On-site calibration of a phase fraction meter by an inverse technique

The formal calibration procedure of a phase fraction meter is based on registering the outputs resulting from imposed phase fractions at known flow regimes. This can be straightforwardly done in laboratory conditions, but is rarely the case in industrial conditions, and particularly for on-site applications. Thus, there is a clear need for less restrictive calibration methods regarding to the prior knowledge of the complete set of inlet conditions. A new procedure is proposed in this work for the on-site construction of the calibration curve from total flown mass values of the homogeneous dispersed phase. The solution is obtained by minimizing a convenient error functional, assembled with data from redundant tests to handle the intrinsic ill-conditioned nature of the problem. Numerical simulations performed for increasing error levels demonstrate that acceptable calibration curves can be reconstructed, even from total mass measured within a precision of up to 2%. Consequently, the method can readily be applied, especially in on-site calibration problems in which classical procedures fail due to the impossibility of having a strict control of all the input/output parameters.

Marine04 marine radiocarbon age calibration, 0-26 cal kyr BP

New radiocarbon calibration curves, IntCal04 and Marine04, have been constructed and internationally ratified to replace the terrestrial and marine components of IntCal98. The new calibration data sets extend an additional 2000 yr, from 0-26 cal kyr BP (Before Present, 0 cal. BP = AD 1950), and provide much higher resolution, greater precision, and more detailed structure than IntCal98. For the Marine04 curve, dendrochronologically-dated tree-ring samples, converted with a box diffusion model to marine mixed-layer ages, cover the period from 0-10.5 call kyr BR Beyond 10.5 cal kyr BP, high-resolution marine data become available from foraminifera in varved sediments and U/Th-dated corals. The marine records are corrected with site-specific C-14 reservoir age information to provide a single global marine mixed-layer calibration from 10.5-26.0 cal kyr BR A substantial enhancement relative to IntCal98 is the introduction of a random walk model, which takes into account the uncertainty in both the calendar age and the C-14 age to calculate the underlying calibration curve (Buck and Blackwell, this issue). The marine data sets and calibration curve for marine samples from the surface mixed layer (Marine04) are discussed here. The tree-ring data sets, sources of uncertainty, and regional offsets are presented in detail in a companion paper by Reimer et al. (this issue).

Developments in radiocarbon calibration for archaeology

This update on radiocarbon calibration results from the 19th International Radiocarbon Conference at Oxford in April 2006, and is essential reading for all archaeologists. The way radiocarbon dates and absolute dates relate to each other differs in three periods: back to 12400 cal BR radiocarbon dates can be calibrated with tree rings, and the calibration curve in this form should soon extend back to 18 000 cal BP Between 12 400 and 26000 cal BR the calibration curves are based on marine records, and thus are only a best estimate of atmospheric concentrations. Beyond 26000 cal BR dates have to be based on comparison (rather than calibration) with a variety of records. Radical variations are thus possible in this period, a highly significant caveat,for the dating of middle and lower Paleolithic art, artefacts and animal and human remains.

Towards radiocarbon calibration beyond 28ka using speleothems from the Bahamas

We present a new speleothem record of atmospheric Δ14C between 28 and 44 ka that offers considerable promise for resolving some of the uncertainty associated with existing radiocarbon calibration curves for this time period. The record is based on a comprehensive suite of AMS 14C ages, using new low-blank protocols, and U–Th ages using high precision MC-ICPMS procedures. Atmospheric Δ14C was calculated by correcting 14C ages with a constant dead carbon fraction (DCF) of 22.7 ± 5.9%, based on a comparison of stalagmite 14C ages with the IntCal04 (Reimer et al., 2004) calibration curve between 15 and 11 ka. The new Δ14C speleothem record shows similar structure and amplitude to that derived from Cariaco Basin foraminifera (Hughen et al., 2004, 2006), and the match is further improved if the latter is tied to the most recent Greenland ice core chronology (Svensson et al., 2008). These data are however in conflict with a previously published 14C data set for a stalagmite record from the Bahamas — GB-89-24-1 (Beck et al., 2001), which likely suffered from 14C analytical blank subtraction issues in the older part of the record. The new Bahamas speleothem ∆14C data do not show the extreme shifts between 44 and 40 ka reported in the previous study (Beck et al., 2001). Causes for the observed structure in derived atmospheric Δ14C variation based on the new speleothem data are investigated with a suite of simulations using an earth system model of intermediate complexity. Data-model comparison indicates that major fluctuations in atmospheric ∆14C during marine isotope stage 3 is primarily a function of changes in geomagnetic field intensity, although ocean–atmosphere system reorganisation also played a supporting role.

