Determinação condutométrica de cloridrato de metformina em formulações farmacêuticas empregando nitrato de prata como titulante

A simple, precise, rapid and low-cost conductometric titration method for the determination of metformin hydrochloride (MET) in pharmaceuticals using silver nitrate as titrant is proposed. The method was based on the chemical reaction between the chloride of metformin hydrochloride molecule and Ag(I) ions, yielding the precipitate AgCl(s). The method was applied for MET determination in three pharmaceuticals and the obtained results with proposed method were in close agreement with those results obtained using an official method of the British Pharmacopoeia, at a 95% confidence level.

Desenvolvimento de um titulador baseado na contagem de gotas

TitDrop II, a practice low-cost titrator based on drop counting is proposed. A microcomputer counts drops in an opto-switch and it receives pH values from a commercial pHmeter with RS-232 serial port. The volume of drops must kept constant and the amount of base in each drop is obtained by standardization in the titrator. A linear behavior between height of reservoir of titrant and drop frequency was observed, but there is no influence of low height on drop volume. Acetic acidity in samples of vinager was compared with volumetric titration, and deviation between -2.6 to 3.9% was observed.

Avaliação da influência de sulfetos solúveis na complexação do cobre em águas superficiais empregando métodos voltamétricos

In this work a sulfide quantification protocol using voltammetric methods was developed to evaluate the effect of dissolved sulfides on copper complexation. On the basis of pH, sulfide release from the dissociation of specific metal sulfide complexes can be electrochemically measured and then removed (as H2S) by a N2 purge. Cathodic stripping square wave voltammetry (CSSWV) was conducted to quantify Cu sulfides complexes which dissociate at pH < 5.0 during the process of acid titration.

Cloreto de n-(2-hidroxil) propil-3-trimetil amônio quitosana como adsorvente de corantes reativos em solução aquosa

The quaternary chitosan was synthesized by reaction of chitosan with glycidyl trimethylammonium chloride. it was characterized by infrared spectra and conductometric titration. Adsorption of reactive blue 4 (RB4) and reactive red 120 (RR120) by quaternary chitosan was studied from aqueous medium. Two kinetic adsorption models were tested: pseudo first-order and pseudo second-order. The experimental data best fitted the pseudo second-order model. The Langmuir isotherm model provided the best fit to the equilibrium data in the concentration range investigated and the maximum adsorption capacity determined was 415 mg (RR120) and 637 mg (RB4) of reactive dye per gram of adsorbent.

Constantes de acidez de ácidos dipróticos a partir de titulações potenciométricas: ilustração dos princípios do cálculo através da construção de um algoritmo muito simples

This work describes the creation of an very simple calculation algorithm, based in basic chemical and mathematic principles, for the calculation of weak diprotic acid dissociation constants as, for example, amino acids, from potentiometric titrations. For an easier understanding of the algorithm the logical reasoning of this calculus is schematized in a diagram of blocks. In the second part of the work the algorithm is applied to an Excel calculation sheet to determine the dissociation constants of Nicotinic Acid and Glycine, from the respective potentiometric titration curves. The values obtained using this algorithm are compared with those estimated by Hyperquad2008 (program generally used for this type of calculus) and also with the values of a stability constants database.

Determinação da constante de dissociação (Ka) do captopril e da nimesulida: experimentos de química analítica para o curso de farmácia

This paper presents the determination of the dissociation constant (Ka) of captopril and nimesulide as contextualized experiments to teach chemical concepts to students of Pharmacy. Captopril is an antihypertensive drug, which presents high water-solubility and weak acid properties. The pKa of carboxylic acid group of captopril is 3.7. Nimesulide is a non-steroidal anti-inflammatory drug sparingly soluble in water. It is weakly acidic (pKa ≈ 6.5) because of its methanesulfonamide functional group. The pKa of captopril was determined by potentiometric titration with NaOH 2.0 x 10-2 moL L ¹. The pKa of nimesulide was determined by using spectrophotometry and photometric titration. The experimental values of pKa of both drugs are in very good agreement with those from literature

Recuperação de compostos de iodo de reagentes e soluções laboratoriais

This work presents simple routes to recover iodine compounds from oxidized laboratory chemicals and aqueous solutions (HI and KI) used in laboratory chemistry classes. These routes are based on the oxidation of iodide ions (I-) to iodine (I2) by an oxidant (H2O2) or reduction of oxidized iodine by red phosphorus or hydrazine. Both routes presented high yields. The oxidative route is of general use whereas the reductive one is appropriate for restoring original iodine reagents. Final wastes were generated in low amounts. This work is appropriate for teaching many laboratory techniques (e.g., distillation, titration and filtration) in the chemical laboratory.

Investigação eletroquímica e calorimétrica da interação de novos agentes antitumorais biscatiônicos com DNA

Biscationic amidines bind in the DNA minor groove and present biological activity against a range of infectious diseases. Two new biscationic compounds (bis-α,ω-S-thioureido, amino and sulfide analogues) were synthesized in good yields and fully characterized, and their interaction with DNA was also investigated. Isothermal titration calorimetry (ITC) was used to measure the thermodynamic properties of binding interactions between DNA and these ligands. A double stranded calf thymus DNA immobilized on an electrode surface was used to study the possible DNA-interacting abilities of these compounds towards dsDNA in situ. A remarkable interaction of these compounds with DNA was demonstrated and their potential application as anticancer agents was furthered.

