An Environmental Friendly Procedure for Photometric Determination of Hypochlorite in Tap Water Employing a Miniaturized Multicommuted Flow Analysis Setup

A photometric procedure for the determination of ClO− in tap water employing a miniaturized multicommuted flow analysis setup and an LED-based photometer is described. The analytical procedure was implemented using leucocrystal violet (LCV; 4,4′,4′′-methylidynetris (N,N-dimethylaniline), C25H31N3) as a chromogenic reagent. Solenoid micropumps employed for solutions propelling were assembled together with the photometer in order to compose a compact unit of small dimensions. After control variables optimization, the system was applied for the determination of ClO− in samples of tap water, and aiming accuracy assessment samples were also analyzed using an independent method. Applying the paired t-test between results obtained using both methods, no significant difference at the 95% confidence level was observed. Other useful features include low reagent consumption, 2.4 μg of LCV per determination, a linear response ranging from 0.02 up to 2.0 mg L−1  ClO−, a relative standard deviation of 1.0% (n = 11) for samples containing 0.2 mg L−1  ClO−, a detection limit of 6.0 μg L−1  ClO−, a sampling throughput of 84 determinations per hour, and a waste generation of 432 μL per determination

Instrumentation and Automated Photometric Titration Procedure for Total Acidity Determination in Red Wine Employing a Multicommuted Flow System

An automated procedure for photometric titration of red wine and associated instrumentation is described. The procedure was based on the flow-batch approach implemented employing multicommutation. The photometric detection was carried out using a homemade LED-based photometer. The mixing device, LED, and photodetector were attached to the titration chamber in order to form a compact and small-sized unit. The flow system comprised an automatic injector and three-way solenoid valves, which were controlled by a microcomputer through an electronic interface card. The software, written in Quick BASIC 4.5, was designed with abilities to accomplish all steps of the titration procedure including data acquisition and real-time processing to decide about the course of titration in the following step and so forth, until the titration endpoint was reached. The usefulness of the proposed titration system was demonstrated by analyzing red wine samples. When results were compared with those obtained using the AOAC reference method, no significant difference was observed at the [Formula: see text] confidence level. A relative standard deviation of ca [Formula: see text] ([Formula: see text]) was obtained when processing a typical red wine sample containing 7.3 [Formula: see text] total acidity expressed as tartaric acid

A Full Automatic Device for Sampling Small Solution Volumes in Photometric Titration Procedure Based on Multicommuted Flow System

In this work, an automatic device to deliver titrant solution into a titration chamber with the ability to determine the dispensed volume of solution, with good precision independent of both elapsed time and flow rate, is proposed. A glass tube maintained at the vertical position was employed as a container for the titrant solution. Electronic devices were coupled to the glass tube in order to control its filling with titrant solution, as well as the stepwise solution delivering into the titration chamber. The detection of the titration end point was performed employing a photometer designed using a green LED (λ=545 nm) and a phototransistor. The titration flow system comprised three-way solenoid valves, which were assembled to allow that the steps comprising the solution container loading and the titration run were carried out automatically. The device for the solution volume determination was designed employing an infrared LED (λ=930 nm) and a photodiode. When solution volume delivered from proposed device was within the range of 5 to 105 μl, a linear relationship (R = 0.999) between the delivered volumes and the generated potential difference was achieved. The usefulness of the proposed device was proved performing photometric titration of hydrochloric acid solution with a standardized sodium hydroxide solution and using phenolphthalein as an external indicator. The achieved results presented relative standard deviation of 1.5%

Automatic flow system for simultaneous determination of iron and chromium in steel alloys employing photometers based on LEDs as radiation source

A multicommutated flow system for simultaneous determination of iron and chromium in steel alloys by photometry is described. The flow network consisted of an automatic injector and four solenoid valves assembled to form two independent analytical pathways, each one comprising reaction coils and a flow cell. The light source (LED) and detector (photodiode) were attached to the flow cells to form a compact unit. The flow system was microcomputer controlled by Quick BASIC 4.5 software, which carried out all steps of the analytical procedure. The feasibility of the system was proved by the determination of iron and chromium in steel alloys and its accuracy was accessed by comparing results with those obtained by plasma atomic emission spectrometry (ICP-AES). No significant difference at the 95% confidence level was observed. Other profitable features such as low reagent consumption (0.33 mg 1,10-phenantroline and 0.03 mg 1,5-diphenylcarbazide per determination); relative standard deviations (n = 5) of 0.4% for iron and 1.2% for chromium; and an analytical throughput of 160 determinations per h were also achieved

Automatic flow analysis procedure for the determination of bromide in L-alanine by chemiluminescence detection

An automatic flow analysis procedure for bromide determination in L-alanine aminoacid employing detection by chemiluminescence is described. The procedure was based on the bromide oxidation by chloramine-T followed by reaction with luminol. Spiking sample with standard solution gave recoveries values ranging from 94 to 106 %. Profitable features such as linear response ranging from 0.01 to 1.000 mg L-1 bromide (R = 0.999); detection limit of 8.9 µg L-1 Br-; relative standard deviation of 3.0% (n = 10); sampling throughput of 18 determination per hour; and reagent consumption 0.07 mg luminol and 0.4 mg chloramine-T per determination were achieved

Multicommuted flow system for the determination of glucose in animal blood serum exploiting enzymatic reaction and chemiluminescence detection