Comparison of the GEANT4 releases 8.2 and 9.2 in terms of a pCT reduced calibration curve

The GEANT4 simulations are essential for the development of medical tomography with proton beams pCT. In the case of thin absorbers the latest releases of GEANT4 generate very similar final spectra which agree well with the results of other popular Monte Carlo codes like TRIM/SRIM, or MCNPX. For thick absorbers, however, the disagreements became evident. In a part, these disagreements are due to the known contradictions in the NIST PSTAR and SRIM reference data. Therefore, it is interesting to compare the GEANT4 results with each other, with experiment, and with diverse code results in a reduced form, which is free from this kind of doubts. In this work such comparison is done within the Reduced Calibration Curve concept elaborated for the proton beam tomography. © 2010 IEEE.

Calibration and simulations of SIXS-P's response to energetic particles

The Solar Intensity X-ray and particle Spectrometer (SIXS) on board BepiColombo's Mercury Planetary Orbiter (MPO) will study solar energetic particles moving towards Mercury and solar X-rays on the dayside of Mercury. The SIXS instrument consists of two detector sub-systems; X-ray detector SIXS-X and particle detector SIXS-P. The SIXS-P subdetector will detect solar energetic electrons and protons in a broad energy range using a particle telescope approach with five outer Si detectors around a central CsI(Tl) scintillator. The measurements made by the SIXS instrument are necessary for other instruments on board the spacecraft. SIXS data will be used to study the Solar X-ray corona, solar flares, solar energetic particles, the Hermean magnetosphere, and solar eruptions. The SIXS-P detector was calibrated by comparing experimental measurement data from the instrument with Geant4 simulation data. Calibration curves were produced for the different side detectors and the core scintillator for electrons and protons, respectively. The side detector energy response was found to be linear for both electrons and protons. The core scintillator energy response to protons was found to be non-linear. The core scintillator calibration for electrons was omitted due to insufficient experimental data. The electron and proton acceptance of the SIXS-P detector was determined with Geant4 simulations. Electron and proton energy channels are clean in the main energy range of the instrument. At higher energies, protons and electrons produce non-ideal response in the energy channels. Due to the limited bandwidth of the spacecraft's telemetry, the particle measurements made by SIXS-P have to be pre-processed in the data processing unit of the SIXS instrument. A lookup table was created for the pre-processing of data with Geant4 simulations, and the ability of the lookup table to provide spectral information from a simulated electron event was analysed. The lookup table produces clean electron and proton channels and is able to separate protons and electrons. Based on a simulated solar energetic electron event, the incident electron spectrum cannot be determined from channel particle counts with a standard analysis method.

Determination of 5-aminosalicylic acid in pharmaceutical formulations by square wave voltammetry at pencil graphite electrodes

An analytical method for the determination of the anti-inflammatory drug 5-aminosalicylic acid (5-ASA) in pharmaceutical formulations using square wave voltammetry at pencil graphite electrodes was developed. After the optimization of the experimental conditions, calibration curves were obtained in the linear concentration range from 9.78 × 10-7 to 7.25 × 10-5 mol L-1 resulting in a limit of detection of 2.12 ± 0.05 x 10-8 mol L-1. Statistical tests showed that the concentrations of 5-ASA in commercial tablets and enemas obtained with the proposed voltammetric method agreed with HPLC values at a 95% confidence level.

Evaluation of laser induced breakdown spectrometry for the determination of macro and micronutrients in pharmaceutical tablets

The aim of this work is to demonstrate the feasibility of laser induced breakdown spectrometry (LIBS) for the determination of macro and micronutrients in multielement tablets. The experimental setup was designed by using a laser Q-switch (Nd:YAG, 10 Hz, lambda = 1064 nm) and the emission signals were collected by lenses into an optical fiber coupled to an echelle spectrometer equipped with a high-resolution intensified charge coupled device (ICCD). Tablets were cryogenically ground and thereafter pelletized before LIBS analysis. Calibration curves were made by employing samples and mixtures of commercial multielement tablets with binders at different ratios. Best results were achieved by using the following experimental conditions: 29 J cm(-2) laser fluence, 165 mm lens to sample distance (f = 200 mm), 2.0 mu s delay time, 5.0 mu s integration time and 5 accumulated laser pulses. In general, the results obtained by the proposed LIBS procedure were in agreement with those obtained by ICP OES from the corresponding acid digests and coefficients variation of LIBS measurements varied from 2 to 16%. The metrological figures of merit indicate that LIBS fits for the intended purposes, and can be recommended for the analysis of multielement tablets and similar matrices aiming the determination of Ca, Cu, Fe, Mg, Mn, P and Zn.

