Evaluating Handheld X-Ray Fluorescence (XRF) Technology in Planetary Exploration: Demonstrating Instrument Stability and Understanding Analytical Constraints and Limits for Basaltic Rocks

NASA Technical Reports Server (NTRS)

Young, K. E.; Hodges, K. V.; Evans, C. A.

2012-01-01

While large-footprint X-ray fluorescence (XRF) instruments are reliable providers of elemental information about geologic samples, handheld XRF instruments are currently being developed that enable the collection of geochemical data in the field in short time periods (approx.60 seconds) [1]. These detectors are lightweight (1.3kg) and can provide elemental abundances of major rock forming elements heavier than Na. While handheld XRF detectors were originally developed for use in mining, we are working with commercially available instruments as prototypes to explore how portable XRF technology may enable planetary field science [2,3,4]. If an astronaut or robotic explorer visited another planetary surface, the ability to obtain and evaluate geochemical data in real-time would be invaluable, especially in the high-grading of samples to determine which should be returned to Earth. We present our results on the evaluation of handheld XRF technology as a geochemical tool in the context of planetary exploration.

Detection of trace metallic elements in oral lichenoid contact lesions using SR-XRF, PIXE, and XAFS

PubMed Central

Sugiyama, Tomoko; Uo, Motohiro; Wada, Takahiro; Omagari, Daisuke; Komiyama, Kazuo; Miyazaki, Serika; Numako, Chiya; Noguchi, Tadahide; Jinbu, Yoshinori; Kusama, Mikio; Mori, Yoshiyuki

2015-01-01

Oral lichen planus (OLP) and oral lichenoid contact lesions (OLCL) are chronic inflammatory mucocutaneous reactions with a risk of malignant transformation that alter the epithelium. OLP and OLCL have similar clinical and histopathological features and it is difficult to distinguish one from the other. Metallic restorations are suspected to generate OLCLs. Trace metal analysis of OLCL specimens may facilitate the discrimination of symptoms and identification of causative metallic restorations. The purpose of this study was to assess OLCL tissue samples for the prevalence of metallic elements derived from dental restorations, and to discriminate OLCL from OLP by using synchrotron radiation-excited X-ray fluorescence analysis (SR-XRF), particle-induced X-ray emission (PIXE), and X-ray absorption fine structure (XAFS). Typical elements of dental materials were detected in the OLCL, whereas no obvious element accumulation was detected in OLP and negative control specimens. The origin of the detected metallic elements was presumed to be dental alloys through erosion. Therefore, our findings support the feasibility of providing supporting information to distinguish OLCL from OLP by using elemental analysis. PMID:26085368

Influence of depositional environment in fossil teeth: a micro-XRF and XAFS study

NASA Astrophysics Data System (ADS)

Zougrou, I. M.; Katsikini, M.; Pinakidou, F.; Papadopoulou, L.; Tsoukala, E.; Paloura, E. C.

2014-04-01

The formation of metal-rich phases during the fossilization of vertebrate fossil teeth, recovered from various deposition environments in northern Greece, is studied by means of synchrotron radiation X-ray fluorescence (SR-XRF) as well as Fe and Mn K edge X-ray absorption fine structure (XAFS) spectroscopy. XRF line-scans from the samples' cross-sections revealed different contamination paths for Mn and Fe. The two-dimensional XRF maps illustrate the spatial distribution of P, Ca, Mn and Fe as well as the precipitation of Fe-rich phases in cementum, dentin and dentinal tubules. Goethite, lepidocrocite and ferrihydrite were detected in the samples' cross-section by means of Fe K edge EXAFS spectroscopy. Moreover the Fe and Mn K edge EXAFS revealed the presence of vivianite and birnessite (MnO2) on the external surface of two samples.

