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Synthesis of bis-arylsulfenyl-benzo-2,1,3-thiadiazoles was accomplished using a Pd-G3 XantPhos as a simple and inexpensive catalyst. Numerous benzene thiols reacted well with 4,7-dibromo-benzo-2,1,3-thiadiazole in DMF, using K2CO3 as the base, obtaining high product yields in a short reaction time. All the synthesized compounds showed remarkable fluorescence properties with emission wavelengths in the visible range. Due to their unique properties, these compounds have potential for application as image probes in fluorescence microscopy. The study found that these compounds have a wide range of potential uses in the area of sensors, as well as displaying other useful photophysical properties.

Ceramics manufactured in Brazil and in other countries were analyzed by laser induced breakdown spectroscopy (LIBS). The LIBS spectra were employed to identify the origin of the tableware as produc...

This work presents a study involving the determination of Cd, Cr and Pb in ceramic tableware by graphite furnace atomic absorption spectrometry (GF AAS) using a simple and practical slurry sampling...

The present study provides information about the total concentration and bioaccessible fraction of metals Al, Ba, Bi, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Pb, Ti and Zn in nine different infant cereal samples. An in vitro digestion method was employed to evaluate the bioaccessibility. The determinations were performed by microwave induced plasma optical emission spectrometry (MIP OES). The bioaccessibility varied according to the type of infant cereal sample. The values of bioaccessible fraction (minimum and maximum) for Cu, Fe, Mn, Pb and Zn were 24–68, 1–10, 7–58, 24–100 and 1–7% of the total concentration, respectively. Al and Ti presented bioaccessibility in only two samples: 6% in the multicereal A and 14% in the rice and oat cereal B, respectively. The concentration of Ba, Bi, Cd, and Cr was below the limit of detection for the bioaccessibility method. The obtained concentrations were lower than the daily recommended intake for essential and toxic elements, with exception of Pb in the rice and oat A sample.

The use of surface-functionalized polymers has shown great potential for application, emphasizing the development of flexible optoelectronic devices (FOD). There are several ways to carry out this functionalization, attributing different characteristics to the resulting material. In the present study, polyethylene terephthalate (PET) films were surface-functionalized with [4-(2-hydroxy naphthyl)diazenyl] benzoic acid using UV radiation and the direct grafting method. The resulting films were characterized using different techniques, which enabled the identification of functional groups characteristic of the compound azo, thus proving that both methods used for surface functionalization were efficient. Subsequently, the sensing capabilities of these films were evaluated by being exposed to solutions of different cations. The fluorescence signal was the measurable response, in which its variation is dependent on the interaction of analytes with the functionalized surface of the PET film. The main advantages observed in this study are simplicity, low cost and the possibility of using recycled polymer, contributing to sustainable development and environmental conservation.

Selenium is an essential micronutrient for living beings, as it helps to maintain the normal physiological functions of the organism. The numerous discoveries involving the importance of this element to the health of human beings have fostered interest in research to develop enriched and functional foods. The present study evaluated the potential for bacterial strains of Enterococcus faecalis (CH121 and CH124), Lactobacillus parabuchneri (ML4), Lactobacillus paracasei (ML13, ML33, CH135, and CH139), and Lactobacillus plantarum (CH131) to bioaccumulate Se in their biomass by adding different concentrations of sodium selenite (30 to 200 mg/L) to the culture medium. Quantification of Se with UV and visible molecular absorption spectroscopy showed that the investigated bacteria were able to bioaccumulate this micromineral into their biomass. Two of the L. paracasei strains (ML13 and CH135) bioaccumulated the highest Se concentrations (38.1 ± 1.7 mg/g and 40.7 ± 1.1 mg/g, respectively) after culture in the presence of 150 mg/L of Se. This bioaccumulation potential has applications in the development of dairy products and may be an alternative Se source in the diets of humans and other animals.

