Preparação de carvão ativado em baixas temperaturas de carbonização a partir de rejeitos de café: utilização de FeCl3 como agente ativante

Ferric chloride as a new activating agent was used to obtain activated carbons from agroindustrial waste. This material was prepared at three temperatures of pyrolysis, 200, 280 and 400 ºC. The carbonaceous materials obtained after the activation processes showed high specific surface areas (BET), with values higher than 900 m² g-1. The materials showed different behaviors in the adsorption of methylene blue dye and reactive red textile dye in water solutions. An important fact in the use of FeCl3 as an activating agent is that the activation temperature is at 280 ºC, well below of those commonly employed in chemical or physical activations described in the literature.

Influência das características das substâncias húmicas aquáticas na eficiência da coagulação com o cloreto férrico

The aim of this study was to verify the influence of the apparent molecular size of aquatic humic substances on the effectiveness of coagulation with ferric chloride. Coagulation-filtration tests using jar test and bench-scale sand filters were carried out on samples of water with true color of approximately 100 Hazen units, prepared with aquatic humic substances of different molecular sizes (F1: < 0.45 µm, F2: 100 kDa - 0.45 µm, F3: 30 - 100 kDa and F4': < 30 kDa). For the water samples with lower apparent molecular size fractions, greater dosages of coagulant was needed to remove the color around 5.0 Hanzen units, mainly because these water samples contain higher concentrations of fulvic acids, which exhibited a larger number of negatively-charged groups.

Fotocatálise heterogênea com TiO2 para oxidação de arsênio e sua remoção de águas por coprecipitação com sulfato férrico

The oxidation of arsenic (As(III) to As(V)) in water samples was performed by heterogeneous photocatalysis using a TiO2 film immobilized inside a photochemical reactor. After oxidation, As(V) was removed from the water samples by coprecipitation with ferric sulfate. The final conditions of oxidation and arsenic removal (TiO2 film prepared with a suspension: 10% (w/v); pH: 7.0; oxidation time: 30 min and Fe3+ concentration: 50 mg L-1) were applied in natural water samples which were supplemented with 1.0 mg L-1 of As(III) to verify the influence of the matrix. After treatment, more than 99% of arsenic was removed from the water.

Estudo da oxidação dos sulfetos sintéticos molibdenita (MoS2) e covelita (CuS) por Acidithiobacillus ferrooxidans via respirometria celular

This paper analyses the oxidation of covellite and molybdenite by Acidithiobacillus ferrooxidans strain LR using respirometric experiments. The results showed that both sulfides were oxidized by A. ferrooxidans, however, the covellite oxidation was much higher than molybdenite. Regarding the kinetic oxidation, the findings revealed that just molybdenite oxidation followed the classical Michaelis-Menten kinetic. It is probably associated with the pathway which these sulfides react to chemistry-bacterial attack, what is influenced by its electronic structures. Besides, experiments conducted in the presence of Fe3+ did not indicate alterations in molybdenite oxidation. Thus, ferric ions seem not to be essential to the sulfide oxidations.

Determinação de citrato de sildenafila e de tadalafila por cromatografia líquida de ultraeficiência com detecção por arranjo de diodos (CLUE-DAD)

A simple ultra-performance liquid chromatographic method for the simultaneous determination of sildenafil citrate and tadalafil was developed and validated. Sample preparation was dissolution in methanol, followed by centrifugation and dilution (1:10) with methanol. Analysis was performed in an Acquity® UPLC system with Acquity® BEH C18 column (2.1 x 50 mm, with 1.7 μm particles). The elution was isocratic with phosphate buffer pH 2.3 and acetonitrile (65:35, v/v) at a flow rate of 0.7 mL/min. The method presented adequate specificity, linearity, precision and accuracy and allowed the determination of the drugs in seized forensic samples.

Degradação de corantes reativos por processo foto-fenton envolvendo o uso de peneira molecular 4A modificada com Fe3+

In this work the preparation and characterization of a supported catalyst intended for degradation of reactive dyes by Fenton-like processes is described. The photocatalyst was prepared by immobilization of Fe3+ into the molecular sieve (4A type) surface and characterized by x-ray diffractometry and infrared, Mössbauer and EPR spectroscopy. The solid containing 0.94% (w/w) of ferric ions was used in degradation studies of aqueous reactive-dyes samples with really promissory results. Generally, Vis-assisted photochemical processes leads to almost total decolorization of all tested dyes at reaction times lower than 30 min. It was also observed that the iron-molecular sieve matrix can be reused.

