Abstract

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.

Highlights

  • Reagent and solutionsA 0.2 mol L-1 carbonate buffer solution was prepared by dissolving 13.8 g of K2CO3 in water (500 mL) and adjusting pH to 10.5 using a 0.1 mol L-1 HCl solution

  • An automatic flow analysis procedure for bromide determination in L-alanine aminoacid employing detection by chemiluminescence is described

  • In the synthesis of the L-alanine, bromide is a constitute of the raw material used in the synthesis line,[1] residual bromide could occur as contamination after the purification step

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Summary

Reagent and solutions

A 0.2 mol L-1 carbonate buffer solution was prepared by dissolving 13.8 g of K2CO3 in water (500 mL) and adjusting pH to 10.5 using a 0.1 mol L-1 HCl solution. A 1.0 mmol L-1 luminol solution was prepared by dissolving 35 mg of salt (Sigma) in 200 mL of carbonate buffer solution. This solution was prepared 24 hours before use and it was maintained in a freezer at 4 oC. Working standard solutions 0.0, 0.10, 0.20, 0.40, 0.60, 0.80, 1.00, 1.50 and 2.00 mg L-1 were daily prepared by dilution with water or in 0.1% (m/v) L-alanine solution. Solutions 0.1% (m/v) L-alanine were prepared everyday by dissolving 0.1 g of solid in 100 mL. A homemade electronic interface to drive the automatic injector and the solenoid valves based on the integrated circuit ULN2803 that was wired to the output port of the PCL711S interface card by mean of a multiline flat cable

Procedure
General comments
Effect of the reagent concentration
Effect of the reaction coil length
Effects of the sampling loop volume and of the sample matrix
Analytical Parameter
Flow system performance and sample analysis
Full Text
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