Document Type

Thesis

Date of Award

5-31-1984

Degree Name

Master of Science in Chemical Engineering - (M.S.)

Department

Chemical Engineering and Chemistry

First Advisor

Barbara B. Kebbekus

Second Advisor

Joseph W. Bozzelli

Third Advisor

R. P. T. Tomkins

Abstract

A new method for the determination of sulfur dioxide, SO2, and sulfur trioxide, SO3, in stack emissions was developed due to questionable results obtained from the EPA Method 8. This new method is a wet chemical procedure utilizing a pH 4.0 formic acid- sodium formate buffered formaldehyde solution to collect both SO2 and SO3 in the same solution. The absorbed SO2 forms a stable adduct, hydroxymethanesulfonate, HOCH2SO3-, in solution with formaldehyde. The SO3 is absorbed as sulfuric acid, H2SO4. The SO3 is determined as sulfate, SO24 , by a photometric titration with barium perchlorate, Ba(C104)2, and Thorin indicator at 520 nm. The hyd_roxymethanesulfonate does not interfere in the sulfate titration. A procedure for concentrating sulfate was developed for determination of low levels of SO3. Sulfate in the presence of hydroxymethanesulfonate is adsorbed on an alumina column. It is then eluted into a smaller volume and analyzed in the same manner. Total sulfur oxides are determined by oxidation of the hydroxymethanesulfonate to sulfate with hydrogen peroxide and subsequent titration with Ba(C104)2. The difference between total sulfur oxides and SO3 is the SO2 concenration. The advantage of this technique is the preservation of SO2 and SO3 in their respective oxidation states allowing accurate speciation of the two. The procedure for concentration of sulfate allows accurate ppm determination of SO3, and allows the separation of sulfate from hydroxymethanesulfonate or complexed sulfite.

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