M. Renata S. Souto

Use of a single air segment to minimise dispersion and improve mixing in sequential injection: turbidimetric determination of sulphate in waters

In this work, we propose the use of an air segment in a sequential injection system to simultaneously improve the overlapping of the stacked zones and minimise dispersion. This strategy was developed for the determination of sulphate in natural and wastewaters. Barium chloride was used as a precipitating agent and the turbidity of the suspension formed was measured at 420 nm. Analysis was performed without sample pre-treatment and the system was able to monitor sulphate concentration at a rate of at least 20 determinations per hour. Slightly different analytical sequences were developed for natural and wastewaters in order to minimise specific interferences. Direct determination of sulphate was possible within a concentration range of 10-100 and 16-100 mg SO(4)(2-) L(-1) for natural and wastewaters, respectively. Results obtained were comparable with those of the reference method with relative deviations lower than 5%. Relative standard deviations between 1.6% and 3.3% were found.

Turbidimetric flow-injection determination of total nitrogen and potassium in vegetables

A turbidimetric flow-injection system was developed for the determination of total nitrogen and potassium in vegetable samples using a single spectrophotometer as detector. As a precipitating agent, 3.0% (w/v) sodium tetraphenylboron solution prepared in 2.0% (w/v) poly(vinyl alcohol) was used. A gas diffusion process was included in the manifold to separate ammonium ions from the rest of the sample and to allow paired analysis. Total nitrogen and potassium determinations were carried out on the solutions remaining in the acceptor and donor streams, respectively. Results obtained were precise (relative standard deviations <2.1 and 1.6% for total N (<25 mg g−1) and K (<55 mg g−1) determinations, respectively) and in agreement with those of reference methods. Analysis can be carried out at a rate of up to 35 samples per hour (corresponding to 70 determinations per hour) within concentration range 87–430 mg N–NH+4 l−1 and 78–390 mg K+ l−1 for the total nitrogen and potassium determinations, respectively.

Cathodic voltammetric detection of diltiazem at a bismuth film electrode: application to human urine and pharmaceuticals

In this work it was developed a novel application of bismuth film electrodes (BiFEs) for the determination of the antihypertensive and coronary vasodilator diltiazem by square wave cathodic voltammetry. The bismuth film was deposited ex situ on a glassy carbon electrode for 90 s at -1.4 V vs. Ag/AgCl, from an acetate buffer (pH 4.5; 0.10 mol L-1) containing 5 or 30 mg L-1 Bi. Diltiazem analytical signal was obtained in phosphate buffer (pH 7.4; 0.25 mol L-1) where reduction takes place at -1.5 V vs. Ag/AgCl. The proposed methodology was applied to the quantification of diltiazem in pharmaceutical samples (dynamic linear range comprised between 90 and 900 µg L-1) and in human urine (dynamic linear range comprised between 45 and 270 µg L-1, and detection limit of 12 µg L-1).

Assay of plant tissues for elemental content by flow injection analysis

Abstract For the effective control of the increasing number of agricultural and environmental samples, new and improved analytical procedures are required. The use of the flow injection analysis (FIA) instrumental procedure for routine plant elemental determinations is discussed. Short descriptions of the flow manifolds are given by highlighting some of their most important features.