The specifi c surface areas of oxyhydrate adsorbents, calculated by the Parsons-Zobel plot method, were compared with the meso-and macropore specifi c surface areas derived from the nitrogen adsorption/desorption isotherms (by the t-plot method).Calculations of the specifi c surface area of oxide adsorbents with the use of the dependence of the surface charge on pH in the point of zero charge (PZC) vicinity, known as Parsons-Zobel (PZ) plots, give the "electrochemical" specifi c surface area available for sorption of charged species [1]. This technique has limitations associated with the pore structure characteristics of samples: Electric double layer is not formed in micropores whose radii do not exceed 1 nm [2]. For samples characterized by bimodal pore radius distribution the most important aspect consists in calculation of the specifi c surface area occupied by meso-and macropores, which is the decisive factor determining their suitability for dynamic sorption process applications. In our previous study [3] we explored the possibility of determining the specifi c surface area of mesoporous Zr, Al, Sn, and Ti oxyhydrates using the dependence of the surface charge on the equilibrium pH in the PZC vicinity for three points, in 0.12, 0.05, and 0.005 M KNO 3 . We found that, for mesoporous oxyhydrates, the specifi c surface area differs from that derived from nitrogen adsorption/desorption isotherms by no larger than 10%. This study was focused on double oxyhydrate adsorbents Al x M 1-x O y ·nH 2 O [M = Ti(IV), Mn(IV), x = 0.5-0.9].Here, we compared the specifi c surface areas of double oxyhydrates, estimated from the nitrogen adsorption/ desorption isotherms, with those derived from the Parsons-Zobel plots.
EXPERIMENTALThe amorphous oxyhydrate adsorbents were prepared by precipitation (coprecipitation in the case of double oxyhydrates) of appropriate hydroxides from the corresponding salt solutions by the sol-gel procedure [4]. For better gelation, urea and urotropine were introduced into the initial solutions; in selected experiments, a modifi er (citric acid) was added. The initial ratio of the components in the synthesis was Al : Mn (Ti) = 1 : 1, as well as 3 : 1 [in the case when MnO(OH) 2 was introduced]. The resulting gels were air dried at 70°C and preliminarily treated (to remove the cations adsorbed during synthesis) by keeping the samples for 1 day in 0.2 M HNO 3 and subsequently rinsing with distilled water to neutral pH. The ratio of the components constituting the double oxyhydrates was determined by quantitative chemical analysis. The oxyhydrate samples were fused with K 2 CO 3 , Na 2 CO 3 ; the metals were leached with hydrochloric and nitric acids, after which Ti in the solution was determined colorimetrically, and Al, Zr, and Sn, titrimetrically (Trilon B).The specifi c surface area S sp and the pore structure parameters were calculated using the data from nitrogen adsorption/desorption, collected with an Autosorb-6B instrument. The specifi c surface area was calculated by