Joanna Bok-Badura

New, hybrid pectin-based biosorbents.

ABSTRACT In this work hybrid pectin-based biosorbents with secondary polysaccharide additives (gellan, carob and xanthan gum, ratio to pectin 1:1, 1:1 and 1:3, respectively) were obtained at two temperatures. The presence of these additives in prepared beads was confirmed by Raman spectra. The SEM micrographs show better homogeneity of blends and grater differences between structures of beads with various additives obtained at higher temperature. The sorption capacity of our hybrid biosorbents as well as sole pectin sorbent is rather the same, and equals 0.85 and 0.70 mmol/g for lead and cadmium, respectively, in pH 4–6.

Hybrid pectin-based biosorbents for zinc ions removal

In this paper, a set of the hybrid biosorbents, made of pectin and polysaccharide additives (arabic, tragacanth, guar, karaya, xanthan, gellan, carob gums, agar-agar) or lecithin (phospholipid), was investigated and tested for zinc ions removal. The immobilization of the polysaccharides into the pectin matrix was proved by the IR spectroscopy. The structure of the working biosorbents was observed in SEM micrographs. The influence of the additive type and pH on the sorption properties and swelling index was investigated. The maximum sorption capacities were achieved in pH above 4 and ranged from 17.7 to 25.4mg/g for lecithin and xanthan gum as additives, respectively. The results show that the hybrid pectin-based beads are promising biosorbents for zinc removal from aqueous solutions.

A versatile method for direct determination of iron content in multi-wall carbon nanotubes by inductively coupled plasma atomic emission spectrometry with slurry sample introduction

Carbon nanotubes (CNTs), due to their unique combination of physicochemical properties, are continuously considered as one of the most interesting materials in contemporary science and industry. Their applicability depends on physical properties, such as number of walls, morphology, diameter and length (aspect ratio), but also on the content of carbonaceous and metallic contaminants (typically present as encapsulated catalyst nanoparticles from catalytic Chemical Vapor Deposition). Therefore, especially for medical and biomedical applications, the concentration of metallic impurities or modifiers should be monitored. In this paper, an inductively coupled plasma atomic emission spectrometry (ICP-AES) technique with slurry nebulization is proposed for direct determination of iron in multi-wall carbon nanotubes (MWCNTs). Slurries of MWCNTs are prepared in a 1% solution of Triton X-100, ultrasonicated to ensure their homogeneity and measured by the ICP-AES apparatus. The optimal range of MWCNTs slurry concentration and plasma radiofrequency (RF) power are established as 40–500 mg L−1 and 1.0 kW, respectively. The precision of the method does not exceed 1.5% of the mean values. Validation of the method is based on the fact that Fe is partly leached from the slurry and the assumption that iron in the leachate gives the same response in ICP-AES as iron in the residual MWCNTs slurry. This behavior was proved by summing both results for Fe (determined in the leachate and in the slurry of post-leaching nanotubes), which always yielded the same total amount of Fe for different degrees of leaching and this value was in full agreement with the iron content in the original, tested sample, as determined by the proposed slurry method. Taking into account all the examinations and obtained results, it can be concluded that the proposed method is applicable for fast, versatile, direct, and simple quantitative analysis of iron in MWCNTs and potentially other nanoallotropes produced by c-CVD.

Sorption studies of cadmium and lead ions on hybrid polysaccharide biosorbents

ABSTRACT The sorption of lead and cadmium ions on hybrid pectin-based biosorbents containing gellan, carob, and xanthan gum has been studied. The rate constant of the metal ions’ sorption on hybrid P + X beads (analyzed with the two kinetic models: pseudo-first-order and pseudo-second–order models) is at least two times higher than obtained on other pectin-based sorbents. The Langmuir equation fits experimental data better than Freundlich model. A greater equilibrium constant B for lead(II) than cadmium(II) indicates a stronger bond between Pb(II) and pectin-based beads. Prepared hybrid materials are promising biosorbents for heavy metals’ removal from waste waters.

Zinc Sorption Studies on Pectin-Based Biosorbents

The previously-obtained and characterized hybrid pectin-based beads containing agar-agar and guar gum, as well as sole pectin beads (P, for comparison) were examined for zinc ions sorption and desorption properties. The sorption kinetics and equilibrium in the studied system was described by two kinetic models (pseudo-first- and pseudo-second-order) and two isotherms (Langmuir and Freundlich), respectively. The desorption kinetics and equilibrium was also investigated by applying various inorganic acids (nitric, hydrochloric, and sulfuric acid) of various concentrations. In the case of guar gum additive, no significant change in sorption capacity compared to sole pectin beads was observed (q: 37.0 ± 2.6 and 34.7 ± 2.0 mg/g, respectively). Addition of agar-agar significantly decreased the sorption capacity to 22.3 ± 1.0 mg/g, but stripping of zinc(II) ions from this biosorbent was complete even with very diluted acids (0.01 M). Total desorption of zinc from sole pectin and pectin-guar gum beads required acid solution of higher concentration (0.1 M). Sorption rates for all biosorbents are roughly the same and maximum sorption is achieved after 4–5 h. Obtained results and the advantage of our sorbent’s shape formation ability, make the pectin-based biosorbents interesting alternative for zinc(II) ions removal.

