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The study focused on the adsorption mechanism of two selected pesticides: carboxin and diuron, on goethite and biochar, which were treated as potential compounds of mixed adsorbent. The authors also prepared a simple mixture of goethite and biochar and performed adsorption measurements on this material. The adsorbents were characterized by several methods, inter alia, nitrogen adsorption/desorption, Boehm titration, Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. The adsorption study included kinetics and equilibrium measurements, in the solution containing one or two pesticides simultaneously. The adsorption data were fitted to selected theoretical models (e.g., Langmuir, Freudlich, Redlich–Peterson, pseudo first-order and pseudo second-order equations). Based on the obtained results, it was stated that, among all tested adsorbents, biochar had the highest adsorption capacity relative to both carboxin and diuron. It equaled 0.64 and 0.52 mg/g, respectively. Experimental data were best fitted to the pseudo second-order and Redlich–Peterson models. In the mixed systems, the adsorption levels observed on biochar, goethite and their mixture were higher for diuron and lower for carboxin, compared to those noted in the single solutions. The presented results may enable the development of new mixed adsorbent for remediation of soils polluted with pesticides.

With the increasing needs of clean water supplies, the use of biomass wastes and residues for environmental remediation is essential for environmental sustainability. In this study, the residues from winery and citrus juice industries, namely grape skin and orange peel, respectively, were first converted to hydrochars by hydrothermal carbonization (HTC) and then a cationic dye (methylene blue) adsorption was studied on hydrochars. Hydrochars from both feedstocks were produced at three different temperatures (180, 220, and 250 °C) and a fixed residence time (1 h) to evaluate the hydrochar’s performance on the dye adsorption. The hydrochars were characterized in terms of their pH, pH at point of zero charge (pHPZC), surface functionalities, and surface area. A batch adsorption study of the dye was carried out with variable adsorbate concentration, pH, and temperature. Two adsorption isotherms namely Langmuir and Freundlich models were fitted at 4, 20, and 36 °C. The thermodynamic properties of adsorption (Gibbs free energy (ΔG), enthalpy (ΔH) and entropy (ΔS)) were evaluated from the isotherms fittings. Results showed that the dye adsorption on both hydrochars was significant and followed Langmuir isotherm. The maximum adsorption capacity on citrus waste hydrochar was higher than the winery waste hydrochar at any corresponding HTC temperature. Although hydrochars showed the lowest surface area (46.16 ± 0.11 and 34.08 ± 1.23 m2/g for citrus and winery wastes, respectively) at 180 °C, their adsorption was the highest, owing to their maximum density of total oxygen functional groups (23.24 ± 0.22 and 32.69 ± 1.39 µmol/m2 for citrus and winery wastes, respectively), which decreased with the increase in HTC temperature. This research shows a sustainable route for the production of highly effective adsorbent materials at lower HTC temperatures from citrus and winery wastes.

Natural graphite, a locally available, eco-friendly, and low-cost carbonaceous source, can be easily transformed into exfoliated graphite (EG) with many surface functional groups via a chemical oxidation route. Combination between EG and magnetic MnFe2O4 is a promising strategy to create a hybrid kind of nanocomposite (EG@MnFe2O4) for the efficient adsorptive removal of Congo red (CR) dye from water. Here, we reported the facile synthesis and characterization of chemical bonds of EG@MnFe2O4 using several techniques such as Fourier-transform infrared spectroscopy (FT-IR), and X-ray photoelectron spectroscopy (XPS). In particular, the quantity method by Boehm titration was employed to identify the content of functional groups: Carboxylic acid (0.044 mmol/g), phenol (0.032 mmol/g), lactone (0.020 mmol/g), and total base (0.0156 mmol/g) on the surface of EG@MnFe2O4. Through the response surface methodology-optimized models, we found a clear difference in the adsorption capacity between EG-decorated MnFe2O4 (62.0 mg/g) and MnFe2O4 without EG decoration (11.1 mg/g). This result was also interpreted via a proposed mechanism to elucidate the contribution of surface functional groups of EG@MnFe2O4 to adsorption efficiency towards CR dye.

