Avaliação das condições de precipitação do azul da Prússia sobre pó de grafite visando o desenvolvimento de eletrodos de pasta de carbono para a quantificação de nitrito

An amperometric FIA method for nitrite quantification based on nitrite electroreduction and employing a carbon paste electrode (CPE) chemically modified with iron hexacyanoferrate (HCF) as an amperometric detector was developed. The influence of experimental conditions on the preparation of the electrode materials was evaluated and the materials obtained in each study were used for the development of modified electrodes. The electrochemical sensors were prepared by a fast, simple, and inexpensive procedure, and the long-term performance of the electrodes were quite satisfactory as the stability was maintained over one year. HCF was an effective redox mediator for nitrite electroreduction in acidic media, allowing nitrite detection at +0.2 V vs. Ag/AgClsat, which is a potential free of possible interfering species that are normally present in food and water samples. The electrochemical cell used in the FIA system was similar to a batch injection analysis cell, enabling recirculation of the carrier solution. This is an attractive feature because it allows the use of a high flow rate (6 mL min-1) leading to high sensitivity and analysis speed, while keeping reagent consumption low. The proposed method had a detection limit of 9 μmol L-1 and was successfully employed for nitrite quantification in spiked water and sausage samples. The obtained results were in good agreement with those provided by the spectrophotometric official method. At a 95 % confidence level it was not observed statistical differences neither in nitrite content nor in the precision provided by both methods. The experimental conditions for the synthesis of HCF were optimized and the best electrode material was prepared by mixing FeCl3, K4[Fe(CN)6] and carbon powder subjected to an acid and thermal treatment (400 ºC), followed by ultrasonic agitation at 4 °C. This material was used to construct an electrode with improved analytical performance to reduce nitrite, which presented greater stability compared to HCF film electrodeposited on the EPC, showing that the preparation procedure of the electrode material is an effective strategy for the development of HCF modified electrodes.

Desenvolvimento de um exoesqueleto para movimentação/reabilita-ção de paraplégicos

People bedridden by paralysis/motor disability are subject to several problems due to lack of movement. Then, it is necessary to use equipments that enable the people bedridden stand up and walk, so as to reduce the problems due to lack of movement and the time of rehabilitation, impacting directly on its quality of life. The aim of this work is the development of an exoskeleton to make the movement of people with paralysis / motor impairment in the lower limbs, without help of third parties, to be activated by the user. To provide support, stability and security to the deficient, it was decided to use a structure formed by four legs, being each leg consisting of a parallel chain. The gait was obtained by combining the movement of two mechanisms: crank/rocker, responsible for oscillatory motion of the leg, and cam/follower, responsible for the foot motion on the desired trajectory. To achieve the aim of this work was conducted a study about the types of exoskeletons for locomotion/rehabilitation of people with lower limb paralysis and presented a study on the movement of the lower limb joints. It also presented a mathematical model to obtain the desired path to the foot of the exoskeleton, the static model and the design of the structure elements. In the sequence is presented the simulation of movements of a people during the human gait, experimental tests and the comparison with the human gait developed by a people without disabilities.