The supply of drinking water in the Metropolitan Area of São Paulo City has been a great and serious challenge in the latest years. This work demonstrates the viability of the evaluation of the degree of contamination of the water reservoirs using analytical procedures, which allow the analysis of several compounds at relatively low cost: stripping square wave voltammetry (SSWV) and capillary zone electrophoresis with contactless conductivity detection (CZE-CCD). The results of ionic composition indicated significant contamination of the Guarapiranga water system by human activities on the reservoir banks. In fact, the Guavirutuba and Itupu streams presented high concentrations of phosphate and ammonium ions. This can be directly related to misuse and unruled occupation of the soil and precarious sanitary infrastructure.

Neste trabalho é descrita a construção de um microssistema em silício para retenção de íons cobre(II). Processo fotolitográfico convencional foi empregado para transferir o padrão de microcanais para o substrato de silício. Utilizando corrosão por íons reativos (RIE) com plasma de SF6, foram produzidos canais de 50 µm de largura e 10 µm de profundidade. Os canais foram selados com vidro de borossilicato utilizando-se a técnica de soldagem anódica. Para promover a retenção dos íons cobre(II), a superfície dos canais foi modificada através de reação de silanização com N-(beta-aminoetil)-gama-aminopropiltrimetóxisilano. Os íons cobre(II) foram detectados amperometricamente na saída do canal utilizando-se um eletrodo de ouro. Os íons cobre(II) foram eluídos com HCl 50 mmol L-1 em um sistema micro-FIA com fluxo de 100 µL min-1. A reprodutibilidade em termos de área e altura do pico foram de 4,6 % e 10 %, respectivamente, para três injeções consecutivas de 600 µL de solução de cobre(II) 10 µmol L-1.

This work describes the construction of a silicon microchip for retention of copper(II) metal ions. Conventional photolithographic process was applied to transfer the generated pattern to silicon wafers. Using Reactive Ion Etching (RIE), SF6 based, channels 50 µm wide and 10 µm deep were produced. The channels were sealed with borosilicate glass using anodic bonding process. The surface of the channels were modified with N-(beta-aminoethyl)-gamma-aminopropyltrimetoxysilane through a silanization reaction to promote the adsorption of copper(II) ions. An amperometric detector was placed at the microchip outlet and copper(II) ions were detected by a gold electrode at 0 V (against Ag/AgCl(KCl sat.) reference electrode). Copper(II) ions were retained and eluted with HCl 50 µmol L-1 in a micro-flow system at a flow rate about 100 µL min-1. Reproducibility in the peak area and height were about 4.6 % and 10 %, respectively, for three consecutive injections of 600 µL of 10 µmol L-1 copper(II) sample.

In this work a simple and versatile procedure is described for treating water samples using small polypropylene (PP) vials (4 mL) for determining heavy metals by square wave voltammetry (SWV). This procedure involves treatment with nitric acid (0.2 mol L-1) and boiling in a water-bath (~ 100 ºC). This process is completed after one hour and allows the pretreatment of several samples simultaneously. The accuracy was estimated using addition/recovery studies and certified water sample analysis, yielding an agreement near to 100%.

Este trabalho apresenta a determinação de diversos analitos em água de coco por eletroforese capilar com detecção condutométrica sem contato (CCD). Foram analisadas 5 diferentes amostras: duas não processadas (naturais) e três industrialmente processadas (comerciais). As amostras foram injetadas sem tratamento prévio e apenas uma simples diluição foi necessária. A técnica foi aplicada para quantificação de 12 analitos: cloreto, sulfato, fosfato, malato, ascorbato, potássio, sódio, cálcio, magnésio, frutose, glicose e sacarose, sendo que seus respectivos limites de detecção (LOD) são: 0,09; 0,12; 0,50; 0,97; 1,2; 0,05; 0,17; 0,12; 0,08; 5,4; 7,4 e 8,9 mg L-1. Para realizar estas análises, foram utilizados quatro tampões de corrida diferentes.

This work presents the determination of several analytes in coconut water by using capillary electrophoresis with contactless conductivity detection (CCD). It was analyzed 5 different samples: two unprocessed (natural) coconut water and three processed (commercial) ones. The samples were injected without pretreatment and only a simple dilution was necessary. The technique was applied to quantify 12 analytes: chloride, sulfate, phosphate, malate, ascorbate, potassium, sodium, calcium, magnesium, fructose, glucose, and sucrose with limit of detection (LOD) of 0.09, 0.12, 0.50, 0.97, 1.2, 0.05, 0.17, 0.12, 0.08, 5.4, 7.4, and 8.9 mg L-1, respectively. These analysis were done utilizing four different running buffers.

