Evidences of turbulent mixing in multi-pumping flow systems

Multi-pumping flow systems exploit pulsed flows delivered by Solenoid pumps. Their improved performance rely on the enhanced radial mass transport inherent to the pulsed flow, which is a consequence of the establishment of vortices thus a tendency towards turbulent mixing. This paper presents several evidences of turbulent mixing in relation to pulsed flows. such as recorded peak shape, establishment of fluidized beds, exploitation of flow reversal, implementation of relatively slow chemical reactions and/or heating of the reaction medium. In addition, Reynolds number associated with the GO period of a pulsed flow is estimated and photographic images of dispersing samples flowing under laminar regime and pulsed flow conditions are presented. (C) 2009 Elsevier B.V. All rights reserved.

Determination of Glyphosate in Water Samples by Multi-pumping Flow System Coupled to a Liquid Waveguide Capillary Cell

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Multi-commutation in spectrometry

We review recent developments in manifold components and the introduction of light-emitting-diode technology in spectroscopic detection in order to evaluate the tremendous possibilities offered by multi-commutation for infield and in-situ measurements, based on the use of multi-pumping and low-voltage, portable batteries, which make possible a dramatic reduction in size, weight and power requirements of spectrometric devices. (C) 2009 Elsevier Ltd. All rights reserved.

Exploiting Pulsed Flows for Heating Improvement: Application to Determination of Total Reducing Sugars in Molasses and Sugar-Cane Juices

Laminar and pulsed flows typical of multi-commuted and multi-pumping flow systems, were evaluated in relation to analytical procedures carried out at high temperatures. As application, the spectrophotometric determination of total reducing sugars (TRS, hydrolyzed sucrose plus reducing sugars) in sugar-cane juice and molasses was selected. The method involves in-line hydrolysis of sucrose and alkaline degradation of the reducing sugars at about 98 degrees C. Better results were obtained with pulsed flows, due to the efficient radial mass transport inherent to the multi-pumping flow system. The proposed system presents favorable characteristics of ruggedness, analytical precision (r.s.d. < 0.013 for typical samples), stability (no measurable baseline drift during 4-h working periods), linearity of the analytical curve (r > 0.992, n = 5, 0.05-0.50% w/v TRS) and sampling rate (65 h(-1)). Results are in agreement with ion chromatography.

A multicommuted flow system with solenoid micro-pumps for paraquat determination in natural waters

A flow system designed with solenoid micro-pumps is proposed for the determination of paraquat in natural waters. The procedure involves the reaction of paraquat with dehydroascorbic acid followed by spectrophotometric measurements. The proposed procedure minimizes the main drawbacks related to the standard chromatographic procedure and to flow analysis and manual methods with spectrophotometric detection based on the reaction with sodium dithionite, i.e. high solvent consumption and waste generation and low sampling rate for chromatography and high instability of the reagent in the spectrophotometric procedures. A home-made 10-cm optical-path flow cell was employed for improving sensitivity and detection limit. Linear response was observed for paraquat concentrations in the range 0.10-5.0 mg L-1. The detection limit (99.7% confidence level), sampling rate and coefficient of variation (n = 10) were estimated as 22 mu g L-1, 63 measurements per hour and 1.0%, respectively. Results of determination of paraquat in natural water samples were in agreement with those achieved by the chromatographic reference procedure at the 95% confidence level. (c) 2008 Elsevier B.V. All rights reserved.

An improved flow-based procedure for microdetermination of total tannins in beverages with minimized reagent consumption

A flow system designed with solenoid micro-pumps is introduced for spectrophotometric determination of total tannins based on the Folin- Denis reaction. The procedure minimizes the main drawbacks related to the AOAC batch procedure, i.e. interferences from reducing species in the samples, high reagent consumption and waste generation, and low sampling rate. Linear response was observed for tannic acid concentrations in the range 2-100 mg L-1, with a detection limit (99.7% confidence level) of 0.3 mg L-1. The sampling rate and coefficient of variation (n = 10) were estimated as 75 measurements per hour and 1.1%, respectively. Results of determination of total tannin in tea, beer and wine samples were in agreement with those achieved by the batch reference procedure at the 95% confidence level. In comparison to the batch procedure, the reagent consumption and effluent generation were 83 and 60-fold lower, respectively.

