This study evaluated the impact of secondary municipal effluent discharge on carbamazepine, diclofenac, and metoprolol concentrations in small and medium rivers in northern Germany and compared the measured environmental concentrations (MECs) to the predicted environmental concentrations (PECs) calculated with four well-established models. During a 1-year sampling period, secondary effluent grab samples were collected at four wastewater treatment plants (WWTPs) together with grab samples from the receiving waters upstream and downstream from the wastewater discharge points. The carbamazepine, diclofenac, and metoprolol concentrations were analyzed with high-performance liquid chromatography-tandem mass spectrometry (HPLC/MS-MS) after solid phase extraction. In the secondary effluents, 84-790 ng/L carbamazepine, 395-2100 ng/L diclofenac, and 745-5000 ng/L metoprolol were detected. The carbamazepine, diclofenac, and metoprolol concentrations analyzed in the rivers downstream from the secondary effluent discharge sites ranged from <5 to 68, 370, and 520 ng/L, respectively. Most of the downstream pharmaceutical concentrations were markedly higher than the corresponding upstream concentrations. The impact of wastewater discharge on the MECs in rivers downstream from the WWTPs was clearly demonstrated, but the correlations of the MECs with dilution factors were poor. The smallest rivers exhibited the largest maximum MECs and the widest ranges of MECs downstream from the wastewater discharge point. Three of the four tested models were conservative, as they showed higher PECs than the MECs in the rivers downstream from the WWTPs. However, the most detailed model underestimated the diclofenac concentrations.
In this study organic compounds in dichloromethane extracts of wastewater samples taken at different stages of a mineral oil refinery wastewater treatment plant were analysed by gas chromatography using a mass selective detector. Main constituents of the raw wastewater were n-alkanes, iso-alkanes, cyclic alkanes, aromatic hydrocarbons, and phenols. Also small concentrations of some heterocycles were detected. The data suggest that flotation is a suitable pre-treatment step for removing the major part of alkanes, aromatics and phenols. The flotation protects biological stages against inhibitory effects of e.g. phenols. The activated sludge process removes most of the remaining gas chromatographically detectable organics and only three iso-alkanes, traces of carboxylic acids and – exhibiting the highest concentration – acetic acid 2-(2-butoxyethoxy)-ethyl ester were found in the clarified effluent of the activated sludge process. These detected substances cannot explain the relatively high COD of the sedimentation effluent and it is assumed that the main part of the COD of the biologically treated mineral oil refinery wastewater is represented by humic material formed in the activated sludge process. As in the raw wastewater also volatile aromatics (e.g. toluene, xylenes, ethylbenzene) were detected it is recommended to collect and treat the off-gas of flotation units applied for petrochemical wastewater purification.
This study was carried out for gathering qualitative information about the potential of photocatalytic oxidation for the removal of trace organics (analysed by gas chromatography coupled to mass spectrometry, GC/MS) from biologicallypretreated greywater to make it suitable for high quality reuse applications like groundwater recharge. Additionally, fractions of bulk organics (humic substances, building blocks, and low molecular weight organic acids) were quantified by liquid chromatography with organic carbon detection.Biologically pretreated greywater was subjected to photocatalytic oxidation in open stirred vessel reactors with UV lamps positioned over the reactors. UV doses of 0, 5, and 15 Wh·L-1 and TiO2 P25 photocatalyst concentrations of 1, 5, 10, and 20 g·L-1 were investigated. Photocatalysis experiments with a 15 Wh·L-1UV dose were also conducted in the presence of 1 g·L-1 powdered activated carbon. Subsequent to mere contact of the photocatalyst to biologically pretreated greywater without UV, GC/MS did not indicate a substantial removal of trace organics, while humic substances were increasingly adsorbed by increasing photocatalyst concentration. A UV dose of 15 Wh·L-1 and TiO2 concentrations > 5 g·L-1 were favorable conditions for photocatalytic oxidation resulting in the removal of most of the trace organics, especially chlorinated phosphate flame retardants. Also humic substances were efficiently removed under these conditions. Photocatalytic oxidation is thus a promising process for advanced greywater treatment prior to groundwater recharge. Addition of powdered activated carbon did not improve trace and bulk organics removal by photocatalysis with a UV dose of 15 Wh·L-1and with photocatalyst concentrations > 5g·L
Wastewater originating from oil reclaiming (COD about 300 mg/l, TOC about 70 mg/l) which was pretreated by equalization, neutralization, adsorption to activated sludge from a publicly owned treatment work, flocculation, and flotation and finally oxidized in an activated sludge process was analyzed for humic acids and gas chromatographically detectable organic compounds. The humic acid concentration was estimated to represent about 15% of the COD. Hydrocarbons were detected in activated sludge, but no hydrocarbons were identified gas chromatographically. In the two analyzed wastewater samples ethers (mainly containing polyethoxy structures), carboxylic acids and carboxylic acid esters were found. In one sample several nitrogen compounds (amines and amides) were detected. Except for l,l'-oxybis-(2-methoxy)-ethane, which was a constituent of both samples, the organic gas chromatographically detectable compounds differed completely from sample to sample. This is obviously due to changing composition of the processed spent oils.
A technique for the determination of titanium and zirconium in human blood serum, after pressurized digestion utilizing ICP-MS coupled to an ultrasonic nebulizer (USN) and desolvating membrane is described. As no CRM for titanium is available, zirconium has been determined in order to demonstrate the accuracy of the technique, as the limits in blood are well known. Bone cement consists basically of a polymer, namely polymethylmethacrylate (PMMA). For better X-ray contrast some manufacturers use incorporated ZrO2 with a volume fraction of 10 to 15%. Thus, the zirconium present in the PMMA matrix can be used as an indicator for the PMMA particulate debris.
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