Prostate-cancer diagnosis by non-invasive prostatic Zinc mapping using X-Ray Fluorescence (XRF)

NASA Astrophysics Data System (ADS)

Cortesi, Marco

At present, the major screening tools (PSA, DRE, TRUS) for prostate cancer lack sensitivity and specificity, and none can distinguish between low-grade indolent cancer and high-grade lethal one. The situation calls for the promotion of alternative approaches, with better detection sensitivity and specificity, to provide more efficient selection of patients to biopsy and with possible guidance of the biopsy needles. The prime objective of the present work was the development of a novel non-invasive method and tool for promoting detection, localization, diagnosis and follow-up of PCa. The method is based on in-vivo imaging of Zn distribution in the peripheral zone of the prostate, by a trans-rectal X-ray fluorescence (XRF) probe. Local Zn levels, measured in 1--4 mm3 fresh tissue biopsy segments from an extensive clinical study involving several hundred patients, showed an unambiguous correlation with the histological classification of the tissue (Non-Cancer or PCa), and a systematic positive correlation of its depletion level with the cancer-aggressiveness grade (Gleason classification). A detailed analysis of computer-simulated Zn-concentration images (with input parameters from clinical data) disclosed the potential of the method to provide sensitive and specific detection and localization of the lesion, its grade and extension. Furthermore, it also yielded invaluable data on some requirements, such as the image resolution and counting-statistics, requested from a trans-rectal XRF probe for in-vivo recording of prostatic-Zn maps in patients. By means of systematic table-top experiments on prostate-phantoms comprising tumor-like inclusions, followed by dedicated Monte Carlo simulations, the XRF-probe and its components have been designed and optimized. Multi-parameter analysis of the experimental data confirmed the simulation estimations of the XRF detection system in terms of: delivered dose, counting statistics, scanning resolution, target-volume size and the

XRF Experiment for Elementary Surface Analysis

NASA Astrophysics Data System (ADS)

Köhler, E.; Dreißigacker, A.; Fabel, O.; van Gasselt, S.; Meyer, M.

2014-04-01

The proposed X-Ray Fluorescence Instrument Package (XRF-X and XRF-E) is being designed to quantitatively measure the composition and map the distribution of rock-surface materials in order to support the target area selection process for exploration, sampling, and mining. While energydispersive X-Ray fluorescence (EDX) makes use of Solar X-Rays for excitation to probe materials over arbitrary distances (by XRF-X), electron-beam excitation can be used for proximity measurements (by XRF-E) over short-distance of up to about 10 - 20m. This design is targeted at observing and analyzing surface compositions from orbital platforms and it is in particular applicable to all atmosphereless solidsurface bodies. While the instrument design for observing objects in the outer solar system is challenging due to low count rates, the Moon and objects of the asteroid belt usually receive solar X-ray radiation that allows to integrate a statistically reliable data basis. Asteroids are attractive targets and have been visited using X-ray fluorescence instruments by orbiting spacecraft in the past (Itokawa, Eros). They are wellaccessible objects for determining elemental compositions and assessing potential mineral resources.

Digital Equivalent Data System for XRF Labeling of Objects

NASA Technical Reports Server (NTRS)

Schramm, Harry F.; Kaiser, Bruce

2005-01-01

A digital equivalent data system (DEDS) is a system for identifying objects by means of the x-ray fluorescence (XRF) spectra of labeling elements that are encased in or deposited on the objects. As such, a DEDS is a revolutionary new major subsystem of an XRF system. A DEDS embodies the means for converting the spectral data output of an XRF scanner to an ASCII alphanumeric or barcode label that can be used to identify (or verify the assumed or apparent identity of) an XRF-scanned object. A typical XRF spectrum of interest contains peaks at photon energies associated with specific elements on the Periodic Table (see figure). The height of each spectral peak above the local background spectral intensity is proportional to the relative abundance of the corresponding element. Alphanumeric values are assigned to the relative abundances of the elements. Hence, if an object contained labeling elements in suitably chosen proportions, an alphanumeric representation of the object could be extracted from its XRF spectrum. The mixture of labeling elements and for reading the XRF spectrum would be compatible with one of the labeling conventions now used for bar codes and binary matrix patterns (essentially, two-dimensional bar codes that resemble checkerboards). A further benefit of such compatibility is that it would enable the conversion of the XRF spectral output to a bar or matrix-coded label, if needed. In short, a process previously used only for material composition analysis has been reapplied to the world of identification. This new level of verification is now being used for "authentication."

