Thermal decomposition of crystalline struvite provides an efficient and well controllable method for the synthesis of mesoporous phosphates.

The contamination by chlorinated organic solvents is a worldwide problem as they can deeply penetrate aquifers, accumulating in the sub-surface as lenses of highly hazardous pollutants. In recent years, so called in situ oxidation processes have been developed to remediate chlorinated organic solvents from groundwater and soil by injecting solutions of oxidising agents such as permanganate or peroxydisulphate. We here present modified layered double hydroxides (LDHs) with intercalated oxidising agents that might serve as new reactants for these remediation strategies. LDHs might serve as support and stabiliser materials for selected oxidising agents during injection, as the uncontrolled reaction and consumption might be inhibited, and guarantee that the selected oxidants persist in the subsurface after injection. In this study, LDHs with hydrotalcite- and hydrocalumite-like structures intercalated with permanganate and peroxydisulphate anions were synthesised and their efficiency was tested in batch experiments using trichloroethene or 1,1,2-trichloroethane as the target contaminants. All samples were characterised using powder X-ray diffraction, thermal analysis coupled with mass spectrometry to directly analyse evolving gases, and Fourier-transform infrared spectroscopy. Additionally, particle size distribution measurements were carried out on the synthesised materials. Results of the batch experiments confirmed the hypothesis that oxidising agents keep their properties after intercalation. Permanganate intercalated LDHs proved to be most efficient at degrading trichloroethene while peroxydisulphate intercalated Ca,Al-LDHs were the most promising studied reactants degrading 1,1,2-trichloroethane. The detection of dichloroethene as well as the transformation of the studied reactants into new LDH phases confirmed the successful degradation of the target contaminant by oxidation processes generated from the intercalated oxidising agent.

Nowadays, the contamination of groundwater and soils by chlorinated organic solvents is a severe and worldwide problem. Due to their swelling properties, Layered Double Hydroxides (LDHs) are potentially excellent compounds to retain chlorinated organic solvents from aquifers. By intercalating organic anions, the polarity of the interlayer space can be changed from hydrophilic to hydrophobic, enhancing the adsorption of chloro-organic molecules onto the alkyl chains of intercalated organic anions. In this study, organically modified LDHs were synthesized and their efficiency was tested in batch experiments with three different chlorinated organic solvents, namely trichloroethylene, 1,1,2-trichloroethane and trichloromethane (chloroform), to examine the influence of the chain length and the functional group of the intercalated organic anion upon the retention ability of a LDH due to different electronic interactions and different sizes of the interlayer space. All synthesized and used samples were characterized using powder X-ray diffraction, thermal analysis coupled with mass spectrometry and Fourier-transform infrared spectroscopy; freshly synthesized materials were additionally analyzed regarding their particle size distribution and specific surface area. Results of the batch experiments showed that only LDHs with intercalated long-chain organic anions could be efficient adsorbents for the removal of chlorinated organic solvents from contaminated water. A selective efficiency towards 1,1,2-trichloroethane and trichloromethane can be proposed for these reactants.

No abstract

Nowadays, the contamination of groundwater and soils by highly hazardous and toxic chlorinated solvents is a global issue. Over the past years, different remediation strategies have been developed, involving injection of reactive solutions and/or particles. However, a major difficulty is the monitoring of injected particles during the injection and after secondary mobilisation by groundwater flow. This study is focussed on the development of directly traceable particles by combining fluorescein with Layered Double Hydroxides (LDHs). We present here the facile and easily tuneable synthesis of fluorescing LDHs (Fluo-LDH) via co-precipitation under supersaturation conditions. Their ability to mimic particle sizes of previously studied reactive LDHs, which proved to be able to adsorb or degrade chlorinated organic solvents from aqueous solutions, was investigated as well. Tests using a novel Optical Image Profiler (OIP) confirmed that the fluorescent LDHs can be easily detected with this tool. Even LDHs with the lowest amount of fluorescent dye were detectable. Together with the use of an OIP, which is capable of exciting the fluorescent material and collecting real-time pictures, this can provide a new, efficient, and cost-effective method for in situ tracing of injected particles in the subsurface.