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- A pilot study combining ultrafiltration with ozonation for the treatment of secondary urban wastewater: organic micropollutants, microbial load and biological effectsPublication . Graça, Cátia A. L.; Ribeirinho-Soares, Sara; Abreu-Silva, Joana; Ramos, Inês I.; Ribeiro, Ana R.; Castro-Silva, Sérgio M.; Segundo, Marcela A.; Manaia, Célia M.; Nunes, Olga C.; Silva, Adrián M. T.Ozonation followed by ultrafiltration (O3 + UF) was employed at pilot scale for the treatment of secondary urban wastewater, envisaging its safe reuse for crop irrigation. Chemical contaminants of emerging concern (CECs) and priority substances (PSs), microbial load, estrogenic activity, cell viability and cellular metabolic activity were measured before and immediately after O3 + UF treatment. The microbial load was also evaluated after one-week storage of the treated water to assess potential bacteria regrowth. Among the organic micropollutants detected, only citalopram and isoproturon were not removed below the limit of quantification. The treatment was also effective in the reduction in the bacterial loads considering current legislation in water quality for irrigation (i.e., in terms of enterobacteria and nematode eggs). However, after seven days of storage, total heterotrophs regrew to levels close to the initial, with the concomitant increase in the genes 16S rRNA and intI1. The assessment of biological effects revealed similar water quality before and after treatment, meaning that O3 + UF did not produce detectable toxic by-products. Thus, the findings of this study indicate that the wastewater treated with this technology comply with the water quality standards for irrigation, even when stored up to one week, although improvements must be made to minimise microbial overgrowth.
- Multisyringe flow system: determination of sulfur dioxide in winesPublication . Segundo, Marcela A.; Rangel, António O. S. S.; Claderab, Andreu; Cerdà, VíctorA multisyringe flow system for the spectrophotometric determination of sulfur dioxide in wines is described. The methodology is based on the well-known reaction among SO2, formaldehyde and pararosaniline. The proposed manifold also includes a gas diffusion unit in order to prevent the colour interference of red wines in the spectrophotometric measurement. The proposed method was successfully applied to the determination of free SO2 (2–75 mg l21) and total SO2 (10–250 mg l21) in wines, just by changing a few operating parameters in the controlling software. A sampling-rate of 25–30 samples per hour was achieved with good repeatability for 10 consecutive injections of wine samples (RSD < 3.2%). The results obtained from 10 wine samples for each determination were statistically comparable to those obtained by the recommended procedure.
- Spectrophotometric determination of bromate in drinking water using a multi-syringe flow injection systemPublication . Oliveira, Sara M.; Segundo, Marcela A.; Lima, José L. F. C.; Cerdà, Victor; Rangel, António O. S. S.
- Automatic flow system for sequential determination of ABTS scavenging capacity and Folin-Ciocalteu index: A comparative study in food productsPublication . Magalhães, Luís M.; Segundo, Marcela A.; Reis, Salette; Lima, José L. F. C.; Tóth, Ildikó V.; Rangel, António O. S. S.In the present work, an automatic flow procedure for the sequential spectrophotometric determination of Folin-Ciocalteu reducing capacity (FC assay) and 2,2 -azinobis(3-ethylbenzothiazoline-6-sulfonic acid) radical cation (ABTS•+) scavenging capacity expressed as the trolox equivalent (TEAC assay) is proposed for a comparative study of antioxidant properties in food products. Exploiting the flexibility of flow management associated to the computer control offered by multisyringe flow injection analysis, both methodologies were carried out in the same manifold using gallic acid and trolox as standard compounds. The proposed system configuration allowed the performance of each method separately or in tandem, providing 24 determinations per hour, which accounts for its application in routine analysis. The present methodology was applied to a large number of beverages (n = 72), namely red and white wines, herbal and tea infusions, juices and beers. The results obtained showed that FC reducing capacity and TEAC values of red wines were significantly different from those obtained for the other beverages, while tea infusions provided significantly higher TEAC values when compared to white wines, herbal infusions, juices and beers. A good correlation was found between TEAC and FC reducing capacity (R > 0.9) for red wines, herbal and tea infusions, and beers. For these beverages, similar slope values were found (106–140 mg L−1 of gallic acid per mM of Trolox), except for beers that showed a higher response for FC assay. These results provided evidence that the correlation between these assays vary according to the type of sample, reinforcing the idea that more than one method should be used for evaluation of antioxidant capacity.
- Kinetic determination of L (-)malic acid in wines using sequential injection analysisPublication . Segundo, Marcela A.; Rangel, António O. S. S.In the present work a sequential injection system for the enzymatic determination of Image (−)malic acid in wines is described. The determination was based on the detection of NADH, formed by oxidation of Image -malate to oxaloacetate, catalysed by Image -malate dehydrogenase. A kinetic method was implemented by stopping the flow when a solution plug containing sample, NAD+ and enzyme reached the detector. The rate of reaction was measured by monitoring absorbance changes at 340 nm during a fixed period of time. A linear calibration curve (rate of reaction versus concentration) was obtained for concentrations of Image (−)malic acid between 0.01 and 0.15 g l−1. The determination rate was about 22 h−1 and samples were diluted 25 or 50 times before introduction to the system. Results obtained from 16 wine samples were comparable to those obtained by the reference method.