Evaluation of laser induced breakdown spectroscopy for cadmium determination in soils

Cadmium is known to be a toxic agent that accumulates in the living organisms and present high toxicity potential over lifetime. Efforts towards the development of methods for microanalysis of environmental samples, including the determination of this element by graphite furnace atomic absorption spectrometry (GFAAS). inductively coupled plasma optical emission spectrometry (ICP OES), and inductively coupled plasma-mass spectrometry (ICP-MS) techniques, have been increasing. Laser induced breakdown spectroscopy (UBS) is an emerging technique dedicated to microanalysis and there is a lack of information dealing with the determination of cadmium. The aim of this work is to demonstrate the feasibility of LIBS for cadmium detection in soils. The experimental setup was designed using a laser Q-switched (Nd:YAG, 10 Hz, lambda = 1064 nm) and the emission signals were collimated by lenses into an optical fiber Coupled to a high-resolution intensified charge-coupled device (ICCD)-echelle spectrometer. Samples were cryogenically ground and thereafter pelletized before LIBS analysis. Best results were achieved by exploring a test portion (i.e. sampling spots) with larger surface area, which contributes to diminish the uncertainty due to element specific microheterogeneity. Calibration curves for cadmium determination were achieved using certified reference materials. The metrological figures of merit indicate that LIBS can be recommended for screening of cadmium contamination in soils. (C) 2009 Elsevier B.V. All rights reserved.

Estimation of hexenuronic acids and kappa number in kraft pulps of Eucalyptus globulus by Fourier transform near infrared spectroscopy and multivariate analysis

Fourier transform near infrared (FT-NIR) spectroscopy was evaluated as an analytical too[ for monitoring residual Lignin, kappa number and hexenuronic acids (HexA) content in kraft pulps of Eucalyptus globulus. Sets of pulp samples were prepared under different cooking conditions to obtain a wide range of compound concentrations that were characterised by conventional wet chemistry analytical methods. The sample group was also analysed using FT-NIR spectroscopy in order to establish prediction models for the pulp characteristics. Several models were applied to correlate chemical composition in samples with the NIR spectral data by means of PCR or PLS algorithms. Calibration curves were built by using all the spectral data or selected regions. Best calibration models for the quantification of lignin, kappa and HexA were proposed presenting R-2 values of 0.99. Calibration models were used to predict pulp titers of 20 external samples in a validation set. The lignin concentration and kappa number in the range of 1.4-18% and 8-62, respectively, were predicted fairly accurately (standard error of prediction, SEP 1.1% for lignin and 2.9 for kappa). The HexA concentration (range of 5-71 mmol kg(-1) pulp) was more difficult to predict and the SEP was 7.0 mmol kg(-1) pulp in a model of HexA quantified by an ultraviolet (UV) technique and 6.1 mmol kg(-1) pulp in a model of HexA quantified by anion-exchange chromatography (AEC). Even in wet chemical procedures used for HexA determination, there is no good agreement between methods as demonstrated by the UV and AEC methods described in the present work. NIR spectroscopy did provide a rapid estimate of HexA content in kraft pulps prepared in routine cooking experiments.

Void fraction measurement and signal analysis from multiple-electrode impedance sensors

Void fraction sensors are important instruments not only for monitoring two-phase flow, but for furnishing an important parameter for obtaining flow map pattern and two-phase flow heat transfer coefficient as well. This work presents the experimental results obtained with the analysis of two axially spaced multiple-electrode impedance sensors tested in an upward air-water two-phase flow in a vertical tube for void fraction measurements. An electronic circuit was developed for signal generation and post-treatment of each sensor signal. By phase shifting the electrodes supplying the signal, it was possible to establish a rotating electric field sweeping across the test section. The fundamental principle of using a multiple-electrode configuration is based on reducing signal sensitivity to the non-uniform cross-section void fraction distribution problem. Static calibration curves were obtained for both sensors, and dynamic signal analyses for bubbly, slug, and turbulent churn flows were carried out. Flow parameters such as Taylor bubble velocity and length were obtained by using cross-correlation techniques. As an application of the void fraction tested, vertical flow pattern identification could be established by using the probability density function technique for void fractions ranging from 0% to nearly 70%.

Gas Chromatographic Analysis of Dimethyltryptamine and beta-Carboline Alkaloids in Ayahuasca, an Amazonian Psychoactive Plant Beverage

Introduction - Ayahuasca is obtained by infusing the pounded stems of Banisteriopsis caapi in combination with the leaves of Psychotria viridis. P. viridis is rich in the psychedelic indole N,N-dimethyltryptamine, whereas B. caapi contains substantial amounts of beta-carboline alkaloids, mainly harmine, harmaline and tetrahydroharmine, which are monoamine-oxidase inhibitors. Because of differences in composition in ayahuasca preparations, a method to measure their main active constituents is needed. Objective - To develop a gas chromatographic method for the simultaneous determination of dimethyltryptamine and the main beta-carbolines found in ayahuasca preparations. Methodology - The alkaloids were extracted by means of solid phase extraction (C(18)) and detected by gas chromatography with nitrogen/phosphorous detector. Results - The lower limit of quantification (LLOQ) was 0.02 mg/mL for all analytes. The calibration curves were linear over a concentration range of 0.02-4.0 mg/mL (r(2) > 0.99). The method was also precise (RSD < 10%). Conclusion - A simple gas chromatographic method to determine the main alkaloids found in ayahuasca was developed and validated. The method can be useful to estimate administered doses in animals and humans for further pharmacological and toxicological investigations of ayahuasca. Copyright (C) 2009 John Wiley & Sons, Ltd.