A novel flow-based procedure for automation of respirometric assays in soils.

A flow-based strategy involving a gas-diffusion sampling probe was proposed for evaluating the respiration rate in soils. The amount of CO2 collected after a pre-defined time interval was proportional to the free CO2 released by the soil ecosystem. The 500-mL incubation flasks typically used for soil respirometric assays were adapted and a special cover was designed for connecting a tubular gas diffusion membrane, a fan, and a septum for adding the CO2(g) standards required for calibration. The method relied on the pH-dependent absorbance variations resulting from the CO2 collection. A 1.3mmolL(-1) bromothymol blue solution (pH 7.0) acted as both acceptor and carrier streams. In order to widen the dynamical working range to 0.003-0.2mmol CO2, two analytical curves were obtained, each related to a different time interval for the CO2 collection. Kinetic curves related to CO2 release by the soil samples were straightforwardly attained. Repeatability and detection limit were estimated as 2.0% and 0.001mmol CO2 (n=10), and accuracy was assessed in relation to a recommended titrimetric procedure.

A multi-purpose flow manifold for the spectrophotometric determination of sulphide, sulphite and ethanol involving gas diffusion: application to wine and molasses analysis.

A simple and rugged flow set up was designed for spectrophotometric determination of sulphide, sulphite and ethanol aiming at quality assessment of wines, control of industrial fermentation, and selection of yeast strain. The different assays involved gas diffusion through a Teflon planar membrane and were carried out after minor modifications in the manifold, namely reagent composition and total flow rate. Main figures of merit: linear analytical curves=0.50-6.0 mg L(-1)S(2-), 2.5-20.0 mg L(-1) SO3(-) and 5.0-25.0% (v/v) of ethanol; detection limits (3σ)=0.035 mg L(-1)S(2-), 0.2 mg L(-1) SO3(-) and 0.18% (v/v) of ethanol; peak height r.s.d.=2.18% for 4.03 mg L(-1)S(2-) spiked molasses, 2.21% for a 9.82 mg L(-1) SO3(-) wine and 2.07% for a typical wine (12.53% v/v of ethanol), sampling rate=15, 57 and 29 h(-1), reagent consumptions=1.9 µmol of N,N-dimethyl-p-phenylenediamine, 1.68 µg of Malachite green and 0.68 mmol Cr(VI) per determination, respectively.

Banana peel as an adsorbent for removing atrazine and ametryne from waters.

The feasibility of using banana peel for removal of the pesticides atrazine and ametryne from river and treated waters has been demonstrated, allowing the design of an efficient, fast, and low-cost strategy for remediation of polluted waters. The conditions for removal of these pesticides in a laboratory scale were optimized as sample volume = 50 mL, banana mass = 3.0 g, stirring time = 40 min, and no pH adjustment necessary. KF(sor) values for atrazine and ametryne were evaluated as 35.8 and 54.1 µg g(-1) (µL mL(-1)) by using liquid scintillation spectrometry. Adsorption was also evaluated by LC-ESI-MS/MS. As quantification limits were 0.10 and 0.14 µg L(-1) for both pesticides, sample preconcentration was not needed. Linear analytical curves (up to 10 µg L(-1)), precise results (RSD < 4.5%), good recoveries (82.9-106.6%), and a > 90% removal efficiency were attained for both pesticides. Water samples collected near an intensively cultivated area were adequately remedied.

A flow system with zone merging and zone trapping in the main reactor applied to spectrophotometric catalytic determination of cobalt in grasses.

A flow system with zone merging and zone trapping in the main reactor was proposed. The sample and reagent inserted aliquots merge together and the resulting zone is directed towards a displaceable reactor inside which its most concentrated portion is trapped. After the pre-set TRAP period, the handled sample is released towards detection. A comparison with an analogous flow system exploiting zone stopping revealed the superior characteristics of sampling rate and system operation; moreover, the sample inserted volume plays little influence on sampling rate. The system was applied to the spectrophotometric determination of cobalt in pastures, and enhanced figures of merit (sampling rate=18 h(-1); peak height r.s.d.=0.7%, detection limit=0.046 µg L(-1) Co; reagent consumption=330 µg of Tiron per measurement; 98%

Spectrophotometric flow injection monitoring of sulfide during sugar fermentation.

A spectrophotometric flow injection procedure involving N,N-dimethyl-p-phenylenediamine (DMPD) is applied to the sulfide monitoring of a sugar fermentation by Saccharomyces cerevisiae under laboratory conditions. The gaseous chemical species evolving from the fermentative process, mainly CO(2), are trapped allowing a cleaned sample aliquot to be collected and introduced into the flow injection analyzer. Measurement rate, signal repeatability, detection limit and reagent consumption per measurement were estimated as 150 h(-1), 0.36% (n=20), 0.014 mg L(-1) S and 120 µg DMPD, respectively. The main characteristics of the monitoring record are discussed. The strategy is worthwhile for selecting yeast strain, increasing the industrial ethanol production and improving the quality of wines.

Zone trapping/merging zones in flow analysis: a novel approach for rapid assays involving relatively slow chemical reactions.

A novel strategy for accomplishing zone trapping in flow analysis is proposed. The sample and the reagent solutions are simultaneously inserted into convergent carrier streams and the established zones merge together before reaching the detector, where the most concentrated portion of the entire sample zone is trapped. The main characteristics, potentialities and limitations of the strategy were critically evaluated in relation to an analogous flow system with zone stopping. When applied to the spectrophotometric determination of nitrite in river waters, the main figures of merit were maintained, exception made for the sampling frequency which was calculated as 189 h(-1), about 32% higher relatively to the analogous system with zone stopping. The sample inserted volume can be increased up to 1.0 mL without affecting sampling frequency and no problems with pump heating or malfunctions were noted after 8-h operation of the system. In contrast to zone stopping, only a small portion of the sample zone is halted with zone trapping, leading to these beneficial effects.

Flow injection spectrophotometric method for chloride determination in natural waters using Hg(SCN)(2) immobilized in epoxy resin.

A flow injection (FI) spectrophotometric method was proposed for the determination of chloride ion in natural waters. The determination of chloride was carried out by reaction with Hg(SCN)(2) immobilized in an epoxy resin bead in a solid-phase reactor (SPR) and the thiocyanate ions released were determined spectrophotometrically at 480nm after complexing reaction with Fe(III). The analytical curve for chloride was linear in the concentration range from 5.6 x 10(-5) to 2.2 x 10(-4)moll(-1) with a detection limit of 1.4 x 10(-5)moll(-1). The relative standard deviation (R.S.D.) was 2.2% for a solution containing 2.2 x 10(-4)moll(-1) (n = 10). The simple manifold allows a routine analytical frequency of 100 determinations per hour. The main advantage of the developed method is the 400% reduction of the Hg waste solution generated when compared to conventional methods for chloride determination based on the same spectrophotometric reaction.