It is well known that surfactant-suspended carbon nanotube (CNT) samples can be purified by centrifugation to decrease agglomerates and increase individually-dispersed CNTs. However, centrifugation is not always part of protocols to prepare CNT samples used in biomedical applications. Herein, using carboxylated multi-walled CNTs (cMWCNTs) suspended in water without a surfactant, we developed a Boehm titrimetric method for the analysis of centrifuged cMWCNT suspensions and used it to show that the surface acidity of oxidized carbon materials in aqueous cMWCNT suspensions was enriched by ∼40% by a single low-speed centrifugation step. This significant difference in surface acidity between un-centrifuged and centrifuged cMWCNT suspensions has not been previously appreciated and is important because the degree of surface acidity is known to affect the interactions of cMWCNTs with biological systems.

The use of the Boehm titration (BT) method as an analytical tool for the quantification of oxygen-containing surface groups is systematically investigated for oxidized carbon black, carbon nanotubes and two active carbons with specific surface areas between 60 and 1750 m2 g−1. The accuracy of the BT method is quantitatively compared with results from elemental analysis (EA), temperature programmed desorption (TPD), and X-ray photoelectron spectroscopy (XPS). Overall, the results from TPD are in line with the values obtained by BT. Both show the equal ratio of the oxygen groups to each other. Within the series of carbon samples, all methods provide similar trends for the total oxygen content yet the absolute numbers are deviating significantly. Reasons for these discrepancies are discussed and linked to the specific characteristics of the different methods. As the BT method is a solution based method, it only probes the surface fraction of the carbon that is accessible to the base solution. That means, it probes the relevant fraction for applications where carbon is in contact to aqueous solutions. Overall, the BT method can be conveniently applied to a broad range of carbon materials as long as the samples are sufficiently hydrophilic and of the enough sample amount is provided.

Practical aspects of the Boehm titration method are evaluated for obtaining reliable results in the quantification of oxygen-containing surface groups in a short time. Analytical criteria such as accuracy, repeatability, precision, and robustness are applied. Oxidized multi-walled carbon nanotubes (MWCNTs) are used as the model substance. Different reaction bases (NaHCO3(aq), Na2CO3(aq), NaOH(aq)) are applied and treatment times are studied. We also show that smaller amounts of carbon material can be reliably analyzed by using an autotitrator combined with a pH electrode. We find that indirect titration with Na2CO3 results in the highest titration precision and accuracy despite the lower base strength compared with NaOH. Therefore, CO2 impurities do not have to be removed and only 7 min is necessary for one titration. The titration error with respect to the proposed method is 0.15% of the aliquot volume. The mixing method during the carbon treatment with bases (stirring, shaking, ultrasound treatment) has no influence on the result as long as one allows a few hours for the reaction to complete. Finally, we provide a standard operating procedure for obtaining results with high precision during Boehm titration.

Points of zero charge, pH(pzc), of various samples of NbC, WC, SiC and TiC powders were investigated using a batch equilibration method. The examined powders were both laboratory prepared (NbC and WC via plasma-chemical method (PCM), while SiC was sol-gel derived) and commercial ones (WC, TiC, and laser derived SiC). The applied solid/liquid ratio ranged from 0.1 to 0.3 g/20 ml. The aqueous solution of KNO3 (10(-3) to 10(-1) mol/l) was used as a background electrolyte. The points of zero charge for all investigated carbides were found to be between 3.2 and 5.0. They were not affected by the concentration of KNO3, indicating its nonspecific nature vis-a-vis studied carbides. The pH(pzc) values were correlated with the physicochemical properties of investigated powders. (c) 2006 Elsevier B.V. All rights reserved.

The aim of this work is to gain a better fundamental understanding of the nature Of Surface oxide sites present on activated carbon cloth (ACC) surface, and their role in the adsorption process. BET surface area of ACC was measured by means of benzene adsorption isotherms. The amount and the type of surface oxygen groups were determined by thermogravimetric analysis and titration following Boehms method. Batch adsorption tests were conducted to evaluate equilibrium adsorption isotherms of phenol on ACC. It was shown that both surface area and surface groups composition had quite an impact on adsorption properties of ACC against phenol. Progress in Advanced Materials and Processes, 5th Conference of the Yugoslav-Materials-Research-Society (Yu-MRS 2003), Sep 15-19, 2003, Herceg Novi, Yugoslavia