Variation of the specific surface area and porosity of anhydrous zinc oxalate with water vapour pressure

Specific surface areas and pore structure studies were carried out on two sets of samples of anhydrous zinc oxalate prepared from the dihydrate by heating at 130 and 180°C in various atmospheres of differing water vapour pressure. The two sets of samples were freshly prepared and aged samples. The variation of specific surface areas with water vapour pressure was found to behave in accordance with the Smith-Topley effect, with a minimum S_BET value located at 3.0 mmHg of water vapour. Analysis of the nitrogen adsorption isotherms by the t-method revealed the existence of both micropores and mesopores in the freshly prepared samples heated both at 130 and 180°C in 8.0 mmHg water vapour, and also in the aged samples prepared at 130°C in vacuo, and at 180°C in 8.0 mmHg water vapour. The rest of the samples possess only wide pores. Complete pore structure analysis for both micro- and mesopores was carried out for all samples investigated, and an attempt was made to correlate the factors affecting the development of surface area and pore structure, both in the presence and absence of water vapour, with those affecting the dehydration rate, and which occasionally lead to the Smith-Topley effect.