Um sistema sensível e seletivo para boro, utilizando um sistema de análise por injeção em fluxo com detecção piezelétrica, é apresentado. O detector é um cristal piezelétrico de quartzo com eletrodo separado recoberto com filme de poliepicloridrina modificada com N-metil-D-glucamina. A capacidade do filme em reter boro possibilita ampliar a faixa de resposta linear e a sensibilidade, variando o volume de amostra injetada. Neste trabalho, o volume de amostra variou de 0,5 a 5,0 mL. Dentre diversos íons analisados, germanato foi o único interferente. Entretanto, essa interferência pode ser eliminada com a adição de sulfeto à amostra. O método se mostrou eficiente na determinação de boro em amostras de água natural (de 1,71 a 309 µg L-1) e produtos derivados da uva (de 2,06 a 6,21 mg L-1). Um pré-tratamento com peróxido de hidrogênio em meio básico foi necessário devido à grande quantidade de carboidratos presentes no suco de uva.

An automated flow injection analysis system with piezoelectric detection is proposed as a sensitive and selective method for boron. The detector is an electrode-separated piezoelectric quartz crystal coated with N-methyl-D-glucamine-modified poly(epichlorohydrin). The film ability to retain boron allows the adjustment of the linear dynamic range and the sensitivity by varying the injected sample volume. In the present work, the sample volumes were varied from 0.5 to 5.0 mL. Among several ionic species, germanate is the only one that can interfere in the method. Nevertheless, it can be eliminated by addition of sulfide to the sample. The method was successfully applied to the determination of boron concentration in samples of natural water (from 1.71 to 309 µL-1) and products derived from grape juice (from 2.06 to 6.21 mg L-1). A pretreatment with hydrogen peroxide in alkaline medium was required due to the great amount of sugars in the grape products.

O controle do conteúdo de íons inorgânicos em combustíveis veiculares tem uma importante função na manutenção do motor. Um método novo e versátil para análise rápida de íons em etanol é apresentado. Eletroforese capilar foi utilizada para quantificar cátions (sódio, potássio, cálcio, magnésio e amônio) e ânions (sulfato, cloreto e nitrato). A injeção direta da amostra no capilar apresentou falta de repetibilidade nos resultados. A evaporação prévia do etanol, seguida pela resuspensão do material residual, levou a resultados confiáveis. Os limites de detecção para os oito íons estiveram na faixa de 0,06 a 0,18 mg L-1. Limites de detecção inferiores podem ser obtidos com o aumento do tempo de injeção e/ou da pressão de injeção.

The control of the content of inorganic ions in vehicular fuels plays an important role in the engine maintenance. A novel and versatile methodology to carry out rapid analysis of ions in ethanol is presented. Capillary electrophoresis was used to quantify cations (sodium, potassium, calcium, magnesium, and ammonium) and anions (sulfate, chloride, and nitrate). The injection of the sample directly in the capillary shows some lack of repeatability of the results. The prior evaporation of the ethanol, followed by a re-suspension of the residual material, leads to reliable results. The detection limits of the eight ions range between 0.06 and 0.18 mg L-1. Lower detection limits could be attained by increasing the injection time and/or the injection pressure.

This article describes a novel approach to the separation of fatty acids ranging from 8 to 20 carbons using capillary electrophoresis with contactless conductivity detection. Complete separation of nine linear chain fatty acids (from C8:0 to C20:0) was achieved in 15 min under normal polarity operation. Limits of detection ranged from 35 to 319 µmol L-1 for C20:0 to C8:0, respectively. The optimized running electrolyte composition was 5.0 mmol L-1 phosphate buffer at pH 7, 4.0 mmol L-1 dimethyl-b-cyclodextrin, 2.0 mmol L-1 trimethyl-b-cyclodextrin, acetonitrile 50% (v/v), and methanol 20% (v/v). The applicability of the separation system was demonstrated by the analysis of coconut vegetable oil.

This paper presents a new way for the construction of silver electrodes utilizing recordable CDs. The new electrodes were explored for the quantification of chloride (by potentiometry/FIA), cyanide (by amperometry/FIA) and for lead analysis (by square wave voltammetry). For the flowing measurements, a digital multimeter, connected to a microcomputer (via RS 232 interface) was used to collect directly the potential signal (for Cl- measurements) or to take the output signal from a potentiostat (for CN- measurements). The square wave voltammetry analysis was performed in a commercial instrument. The results shown good performance of the new electrodes and the detection limit (s/n = 3) attained for these three analytes were: 0.2, 50, and 200 µg L-1 for Pb2+, Cl-, and CN- respectively.