Hemoglobina extracelular gigante de Glossoscolex paulistus: um extraordinário sistema supramolecular hemoproteico

Giant extracellular hemoglobins are considered the summit of complexity in systems that carry oxygen, constituting an extraordinary model system to the study of hemoproteins. This class includes the hemoglobin of the annelid Glossoscolex paulistus that presents high cooperativity, great oligomeric and redox stabilities and ability of oligomeric reassociation. These properties have motivated evaluations about its utilization as prototype of artificial blood and biosensor. Kinetic studies involving autoxidation and detailed spectroscopic characterizations of its ferrous and ferric species have propitiated information about the structure-activity relationship of this macromolecule. The present review analyzes several biochemical issues, evaluating the state-of-art of this subject.

Método QuEChERS para determinação de ocratoxina a e citrinina em arroz e farelo de arroz

The present study was carried out to establish the optimal conditions for performing ochratoxin A (OTA) and citrinin (CIT) extraction using the QuEChERS method in rice. Employing the factorial experimental design, variables that significantly influenced the extraction stages were determined. The following variables were analyzed: addition of water, acidification of acetonitrile with glacial acetic acid, as well as amounts of magnesium sulfate, sodium acetate, sodium citrate and diatomaceous earth. The best combining procedure resulted in a predictive model using more water and less diatomaceous earth. Recoveries of CIT and OTA were 78-105%.

Zn-edta degradation by catechol-driven fenton reaction

Zn-EDTA degradabilty by catechol-driven Fenton reaction was studied. Response surface methodology central composite design was employed to maximize this complex degradation. Theoretical speciation calculations were in good agreement with the experimental results. Fenton and Fenton type treatments are typically thought to be applicable only in the highly acidic range, representing a major operational constraint. Interestingly, at optimized concentrations, this CAT-driven Fenton reaction at pH 5.5 achieved 100% Zn-EDTA degradation; 60% COD and 17% TOC removals, using tiny amounts of CAT (50 µM), Fe(III) (445 µM) and H2O2 (20 mM) with no evident ferric sludge.

Preparação de nanopartículas de prata e ouro: um método simples para a introdução da nanociência em laboratório de ensino

A new practical experiment involving silver and gold nanoparticle syntheses was introduced in an inorganic chemistry laboratory course for undergraduate students at the Institute of Chemistry, UNICAMP. The nanoparticles were synthesized by the reduction of silver nitrate and tetrachloroauric acid with sodium borohydride and sodium citrate in an aqueous medium. Stabilities of the suspensions were tested using several different reactants including sodium chloride, polyvinylpyrrolidone, polyvinyl alcohol and cistamine. Changes in optical properties were observed by electronic spectra and also by transmission electronic microscopy, which also yielded data for estimating particle size.

Synthesis of 1H-benzoxazine-2,4-diones from heterocyclic anhydrides: evaluation of antioxidant and antimicrobial activities

A facile one-step synthesis of 1H-benzoxazine-2,4-diones from heterocyclic anhydrides and TMSA was described. This paper determines their antimicrobial activity against nine human bacterial pathogens by the broth microdilution method; antioxidant activity by DPPH• inactivation and a ferric-reducing power assay; and toxicity by a brine shrimp, Artemia salina, assay. The 1H-benzoxazine-2,4-dione yields were in the range of 57 to 98%. The novel compound 1H-pyrazino[2,3-][1,3]oxazine-2,4-dione 4c showed the highest antioxidant capacity (DPPH 35.4% and FRAP 0.063 µmol TEs/µmol).