- Food, Beverages and Agricultural ApplicationsPublication . Tóth, Ildikó V.; Segundo, Marcela A.; Rangel, António O. S. S.This chapter provides an overview of the flow methods described for the analysis of food, beverage, and agricultural samples. A beverage is a drink specifically prepared for human consumption, other than water, such as alcoholic drinks, coffee, fruit juices, and tea. The evolution of flow-injection application to food analysis is described along with distribution by commodity. Some of the analytical features of flow methods for alcoholic beverages, meat, and fish products are tabulated. The analytes illustrate the dual role that flow-based methods have in food analysis. These include flow systems devised for routine analysis based on well-established methods. However, flow systems are also applied to novel analytical tasks, such as the determination of analytes related to sensory properties or to characteristics that contribute to a value-added product. Modern agricultural economies are highly dependent on the use of pesticides. A group of key analytes of interest in monitoring food safety is the antimicrobial agents. The evaluation of freshness and the quality of meat and fish products is based on sensorial evaluation. The application of flow systems to the determination of parameters can be correlated to astringency, bitterness, body, and smoothness.
- A gas diffusion sequential injection system for the determination of sulphur dioxide in winesPublication . Segundo, Marcela A.; Rangel, António O. S. S.In the present work, a sequential injection system with spectrophotometric detection was developed for the determination of free and total sulphur dioxide in wines. It was based on the formation of a coloured product from the reaction among SO2, formaldehyde and pararosaniline. A gas diffusion unit (GDU) was incorporated into the manifold to prevent the wine matrix interference in the spectrophotometric measurement. An acid solution was added to the sample prior to its passage through the donor channel of the GDU to promote gaseous SO2 formation. For the free SO2 determination, the sample was directly aspirated into the holding coil; for the total SO2 determination, the sample was processed after previous in-line hydrolysis of bound SO2 with an alkali solution. Two second-order calibration curves were established, defining two concentration ranges: 2–40 mg l−1 for the free SO2 determination and 25–250 mg l−1 for the total SO2 determination. Relative standard deviations (n=10) were lower than 1.2% for the determination of free SO2 and lower than 2.3% for the determination of total SO2. The sample frequency was about 16 h−1. This methodology was applied to the determination of free and total sulphur dioxide in 10 table wines and the results were statistically comparable with those furnished by the recommended procedure.
- Multi-syringe flow injection system for the determination of available phosphorus in soil samplesPublication . Almeida, M. Inês G. S.; Segundo, Marcela A.; Lima, José L. F. C.; Rangel, António O. S. S.Considering the importance of monitoring the levels of nutrients present in soils and their availability to plants, an automatic methodology is proposed based on multi-syringe flow injection analysis (MSFIA) for the spectrophotometric determination of available phosphorus in soil extracts. This fully computerized flow technique allowed the development of a flow network where sample and reagents were intercalated and sent further towards the detection system. The colorimetric determination was based on the molybdenum blue method with ascorbic acid as reducing reagent and the Egner–Riehm method was applied to extract phosphorus from soil samples. A linear calibration curve was obtained between 0.75 and 15.0mgL-1. A determination frequency of 15 h-1 was achieved, with good repeatability for 12 consecutive injections of soil extracts (RSD<1.7%). The results obtained from 12 soil samples were statistically comparable to those attained by the usual batch method.
- Avaliação comparativa da utilização de compostos da família das fenotiazinas para a determinação do ião bromatoPublication . Oliveira, Sara M.; Segundo, Marcela A.; Lima, José L. F. C.; Cerdà, Victor; Rangel, António O. S. S.
- Sequential injection flow system with improved sample throughput: determination of glycerol and ethanol in winesPublication . Segundo, Marcela A.; Rangel, António O.S.S.The performance of sequential injection (SI) systems has often been criticized for its low sampling frequency. The present work describes a SI system where an injection valve and an additional pump were incorporated to enhance sample throughput rate. The proposed systemwas applied to the enzymatic determination of glycerol and ethanol in wines, using spectrophotometric detection and immobilized glycerol and alcohol dehydrogenases. The method proposed was applied to the determination of ethanol between 0.10 and 0.50% (v/v) and glycerol between 0.03 and 0.30 g l−1. These ranges were appropriate for determination in table and port wines, since samples were diluted 50 times before introduction into the system. The results obtained from 15 wine samples were statistically comparable to those obtained by the reference methods, with good repeatability (R.S.D. < 3.4%, n = 10). The sampling rate was 22.5 h−1, corresponding to 45 determinations per hour. This way, the time required for each determination was decreased by 30% when compared to a conventional SI system.
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