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- 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.
- Spectrophotometric determination of Bromate in water using multisyringe flow injection analysisPublication . Oliveira, Sara M.; Segundo, Marcela A.; Rangel, António O. S. S.; Lima, José L. F. C.; Cerdà, VíctorA multisyringe flow injection system for the spectrophotometric determination of bromate in water is proposed, based on the oxidation of phenothiazine compounds by bromate in acidic medium. Several phenothiazines were tested, including chlorpromazine, trifluoperazine, and thioridazine. Higher sensitivity and lower LOD were attained for chlorpromazine. Interference from nitrite, hypochlorite, and chlorite was eliminated in-line, without any changes in the manifold. The automatic methodology using chlorpromazine allowed the determination of bromate between 25 and 750 lgL 1, with LOD of 6 lgL 1, good precision (RSD<1.6%, n¼10), and determination frequency of 35 h 1.