EVALUATION OF A BUFFERED SOLID PHASE DISPERSION PROCEDURE ADAPTED FOR PESTICIDE ANALYSES IN THE SOIL MATRIX

An evaluation of the pesticides extracted from the soil matrix was conducted using a citrate-buffered solid phase dispersion sample preparation method (QuEChERS). The identification and quantitation of pesticide compounds was performed using gas chromatography-mass spectrometry. Because of the occurrence of the matrix effect in 87% of the analyzed pesticides, the quantification was performed using matrix-matched calibration. The method's quantification limits were between 0.01 and 0.5 mg kg-1. Repeatability and intermediate precision, expressed as a relative standard deviation percentage, were less than 20%. The recoveries in general ranged between 62% and 99%, with a relative standard deviation < 20%. All the responses were linear, with a correlation coefficient (r) ≥0.99.

Direct and simultaneous spectrophotometric determination of Ni (II) and Co (II) using diethanoldithiocarbamate as complexing agent

A direct spectrophotometric method for simultaneous determination of Co(II) and Ni(II), with diethanoldithiocarbamate (DEDC) as complexing agent, is proposed using the maximum absorption at 360 and 638 nm (Co(II)/DEDC) and 390 nm (Ni/DEDC). Adjusting the best metal/ligand ratio, supporting eletrolite, pH, and time of analysis, linear analytical curves from 1.0 10-6-4.0 10-4 for Co(II) in the presence of Ni 1.0 10-6-1.0 10-4 mol L-1 were observed. No further treatment or calculation processes have been necessary. Recoveries in different mixing ratios were of 99%. Interference of Fe(III), Cu(II), Zn(II) and Cd(II), and anions as NO3-, Cl-, ClO4-, citrate and phosphate has been evaluated. The method was applied to natural waters spiked with the cations.

Method to obtain platelet-rich plasma from rabbits (Oryctolagus cuniculus )

Abstract: Platelet-rich plasma (PRP) is a product easy and inxpesnsive, and stands out to for its growth factors in tissue repair. To obtain PRP, centrifugation of whole blood is made with specific time and gravitational forces. Thus, the present work aimed to study a method of double centrifugation to obtain PRP in order to evaluate the effective increase of platelet concentration in the final product, the preparation of PRP gel, and to optimize preparation time of the final sample. Fifteen female White New Zealand rabbits underwent blood sampling for the preparation of PRP. Samples were separated in two sterile tubes containing sodium citrate. Tubes were submitted to the double centrifugation protocol, with lid closed and 1600 revolutions per minute (rpm) for 10 minutes, resulting in the separation of red blood cells, plasma with platelets and leucocytes. After were opened and plasma was pipetted and transferred into another sterile tube. Plasma was centrifuged again at 2000rpm for 10 minutes; as a result it was split into two parts: on the top, consisting of platelet-poor plasma (PPP) and at the bottom of the platelet button. Part of the PPP was discarded so that only 1ml remained in the tube along with the platelet button. This material was gently agitated to promote platelets resuspension and activated when added 0.3ml of calcium gluconate, resulting in PRP gel. Double centrifugation protocol was able to make platelet concentration 3 times higher in relation to the initial blood sample. The volume of calcium gluconate used for platelet activation was 0.3ml, and was sufficient to coagulate the sample. Coagulation time ranged from 8 to 20 minutes, with an average of 17.6 minutes. Therefore, time of blood centrifugation until to obtain PRP gel took only 40 minutes. It was concluded that PRP was successfully obtained by double centrifugation protocol, which is able to increase the platelet concentration in the sample compared with whole blood, allowing its use in surgical procedures. Furthermore, the preparation time is appropriate to obtain PRP in just 40 minutes, and calcium gluconate is able to promote the activation of platelets.

A new allele of peptidase-B in cattle

Electrophoretic analyses of peptidase-B were carried out on red cell hemolysates from Holstein, Mantiqueira and Gyr cattle, using cornstarch, known in Brazil as Penetrose-30. We describe a new peptidase-B allele, denoted Pep-B1, in Mantiqueira cattle, belonging to the Bos taurus group, which are the result of a cross of native cattle of Portuguese origin introduced in Brazil during colonial times (16th century) with Holstein and Caracu cattle. The genetic control of peptidase-B was determined by typing parents and progeny segregating for all three alleles, confirming that peptidase B is controlled by a single autosomal locus with three codominant alleles, denoted Pep-B1, Pep-B2 and Pep-B3 The use of the citrate-phosphate buffer system, at pH 5.9, on 14% gel, under the electrophoretic conditions standardized in this study permitted good visualization of all peptidase-B variants.