Technological quality determination of pharmaceutical disintegrant by DSC cooling and DSC photovisual

A number of disintegrants are available on the market. They improve tablets’ disintegration. The objective of this work is the comparison of the technological quality parameters of disintegrants using different analytical techniques. Three batches of disintegrants and their binary mixtures (water:disintegrants) were investigated. Cooling experiments were used from –30 up to 200°C. The data obtained showed calorimetric differences between the samples. In the binary mixtures water showed different crystallization behaviour from the one found in the literature. According to the results DSC technique helped the quality control of different disintegrants.     

Preconcentration of heavy metals ions from aqueous solutions by means of cellulose phosphate: an application in water analysis

Cellulose phosphate (CELLPHOS) was studied as a collector for analytical preconcentration of traces of Cd(II), Cr(III), Cu(II) and Ni(II) from aqueous sample solution. It has been proved that using chromatographic columns packed with CELLPHOS for preconcentration and 1.0 mol 1(-1) HCl for elution the adsorbed analytes are quantitatively enriched. An enrichment factor of 20 (100 ml sample, 5 ml concentrate) was achieved by this separation procedure, which was applied to a series of water analyses (river, sea, bog water).     

Determination of manganese and zinc in powdered chocolate samples by slurry sampling using sequential multi-element flame atomic absorption spectrometry

In the present work, a slurry sampling flame atomic absorption spectrometric method to determine directly manganese and zinc in powdered chocolate samples is proposed. The optimization step was performed using univariate methodology involving the following factors: nature and concentration of the acid solution, sonication time, and particle size. The established conditions led to the use of a sample mass of 150 mg, 2.0 mol L^− 1 nitric acid solution, sonication time of 15 min, and a slurry volume of 50 mL. This method allows the determination of manganese and zinc with detection limit of 52 and 61 ng g^− 1, respectively, and a precision expressed as relative standard deviation (RSD) of 2.6% and 3.2% (both, n = 10) for contents of manganese and zinc of 52.4 and 100.0 μg g^− 1, respectively. The proposed method was applied for determination of manganese and zinc in five powdered chocolate samples. In these, the manganese content varied from 42.8 to 52.7 and from 88.6 to 102.4 μg g^− 1 of zinc. The analytical results were compared with the results obtained by analysis of these samples after digestion using open vessel and acid bomb digestion procedures and determination using FS-FAAS. The statistical comparison by t-test (95% confidence level) showed no significant difference between these results.     

Counterions in poly(allylamine hydrochloride) and poly(styrene sulfonate) layer-by-layer films

The amount of counterions in layer-by-layer (LBL) films of poly(allylamine hydrochloride) (PAH) and poly(styrene sulfonate) (PSS) has been determined with X-ray photoelectron spectroscopy (XPS) for films prepared from solutions with various NaCl concentrations. Sodium and chloride counterions are present in LBL films produced from salt solutions, which are located at the surface and in the bulk of the films. The percentage of bulk counterions increases with the ionic strength of the polyelectrolyte before reaching a constant value. The bulk sodium/sulfur percentage ratios tend to 0.8 for samples washed with pure water and for samples washed with NaCl aqueous solutions, while the bulk chlorine/nitrogen percentage ratios tend to 0.5 for the same samples. The ratio between the percentages of polyelectrolyte ionic groups lies close to unity for all samples, indicating that counterions do not contribute to charge compensation in the polyelectrolyte during the adsorption process. The presence of counterions in LBL films is explained by Manning condensation near the polyelectrolyte ionic groups, leading to inter-polyelectrolyte ionic bondings via ionic networks. It is believed that condensation leads to the formation of NaCl crystallites in these LBL films, which was confirmed by X-ray diffraction measurements.     

Preliminary test for nitrogen- and oxygen-containing groups in organic compounds

Summary Organic Compounds carrying groups containing both nitrogen and oxygen, such as nitro- and nitroso compounds, oximes, hydroxamic acids, azoxy compounds, and amine oxides yield nitrous acid when they are heated dry (pyrolysis). This product can be readily detected in the gas phase by theGriess nitrite reaction. This behavior provides a rapid preliminary test for members of these classes of compounds. Micro analytical limits of identification are readily obtained within the technique of spot test analysis.

