Thermal analysis of some novel pyrimidine derivatives / Análisis térmico de algunos nuevos derivados de pirimidina

SUMMARY Some new pyrimidine derivatives have been synthesized and their decomposition characteristics have been studied by thermogravimetric and differential scanning calorimetric analysis. The thermal stability and some kinetics parameters of decomposition were evaluated from thermograms. It is observed that depending upon the structure, substitutions, thermal stability and decomposition kinetics varies in different compounds.

RESUMEN Se sintetizaron algunos nuevos derivados de pirimidina y se estudiaron sus características de descomposición mediante análisis termogravimétrico y calorimétrico diferencial de barrido. La estabilidad térmica y algunos parámetros cinéticos de descomposición se evaluaron a partir de los respectivos termogramas. Se observa que, dependiendo de la estructura y las sustituciones, la estabilidad térmica y la cinética de descomposición varían entre los diferentes compuestos.

Instrumental Analysis Of Novel Siddha Formulation Poonaga Parpam

Poonaga parpam (PNP) is an animal origin siddha formulation mentioned in the Siddha text “Sikicha Rathina Deepam”. The trial drug was prepared as per the standard operative procedure and subjected to various studies to reveal its potency. Materials and methods: The aim of the study was to standardize the PNP by modern instrumental techniques such as Fourier Transform Infra-Red Spectroscopy (FTIR), Inductively Coupled Plasma Optical Emission Spectroscopy (ICPOES), Scanning Electron Microscope with Energy Dispersive X-Ray Analysis (SEM with EDAX), X-Ray Diffractometer (XRD), Thermo Gravimetric Analysis (TGA). Results and Discussion: ICP-OES revealed the heavy metals like As, Cd, Pb, Hg and trace element like Ni were below detectable level. The stretches and bonds present in the FTIR analysis indicated the presence of some organic functional groups such as alcohol, aromatic, alkane, carbonyl, ketone, alkane, amine and alkyl halide which may be the reason for the therapeutic potency of the drug. XRD results revealed that the copper and iron may be the key ingredients present in the test drug PNP and the SEM picture indicated the existence of nanoparticles. TGA results revealed that the test drug PNP seems to be stable at varying temperature ranges from 50 to 400°C. Based on the results, Poonaga Parpam is preferably non-toxic to human in its therapeutic dose.

Técnicas de titulación ácido-base: consideraciones metrológicas / Acid-base titration techniques: metrological considerations / Técnicas de titulação ácido-base: considerações metrológicas

Resumen Se evaluaron diferentes sistemas de medición para titulaciones ácido-base, con el propósito de determinar cuál presenta mejores características metrológicas. Estos sistemas incluyen volumetrías y gravimetrías, las cuales se combinaron con diferentes métodos de detección del punto de equivalencia: (i) potenciometría, (ii) indicador ácido-base y (iii) conductividad electrolítica. Este artículo propone una nueva aproximación para la estimación de la incertidumbre de medición asociada a la detección del punto de equivalencia. Los resultados indicaron que, para la determinación del punto de equivalencia, las incertidumbres más bajas se obtienen mediante el método potenciométrico en comparación con el método conductimétrico cuyo sesgo es hasta 78 veces mayor. Sin embargo, se encontró que el método potenciométrico es fuertemente dependiente de la resolución del instrumento y/o la cantidad de agente titulante que se adiciona en la cercanía al punto de equivalencia. También se encontró que la incertidumbre disminuye cerca del 40% empleando métodos gravimétricos en comparación con los volumétricos. Al realizar la evaluación del sesgo de los sistemas de medición acorde con la guía ISO 33:2015, los resultados mostraron que, de los métodos evaluados, el método gravimétrico con detección potenciométrica presentó las mejores características metrológicas, pues se obtuvieron sesgos e incertidumbres menores.

Abstract Different measurement systems for acid-base titrations were evaluated to determine which one had the best metrological characteristics. These systems included volumetric and gravimetric titrations, which were combined with different detection systems: (i) potentiometry, (ii) acid-base indicator, and (iii) electrolytic conductivity. This article proposes a new approach for estimating the measurement uncertainty associated with the detection of the equivalence point. The results showed that, for the determination of the equivalence point, the lowest uncertainties were obtained by the potentiometric method in comparison with the conductometric method, whose bias was 78 times higher. The potentiometric method, however, was strongly dependent on the instrument resolution and/or the titrant amount that is added close to the equivalence point. It was also found that uncertainty decreases about 40% using gravimetric methods as compared to volumetric methods. When performing bias evaluation of the measurement systems according to the ISO 33:2015 guide, results showed that, among the evaluated methods, the gravimetric method with potentiometric detection presented the best metrological characteristics, with the lowest biases and uncertainties.