The present work describes a sample preparation method using acid decomposition in reflux system for the determination of Hg on xanthan gum samples by cold vapor atomic absorption spectrometry (CV AAS). The best conditions of sample preparation method were optimized. This procedure proved to be safe for the quantification of this analyte, because no significant losses of Hg by volatilization, which is due to the efficient reflux system. The limits of detection and quantification were 0.0049 and 0.0163 μg g−1, respectively. The accuracy was evaluated through recovery tests performed with different species of Hg and CRM analysis, obtaining excellent recoveries. The values of Hg were below the LOD(m) for xanthan gum samples A and B. However, the other samples showed concentrations in the range of 0.027–0.325 μg g−1. The method proves suitable for the quantification of Hg, which is important due to the wide applicability of xanthan gum.

In the present study, the microwave induced plasma optical emission spectrometry (MIP OES) and laser-induced breakdown spectroscopy (LIBS) complementary techniques are used to determine and locate metals in ceramic tableware samples. For quantitative analysis by MIP OES, a new method for sample treatment is proposed, preparing the samples using ultrasonic decomposition aided by an acid mixture containing HNO3 and HF. The highest average concentrations were found in the group of Brazilian samples for most of the analytes. The accuracy of the quantitative method was assessed by comparing the results with two methods described in the literature. No significant differences were detected. Aiming at qualitative analysis and analyte locating by LIBS, a sample fragment was already sufficient for the analysis, being possible to observe that Al, Ba, Ca, Fe, K, Li, Mg, Na and Ti are present in the ceramic mass and decorated surface, while Cd, Co, Cr, Cu, Mn, Pb and Zn are found only on the sample surface. Besides, according to LIBS results, it would be essential to pay attention to pigmentation, which contains most of the potentially toxic elements, at locations in direct contact with food to minimize the risk of leaching and avoid human contamination. This study shows that MIP OES and LIBS can be used complementarily to improve the analytical information used to control the ceramic tableware quality and safety. The conclusions of this work can be extended to several other types of samples where both the average contents and the location of the elements are relevant.

Este trabalho apresenta uma metodologia na determinação de Mn e Zn em amostras a base de sílica por espectrometria de absorção atômica com chama após tratamento em microescala para a caracterização de óxidos mistos. Para o tratamento das amostras, foram utilizados cerca de 10 mg de óxido misto, 50 µL de HF, 50 µL de HNO3, 25 µL de H2O2 com aquecimento por micro-ondas e diluição final de 2,0 mL. O procedimento foi aplicado para a determinação de Mn e Zn, e os resultados foram comparados com a técnica semiquantitativa de fluorescência de raios-X. A exatidão foi avaliada por testes de recuperação (93,5 a 100,7 %) e RSD abaixo de 9 %.

As an alternative, cuticles from edible insects was proposed as an unconventional but viable source of chitin and chitosan. The chitin present in the mealworm's (Tenebrio molitor) cuticles was obtained biotechnologically in one step of enzymatic deproteinization and after deacetylated. Differences in the physicochemical characteristics and the properties of the cuticles, chitin, and chitosan were investigated in this study. Commercial chitosan was used as a reference sample to validate the methods used. The enzymatic deproteinization used to obtain chitin showed an efficiency of 85%. The global yield of the process (cuticle-to-chitosan) was 31.9%. The characterization results of these polymers using DSC, FT-IR, XRD, TGA, and SEM techniques demonstrate consistency with the degree of deacetylation of the obtained chitosan, allowing the differentiation between chitin and chitosan. This study suggests that the wastes of edible insect breeding should be collected and evaluated as an alternative of chitin/chitosan source.

In this paper, a comparative study between three acid decomposition procedures of milk powder samples for the determination of Ca, Cu, Fe, K, and Na by optical emission spectrometry with inductively coupled plasma is presented. Utilizing a reflux system, it was possible to increase the temperature of the digester block above the boiling point of the reaction medium, avoiding the loss of analyte and the excessive evaporation of the acids during the heating. Conditions of acidity (10 mL HNO3/H2SO4), temperature (350 °C), and decomposition time (4 h) were defined by evaluation of residual carbon content. Acid digestion in an open system with a cold finger was compared with a conventional open system (4 h ate 120 °C), as well as with microwave digestion (heating ramp to 180 °C by the time 45 min), for four commercial samples of milk powder. For the three sample preparation procedures, the values of the analyte concentrations in all analyzed samples were similar. The accuracy of the acid digestion procedures for Ca, Cu, Fe, K, and Na was assessed by the analysis of a certified reference material of milk (infant formula), and good agreement between the certified values and the measured value was obtained. The limits of quantification for the acid digestion with reflux system for Ca, Cu, Fe, K, and Na, in milligram per kilogram, were 7.48, 0.31, 1.0, 8.20, and 25.81, respectively, and for the microwave digestion were 14.0, 0.57, 1.78, 14.65, and 46.08, respectively. The decomposition procedure using a cold finger in an open system is effective, presenting the lowest residual carbon content (6 %), good accuracy, and relative standard deviation lower than 5 %, and appears to be a suitable procedure for sample preparation for routine analysis.