Use of x-ray fluorescence for in-situ detection of metals

NASA Astrophysics Data System (ADS)

Elam, W. T. E.; Whitlock, Robert R.; Gilfrich, John V.

1995-01-01

X-ray fluorescence (XRF) is a well-established, non-destructive method of determining elemental concentrations at ppm levels in complex samples. It can operate in atmosphere with no sample preparation, and provides accuracies of 1% or better under optimum conditions. This report addresses two sets of issues concerning the use of x-ray fluorescence as a sensor technology for the cone penetrometer, for shipboard waste disposal, or for other in-situ, real- time environmental applications. The first issue concerns the applicability of XRF to these applications, and includes investigation of detection limits and matrix effects. We have evaluated the detection limits and quantitative accuracy of a sensor mock-up for metals in soils under conditions expected in the field. In addition, several novel ways of improving the lower limits of detection to reach the drinking water regulatory limits have been explored. The second issue is the engineering involved with constructing a spectrometer within the 1.75 inch diameter of the penetrometer pipe, which is the most rigorous physical constraint. Only small improvements over current state-of-the-art are required. Additional advantages of XRF are that no radioactive sources or hazardous materials are used in the sensor design, and no reagents or any possible sources of ignition are involved.

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF TECHNOLOGIES FOR MEASURING TRACE ELEMENTS IN SOIL AND SEDIMENT NITON XLT700 SERIES XRF ANALYZER

EPA Science Inventory

The Niton XLt 700 Series (XLt) XRF Services x-ray fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at ...

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF TECHNOLOGIES FOR MEASURING TRACE ELEMENTS IN SOIL AND SEDIMENT RIGAKU ZSX MINI 11 XRF ANALYZER

EPA Science Inventory

The Rigaku ZSX Mini II (ZSX Mini II) XRF Services x-ray fluorescence (XRF) analyzer was demon-strated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2...

Application of GEM-based detectors in full-field XRF imaging

NASA Astrophysics Data System (ADS)

Dąbrowski, W.; Fiutowski, T.; Frączek, P.; Koperny, S.; Lankosz, M.; Mendys, A.; Mindur, B.; Świentek, K.; Wiącek, P.; Wróbel, P. M.

2016-12-01

X-ray fluorescence spectroscopy (XRF) is a commonly used technique for non-destructive elemental analysis of cultural heritage objects. It can be applied to investigations of provenance of historical objects as well as to studies of art techniques. While the XRF analysis can be easily performed locally using standard available equipment there is a growing interest in imaging of spatial distribution of specific elements. Spatial imaging of elemental distrbutions is usually realised by scanning an object with a narrow focused X-ray excitation beam and measuring characteristic fluorescence radiation using a high energy resolution detector, usually a silicon drift detector. Such a technique, called macro-XRF imaging, is suitable for investigation of flat surfaces but it is time consuming because the spatial resolution is basically determined by the spot size of the beam. Another approach is the full-field XRF, which is based on simultaneous irradiation and imaging of large area of an object. The image of the investigated area is projected by a pinhole camera on a position-sensitive and energy dispersive detector. The infinite depth of field of the pinhole camera allows one, in principle, investigation of non-flat surfaces. One of possible detectors to be employed in full-field XRF imaging is a GEM based detector with 2-dimensional readout. In the paper we report on development of an imaging system equipped with a standard 3-stage GEM detector of 10 × 10 cm2 equipped with readout electronics based on dedicated full-custom ASICs and DAQ system. With a demonstrator system we have obtained 2-D spatial resolution of the order of 100 μm and energy resolution at a level of 20% FWHM for 5.9 keV . Limitations of such a detector due to copper fluorescence radiation excited in the copper-clad drift electrode and GEM foils is discussed and performance of the detector using chromium-clad electrodes is reported.