An expert flow system involving in-line prior assay for turbidimetric determination of chloride and sulphate in natural waters

A multi-pumping flow system exploiting prior assay is proposed for sequential turbidimetric determination of sulphate and chloride in natural waters. Both methods are implemented in the same manifold that provides facilities for: in-line sample clean-up with a Bio-Rex 70 mini-column with fluidized beads: addition of low amounts of sulphate or chloride ions to the reaction medium for improving supersaturation; analyte precipitation with Ba(2+) or Ag(+); real-time decision on the need for next assay. The sample is initially run for chloride determination, and the analytical signal is compared with a preset value. If higher, the sample is run again, now for sulphate determination. The strategy may lead to all increased sample throughput. The proposed system is computer-controlled and presents enhanced figures of merit. About 10 samples are run per hour (about 60 measurements) and results are reproducible and Unaffected by the presence of potential interfering ions at concentration levels usually found in natural waters. Accuracy was assessed against ion chromatography. (C) 2008 Elsevier B.V. All rights reserved.

LOW COST ANALYZER FOR THE DETERMINATION OF PHOSPHORUS BASED ON OPEN-SOURCE HARDWARE AND PULSED FLOWS

The need for automated analyzers for industrial and environmental samples has triggered the research for new and cost-effective strategies of automation and control of analytical systems. The widespread availability of open-source hardware together with novel analytical methods based on pulsed flows have opened the possibility of implementing standalone automated analytical systems at low cost. Among the areas that can benefit from this approach are the analysis of industrial products and effluents and environmental analysis. In this work, a multi-pumping flow system is proposed for the determination of phosphorus in effluents and polluted water samples. The system employs photometric detection based on the formation of molybdovanadophosphoric acid, and the fluidic circuit is built using three solenoid micropumps. The detection is implemented with a low cost LED-photodiode photometric detection system and the whole system is controlled by an open-source Arduino Uno microcontroller board. The optimization of the timing to ensure the color development and the pumping cycle is discussed for the proposed implementation. Experimental results to evaluate the system behavior are presented verifying a linear relationship between the relative absorbance and the phosphorus concentrations for levels as high as 50 mg L-1.

Automated two-dimensional separation flow system with electrochemical preconcentration, stripping, capillary electrophoresis and contactless conductivity detection for trace metal ion analysis

This paper describes the automation of a fully electrochemical system for preconcentration, cleanup, separation and detection, comprising the hyphenation of a thin layer electrochemical flow cell with CE coupled with contactless conductivity detection (CE-C(4)D). Traces of heavy metal ions were extracted from the pulsed-flowing sample and accumulated on a glassy carbon working electrode by electroreduction for some minutes. Anodic stripping of the accumulated metals was synchronized with hydrodynamic injection into the capillary. The effect of the angle of the slant polished tip of the CE capillary and its orientation against the working electrode in the electrochemical preconcentration (EPC) flow cell and of the accumulation time were studied, aiming at maximum CE-C(4)D signal enhancement. After 6 min of EPC, enhancement factors close to 50 times were obtained for thallium, lead, cadmium and copper ions, and about 16 for zinc ions. Limits of detection below 25 nmol/L were estimated for all target analytes but zinc. A second separation dimension was added to the CE separation capabilities by staircase scanning of the potentiostatic deposition and/or stripping potentials of metal ions, as implemented with the EPC-CE-C(4)D flow system. A matrix exchange between the deposition and stripping steps, highly valuable for sample cleanup, can be straightforwardly programmed with the multi-pumping flow management system. The automated simultaneous determination of the traces of five accumulable heavy metals together with four non-accumulated alkaline and alkaline earth metals in a single run was demonstrated, to highlight the potentiality of the system.

Desenvolvimento de métodos quantitativos e de sistemas de screening para a determinação de glifosato

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Desenvolvimento de um método simples, limpo e rápido para a determinação de fluoroquinolonas em formulações farmacêuticas

Pós-graduação em Química - IQ

Feasibility study and flow scheduling optimization of a multi-product pipeline system