In this work, three vapor generation methods (photochemical vapor generation, cold vapor generation with NaBH4 or with SnCl2) coupled with atomic absorption spectrometry were compared for the analysis of mercury (Hg) in pure glycerin and residual glycerin from biodiesel production. For these methods, a simple sample treatment step was employed through a dilution with formic acid or water and all parameters used were optimized. The limits of detection for the methods PVG-CV AAS, CV AAS with NaBH4, and CV AAS with SnCl2, were 0.12, 0.11, and 0.04 μg L–1, respectively. Because no adequate certified reference material was available, the accuracy was evaluated by assessing the recoveries of Hg2+ spikes in all samples (84%–108.3%). When methods were compared, the PVG-CV AAS presented adequate sensitivity and simplicity, and provided a direct approach to the generation of Hg vapor from glycerin samples while promoting green chemistry. In addition, PVG-CV AAS provided limits of detection that are comparable to co...

The present paper describes the validation of a spectrophotometry method involving molecular absorption in the visible ultraviolet-visible (UV-Vis) region for selenium (Se) determination in the bacterial biomass produced by lactic acid bacteria (LAB). The method was found to be suitable for the target application and presented a linearity range from 0.025 to 0.250 mg/L Se. The angular and linear coefficients of the linear equation were 1.0678 and 0.0197 mg/L Se, respectively, and the linear correlation coefficient (R2) was 0.9991. Analyte recovery exceeded 96% with a relative standard deviation (RSD) below 3%. The Se contents in LAB ranged from 0.01 to 20 mg/g. The Se contents in the bacterial biomass determined by UV-Vis were not significantly different (p > 0.05) those determined by graphite furnace atomic absorption spectrometry. Thus, Se can be quantified in LAB biomass using this relatively simpler technique.

This paper presents studies involving the determination of Hg in biological samples by cold vapor atomic absorption spectrometry (CV-AAS) using a simple and inexpensive system for sample digestion. The system consists of a glass tube that is closed with a small glass tube filled with cold water, which is called cold finger, and helps the recirculation of the acids within the bigger tube. The use of cold finger avoided the loss of analyte and the excessive evaporation of the acids during the heating. Thus, lower amount of acid was required, decreasing the risk of contamination. Studies of temperature of the digester block were performed with aqueous standard solutions in an interval between 80 and 120 °C. No significant loss of analyte was observed when compared with the open system. Certified reference materials (CRMs) were used to evaluate the accuracy of the proposed methodology. For this process, samples were digested with HNO3 for 2 h in a digester block between 90 and 120 °C, using the open system with the cold finger. The use of the cold finger system was efficient with similar results to those expected for CRMs for mercury (Hg) concentrations. For the open system, loss of analyte was observed when the digestion temperature was increased. The limit of detection (LOD) was 0.08 μg L− 1. The digestion procedure using cold finger in an open system is useful, at boiling point solution temperature, safe and simple for Hg determination in biological samples. Moreover, it can be used as an alternative to microwave-assisted digestion.