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF TECHNOLOGIES FOR MEASURING TRACE ELEMENTS IN SOIL AND SEDIMENT OXFORD X-MTE 3000TX XRF ANALYZER

EPA Science Inventory

The Elvatech, Ltd. ElvaX (ElvaX) x-ray fluorescence (XRF) analyzer distributed in the United States by Xcalibur XRF Services (Xcalibur), was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field por...

SU-G-IeP3-07: High-Resolution, High-Sensitivity Imaging and Quantification of Intratumoral Distributions of Gold Nanoparticles Using a Benchtop L-Shell XRF Imaging System

DOE Office of Scientific and Technical Information (OSTI.GOV)

Manohar, N; Diagaradjane, P; Krishnan, S

2016-06-15

Purpose: To demonstrate the ability to perform high-resolution imaging and quantification of sparse distributions of gold nanoparticles (GNPs) within ex vivo tumor samples using a highly-sensitive benchtop L-shell x-ray fluorescence (XRF) imaging system. Methods: An optimized L-shell XRF imaging system was assembled using a tungsten-target x-ray source (operated at 62 kVp and 45 mA). The x-rays were filtered (copper: 0.08 mm & aluminum: 0.04 mm) and collimated (lead: 5 cm thickness, 3 cm aperture diameter) into a cone-beam in order to irradiate small samples or objects. A collimated (stainless steel: 4 cm thickness, 2 mm aperture diameter) silicon drift detector,more » capable of 2D translation, was placed at 90° with respect to the beam to acquire XRF/scatter spectra from regions of interest. Spectral processing involved extracting XRF signal from background, followed by attenuation correction using a Compton scatter-based normalization algorithm. Calibration phantoms with water/GNPs (0 and 0.00001–10 mg/cm{sup 3}) were used to determine the detection limit of the system at a 10-second acquisition time. The system was then used to map the distribution of GNPs within a 12×11×2 mm{sup 3} slice excised from the center of a GNP-loaded ex vivo murine tumor sample; a total of 110 voxels (2.65×10{sup −3} cm{sup 3}) were imaged with 1.3-mm spatial resolution. Results: The detection limit of the current cone-beam benchtop L-shell XRF system was 0.003 mg/cm{sup 3} (3 ppm). Intratumoral GNP concentrations ranging from 0.003 mg/cm{sup 3} (3 ppm) to a maximum of 0.055 mg/cm{sup 3} (55 ppm) and average of 0.0093 mg/cm{sup 3} (9.3 ppm) were imaged successfully within the ex vivo tumor slice. Conclusion: The developed cone-beam benchtop L-shell XRF imaging system can immediately be used for imaging of ex vivo tumor samples containing low concentrations of GNPs. With minor finetuning/optimization, the system can be directly adapted for performing routine preclinical in

Detection Limit of Smectite by Chemin IV Laboratory Instrument: Preliminary Implications for Chemin on the Mars Science Laboratory Mission

NASA Technical Reports Server (NTRS)

Archilles, Cherie; Ming, D. W.; Morris, R. V.; Blake, D. F.

2011-01-01

The CheMin instrument on the Mars Science Laboratory (MSL) is an miniature X-ray diffraction (XRD) and X-ray fluorescence (XRF) instrument capable of detecting the mineralogical and elemental compositions of rocks, outcrops and soils on the surface of Mars. CheMin uses a microfocus-source Co X-ray tube, a transmission sample cell, and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D XRD patterns and energy-dispersive X-ray histograms from powdered samples. CRISM and OMEGA have identified the presence of phyllosilicates at several locations on Mars including the four candidate MSL landing sites. The objective of this study was to conduct preliminary studies to determine the CheMin detection limit of smectite in a smectite/olivine mixed mineral system.

PyXRF: Python-based X-ray fluorescence analysis package

NASA Astrophysics Data System (ADS)

Li, Li; Yan, Hanfei; Xu, Wei; Yu, Dantong; Heroux, Annie; Lee, Wah-Keat; Campbell, Stuart I.; Chu, Yong S.

