mass loss can be calculated using molar masses of the individual components. Table 1 shows the decomposition reactions as well as the theoretical mass loss of CaC2O4H2O. Table 1: Thermal Decomposition Reactions of Calcium Oxalate Monohydrate Reaction CaC2O4H2O CaC2O4 + H2O CaC2O4 CaCO3 + CO CaCO3 CaO + CO2 Theoretical Mass Loss 12.33% 19.17% 30.12% Measured Mass Loss ?
? ?

(i) Calculate the measured mass losses of all reactions shown in Table 1. (ii) Is there any difference in the mass loss between theoretical calculation and actual measurement for decomposition of CaC2O4? Give reasons to your answer. (6 marks)

Figure 1. Thermal Decomposition of Calcium Oxalate Monohydrate. Q3. The specific heat of 29 g of chicken meat sample was determined with the aid of 77 g of vacuum jacketed calorimeter. The calorimeter cup and the sample were first brought to 11C and then 55 g of water at 5.1C was poured into the cup. The system was then sealed and brought to equilibrium. The equilibrium temperature was recorded to be 6.9C. The specific heats of water and calorimeter cup are 4198 J kg-1 C-1 and 383 J kg-1 C-1, respectively. The calorimeter was well insulated and the heat loss to the surrounding was negligible. (i) (ii) Based on the scenario given above, what is the suitable method to measure the specific heat of the sample? Why? Calculate the specific heat of the sample. (6 marks)

ANSWER SCHEME

Q1. Thermal stability and moisture content of materials can be measured via Thermogravimetric analysis (TGA) Instrument. Thermogravimetric analysis (TGA) is a type of analysis that determines the mass change of a sample over time as it is heated. This analysis requires that the test instrument be able to accurately measure mass, temperature, and temperature change. Typically, samples are analyzed in an inert atmosphere although an oxidizing or reducing atmosphere can be used when necessary. TGA is widely employed in research and development, testing and characterization of all kinds of materials from metals and alloys to polymeric and ceramic composites. Typical applications of TGA may include determination of polymer degradation and decomposition temperatures, moisture content of materials, oxidation resistance and dynamics, volatile and non-volatile components, thermal stability, etc. Q2. (i) Calculate measured mass loss from Figure 1

Table 1: Thermal Decomposition Reactions of Calcium Oxalate Monohydrate Reaction Theoretical Mass Loss Measured Mass Loss CaC2O4H2O CaC2O4 + H2O 12.33% 12.30% CaC2O4 CaCO3 + CO 19.17% 18.90% CaCO3 CaO + CO2 30.12% 29.93% (ii) There is a slight difference in the mass loss between theoretical calculation and actual measurement for decomposition of CaC2O4. This is due to a redox reaction during which a reactant is simultaneously oxidized and reduced, thus forming two different products of CO into CO2 and carbon.

This scenario is highly dependent on the impurities within the sample as well as the cleanliness and material of the sample holder. Q3. (i) The method of mixture is a suitable method to measure the specific heat of the sample. This is because a known quantity of liquid (typically water) at a known initial temperature is mixed with a sample of known mass and temperature within an insulated container. The equilibrium temperature of the mixture is determined and the specific heat may be calculated from the simple energy balance:

(ii)

(77 x 10-3)(383)(11-6.9) + (29 x 10-3) Cps (11-6.9) = (55 x 10-3) (4198) (6.9-5.1) Cps = ___________ J kg-1 C-1