Zinc Sorption on Modified Waste Poly(methyl methacrylate)

The new one-pot hydrolysis-crosslinking reaction was used to synthesize a new, waste poly(methyl methacrylate) (PMMA)-based material for zinc(II) ions removal. The alkaline hydrolysis of PMMA in diethylene glycol diethyl ether was used to obtain polymer matrix and it was then crosslinked with Ca and Mg ions to obtain the sorbent. As a result, the macroporous materials were obtained with a yield of 87% when waste PMMA was used, and about 95% when the commercial PMMAs were used. The degree of hydrolysis was similar, from 32% to 35%. New materials were then tested for their affinity towards zinc(II) ions. Two kinetic models (pseudo-first and pseudo-second order), as well as two isotherms (Langmuir and Freundlich), were used to describe the kinetics and equilibrium of zinc(II) ion sorption on the studied materials, respectively. All the prepared PMMA-based sorbents showed similar or higher sorption capacity (q up to 87.7 mg/g) compared to commercially available materials in a broad pH range (4–7). The study shows sorption was fast—above 80% of equilibrium capacity was achieved after ca. 0.5 h. Presented results show that waste PMMA may be an interesting raw material for the preparation of sorbents for zinc(II) ions removal.

A Method for Determination of Metals in Hybrid Metal Oxide/Metal-Carbon Nanotubes Catalysts

Carbon nanotubes (CNTs), due to their special structure and unique properties, are still one of the most interesting materials for scientists. Recently, carbon nanotubes were proposed as a new type of carbon support for catalysts. Fe, Pt, Ni, Co, and other metals anchored to CNTs are used in various reactions. Due to the fact that production processes are usually unpredictable and the total amount of metal/metal oxide deposited on the CNTs may only be estimated, the methods for examining the chemical composition are necessary. In this study, fast and simple inductively coupled plasma atomic emission spectrometry (ICP-AES) with slurry nebulization was proposed for metal content determination in hybrid CeZrO2/CNT, Ni-CeZrO2/CNT, and Ni/CNT materials. Slurries were prepared by 30 min ultrasonication of appropriate amount of investigated material in 1% Triton X-100 solution. Optimal range of slurry concentration and optimal RF plasma power were established (40–400 mg L−1, 1.2 kW, resp.). Obtained results proved that this method may be applied for determination of Ce, Zr, and Ni in hybrid CNT-based materials.

Sorption studies of heavy metal ions on pectin-nano-titanium dioxide composite adsorbent

ABSTRACT The Cu(II), Cd(II), Zn(II), and Pb(II) sorption kinetics and equilibrium on hybrid material, composed of pectin and titanium dioxide nanopowder, were examined. Parameters, such as pH and adsorbent dose, were also investigated. The experimental data were better described by the Langmuir model. The maximum adsorption capacities were 1.37, 0.68, 0.51, and 0.83 mmol/g for Cu(II), Cd(II), Zn(II), and Pb(II), respectively. The introduction of nano-TiO2 improved the kinetics of the metal ion sorption. The titanium dioxide, despite its small content (6%), contributes to the removal of the examined metal ions and eventually to the adsorption capacity of hybrid beads.

Fast and Simple Analytical Method for Direct Determination of Total Chlorine Content in Polyglycerol by ICP-MS

The fast and simple method for total chlorine determination in polyglycerols using low resolution inductively coupled plasma mass spectrometry (ICP-MS) without the need for additional equipment and time-consuming sample decomposition was evaluated. Linear calibration curve for 35Cl isotope in the concentration range 20–800 µg/L was observed. Limits of detection and quantification equaled to 15 µg/L and 44 µg/L, respectively. This corresponds to possibility of detection 3 µg/g and determination 9 µg/g of chlorine in polyglycerol using studied conditions (0.5% matrix-polyglycerol samples diluted or dissolved with water to an overall concentration of 0.5%). Matrix effects as well as the effect of chlorine origin have been evaluated. The presence of 0.5% (m/m) of matrix species similar to polyglycerol (polyethylene glycol—PEG) did not influence the chlorine determination for PEGs with average molecular weights (MW) up to 2000 Da. Good precision and accuracy of the chlorine content determination was achieved regardless on its origin (inorganic/organic). High analyte recovery level and low relative standard deviation values were observed for real polyglycerol samples spiked with chloride. Additionally, the Combustion Ion Chromatography System was used as a reference method. The results confirmed high accuracy and precision of the tested method.

Zinc Ion Removal on Hybrid Pectin-Based Beads Containing Modified Poly(Methyl Methacrylate) Waste

A new hybrid sorbent in the form of round beads containing modified poly(methyl methacrylate) (PMMA) waste immobilized in pectin and crosslinked with calcium ions was prepared. A previously obtained and characterized powdered poly(methyl methacrylate)–based sorbent was used. Batch and column studies on the new material’s sorption-desorption properties were performed. Two kinetic models (pseudo-first- and pseudo-second-order) and three isotherms (Langmuir, Langmuir bisite and Freundlich) were used to describe the results. Breakthrough and elution curves were also obtained. Nitric, hydrochloric, and sulfuric acid of various concentrations were used in the desorption studies. Higher sorption affinity of zinc(II) ions to hybrid sorbent than to pectin alone, reflected by higher values of the Langmuir and Freundlich model parameters, was observed. The maximum sorption capacities, calculated based on the best-fitted models, were 50.2 mg/g (Langmuir bisite) and 42.2 mg/g (Langmuir) for hybrid and only pectin beads, respectively. The stripping of Zn ions using 0.1 M solutions of mineral acids was similarly effective in the case of both sorbents. The mass balance calculated for the column studies showed about 100% recovery of zinc in a sorption-desorption cycle. By applying the hybrid sorbent under the studied conditions it is possible to purify Zn in water to the level permitted by law and concentrate Zn(II) ions by about 60 times.