Semi-automated Analysis of Fluoride in Biological Materials

Abstract

A semi-automated method for determination of fluorine in biological materials has been developed incorporating the Technicon AutoAnalyzer. One-half gram of dried, ground plant material is ashed, alkali-fused, diluted with water, and the suspension is pumped, along with H₂SO₄, at controlled rates, into the hot revolving glass helix of a digestor unit. As the acid-digest mixture passes through the heated coil, volatile fluoride and water vapor are evolved. The volatile fluoride and water vapor are pulled from the helix under reduced pressure through a tube which projects into the helix. The tube, in turn, is connected to a water-jacketed condenser and then to an impinger where the sample is continuously mixed. An aliquot of the impinger liquid is being constantly withdrawn. This sample is then air-segmented and mixed with a reagent containing alizarin complexone, pH 4 acetate buffer, lanthanum nitrate, acetone, and water. The sample-reagent combination passes through 4 full-length mixing coils where color development takes place. Upon reacting with fluoride, the wine-red alizarin complexone-La(III) reagent forms a lilac blue fluoride complex. The solution is pumped from the mixing coils through the tubular flow cell of the colorimeter. The absorbence of the solution is measured at 624 mμ, and the signal is transmitted to a recorder where the results are plotted on absorbency paper. The absorbence at the apex of the peak is proportional to the amount of fluoride in the sample between the range of 2.5-80 μg °F. Samples are analyzed at a rate of 12 per hour. Results compare favorably with those obtained by Willard-Winter distillation. Recent studies indicate that the F content of plant tissues can be estimated without prior ashing and fusion