The acid decomposition method was applied for the sample preparation of processed fruit juice. The decomposition of 15mL of juice sample using HNO3 and H2O2 was performed in a digester block with reflux system and heated at 200°C for 150min. The limits of detection were 0.03; 0.24; 0.8; 0.008; 0.026 and 0.056mgL-1 for Cr, Cu, K, Mg, Na and Zn, respectively and for Pb was 0.99μgL-1. The accuracy was evaluated by spiked experiments (80 to 119%). Four processed fruit juice samples commercialized in Brazil (strawberry, mango, peach, and orange) were analyzed and indicated the absence of Cr, Zn and Cu in the samples, except for Cu in strawberry juice. Pb was found in the mango juice sample (17.8±0.9μgL-1) and the concentration is below the maximum values recommended by Brazilian legislation for juices of citric fruits (0.3mgkg-1).

In this work, the photochemical vapor generation (PVG) coupled with atomic absorption spectrometry and a pre-concentration step with an Au column was used for the determination of Hg in biological samples and ethanol fuel. PVG with pre-concentration showed an up to 250-fold higher sensitivity compared to the approach without pre-concentration. The accuracy of analysis of biological samples was evaluated using certified reference materials (fish tissues), while for ethanol fuel samples, recovery tests were employed (91%). Analytical curves were linear (R > 0.99) in the studied range of 2.5 to 10 µg L-1 for conventional PVG and 0.2 to 0.5 µg L-1 for PVG with the pre-concentration step. For the last, the limits of detection reached for biological samples and ethanol fuel were 0.02 and 0.01 µg L-1, respectively. The systems presented are simple, sensitive and safe for the control of low Hg concentrations in different samples. However, only the system using pre-concentration with an Au column was capable of obtaining the reproduced signals of Hg in low concentrations of the order of 0.2 µg L-1.

The aim of this study was to evaluate the performance of a reflux system adapted in the digestion tubes in sample preparation of xanthan gum for subsequent determination of Ca, Cu, K, Mg, Na and Zn by using spectrometric techniques. Through the proposed method, the samples were digested with HNO3 for 3 h in a digester block at 220 °C. The accuracy of the method was evaluated by comparing the results with another sample preparation method and by using recovery tests, which results vary between 83 and 103%. The efficiency of digestion was assessed and significant results were verified through residual carbon values, which were five times lower compared to conventional acid digestion in open system, with use of HNO3 and HClO4. The proposed methodology is a simple and accurate analytical strategy, which does not require the use of special equipment, neither a mixture of strong oxidizing acid in the sample preparation.

This paper describes the evaluation of a method for determination of Cd and Pb in xanthan gum samples by Graphite Furnace Atomic Absorption Spectrometry (GF AAS) using NH4H2PO4 as the chemical modifier. The sample preparation was performed using a reflux system adapted in the digestion tubes. With this system it was possible to increase the temperature of the digester block above the boiling point of the reaction medium, preventing loss of analyte and excessive evaporation of acids during heating. Samples were digested with HNO3 for 3 h in a digester block at 220 oC. The limits of detection for Cd and Pb were 2.2 and 33.8 ng g-1, respectively. The RSDs for both analytes were, on average, lower than 5.0% and accuracy was verified by recovery tests, yielding values in the 83-100% range.