An automatic flow procedure based on multicommutation dedicated for the determination of glucose in animal blood serum using glucose oxidase with chemiluminescence detection is described. The flow manifold consisted of a set of three-way solenoid valves assembled to implement multicommutation. A microcomputer furnished with an electronic interface and software written in Quick BASIC 4.5 controlled the manifold and performed data acquisition. Glucose oxidase was immobilized on porous silica beads (glass aminopropyl) and packed in a minicolumn (15 × 5 mm). The procedure was based on the enzymatic degradation of glucose, producing hydrogen peroxide, which oxidized luminol in the presence of hexacyanoferrate(III), causing the chemiluminescence. The system was tested by analysing a set of serum animal samples without previous treatment. Results were in agreement with those obtained with the conventional method (LABTEST Kit) at the 95% confidence level. The detection limit and variation coefficient were estimated as 12.0 mg l(−1) (99.7% confidence level) and 3.5% (n = 20), respectively. The sampling rate was about 60 determinations h(−1) with sample concentrations ranging from 50 to 600 mg l(−1) glucose. The consumptions of serum sample, hexacyanoferrate(III) and luminol were 46 μl, 10.0 mg and 0.2 mg/determination, respectively

An improved flow system for spectrophotometric determination of anions exploiting multicommutation and multidetection

Abstract A multicommutated flow system is proposed for the determination of anions in water samples. The flow set up was assembled with a set of computer-controlled three-way solenoid valves in order to manage the addition of different reagents by binary sampling. An optical-fiber CCD-array spectrophotometer with a tungsten-halogen lamp was employed for multidetection. Water samples were used as carrier and the chromogenic reagents were intermittently added, allowing the sequential determination of nitrate, nitrite, chloride and phosphate with or without in-line concentration by ion exchange. In-line concentration of the analytes was performed during the signal measurements of the other species. In this way, a 180 s loading time was implemented without impairing the sampling rate (estimated as 50 determinations per hour). Under the proposed conditions, the procedure can be used for samples containing 30-300 g l −1 N-NO 2 − , 0.1-1.0 mg l −1 N-NO 3 − , 1.0-10 mg l −1 Cl − , and 0.05-2.5 mg l −1 P-PO 4 3− . Detection limits were estimated as 6 g l −1 N-NO 2 − , 40 g l −1 N-NO 3 − , 400 g l −1 Cl − and 30 g l −1 P-PO 4 3− at 99.7% confidence level. Coefficients of variation were estimated (n = 20) as 1.6, 2.2, 2.3 and 1.5% for nitrite, nitrate, chloride and phosphate, respectively. The reagent consumption was reduced from 3-to 40-fold and from 20-to 760-fold regarding the conventional FIA systems and batch procedures, respectively. Results for river water samples agreed with those obtained by single-analyte FIA procedures at the 95% confidence level

Evaluation of a Multicommuted Flow System for Photometric Environmental Measurements

A portable flow analysis instrument is described for in situ photometric measurements. This system is based on light-emitting diodes (LEDs) and a photodiode detector, coupled to a multipumping flow system. The whole equipment presents dimensions of 25  cm × 22  cm × 10  cm, weighs circa 3 kg, and costs 650 €. System performance was evaluated for different chemistries without changing hardware configuration for determinations of (i) Fe3+ with SCN-, (ii) iodometric nitrite determination, (iii) phenol with sodium nitroprusside, and (iv) 1-naphthol-N-methylcarbamate (carbaryl) with p-aminophenol. The detection limits were estimated as 22, 60, 25, and 60 ng mL -1 for iron, nitrite, phenol, and carbaryl at the 99.7% confidence level with RSD of 2.3, 1.0, 1.8, and 0.8%, respectively. Reagent and waste volumes were lower than those obtained by flow systems with continuous reagent addition. Sampling rates of 100, 110, 65, and 72 determinations per hour were achieved for iron, nitrite, phenol, and carbaryl determination

Monosegemented flow potentiometric titration for the determination of chloride in milk and wine

An automated flow potentiometric titration procedure for the determination of chloride in milk and wine exploiting the monosegmented flow approach is described. The flow network was designed based on a six-way solenoid valve, controlled by a microcomputer running software written in VisualBasic 3.0, allowing selection of the titration conditions. An Ag2S tubular electrode selective for Cl- and a conventional Ag/AgCl electrode were employed as indicator and reference, respectively. An algorithm based on the potential difference between two subsequent titrant additions was developed, allowing to reach the end point in less than 10 attempts, with a precision better than 1.0%. The proposed system was evaluated by determining chloride in milk and wine, using a standard AgNO3 solution as titrant. Accuracy was ascertained by comparing the results with those obtained using the AOAC procedure. No significant difference at a 95% confidence level was observed.Este trabalho descreve um procedimento automático em fluxo monossegmentado para titulação potenciométrica aplicado à determinação de cloreto em leite e vinho. O sistema de fluxo foi desenvolvido com base em uma válvula solenóide de 6 vias, controlada por um microcomputador através de um programa escrito em VisualBasic 3.0. Um eletrodo indicador tubular de Ag2S seletivo a Cl- e um eletrodo de referência convencional de Ag/AgCl foram empregados. Um algoritmo baseado na diferença de potencial entre duas adições subsequentes de titulante foi desenvolvido, possibilitando a determinação do ponto final da titulação em, no máximo, 10 tentativas, com uma precisão melhor que 1,0%. O sistema proposto foi avaliado pela determinação de cloreto em leite e vinho, usando uma solução padrão de AgNO3 como titulante. A exatidão foi avaliada comparando-se os resultados com aqueles obtidos pelo método da AOAC, não sendo encontradas diferenças significativas ao nível de confiança de 95%.259264Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP