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- Use of tetramethylbenzidine for the spectrophotometric sequential injection determination of free chlorine in watersPublication . Mesquita, Raquel B. R.; Noronha, M. Lúcia F.O. B.; Pereira, Ana I. L.; Santos, Arménia C. F.; Torres, André F.; Víctor, Cerdà; Rangel, António O. S. S.A sequential injection (SI) method was developed for the spectrophotometric determination of chlorine based on the reaction between tetramethylbenzidine (TMB) and free chlorine. The advantages resulting from the use of TMB are considerable: TMB is highly selective for chlorine, it enables a fairly low quantification limit and represents a less toxic alternative to reagents such as tolidine. The use of this reaction in SI adds other advantages as it enhances the degree of automation, minimisation of reagent consumption (6.8 g TMB/assay) and low effluent production (2.5 mL/determination). The developed method allowed a quantification limit of 90 g/L with a working range of 0.09–1.30 mg OCl−/L and a determination rate of 60 det./h. Based on these features, the system was applied to tap-water and surface water samples with no previous treatment required. The results obtained with the developed system were compared to the reference method, diethyl-p-phenylelediamine (DPD) colorimetric method, and proved not to be statistically different.
- Development of a flow method for the determination of phosphate in estuarine and freshwaters - Comparison of flow cells in spectrophotometric sequential injection analysisPublication . Mesquita, Raquel B. R.; Ferreira, M. Teresa S. O. B.; Tóth, Ildikó V.; Bordalo, Adriano A.; McKelvied, Ian D.; Rangel, António O. S. S.A sequential injection system with dual analytical line was developed and applied in the comparison of two different detection systems viz; a conventional spectrophotometer with a commercial flow cell, and a multi-reflective flow cell coupled with a photometric detector under the same experimental conditions. The study was based on the spectrophotometric determination of phosphate using the molybdenum-blue chemistry. The two alternative flow cells were compared in terms of their response to variation of sample salinity, susceptibility to interferences and to refractive index changes. The developed method was applied to the determination of phosphate in natural waters (estuarine, river, well and ground waters). The achieved detection limit (0.007 mu M PO43-) is consistent with the requirement of the target water samples, and a wide quantification range (0.024-9.5 mu M) was achieved using both detection systems.
- A flow system for the spectrophotometric determination of lead in different types of waters using ion-exchange for pre-concentration and elimination of interferencesPublication . Mesquita, Raquel B. R.; Fernandes, Sílvia M.V.; Rangel, António O.S.S.A flow system for the spectrophotometric determination of lead in natural and waste waters is proposed. The determination is based on the colorimetric reaction between malachite green and iodide, followed by the formation of a ternary complex between those reagents and lead cations. The developed flow system includes a lead pre-concentration step in a column packed with a cationic resin (Chelex 100) operating in a sequential injection mode. To improve the mixture of sample and reagents, a flow injection approach was adopted for the colorimetric determination. This way a hybrid flow system, involving both sequential and flow injection concepts was designed. Another feature of the proposed system is the efficient elimination of major interferent species, such as cadmium and copper. The elimination of cadmium interference is obtained by complexing Cd2+ with chloride and retaining the formed negatively charged complexes in an anionic resin, AG1 X-8. As for copper, with the presence of both ionic resins as well as the conditions for cadmium elimination, it no longer acts as an interferent. Different ranges of lead concentration (50–300 and 300–1000 g l−1) can be determined with minor changes in the controlling software, useful for application to both natural and waste waters. Therefore, a detection limit of 25 g l−1 was achieved. Repeatability was evaluated from 10 consecutive determinations being the results better than 4%. The recoveries of lead spikes added to the samples ranged from 93 to 102%. The sampling frequency was 17 and 24 determinations per hour, for 50–300 and 300–1000 g l−1 ranges, respectively.
- Gas diffusion sequential injection system for the spectrophotometric determination of free chlorine with o-dianisidinePublication . Mesquita, Raquel B. R.; Rangel, António O. S. S.A gas diffusion sequential injection system for spectrophotometric determination of free chlorine is described. The detection is based in the colorimetric reaction between free chlorine and a low toxicity reagent o-dianisidine. A gas diffusion unit is used to isolate free chlorine from the sample in order to avoid possible interferences. This feature results from the conversion of free chlorine to molecular chlorine (gaseous) with sample acidification. With minor changes in the operating conditions, two different dynamic ranges were obtained enhancing the application both to water samples and bleaches. The results obtained with the developed system were compared to the reference method, iodometric titration and proved not to be statistically different. A detection limit of 0.6 mg ClO−/L was achieved. Repeatability was evaluated from 10 consecutive determinations being the results better than 2%. The two dynamic ranges presented different determination rates: 15 h−1 for 0.6–4.8 mg ClO−/L (water samples) and 30 h−1 for 0.047–0.188 g ClO−/L (bleaches).
- Spectrophotometric determination of carbon dioxide and sulphur dioxide in wines by flow injectionPublication . Atanassov, G.T.; Lima, R.C.; Mesquita, Raquel B. R.; Rangel, António O. S. S.; Tóth, I.V.Flow injection analysis (FIA) methods for the spectrophotometric determination of CO2 and SO2 in wines are described. The determination of CO2 is based on the colour change of a low capacity buffer (containing an acid-base indicator) due to the dissolved carbon dioxide. The determination of SO2 is based on the decoloration of malachite green by sulphur dioxide. Two FIA manifolds are presented; one for the determination of CO2 in sparkling wines and another for the simultaneous determination of CO2 and SO2 in table wines. The analytes are isolated inside the manifold from the sample matrix using gas-diffusion units. Regression equations (FIA versus reference methods) showed no statistical difference, at 95 % confidence level, between the two sets of results for both determinations; additionally, for the determination of CO2, recovery values between 93.5 % and 111 % were found. RSD lower than 4.5 % for SO2 and 2.4 % for the CO2 determination were found. The sampling rates achieved were: 30 h–1 for the uniparametric system and 40 h–1 for the biparametric system. The single determination manifold is applicable in the concentration ranges of 0.5 to 4 g L–1 of CO2, and the simultaneous determination manifold in the range of 0.25 to 3 g L–1 of CO2 and 0.05 to 0.3 g L–1 of SO2
- Iodine speciation in coastal and inland bathing waters and seaweeds extracts using a sequential injection standard addition flow-batch methodPublication . Santos, Inês C.; Mesquita, Raquel B. R.; Bordalo, Adriano A.; Rangel, António O. S. S.The present work describes the development of a sequential injection standard addition method for iodine speciation in bathing waters and seaweeds extracts without prior sample treatment. Iodine speciation was obtained by assessing the iodide and iodate content, the two inorganic forms of iodine in waters. For the determination of iodide, an iodide ion selective electrode (ISE) was used. The indirect determination of iodate was based on the spectrophotometric determination of nitrite (Griess reaction). For the iodate measurement, a mixing chamber was employed (flow batch approach) to explore the inherent efficient mixing, essential for the indirect determination of iodate. The application of the standard addition method enabled detection limits of 0.14 µM for iodide and 0.02 µM for iodate, together with the direct introduction of the target water samples, coastal and inland bathing waters. The results obtained were in agreement with those obtained by ICP-MS and a colorimetric reference procedure. Recovery tests also confirmed the accuracy of the developed method which was effectively applied to bathing waters and seaweed extracts.
- Use of solid phase extraction for the sequential injection determination of alkaline phosphatase activity in dynamic water systemsPublication . Santos, Inês C.; Mesquita, Raquel B.R.; Bordalo, Adriano A.; Rangel, António O.S.S.In this work, a solid phase extraction sequential injection methodology for the determination of alkaline phosphatase activity in dynamic water systems was developed. The determination of the enzymatic activity was based on the spectrophotometric detection of a coloured product, p-nitrophenol, at 405 nm. The p-nitrophenol is the product of the catalytic decomposition of p-nitrophenyl phosphate, a noncoloured substrate. Considering the low levels expected in natural waters and exploiting the fact of alkaline phosphatase being a metalloprotein, the enzyme was pre-concentrated in-line using a NTA Superflow resin charged with Zn2þ ions. The developed sequential injection method enabled a quantification range of 0.044–0.441 unit mL 1 of enzyme activity with a detection limit of 0.0082 unit mL 1 enzyme activity (1.9 mmol L 1 of pNP) and a determination rate of 17 h 1. Recovery tests confirmed the accuracy of the developed sequential injection method and it was effectively applied to different natural waters and to plant root extracts.
- Development of sequential injection methodologies for the spectrophotometric direct and kinetic determination of aluminium in natural and waste watersPublication . Mesquita, Raquel B. R.; Rangel, António O. S. S.Two sequential injection methodologies for the spectrophotometric determination of reactive aluminium in water samples are proposed, based on the reaction between chrome azurol S (CAS) and aluminium. The two methods involve a direct and a kinetic methodology (for its application to coloured waste waters), both accommodated within the same manifold. The working ranges obtained were: 0.040-0.500 mg Al Lˉ¹ for direct method and 0.050-0.300 mg Al Lˉ¹ for the kinetic method. The described system has high degree of automation, enabling sampling throughputs of 31 and 57 hˉ¹ for the kinetic method and direct methods, respectively. The reagents consumption per determination is low: 46 μg of CAS, 3.75 mg of sodium acetate and 25 μg of ascorbic acid. The volume of effluent produced per determination is only around 2.8 mL in the direct method and 3.4 mL in the kinetic method.
- Screening of cadmium and lead in potentially contaminated waters using a spectrophotometric sequential injection lab-on-valve methodologyPublication . Santos, Inês C.; Mesquita, Raquel B. R.; Rangel, António O. S. S.The present work describes the development of a µSI-LOV method for the simultaneous screening of cadmium and lead in potentially contaminated water samples. To attain the biparametric determination, dithizone was chosen as the spectrophotometric reagent as it forms a colored complex with both metal ions, at different pH conditions. The cadmium determination was attained in strong alkaline conditions (pH≈12); the lead determination was calculated by the difference with the determination of both metals in mild alkaline conditions (pH≈8). The colored complex was measured at 550 nm and the method presented a LOD of 34 μg L−1 for cadmium and 56 μg L−1 for lead, with a sample consumption of 20 µL per assay and a determination rate of 55 h−1. The results obtained were in agreement with those obtained by FAAS. The developed method was efficiently applied to the screening of cadmium and lead in marine port waters.