Poly (3-hydroxybutyrate) (P(3HB)) is the most studied thermoplastic biopolymer belonging to the polyhydroxyalkanoate (PHA) family, the main features of which include rapid biodegradability and biocompatibility. The bioplastic recovery process is an important step during production and can directly influence the characteristics of PHAs. However, more efficient methods for the production of P(3HB) are necessary to make it economically viable. The aim of the present study was to improve the standard, chloroform-based, extraction step for the recovery of P(3HB). The polymer was produced using a Ralstonia solanacearum strain. The following parameters were improved in the recovery process: heating time, separation method (filtration or liquid-liquid phase separation), biomass state (fresh or dry cell concentrate) and the solvent:biomass ratio. By improving the chemical extraction of P(3HB) we recovered 98% of the cumulative polymer and reduced the heating time by 75%. Furthermore, we improved the separation process and developed an extraction solution that was faster and more economical.

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.

O presente trabalho teve como objetivo determinar a adequabilidade de três amostras de biopolímero xantana (Xa 06, Xa 82 e Xa 106) e uma clairana como viscosificantes de fluidos de perfuração de poços de petróleo, comparando com uma amostra de xantana comercial, Xanvis®. Foram realizadas análises reológicas, determinados os conteúdos de acetil, piruvato e íons Na+ K+ e Ca2+, e avaliada a capacidade viscosificante segundo norma específica da Petrobras. Os conteúdos de grupos acetil e piruvato para as xantanas e clairana diferiram significativamente entre si, mas foram compatíveis com valores preconizados ou citados na literatura concernente. Com relação ao conteúdo de íons, a xantana comercial apresentou quantidade de cálcio superior, as amostras Xa 06, Xa 82 e Xa 106 tiveram maior teor de potássio e a clairana maior teor de sódio. A viscosidade e a viscoelasticidade da amostra de xantana comercial foram superiores às demais amostras analisadas. Na análise como viscosificante para fluidos de perfuração as amostras de xantana comercial e Xa 106 atingiram os requisitos estabelecidos para os parâmetros n, K e força gel da norma Petrobras N-2605. Com a interpretação conjunta dos resultados obtidos pode-se inferir que apenas as xantanas Xanvis® e Xa 106 apresentam características adequadas à utilização como viscosificante em fluido de perfuração de petróleo. As demais amostras possuem características reológicas adequadas à utilização como espessantes ou estabilizantes em outros segmentos industriais, como em alimentos, tintas e cosméticos.

The aim of this study was to determine the suitability of three xanthans (Xa 06, Xa 82 and Xa 106) and a clairana biopolymer for use as drilling fluid thickeners and comparing them against a commercial sample, Xanvis®. Rheological analyses were performed to determine the acetyl, pyruvate and Na+ K+ and Ca2+ ion content and their thickening ability, according to Petrobras guidelines. The pyruvate and acetyl group content for the xanthans and the clairana biopolymer differed significantly, but they were consistent with the recommended values or those previously cited in the literature. With regard to the ion content, the commercial xanthan contained higher amounts of calcium, while Xa 06, Xa 82 and Xa 106 samples contained higher potassium levels and clairana had a higher sodium level. The viscosity and viscoelasticity of the commercial xanthan sample were higher than for the other samples. In the viscosity analysis of drilling fluids, Xanvis® and Xa 06 met the required parameters for n, K and gel strength (Petrobras regulation N-2605). In an analysis of the results obtained, only Xanvis® and Xa 106 presented the desired characteristics for use as drilling fluid thickeners. The other samples presented adequate rheological characteristics for use as thickeners and stabilizers in many industrial applications, such as food, paints and cosmetics.

With the aim of adapting a method for removal of acetyl groups from xanthan, reactions of chemical deacetylation were carried out with natural xanthan (Jungbunzlauer®) with variations on the following parameters: biopolymer and alkali concentration (sodium and potassium hydroxide). The deacetylation reaction was performed at 25 ºC for three hours. The proposed methodology was efficient to promote the deacetylation reaction. The viscosity of xanthan increased when the alkali concentration was higher in the deacetylation reaction. Xanthan concentration in the solution used in the deacetylation reaction did not influence the solutions viscosity, as similar results in both tested biopolymer concentrations (0.5 and 1%) were obtained for all experiments in different shear rates. Deacetylation reactions at 25 ºC for three hours with sodium and potassium hydroxide in 0.01 mol.L-1 showed a viscosity of 410 and 420 mPa.s at 10 s-1 and acetylation degree 1.3 e 1.4%, respectively.

O trabalho objetivou avaliar xantanas produzidas por Xanthomonas arboricola pv pruni como viscosificante de fluido para aplicação na perfuração de poços de petróleo, comparando-as com três amostras comerciais utilizadas para este fim. Para isto, a viscosidade de soluções aquosas e salinas (NaCl, KCl e CaCl2) das diferentes xantanas, em distintas temperaturas (25, 45, 65 e 80 ºC), foi determinada em reômetro. Os parâmetros reológicos índice de consistência (K) e o índice de fluxo (n) foram obtidos pelo ajuste do modelo de Ostwald-de-Waelle. A força gel (G0, G10 e G30) foi determinada em viscosímetro, e a concentração de sais monovalentes (sódio e potássio) e divalentes (cálcio e magnésio) foi determinada em fotômetro de chama e em espectrômetro de absorção atômica, respectivamente. De uma forma geral, os resultados obtidos neste estudo mostram que as xantanas produzidas pelo patovar pruni, Xp 106-600 e Xp 115-600, por conterem baixa concentração de sais, apresentaram potencial para aplicação em fluido de perfuração de poços de petróleo, quando utilizada solução salina. Já os polímeros comerciais apresentaram melhores resultados quando utilizados em solução aquosa, pois continham alta concentração de sais.

The aim of this work was to evaluate xanthans produced by Xanthomonas arboricola pv pruni to be used for increasing the viscosity of fluids applied in the perforation of oil wells, which were compared with three commercial samples. In order to do that, the viscosity of aqueous and saline solutions (NaCl, KCl and CaCl2) from different xanthans, at different temperatures (25, 45, 65 and 80 ºC), was determined in a rheometer. The rheological parameters consistency index (K) and flow behaviour index (n) were obtained by adjusting the data with the Ostwald-de-Waelle model. Gel strength (G0, G10 e G30) was determined in a viscometer, and the concentration of monovalent (sodium and potassium) and divalent salts (calcium and magnesium) was determined in flame photometer and in atomic absorption spectrometer, respectively. Taken together, the results obtained in this study showed that xanthans produced by patovar pruni, Xp 106-600 and Xp 115-600, are promising for fluids used in oil well perforation with saline solutions, because they have low concentration of salts. As for the commercial polymers, they presented the best results when used in aqueous solution, because they had high salt concentrations.