It is presented an alternative procedure for preparation of biodiesel samples for elemental determination by inductively coupled plasma optical emission spectrometry (ICP OES), based on the sample (10% m/v) emulsion formation with formic acid (15% v/v) and Triton X-100 (0.1% m/v). These concentrations were optimized and the stability of emulsified aqueous standards and samples was found to be of at least 3 h. Experimental conditions (1500 W of RF power and 0.5 L min-1 of Ar nebulizer flow rate) were optimized from those recommended by the equipment manufacturer, with a solution containing 10 mg L-1 of each analyte prepared with mineral oil in the same conditions of the emulsion. Matrix effects were investigated by observing the slopes of analyte addition curves for different biodiesel samples. Results showed that external calibration with inorganic aqueous standard solutions in the emulsion medium should be used. Limits of detection obtained (in mg kg-1) were 0.121, 0.008, 0.006, 0.001, 0.006, 0.071, 0.241 and 0.024 for Ca, Cu, Fe, Mn, Mg, Na, K and Si, respectively. The accuracy of the procedure for Ca, Mg, K and Na was assessed by the analysis of a multi-element standards B100 biodiesel (Conostan) and the recoveries ranged from 91 to 107%. The proposed procedure used low toxicity reagents and showed to be a simple and straightforward alternative of sample preparation for metal determination in biodiesel by ICP OES with limits of detection adequate for those analyses. Apresenta-se um procedimento alternativo para o preparo das amostras de biodiesel para a determinação elementar por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES), baseado na formação de emulsão da amostra (10% m/v) com ácido fórmico (15% v/v) e Triton X-100 (0,1% m/v). Estas concentrações foram otimizadas e os padrões e amostras emulsionados mostraram-se estáveis por pelo menos 3 h. As condições experimentais (1500 W de potência da radiofrequência e 0,5 L min-1 de vazão do Ar nebulizador) foram otimizadas a partir das recomendadas pelo fabricante do equipamento, com uma solução contendo 10 mg L-1 de todos os analitos, preparada com óleo base nas mesmas condições da emulsão. Os efeitos de matriz foram investigados, observando as inclinações das curvas de adição de analito para diferentes amostras de biodiesel. Os resultados mostraram que a calibração externa com soluções contendo padrões inorgânicos emulsionados pode ser utilizada. Os limites de detecção encontrados (em mg kg-1) foram 0,121; 0,008; 0,006; 0,001; 0,006; 0,071; 0,241 e 0,024 para Ca, Cu, Fe, Mn, Mg, Na, K e Si, respectivamente. A exatidão do procedimento para o Ca, Mg, K e Na foi avaliada por meio da análise de um padrão multielementar de biodiesel B100 (Conostan) e as recuperações variaram entre 91 a 107%. O procedimento proposto usa reagentes com baixa toxicidade e mostrou ser uma alternativa simples e direta de preparação de amostras para determinação de metais em biodiesel por ICP OES com limites de detecção adequados para essas análises.

Two different sample preparation methods were evaluated for meat samples employing the solubilization in alkaline or acidic media. The aim of this study was to determine Na and K levels after sample solubilization with tetramethylammonium hydroxide (TMAH) at room temperature, and with formic acid and heating in a digester block at 50 ºC for ca. 2 h. The alkaline solubilization showed to be a simple and robust method and the better alternative in relation to the mineralization conventional procedures, allowing the complete solubilization of the samples even when small quantities of TMAH were used. The method was validated by using certified reference material as well as by comparing with samples digested with nitric acid. The limits of detection obtained were 0.8 and 2.0 μg g-1 for Na and K, respectively, and showed to be adequate for the analysis purposes. Foram avaliados dois métodos diferentes de preparo de amostras de carnes baseados na solubilização em meios alcalino ou ácido. O objetivo deste estudo foi determinar os teores de Na e K após solubilização com hidróxido de tetrametilamônio (TMAH) temperatura ambiente, e com ácido fórmico e aquecimento em bloco de digestão a 50 ºC por cerca de 2 h. A solubilização alcalina se apresentou como uma metodologia simples e robusta e a melhor alternativa frente aos procedimentos de mineralização convencional, permitindo a solubilização completa das amostras usando pequenas quantidades de TMAH. O método foi validado empregando-se materiais de referência certificada assim como pela comparação com método de digestão convencional com ácido nítrico. Os limites de detecção obtidos foram de 0,8 e 2,0 mg g-1 para Na e K, respectivamente, e se mostraram adequados para o objetivo das análises.

