AN OPTIMIZED PROCEDURE FOR BORON SEPARATION AND MASS SPECTROMETRY ANALYSIS FOR RIVER SAMPLES

Abstract

An optimized procedure for the separation of boron from natural river samples and an improved mass spectrometry determination of boron isotopic ratio are presented. The chemical procedure, based on the use of the boron-specific resin Amberlite IRA 743, is especially efficient in separating boron from natural organic matter-rich samples like river waters.The properties of Amberlite IRA 743 have been investigated. The two factors important in determining the boron affinity for the resin are: the pH value and the ionic strength of the solution from which B is to be extracted. A logarithmic relationship between B partition coefficients and pH values is found. High ionic strength significantly lowers the fixation of B onto the Amberlite resin.The knowledge of the factors controlling the affinity of the resin Amberlite IRA 743 for boron enables us to design a simple and miniaturized chemical separation procedure characterized by (i) three chromatographic steps using, respectively, 50, 10 and 3 μl of resin, (ii) no evaporation step between each column, and (iii) final separation of boron from residual organic matter by sublimation of boric acid at 75 °C.Boron isotopic ratios are measured using an improved cesium metaborate technique, with graphite and mannitol. Adequate loading conditions enable us to obtain typical signal intensities of 5x10-12 A for 250 ng of boron. No in-run isotopic fractionation is observed, the external reproducibility for standards processed through the entire chemical procedure, as well as for samples, corresponds to 0.35%% (+/-2σ). According to this precision, a slight, but reproducible isotopic fractionation of 0.4%% is observed for standards processed through the entire chemical procedure whose origin is discussed, but is still unclear.