Hollow fiber liquid phase microextraction as a preconcentration and clean-up step after pressurized hot water extraction for the determination of non-steroidal anti-inflammatory drugs in sewage sludge

A method for the quantitative determination of non-steroidal anti-inflammatory drugs (NSAIDs) in sewage sludge was developed and validated. The target compounds were extracted using pressurized hot water extraction (PHWE) and then purified and preconcentrated by three-phase hollow fiber liquid phase microextraction (HF-LPME) followed by LC–ESI-MS analysis. The PHWE was optimized with regard to the pH of solvent as well as other operational parameters. The optimum conditions were 0.01 M NaOH as the extraction solvent, temperature of 120 °C, pressure of 100 bar, static time 5 min, 5 cycles, flush volume 90% and purge time 60 s. Spike recoveries for sludge samples spiked at 200 ng g⁻¹ were in the range of 101–109% but for the native drugs in non-spiked sludge samples, recoveries were 38.9%, 59.8%, 90.3% and 47.8% for ketoprofen, naproxen, diclofenac and ibuprofen, respectively. Donor phase pH, ionic strength and extraction time were optimized for HF-LPME after PHWE. The optimum conditions were 2 h extraction at pH 1.5 without salt addition. Enrichment factors in the range of 947–1213 times were achieved (extraction recoveries were 23.6–30.3%) for HF-LPME after PHWE. The matrix effect on the ionization of drugs in LC–ESI-MS was also investigated. The results show that there is a smaller matrix effect (−8.9% to +14.6%) in comparison with other published values obtained using solid phase extraction (SPE) for clean-up after pressurized liquid extraction (PLE). Method detection limits (MDLs) and method quantification limits (MQLs) for different drugs were in the range of 0.4–3.7 ng g⁻¹ and 1.5–12.2 ng g⁻¹ in dried sludge samples, respectively. The characteristics of the proposed method were compared with those of other published works. The considerably lower ion suppression/enhancement and minimum use of organic solvents (a few microliters of di-n-hexyl ether) in the sample preparation step are two highlighted advantages of the proposed method in comparison with previously published works. The method was applied to determine NSAIDs in sewage sludge from Källby wastewater treatment plant (Lund, Sweden) in April, June, August and October 2010. The highest concentration level was recorded for ibuprofen in the April sewage sludge sample (588 ng g⁻¹) and all of the selected NSAIDs were detected in all the samples analyzed.     

Development of a turbulent boundary layer after a step from smooth to rough surface

The flow developing downstream of a step change from smooth to rough surface condition is studied in the light of Townsend’s wall similarity hypothesis. Previous studies seem to support the hypothesis for channel and pipe flows, but there are considerable controversies about its application to boundary layers and in particular to surface roughness formed by spanwise bars. It has been suggested that this controversy arises from insufficient separation of scales between the boundary layer thickness and the roughness length scale. An experimental investigation has therefore been undertaken where the flow evolves from a fully developed smooth wall boundary layer at high Reynolds numbers over a step in surface roughness (Re _θ = 13,400 at the step). The flow is mapped through the development of the internal layer until the flow is fully developed over the rough wall. The internal layer is found to grow as δ ∼ X ^0.73, and after about 15 boundary layer thicknesses at the step, the internal layer has reached the outer edge of the incoming layer. At the last rough wall measurement station, the Reynolds number has grown to Re _θ ≈ 32,600 and the ratio of boundary layer to roughness length scales is δ/k ≈ 140. The outer layer differences between the smooth and the rough wall data were found to be sufficiently small to conclude that for this setup the Townsend’s wall similarity hypothesis appears to hold.     

Magnetic Properties of Nanoparticles of Antiferromagnetic Materials

Hyperfine Interactions - The magnetic properties of antiferromagnetic nanoparticles have been studied by Mössbauer spectroscopy and neutron scattering. Temperature series of Mössbauer...     

Stable convergence acceleration using Laplace transforms

Summary We consider the general class of power series where the terms may be expressed as the Laplace transforms of known functions. The sum of the series can then be evaluated efficiently and accurately by means of quadrature schemes, recently published by Frank Stenger. The method works also far outside the region of convergence as will be illustrated by numerical examples.Dedicated to Professor Lothar Collatz on the occasion of his 75th birthday     

SCF and limited CI calculations for assignment of the Auger spectrum and of the satellites in the soft X-ray spectrum of H2O

SCF and limited CI calculations have been performed for a number of excited states of doubly ionized water. The calculations allowed an assignment of both the Auger spectrum and most of the satellites in the soft X-ray spectrum. The assignment for the two highest peaks in the Auger spectrum was ambiguous. SCF calculations of the K emission spectrum of H₂O were also performed. It was found that limited CI calculations were of importance for some states with two open shells in one symmetry. Such effects are caused by large off-diagonal lagrangian multiplies connecting the open shells in the reference configuration.     

Valence electron shake-up in photoelectron spectra

Valence electron shake-up phenomena are important in ultraviolet photoelectron spectroscopy because extra bands are formed which may complicate the interpretation, and because the primary bands are displaced in energy which may invalidate comparisons with calculated ionization energies. It would be of value during experimental work to have access to simple methods for an approximate estimation of these effects. Such methods are presented here together with applications to the photoelectron spectra of ethylene and benzene.     

Hadronization of excited nucleons in nuclear collisions at ISR energies

Calorimeters downstream of the intersection of pα and αα beams in the ISR have been used to study the hadronization of excited nucleons. These data extend and support the conclusions from previous studies of the A-dependence of particle multiplicities in ultrarelativistic p-nucleus collisions, which provided evidence that the proton hadronizes outside the nuclear volume.     

Analysis of hashing with chaining in the prime area

The expected performance of hashing with chaining in the prime area is analyzed. The method analyzed is briefly characterized as hashing with chaining of overflow records in the prime storage area, using one or several noncoalescing chains per bucket, and with random search for empty space. The analysis is asymptotic, and it is assumed that deletions do not occur. Simple closed formulas cannot be obtained, except in the case of bucket size one, but numerical results are readily computed. The expected performance compares favorably with that of other methods for handling overflow records.