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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.
- 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.
- Use of a Mixing Chamber for Sample Preparation and Multiple Collection in Sequential Injection Analysis: Determination of Sulfate in WinesPublication . Silva, Helena R.; Segundo, Marcela A.; Rangel, António O. S. S.A sequential injection system for determination of sulfate in wines was developed. It was based on the formation of BaSO4, measured turbidimetrically at 420 nm. As sample dilution and acidification were required, both sample and acid were sent to a mixing chamber placed in a lateral port of the selection valve; after thorough mixing, up to six aliquots could be drawn and analyzed. A linear calibration curve was established using 10% v/v ethanol standards with concentrations between 300 and 1500 mg L-1 of K2SO4. The results obtained by the present methodology were statistically comparable with those furnished by the reference procedure, with relative deviations < 3.5%. The sample frequency was about 5 samples per h with relative standard deviations (RSD) < 10%.
- Automatic flow systems based on sequential injection analysis for routine determinations in winesPublication . Segundo, Marcela A.; Lima, José L.F.C.; Rangel, António O.S.S.Sequential injection systems for wine analysis have been developed in recent years for determination of more than 20 species. Several aspects of these systems are reviewed in the present paper. Special focus is given to implementation of in-line sample treatment and adaptation of system operation through software control to enable determination in different types of wine. The strategies used to enhance selectivity and the capacity for multi-parameter determination are also addressed.