Antocianinas em extratos vegetais: aplicação em titulação ácido-base e identificação via cromatografia líquida/espectrometria de massas

Anthocyanins extracted from picao, quaresmeira, petunia, flamboyant, purple ipe, lobeira, pata de vaca, jaboticaba, purple cabbage and jambul were evaluated as natural acid-base indicators. Anthocyanins in extracts were identified using HPLC/MS. Clear, rapid change in color at final-point titration was observed for extracts but only picao showed strong change in pH. Indirect determination of carbonate in limestone using a natural indicator was performed and results compared with phenolphthalein indicator and potentiometer titration. Optimal results were obtained with picao but other extracts showed good accuracy and precision.

Miniprojeto para ensino de química geral experimental baseado na fermentação do caldo de cana-de-açúcar

This paper describes a five-week mini-project for a general chemistry laboratory course. Activities are included preparations of ethanol and sucrose solutions, calculation of concentrations, determination of densities with densimeters, sugarcane juice fermentation with CO2 capture in alkaline solution, distillation, and determination of amounts of ethanol and CO2 formed. Abilities and concepts normally present in practical general chemistry courses are covered: use of balances, volumetric glassware and densimeters, preparation of solutions, performing of dilutions, determination of solution densities, observation of chemical reactions, stoichiometric calculations, separation of mixtures, and titration.

Use of new silica fillers as additives for polymers used in packaging of fruit

The objective of this work was to synthesize nanosilicas with different degree of hydrophobicity by the sol-gel method, using tetraethyl orthosilicate as a precursor. For this purpose, 3-aminopropyl triethoxysilane (APS) and 1,1,1,3,3,3 - hexamethyldisilazane (HMDS), were added during synthesis as modifiers. A commercial biopolymer (Hexamoll Dinch, BASF) intended for packaging of apples, was added to the new nanosilicas. The materials obtained were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, potentiometric titration, porosity, specific surface area and hydrophobicity/hydrophilicity by wetting test. Colorimetry was used to evaluate change in apple pulp color after contact with the different silicas.

Monitoring of praseodymium(III) ions in aqueous solutions, soil and sediment samples by a PVC membrane sensor based on a furan-triazole derivative

A furan-triazole derivative has been explored as an ionophore for preparation of a highly selective Pr(III) membrane sensor. The proposed sensor exhibits a Nernstian response for Pr(III) activity over a wide concentration range with a detection limit of 5.2×10-8 M. Its response is independent of pH of the solution in the range 3.0-8.8 and offers the advantages of fast response time. To investigate the analytical applicability of the sensor, it was applied successfully as an indicator electrode in potentiometric titration of Pr(III) solution and also in the direct and indirect determination of trace Pr(III) ions in some samples.

Contextualizando reações ácido-base de acordo com a teoria protônica de Brönsted-Lowry usando comprimidos de propranolol e nimesulida

This paper reports the use of alternative materials for teaching experimental chemistry. In this context, nimesulide and propranolol tablets were used to teach chemical concepts about acid-base reactions according to Brönsted-Lowry protonic Theory. Important topics of Organic, Analytical and Pharmaceutical Chemistry were discussed, such as purification by acid-base extraction, solubility of organic compounds in aqueous solutions, buffers, the dissociation constant (pKa), potentiometric titration and ionization of drugs in biological fluids. The purification of propranolol and nimesulide from tablets produced yields of 75% and 90%, respectively. The experimental values of pKa for both drugs were in agreement with those from the literature.

Equilibrium studies of 2,2'-(5-bromo-6-methylpyrimidine-2,4-diyl)bis(azanediyl)dipropanoic acid with some transition-metal ions in aqueous solution

The stability constants of the 1:1 complexes formed between M2+ (M2+: Mn2+, Ni2+, Cu2+, or Cd2+) and BMADA2- (BMADA: 2,2'-(5-bromo-6-methylpyrimidine-2,4 diyl)bis(azanediyl)dipropanoic acid) were determined by potentiometric pH titration in aqueous solution (I = 0.1 mol L-1, NaNO3, 25 °C). The stability of the binary M - BMADA complexes is determined by the basicity of the carboxyl or amino groups. All the stability constants reported in this work exhibit the usual trend, and the order obtained was Mn2+< Ni2+ < Cu2+ > Cd2+. The observed stability order for BMADA approximately follows the Irving - Williams sequence. In the M - BMADA complexes, the M ion is able to form a macrochelate via the pyrimidine group of BMADA.

Potentiometric determination of Nickel (II) ion using 2-hydroxy-1-naphthylidene-N-cyanoacetohydrazone as electroactive material

A potentiometric Nickel sensor was prepared using 2-hydroxy-1-naphthylidene-N-cyanoacetohydrazone as electro-active material and epoxy resin as a binding material. A membrane composed of 40% Schiff's base and 60% epoxy resin exhibited the best performance. The membrane showed excellent response in the concentration range of 0.15 ppm to 0.1 mol L- 1 Ni+2 ions with non-Nernstian slope of 22.0 mV/decade, had a rapid response time (less than 10 s), and can be used for three months without any considerable loss of potential. The sensor was useful within the pH range of 1.3 to 9.6, and was able to discriminate between Ni2+ and a large number of alkaline earth and transition metal ions. The practical utility of the sensor has been demonstrated by using it successfully as an indicator electrode in the potentiometric titration of Ni2+ with EDTA and oxalic acid.