This paper was accepted for publication in the journal Carbon and the definitive published version is available at http://dx.doi.org/10.1016/j.carbon.2014.08.081© 2014 Elsevier Ltd. All rights reserved.Two commercial carbons, coconut shell- and wood-based were chosen to evaluate the mechanisms of carbamazepine (CBZ) and sulfamethoxazole (SMX) adsorption from a low (ppm level) concentration of these pharmaceuticals. The initial sample and those after adsorption were extensively characterized using potentiometric titration, thermal analysis combined with mass spectroscopy, FTIR, and XPS. It was found that not only porosity but also surface chemistry plays an important role in the adsorption process. The results show that extensive surface reactions take place during adsorption and adsorbates undergo significant transformations in the pore system. The ability of carbon surfaces to form superoxide ions results in the oxidation of CBZ and SMX, and their partial decomposition. Surface chemistry also promotes dimerization of the latter species. Moreover, functional groups of CBZ and SMX, mainly amines, react with oxygen groups of the carbon surface. Thus not only microporous carbons with sizes of pores similar to those of adsorbate molecules, but the carbons with large pores, rich in oxygen groups, can efficiently remove these pharmaceuticals following the reactive adsorption mechanism

This study was undertaken to understand the extent and nature of problems in x-ray photoelectron spectroscopy (XPS) data reported in the literature. It first presents an assessment of the XPS data in three high-quality journals over a six-month period. This analysis of 409 publications showing XPS spectra provides insight into how XPS is being used, identifies the common mistakes or errors in XPS analysis, and reveals which elements are most commonly analyzed. More than 65% of the 409 papers showed fitting of XP spectra. An ad hoc group (herein identified as “the committee”) of experienced XPS analysts reviewed these spectra and found that peak fitting was a common source of significant errors. The papers were ranked based on the perceived seriousness of the errors, which ranged from minor to major. Major errors, which, in the opinion of the ad hoc committee, can render the interpretation of the data meaningless, occurred when fitting protocols ignored underlying physics and chemistry or contained major errors in the analysis. Consistent with other materials analysis data, ca. 30% of the XPS data or analysis was identified as having major errors. Out of the publications with fitted spectra, ca. 40% had major errors. The most common elements analyzed by XPS in the papers sampled and researched at an online database, include carbon, oxygen, nitrogen, sulfur, and titanium. A scrutiny of the papers showing carbon and oxygen XPS spectra revealed the classes of materials being studied and the extent of problems in these analyses. As might be expected, C 1s and O 1s analyses are most often performed on sp2-type materials and inorganic oxides, respectively. These findings have helped focus a series of XPS guides and tutorials that deal with common analysis issues. The extent of problematic data is larger than the authors had expected. Quantification of the problem, examination of some of the common problem areas, and the development of targeted guides and tutorials may provide both the motivation and resources that enable the community to improve the overall quality and reliability of XPS analysis reported in the literature.