Um metodo simples para o tratamento de amostras de carne fresca e processada com hidroxido de tetrametilamonio (TMAH) e proposto para a determinacao de Ca, Fe e Mg por espectrometria de absorcao atomica com chama (FAAS) e Cu por espectrometria de absorcao atomica com forno de grafite (GFAAS). A exatidao foi avaliada por comparacao dos resultados usando outros dois procedimentos de preparo de amostra e por analise de materiais de referencia certificados. Nao houve diferenca significativa entre os resultados obtidos, em um nivel de confianca de 95%. Os limites de deteccao para Ca, Cu, Fe e Mg foram 45,0, 0,2, 16,0 e 0,3 µg g -1 , respectivamente. A espectrometria de absorcao atomica de alta resolucao com fonte continua em forno de grafite (HR-CS GFAAS) foi empregada para avaliar as interferencias espectrais na determinacao de Cu. Entretanto, nenhuma interferencia foi encontrada. O metodo proposto e simples, rapido e confiavel para analise de produtos carneos e nao requer o uso de equipamentos especiais nem de acidos fortes no preparo das amostras. A simple method for treating fresh and processed meat with tetramethylammonium hydroxide (TMAH) is proposed for the determination of Ca, Fe and Mg by flame atomic absorption spectrometry (FAAS) and Cu by graphite furnace atomic absorption spectrometry (GFAAS). The accuracy was evaluated by comparison of the results by using two other sample preparation procedures and by the analysis of certified reference materials. No significant differences between the results were found at the 95% confidence level. Limits of detection for Ca, Cu, Fe and Mg were 45.0, 0.2, 16.0 and 0.3 µg g -1 , respectively. High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) was employed to evaluate the spectral interference in the determination of Cu. However, no interference was found. The proposed method is simple, fast and reliable for meat products analysis and does not require especial equipment, neither strong acid for sample preparation.

The aim of this study was to present three sample preparation methods for the determination of Cd, Pb and Sn in meat by Graphite Furnace Atomic Absorption Spectrometry (GFAAS): acid digestion, solubilization with tetramethylammonium hydroxide and formic acid. For the digestion with HNO3, a conventional open system with a cold finger was used. This system helped to avoid losses of analytes and reagents by volatilization, permitting to operate at high temperatures applied at a digester block and reducing the digestion time (∼1 h). Solubilizations were performed at room temperature. The slurry was left standing overnight and remained closed until achieving complete solubilization. The temperature program of the graphite furnace was optimized for each element in the different means of preparation samples using a mixture of Pd–Mg. The figures of merit were similar for all sample preparation methods evaluated. The limits of detection obtained for the acid digestion procedure were 0.0006, 0.0164 and 0.0520 μg g−1 for Cd, Pb and Sn, respectively. In order to evaluate the accuracy of the results obtained by the three sample preparation methods, recovery tests for four real meat samples were performed and the recoveries ranged from 93.7 to 109%, supporting the accuracy of the method. Also, different certified reference materials of meat were analyzed and the results obtained were in agreement with the certified value at 95% of confidence (t-test). The best results were obtained by the acid digestion procedure with the cold finger system. This procedure is faster, the system is semi-closed with no significant contamination or loss of analytes by volatilization and it provides a better signal/noise ratio.

A new procedure based on exposure of ethanol biofuel samples to UV radiation in the presence of low molecular weight organic acids was developed for the determination of total Hg (inorganic and organometallic species: Hg2+, CH3Hg+ and CH3CH2Hg+) by photochemical vapor generation coupled with atomic absorption spectrometry (photo-CV-AAS). For each species, the optimum conditions for photochemical generation were investigated, including the effects of medium composition, exposure time to the UV radiation and transfer gas flow rate. The accuracy was evaluated by assessing the recoveries of species-specific spikes (91–107%) as well as by assessing recovery from a mixture of all species of the mercury added to the ethanol biofuel samples based on calibration standards prepared in high purity bidistilled ethanol. The limits of detection ranged from 0.05 to 0.09 μg L−1 for all addition and recovery tests, enabling the determination of total Hg. The proposed method is sensitive, simple (no sample pretreatment) and provides a direct approach to the generation of mercury vapor from ethanol biofuel samples while promoting “green” chemistry.

This paper describes a sample preparation method for domestic ceramics, based on the acid decomposition assisted by ultrasound for further determination of Cu, Fe, Mg and Zn by Flame Atomic Absorption Spectrometry technique. The main optimized conditions were: particle size (25 µm); sample mass (25 mg) and the acid volume (0.5 mL of HNO3 and 0.5 mL of HF). The samples were placed in an ultrasonic bath for 2 hours at 40 oC. The method was employed for eight commercial samples of domestic ceramic, which showed different concentrations for all analytes investigated, showing the existing variety of raw materials. The method showed good accuracy and precision, attested by the addition and recovery test, with values of 87 to 112% for all analytes and relative standard deviation lower than 3.0%.