Development of an FIA system with amperometric detection for determination of bentazone in estuarine waters

On the basis of its electrochemical behaviour a new flow-injection analysis (FIA) method with amperometric detection has been developed for quantification of the herbicide bentazone (BTZ) in estuarine waters. Standard solutions and samples (200 µL) were injected into a water carrier stream and both pH and ionic strength were automatically adjusted inside the manifold. Optimization of critical FIA conditions indicated that the best analytical results were obtained at an oxidation potential of 1.10 V, pH 4.5, and an overall flow-rate of 2.4 mL min–1. Analysis of real samples was performed by means of calibration curves over the concentration range 2.5x10–6 to 5.0x10–5 mol L–1, and results were compared with those obtained by use of an independent method (HPLC). The accuracy of the amperometric determinations was ascertained; errors relative to the comparison method were below 4% and sampling rates were approximately 100 samples h–1. The repeatability of the proposed method was calculated by assessing the relative standard deviation (%) of ten consecutive determinations of one sample; the value obtained was 2.1%.

Amperometric and spectrophotometric determination of carbaryl in natural waters and commercial formulations

The work presented describes the development and evaluation of two flow-injection analysis (FIA) systems for the automated determination of carbaryl in spiked natural waters and commercial formulations. Samples are injected directly into the system where they are subjected to alkaline hydrolysis thus forming 1-naphthol. This product is readily oxidised at a glassy carbon electrode. The electrochemical behaviour of 1-naphthol allows the development of an FIA system with an amperometric detector in which 1-naphthol determination, and thus measurement of carbaryl concentration, can be performed. Linear response over the range 1.0×10–7 to 1.0×10–5 mol L–1, with a sampling rate of 80 samples h–1, was recorded. The detection limit was 1.0×10–8 mol L–1. Another FIA manifold was constructed but this used a colorimetric detector. The methodology was based on the coupling of 1-naphthol with phenylhydrazine hydrochloride to produce a red complex which has maximum absorbance at 495 nm. The response was linear from 1.0×10–5 to 1.5×10–3 mol L–1 with a detection limit of 1.0×10–6 mol L–1. Sample-throughput was about 60 samples h–1. Validation of the results provided by the two FIA methodologies was performed by comparing them with results from a standard HPLC–UV technique. The relative deviation was <5%. Recovery trials were also carried out and the values obtained ranged from 97.0 to 102.0% for both methods. The repeatability (RSD, %) of 12 consecutive injections of one sample was 0.8% and 1.6% for the amperometric and colorimetric systems, respectively.

Measurements of environmental background radiation in the surrounding area of a coal-fired power plant

Certain materials used and produced in a wide range of non-nuclear industries contain enhanced activity concentrations of natural radionuclides. In particular, electricity production from coal is one of the major sources of increased exposure to man from enhanced naturally occurring materials. Over the past decades there has been some discussion about the elevated natural background radiation in the area near coal-fired power plants due to high uranium and thorium content present in coal. This work describes the methodology developed to assess the radiological impact due to natural radiation background increasing levels, potentially originated by a coal-fired power plant’s operation. Gamma radiation measurements have been done with two different instruments: a scintillometer (SPP2 NF, Saphymo) and a gamma ray spectrometer with energy discrimination (Falcon 5000, Canberra). A total of 40 relevant sampling points were established at locations within 20 km from the power plant: 15 urban and 25 suburban measured stations. The highest values were measured at the sampling points near to the power plant and those located in the area within the 6 and 20 km from the stacks. This may be explained by the presence of a huge coal pile (1.3 million tons) located near the stacks contributing to the dispersion of unburned coal and, on the other hand, the height of the stacks (225 m) which may influence ash’s dispersion up to a distance of 20 km. In situ gamma radiation measurements with energy discrimination identified natural emitting nuclides as well as their decay products (212Pb, 214Pb, 226Ra 232Th, 228Ac, 234Th 234Pa, 235U, etc.). This work has been primarily done to in order to assess the impact of a coal-fired power plant operation on the background radiation level in the surrounding area. According to the results, an increase or at least an influence has been identified both qualitatively and quantitatively.