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Zusammenfassung Organische Verbindungen mit Stickstoff- und sauerstoffhaltigen Atomgruppen, demnach Nitro- und Nitrosoverbindungen, Oxime, Hydroxamsäuren, Azoxy verbindungen und Aminoxyde spalten bei trockenem Erhitzen (Pyrolyse) salpetrige Säure ab, die in der Gasphase durch dieGriesssche Nitritreaktion empfindlich nachweisbar ist. Dieses Verhalten ermöglicht eine schnelle Vorprüfung auf Angehörige der genannten Verbindungsklassen. In der Technik der Tüpfelanalyse werden mikroanalytische Erfassungsgrenzen erreicht.

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Résumé Les combinaisons organiques porteuses d'un groupement azoté et oxygéné telles que les combinaisons nitrées et nitrosées, les oximes, les acides hydroxamiques, les composés azoxy et les oxydes d'aminés, libèrent de l'acide nitreux par chauffage à sec (pyrolyse); cet acide peut être identifié en phase gazeuse par la sensible réaction deGriess des nitrites. Ce comportement permet d'effectuer un essai préliminaire rapide sur les composés appartenant aux classes précédentes. Lorsqu'on met en oeuvre la technique de l'analyse à la touche, les limites de sensibilité atteintes permettent de travailler dans le domaine microanalytique.

     

Selective extraction of benzoic acid from landfill leachate by solid-phase extraction and ion-exchange chromatography

In this work a simple method was described for selective extraction of benzoic acid from landfill leachate samples. The samples were submitted to solid-phase extraction (SPE) with XAD-4 resin as the stationary phase and ion-exchange chromatography (IEC) using the ion-exchange resin Amberlyst A-27. The instrumental analysis was performed by gas chromatography with mass spectrometric detection (GC-MSD). Benzoic acid was isolated, identified and quantified. The extraction process is rapid, simple and of low cost. It was also environmental friendly, that is, it was used a minimum amounts of hazardous organic solvents and produced also minimum quantities of residues.     

Preliminary investigation of the application of on-line membrane extraction of trifluoroacetic acid as an aid to improvement of negative ion electrospray mass spectrometry data

We have recently investigated the biodegradation of a number of acidic aromatic compounds that give excellent chromatography using trifluoroacetic acid (TFA) based HPLC methods. Unfortunately HPLC methods using TFA are not usually compatible with detection by negative ion mass spectrometry as TFA suppresses ionisation of the analyte during the electrospray process. We present a preliminary investigation of the use of an anion-exchange micro-membrane suppressor to remove TFA on-line post column with the aim of improvement of mass spectral data using an aromatic acid as an example, Thus LC-MS using a TFA based HPLC method with negative ion mass spectral detection is shown to be possible with good sensitivity.     

Adsorption of Co(II), Ni(II), Cu(II), and Zn(II) on hexagonal templated zirconia obtained thorough a sol-gel process: the effects of nanostructure on adsorption features

Using zirconium tetrabutoxide, diaminedecane, and diamineoctane as precursors, a templated hexagonal zirconia matrix is synthesized and characterized by X-ray diffractometry and scanning electron microscopy. The adsorption capacity of such a matrix toward Co(II), Ni(II), Cu(II), and Zn(II) from aqueous solutions is studied. The adsorption affinity of the synthesized hexagonal templated zirconia toward the cations is Cu(II)>Zn(II) >Ni(II)>Co(II). It is also verified that the adsorption of the cations follows a Langmuir and not a Freundlich isotherm. All obtained isotherms are of type I, according to the IUPAC classification. The observed adsorption affinity sequence can be explained by taking into account the velocity constant for the substitution of water molecules into the cation coordination spheres, as well as the Irving-Williams series.     

Prediction of intracellular storage polymers using quantitative image analysis in enhanced biological phosphorus removal systems

The present study focuses on predicting the concentration of intracellular storage polymers in enhanced biological phosphorus removal (EBPR) systems. For that purpose, quantitative image analysis techniques were developed for determining the intracellular concentrations of PHA (PHB and PHV) with Nile blue and glycogen with aniline blue staining. Partial least squares (PLS) were used to predict the standard analytical values of these polymers by the proposed methodology. Identification of the aerobic and anaerobic stages proved to be crucial for improving the assessment of PHA, PHB and PHV intracellular concentrations. Current Nile blue based methodology can be seen as a feasible starting point for further enhancement. Glycogen detection based on the developed aniline blue staining methodology combined with the image analysis data proved to be a promising technique, toward the elimination of the need for analytical off-line measurements.