Um dos usos mais comuns da eletroforese capilar com detecção condutométrica é a análise de vários tipos de amostras contendo metais alcalinos e alcalinos terrosos. No entanto, a alta concentração de sódio, a qual é uma ocorrência bastante comum, pode causar perda de resolução de alguns picos. Neste trabalho, as condições e o eletrólito de corrida conveniente para análises de soro e fluído para hemodiálise são apresentados. A idéia básica é deslocar os picos de Ca2+ e Mg2+ pela redução de suas mobilidades pela adição de lactato e metanol ao eletrólito de corrida. Limites de detecção da ordem de 0,5 a 1,0 mmol L-1 e razão molar Na+/Ca2+ da ordem de 1000 foram obtidos. Estas condições excedem as necessidades da aplicação pretendida.

One of the most common uses of capillary electrophoresis with conductometric detection is the analysis of different samples containing alkaline and alkaline earth metals. However, the high sodium content, which is a very common occurrence, may cause loss of resolution of some peaks. In this work, the conditions and a running buffer suitable for serum and hemodialysis fluid analyses are presented. The approach basically consists in the reduction of mobilities of Ca2+ and Mg2+ by addition of methanol and lactate in the running buffer. Limits of detection in the range from 0.5 to 1.0 mmol L-1 with molar Na+/Ca2+ ratios as high as 1000 were obtained, which are conditions that exceed the requirements of the proposed determination.

Um sensor a cristal piezelétrico de quartzo com eletrodos separados e superfície quimicamente modificada foi proposto. A silanização com N-2-aminoetil-3-aminopropiltrimetoxisilano permitiu a imobilização do grupo N-2-aminoetil-3-aminopropilsilano sobre a superfície de um cristal de quartzo de 3,5 MHz. Uma cela em fluxo foi fabricada em poli(metacrilato de metila) com dois eletrodos de latão. Nesta cela, a solução entra em contato somente com um lado do cristal e o eletrodo é recoberto com um filme de poliéster, prevenindo assim a corrosão do eletrodo. Esta inovação reduz o custo da cela e proporciona o desacoplamento DC. O cristal modificado mostrou-se mais sensível a íons cobre (II) do que a magnésio(II), níquel(II), zinco(II) e cobalto(II). Para injeções de 100 miL de amostra, o limite de detecção para cobre(II) foi de 6 mimol L-1 que é um resultado significativo comparado com aqueles obtidos com cristal não modificado.

An electrode-separated piezoelectric quartz crystal sensor with a chemically modified surface was proposed. The modification was carried out by a silanization procedure with N-2-aminoethyl-3-aminopropyltrimethoxysilane, yielding the immobilised N-2-aminoethyl-3-aminopropylsilane group over the surface of a 3.5 MHz piezoelectric quartz crystal. A flow cell was manufactured with poly(methyl methacrylate) and brass, instead of noble metals, for the electrodes. In this cell, the solution touches only one side of the crystal and the related electrode is coated with a polyester film, which prevents corrosion and does not disturb the oscillation process. This innovation reduces the cost of the cell and renders an electronics non DCcoupled to the solution. The modified crystal proved to be more sensitive to copper(II) ions than magnesium(II), nickel(II), zinc(II), and cobalt(II). For 100muL sample injections, the limit of detection for copper(II) was 6 mumol L-1, which is an impressive result when compared with that for an unmodified crystal.

A piezoelectric detector based on a commercial quartz crystal of 3.57MHz is shown. A PTFE cell attached to the GC-column outlet holds the polymer-coated crystal, whose terminals were removed. Two TTL oscillators (reference and sensor) are used and the beating of their frequencies is monitored through a home-made counter card inserted in a microcomputer. The original thermal conductivity detector was also interfaced, but through a 12-bit analog-to-digital converter. In spite of the well-known fact that QCM has low sensitivity at high temperatures, results show significant peak deformation for low temperatures. In addition, the phenomenon is also dependent on the chemical composition of the absorbent film besides instantaneous partial pressure and chemical composition of the analyte.

A simple and inexpensive device to automate a water distilling apparatus is shown. It is composed by a magnetic floater placed in the water reservoir and a level control unit, which acts over the heating element circuit. In order to provide water saving, an electromagnetic valve is inserted in the water supply inlet. Some suggestions for the adaptation to other types of equipment are also offered.