Agata Jakóbik-Kolon

Preparation of Pectin-Based Biosorbents for Cadmium and Lead Ions Removal

The optimal formation conditions of pectin-based, as well as new hybrid pectin-guar gum, biosorbents were found. The lead affinity for obtained biosorbents was very strong even in solution of pH = 1, in opposite to cadmium, which was adsorbed from solutions of pH ≥ 2. The sorption capacities in the studied conditions were about 0.6 and 0.8 mmol/g for cadmium and lead, respectively. The cadmium removal could be fast and it is almost quantitatively desorbed using 0.25 M HNO3, while desorption of lead required 1 M HNO3 to achieve a removal efficiency of ca. 75% from pectin-based beads. The possibility of biosorbents’ reuse was also proved. Addition of guar gum to pectin biosorbent did not change its sorption properties significantly.

Determination of microamounts of hafnium in zirconium using inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry during their separation by ion exchange on Diphonix chelating resin.

Inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICPMS) methods were applied to check the possibility of determination of hafnium in zirconium at a level lower than 100 ppm. A zirconium matrix of hafnium content lower than 10 ppm was obtained using a worked-out separation method exploiting ion exchange on Diphonix resin. Both methods give results in good agreement with each other as well as with those for certified reference material BCR-098 (Zircaloy-4). They were utilized in determination of Hf in the samples collected during separation of microamounts of hafnium from zirconium by the mentioned ion exchange. These results proved the earlier described method of separation on Diphonix resin to be effective even when the initial concentration of hafnium in zirconium decreases from 2.4% to 0.0082%.

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.

Extraction of Zirconium and Hafnium in Polyethylene Glycol‐Based Aqueous Biphasic System

Abstract The behavior of zirconium and hafnium in PEG 2000‐Na2SO4‐HCl aqueous biphasic system has been investigated. The dependences of HCl concentration (0.185–0.55 M), extraction temperature (298–318 K), and extraction time (5–120 min) on distribution ratios have been determined. Extraction of this metals in PEG 2000‐Na2SO4‐H2SO4 and PEG 2000‐Na3Cit‐HCl systems has been also studied. The sulfate and citrate complexes of Zr and Hf prefer salt‐rich phase in contrast to chloride complexes which pass into PEG rich phase in about 50% (w/w) to the greatest degree in room temperature and at short extraction time. The increase of distribution ratios (D*Zr=3.75, D*Hf=4.31) was observed after addition of water soluble organic ligand ‐ tiron (4,5‐dihydroxy‐m benzenedisulfonic acid disodium salt). The results obtained in studied conditions are not very useful for the separation of zirconium and hafnium.

Study on the electrodialytic nickel concentration from electroplating industry waste

ABSTRACT Owing to the ability of electrodialysis to produce highly concentrated solutions from dilute stream, in this paper, the possibility of nickel recovery and concentration from real electroplating industrial waste was discussed. The results showed that the nickel content in solutions after electrodialysis was approximately two times higher than in the initial working solutions, and the nickel recovery exceeded 85%. The nickel electric current efficiency (CENi) depended upon the type of electroplating bath and its acidic behaviour. The CENi was in the range of 52.3–70.6%. Moreover, high boron and the total organic carbon retention coefficients equal to 88.92% and 93.93% respectively, were observed.

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.