The first goal of this study is to analyse a real-world multiproduct onshore pipeline system in order to verify its hydraulic configuration and operational feasibility by constructing a simulation model step by step from its elementary building blocks that permits to copy the operation of the real system as precisely as possible. The second goal is to develop this simulation model into a user-friendly tool that one could use to find an “optimal” or “best” product batch schedule for a one year time period. Such a batch schedule could change dynamically as perturbations occur during operation that influence the behaviour of the entire system. The result of the simulation, the ‘best’ batch schedule is the one that minimizes the operational costs in the system. The costs involved in the simulation are inventory costs, interface costs, pumping costs, and penalty costs assigned to any unforeseen situations. The key factor to determine the performance of the simulation model is the way time is represented. In our model an event based discrete time representation is selected as most appropriate for our purposes. This means that the time horizon is divided into intervals of unequal lengths based on events that change the state of the system. These events are the arrival/departure of the tanker ships, the openings and closures of loading/unloading valves of storage tanks at both terminals, and the arrivals/departures of trains/trucks at the Delivery Terminal. In the feasibility study we analyse the system’s operational performance with different Head Terminal storage capacity configurations. For these alternative configurations we evaluated the effect of different tanker ship delay magnitudes on the number of critical events and product interfaces generated, on the duration of pipeline stoppages, the satisfaction of the product demand and on the operative costs. Based on the results and the bottlenecks identified, we propose modifications in the original setup.

Doehlert Design-desirability Function Multi-criteria Optimal Separation Of 17 Phenolic Compounds From Extra-virgin Olive Oil By Capillary Zone Electrophoresis.

In Brazil, the consumption of extra-virgin olive oil (EVOO) is increasing annually, but there are no experimental studies concerning the phenolic compound contents of commercial EVOO. The aim of this work was to optimise the separation of 17 phenolic compounds already detected in EVOO. A Doehlert matrix experimental design was used, evaluating the effects of pH and electrolyte concentration. Resolution, runtime and migration time relative standard deviation values were evaluated. Derringer's desirability function was used to simultaneously optimise all 37 responses. The 17 peaks were separated in 19min using a fused-silica capillary (50μm internal diameter, 72cm of effective length) with an extended light path and 101.3mmolL(-1) of boric acid electrolyte (pH 9.15, 30kV). The method was validated and applied to 15 EVOO samples found in Brazilian supermarkets.

Behavior Of Listeria Monocytogenes In A Multi-species Biofilm With Enterococcus Faecalis And Enterococcus Faecium And Control Through Sanitation Procedures.

The formation of mono-species biofilm (Listeria monocytogenes) and multi-species biofilms (Enterococcus faecium, Enterococcus faecalis, and L. monocytogenes) was evaluated. In addition, the effectiveness of sanitation procedures for the control of the multi-species biofilm also was evaluated. The biofilms were grown on stainless steel coupons at various incubation temperatures (7, 25 and 39°C) and contact times (0, 1, 2, 4, 6 and 8days). In all tests, at 7°C, the microbial counts were below 0.4 log CFU/cm(2) and not characteristic of biofilms. In mono-species biofilm, the counts of L. monocytogenes after 8days of contact were 4.1 and 2.8 log CFU/cm(2) at 25 and 39°C, respectively. In the multi-species biofilms, Enterococcus spp. were present at counts of 8 log CFU/cm(2) at 25 and 39°C after 8days of contact. However, the L. monocytogenes in multi-species biofilms was significantly affected by the presence of Enterococcus spp. and by temperature. At 25°C, the growth of L. monocytogenes biofilms was favored in multi-species cultures, with counts above 6 log CFU/cm(2) after 8days of contact. In contrast, at 39°C, a negative effect was observed for L. monocytogenes biofilm growth in mixed cultures, with a significant reduction in counts over time and values below 0.4 log CFU/cm(2) starting at day 4. Anionic tensioactive cleaning complemented with another procedure (acid cleaning, disinfection or acid cleaning+disinfection) eliminated the multi-species biofilms under all conditions tested (counts of all micro-organisms<0.4 log CFU/cm(2)). Peracetic acid was the most effective disinfectant, eliminating the multi-species biofilms under all tested conditions (counts of the all microorganisms <0.4 log CFU/cm(2)). In contrast, biguanide was the least effective disinfectant, failing to eliminate biofilms under all the test conditions.

A multi-screening approach for marine-derived fungal metabolites and the isolation of cyclodepsipeptides from Beauveria felina

Extracts obtained from 57 marine-derived fungal strains were analyzed by HPLC-PDA, TLC and ¹H NMR. The analyses showed that the growth conditions affected the chemical profile of crude extracts. Furthermore, the majority of fungal strains which produced either bioactive of chemically distinctive crude extracts have been isolated from sediments or marine algae. The chemical investigation of the antimycobacterial and cytotoxic crude extract obtained from two strains of the fungus Beauveria felina have yielded cyclodepsipeptides related to destruxins. The present approach constitutes a valuable tool for the selection of fungal strains that produce chemically interesting or biologically active secondary metabolites.