2017-09-01

We developed a python-based fluorescence analysis package (PyXRF) at the National Synchrotron Light Source II (NSLS-II) for the X-ray fluorescence-microscopy beamlines, including Hard X-ray Nanoprobe (HXN), and Submicron Resolution X-ray Spectroscopy (SRX). This package contains a high-level fitting engine, a comprehensive commandline/ GUI design, rigorous physics calculations, and a visualization interface. PyXRF offers a method of automatically finding elements, so that users do not need to spend extra time selecting elements manually. Moreover, PyXRF provides a convenient and interactive way of adjusting fitting parameters with physical constraints. This will help us perform quantitative analysis, and find an appropriate initial guess for fitting. Furthermore, we also create an advanced mode for expert users to construct their own fitting strategies with a full control of each fitting parameter. PyXRF runs single-pixel fitting at a fast speed, which opens up the possibilities of viewing the results of fitting in real time during experiments. A convenient I/O interface was designed to obtain data directly from NSLS-II's experimental database. PyXRF is under open-source development and designed to be an integral part of NSLS-II's scientific computation library.

Online sorting of recovered wood waste by automated XRF-technology: part II. Sorting efficiencies.

PubMed

Hasan, A Rasem; Solo-Gabriele, Helena; Townsend, Timothy

2011-04-01

Sorting of waste wood is an important process practiced at recycling facilities in order to detect and divert contaminants from recycled wood products. Contaminants of concern include arsenic, chromium and copper found in chemically preserved wood. The objective of this research was to evaluate the sorting efficiencies of both treated and untreated parts of the wood waste stream, and metal (As, Cr and Cu) mass recoveries by the use of automated X-ray fluorescence (XRF) systems. A full-scale system was used for experimentation. This unit consisted of an XRF-detection chamber mounted on the top of a conveyor and a pneumatic slide-way diverter which sorted wood into presumed treated and presumed untreated piles. A randomized block design was used to evaluate the operational conveyance parameters of the system, including wood feed rate and conveyor belt speed. Results indicated that online sorting efficiencies of waste wood by XRF technology were high based on number and weight of pieces (70-87% and 75-92% for treated wood and 66-97% and 68-96% for untreated wood, respectively). These sorting efficiencies achieved mass recovery for metals of 81-99% for As, 75-95% for Cu and 82-99% of Cr. The incorrect sorting of wood was attributed almost equally to deficiencies in the detection and conveyance/diversion systems. Even with its deficiencies, the system was capable of producing a recyclable portion that met residential soil quality levels established for Florida, for an infeed that contained 5% of treated wood. Copyright © 2010 Elsevier Ltd. All rights reserved.

Assessment of chemical analyses by means of portable XRF in the Roman mortars of Complutum archaeological site (Spain)

NASA Astrophysics Data System (ADS)

Ergenç, Duygu; Freire, David; Fort, Rafael

2016-04-01

The chemical characterization of lime mortars used in Roman period has a great significance and plays a key role in the acquisition of knowledge with respect to construction technology, raw materials and, accordingly, in its conservation works. When it comes to cultural heritage studies, sampling is always complicated since the minimum damage is the primary concern. The use of non-destructive techniques and direct measurements with portable devices reduce the amount of samples and time consumed in analyses, consequently it could be stated that such techniques are extremely useful in conservation and restoration works. In this study, the portable XRF device was used to determine the composition of chemical elements which compose the Roman lime mortars in the archaeological site of Complutum, Alcalá de Henares (Madrid, Spain) which is listed as a World Heritage Site by UNESCO since 1998. Portable XRF devices have some detection limits below the ones of the laboratory equipment that are immovable and require sampling. In order to correlate the results, sampling and grinding were initially done to prepare the powders for the laboratory XRF analysis with the following elements: Si, Al, Fe, Ca, Mg, K, Ti, Nb, Zr, Sr, Rb, Pb, Zn and Cr. The analyses of the powdered samples were conducted with the laboratory equipment PHILIPS Magix Pro (PW-2440) from the Centre of Scientific Instrumentation CIC in the University of Granada, and the results were compared to the results gathered with X Ray Florescence (EDTRX) THERMO NITON model XL3T from the Petrophysics Laboratory Geosciences Institute IGEO (CSIC-UCM). Analyses were performed on the surfaces of the samples -without any previous preparation-, and on the powdered samples to compare the variations between both traditional XRF analyses and the portable XRF. A good correlation was found among the results obtained by the laboratory equipment, the portable device as well as the surface measurements. The results of this study

Portable XRF analysis of occupational air filter samples from different workplaces using different samplers: final results, summary and conclusions.