Resumo Foram avaliados diferentes sistemas de medida para titulações ácido-base, a fim de determinar quais possuem as melhores características metrológicas. Estes sistemas incluem titulações e gravimétricas, que foram combinadas com diferentes sistemas de detecção do ponto de equivalência: (i) potenciometria, (ii) indicador ácido-base e (iii) condutividade electrolítica. Este artigo propõe uma nova abordagem para estimar a incerteza de medição associada à detecção do ponto de equivalência. Os resultados indicaram que, para a determinação do ponto de equivalência, as incertezas mais baixas são obtidas pelo método potenciométrico enquanto que a incerteza do método condutométrico é até 78 vezes maior que a obtida pela potenciometria. Além disso, a potencimetria é altamente dependente da resolução do instrumento e/ou da quantidade de titulante para ser adicionado na proximidade com o ponto de equivalência. Também verificou-se que a incerteza diminui em torno de 40% utilizando métodos gravimétricos. De acordo à guia de norma ISO 33:2015, os resultados mostraram que os métodos de titulação ácido-base avaliados gravimetricamente com detecção potenciométrica proporcionaram as melhores características de metrologia, porque obtiveram os menores distorções e incertezas.

Radiation induced graft copolymerization of acrylamide onto poly (3-hydroxybutyrate) / Copolimerización por injerto radioinducido de acrilamida en el poli (3-hidroxibutirato)

The graft copolymer poly (3-hydroxybutyrate)-g- polyacrylamide[P (HB-g-AAm)] was synthesized by radiation induced graft copolymerization of acrylamide onto poly (3-hydroxybutyrate). The study was conducted by the simultaneous irradiation method. The structure of [P (HB-g-AAm)] was identified by Fourier Transform Infrared (FTIR) spectroscopy. Thermal behavior of the graft copolymer was also studied by Thermal Gravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC). According to the results, FTIR studies showed new signals (stretching-N-H) as an important evidence of grafting. The grafting degree, determined by ATG, was 10% and changes in thermodynamic parameter obtained from the DSC were detected. Such changes show a decrease in crystallinity and an increase in the glass transition temperature. These results demonstrate that the gamma radiation-induced graft copolymerization reaction of acrylamide onto PHB was successively achieved.

En el trabajo se realizó la síntesis del copolímero por injerto poli (3-hidroxibutirato)-g- poliacrilamida [P (HB-g-AAm)] por copolimerización de injerto radioinducido del monómero acrilamidaen el PHB. El estudio se llevó a cabo por el método de la irradiación simultánea. La estructura del copolímero se identificó por espectroscopía Infrarrojo por Transformada de Fourier (FTIR). Además, se realizó el estudio térmico del compuesto obtenido por análisis termogravimétrico (TGA) y calorimetría diferencial de barrido (DSC). De los resultados se encontraron señales (vibraciones de valencia -N-H) por FTIR que constituyen una importante evidencia de la reacción de injerto. El grado de injerto determinado por ATG fue de 10% y se detectaron cambios en los parámetros termodinámicos estudiados por DSC, que muestran una disminución de la cristalinidad y un aumento de la temperatura de transición vítrea. Los resultados demostraron la formación del copolímero por injerto inducido por radiaciones gamma.

Determination of Potassium Chloride in Compound Sodium Chloride Injection by Sodium Tetraphenylborate Volumetric Method / 中国药房

OBJECTIVE:To establish sodium tetraphenylborate volumetric method in place of gravimetric analysis method for the determination of the content of potassium chloride in compound sodium chloride injection.METHODS:The contents of potassium chloride in compound sodium chloride injection were determined by sodium tetraphenylborate volumetric method and sodium tetraphenylborate gravimetric method respectively,the results of which were compared.RESULTS:The average recovery of volumetric method was99.75%(RSD=0.46%,n=9),there was no significant difference in the t-test comparison between the determination results of volumetric method and that of the gravimetric method.CONCLUSION:The sodium tetraphenylborate volumetric method is simple,fast and accurate,which can take the place of gravimetric method for the deter?mination of contents of potassium chloride in compound sodium chloride injection.