Laboratory test to evaluate the resistance of cementitious materials to biodeterioration in sewer network conditions

The biodeterioration of cementitious materials in sewer networks has become a major economic, ecological, and public health issue. Establishing a suitable standardized test is essential if sustainable construction materials are to be developed and qualified for sewerage environments. Since purely chemical tests are proven to not be representative of the actual deterioration phenomena in real sewer conditions, a biological test–named the Biogenic Acid Concrete (BAC) test–was developed at the University of Toulouse to reproduce the biological reactions involved in the process of concrete biodeterioration in sewers. The test consists in trickling a solution containing a safe reduced sulfur source onto the surface of cementitious substrates previously covered with a high diversity microbial consortium. In these conditions, a sulfur-oxidizing metabolism naturally develops in the biofilm and leads to the production of biogenic sulfuric acid on the surface of the material. The representativeness of the test in terms of deterioration mechanisms has been validated in previous studies. A wide range of cementitious materials have been exposed to the biodeterioration test during half a decade. On the basis of this large database and the expertise gained, the purpose of this paper is (i) to propose a simple and robust performance criterion for the test (standardized leached calcium as a function of sulfate produced by the biofilm), and (ii) to demonstrate the repeatability, reproducibility, and discriminability of the test method. In only a 3-month period, the test was able to highlight the differences in the performances of common cement-based materials (CEM I, CEM III, and CEM V) and special calcium aluminate cement (CAC) binders with different nature of aggregates (natural silica and synthetic calcium aluminate). The proposed performance indicator (relative standardized leached calcium) allowed the materials to be classified according to their resistance to biogenic acid attack in sewer conditions. The repeatability of the test was confirmed using three different specimens of the same material within the same experiment and the reproducibility of the results was demonstrated by standardizing the results using a reference material from 5 different test campaigns. Furthermore, developing post-testing processing and calculation methods constituted a first step toward a standardized test protocol

Long term analysis of N2O emission from partial nitritation anammox process under oxygen limitation

International audiencePartial nitritation with anammox (PNA) process was achieved during 300 days to investigate the fate of N2O and NO. N2O emission factor increased from 0.4 ± 0.1 % up to 6.1 ± 0.3 % during intensification phase of 5 months and progressively stabilized at 2.0 ± 0.1 % after 10 months without any significant emission of NO. The emission of N2O correlated with the ammonium consumption rate and the oxygen transfer rate. Experiment carried out in anoxic condition suggested that heterotrophic denitrification poorly contributed. Measurements of δ15N, δ18O and SP of N2O demonstrated that its production resulted from the reduction of nitrite. The stimulating effect of nitrite on N2O production was demonstrated with specific tests and observed during transient nitrite accumulation periods. This study highlighted the importance of nitrite and oxygen transfer rate control for future control strategies aiming to mitigate N2O emission in PNA system

Modelling PAHs removal in activated sludge process: effect of disintegration

International audienceThe removal of polycyclic aromatic hydrocarbons (PAHs) in activated sludge was evaluated using two laboratory-scale bioreactors, coupled or not with a disintegration system (sonication). Mass balances performed on each system underlined that PAHs removal was significantly improved after sludge disintegration, especially for the higher molecular weight PAHs studied, which tended to adsorb to suspended matter. A model was developed in order to study the effect of sludge disintegration on the content of dissolved and colloidal matter (DCM), and to predict the potential impacts on PAHs availability and degradation. Results showed that this new model was efficient for capturing apparent degradation improvement trends and for discriminating between the involved mechanisms. This study showed that DCM content increased after sludge disintegration, and proved to be the main driver for improving PAHs apparent degradation

Combining thermophilic aerobic reactor (TAR) with mesophilic anaerobic digestion (MAD) improves the degradation of pharmaceutical compounds

International audienceThe removal efficiency of nine pharmaceutical compounds from primary sludge was evaluated in two different operating conditions: (i) in conventional Mesophilic Anaerobic Digestion (MAD) alone and (ii) in a co-treatment process combining Mesophilic Anaerobic Digestion and a Thermophilic Aerobic Reactor (MAD-TAR). The pilot scale reactors were fed with primary sludge obtained after decantation of urban wastewater. Concerning the biodegradation of organic matter, thermophilic aeration increased solubilization and hydrolysis yields of digestion, resulting in a further 26% supplementary removal of chemical oxygen demand (COD) in MAD-TAR process compared to the conventional mesophilic anaerobic digestion. The highest removal rate of target micropollutants were observed for caffeine (CAF) and sulfamethoxazole (SMX) (>89%) with no substantial differences between both processes. Furthermore, MAD-TAR process showed a significant increase of removal efficiency for oxazepam (OXA) (73%), propranolol (PRO) (61%) and ofloxacine (OFL) (41%) and a slight increase for diclofenac (DIC) (4%) and 2 hydroxy-ibuprofen (2OH-IBP) (5%). However, ibuprofen (IBP) and carbamazepine (CBZ) were not degraded during both processes. Anaerobic digestion affected the liquid-solid partition of most target compounds. Sorbed fraction of pharmaceutical compounds on the sludge tend to decrease after digestion, this tendency being more pronounced in the case of the MAD-TAR process due to much lower concentration of solids

Development and validation of QuEChERS-based extraction for quantification of nine micropollutants in wastewater treatment plant

Early AccessInternational audienceA modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was established for simultaneous quantification of eight pharmaceutical molecules (2-hydroxyibuprofen, diclofenac, ibuprofen, propranolol, ofloxacin, oxazepam, sulfamethoxazole, carbamazepine) and caffeine in environmental matrices. Analysis was performed by ultra-high-performance liquid chromatography with tandem mass spectrometry (UHPLC-MS-MS). Quantification was performed by using the 13C internal standard method for each molecule. Two methods were firstly optimized on freeze-dried waste activated sludge and then applied and validated on real complex matrices, which have contrasted physicochemical properties, i.e., clarified wastewater and primary sludge. The combination of acetate buffer with MgSO4 (protocol A) and citrate buffer with Na2SO4 (protocol B) was found necessary to recover the nine targeted compounds. Adding a higher salts quantity of Na2SO4 (protocol B) compared to MgSO4 (protocol A) is crucial to increase the ionic strength of the aqueous solution and to obtain comparable extraction recoveries of the targetedmolecules. Adding two times solvent volume to the aqueous phase leads to increased absolute recovery for all molecules and both protocols. After demonstration of the final protocol’s performance on the control matrix, its robustness was tested on the matrices of interest. As a result, the two proposed detection methods exhibit good reproducibility, high sensitivity, and high reliability