PubMed

Harper, Martin; Pacolay, Bruce; Hintz, Patrick; Bartley, David L; Slaven, James E; Andrew, Michael E

2007-11-01

elsewhere. The results, based on data from the three workplaces where lead was the major element present in the samples, are summarized here. A limit of detection and a limit of quantitation are provided. Analysis of some samples using a second analyzer with a different X-ray source technology indicated reasonable agreement for some metals (but this was not evaluated for lead). Provided it is only necessary to analyze the filters, most personal samplers will provide acceptable results when used with portable XRF analysis for lead around applicable limit values.

Rapid limit tests for metal impurities in pharmaceutical materials by X-ray fluorescence spectroscopy using wavelet transform filtering.

PubMed

Arzhantsev, Sergey; Li, Xiang; Kauffman, John F

2011-02-01

We introduce a new method for analysis of X-ray fluorescence (XRF) spectra based on continuous wavelet transform filters, and the method is applied to the determination of toxic metals in pharmaceutical materials using hand-held XRF spectrometers. The method uses the continuous wavelet transform to filter the signal and noise components of the spectrum. We present a limit test that compares the wavelet domain signal-to-noise ratios at the energies of the elements of interest to an empirically determined signal-to-noise decision threshold. The limit test is advantageous because it does not require the user to measure calibration samples prior to measurement, though system suitability tests are still recommended. The limit test was evaluated in a collaborative study that involved five different hand-held XRF spectrometers used by multiple analysts in six separate laboratories across the United States. In total, more than 1200 measurements were performed. The detection limits estimated for arsenic, lead, mercury, and chromium were 8, 14, 20, and 150 μg/g, respectively.

XRF measurements of tin, copper and zinc in antifouling paints coated on leisure boats.

PubMed

Ytreberg, Erik; Bighiu, Maria Alexandra; Lundgren, Lennart; Eklund, Britta

2016-06-01

Tributyltin (TBT) and other organotin compounds have been restricted for use on leisure boats since 1989 in the EU. Nonetheless, release of TBT is observed from leisure boats during hull maintenance work, such as pressure hosing. In this work, we used a handheld X-ray Fluorescence analyser (XRF) calibrated for antifouling paint matrixes to measure tin, copper and zinc in antifouling paints coated on leisure boats in Sweden. Our results show that over 10% of the leisure boats (n = 686) contain >400 μg/cm(2) of tin in their antifouling coatings. For comparison, one layer (40 μm dry film) of a TBT-paint equals ≈ 800 μg Sn/cm(2). To our knowledge, tin has never been used in other forms than organotin (OT) in antifouling paints. Thus, even though the XRF analysis does not provide any information on the speciation of tin, the high concentrations indicate that these leisure boats still have OT coatings present on their hull. On several leisure boats we performed additional XRF measurements by progressively scraping off the top coatings and analysing each underlying layer. The XRF data show that when tin is detected, it is most likely present in coatings close to the hull with several layers of other coatings on top. Thus, leaching of OT compounds from the hull into the water is presumed to be negligible. The risk for environmental impacts arises during maintenance work such as scraping, blasting and high pressure hosing activities. The data also show that many boat owners apply excessive paint layers when following paint manufacturers recommendations. Moreover, high loads of copper were detected even on boats sailing in freshwater, despite the more than 20 year old ban, which poses an environmental risk that has not been addressed until now. Copyright © 2016 The Authors. Published by Elsevier Ltd.. All rights reserved.

Material limitations on the detection limit in refractometry.

PubMed

Skafte-Pedersen, Peder; Nunes, Pedro S; Xiao, Sanshui; Mortensen, Niels Asger

2009-01-01

We discuss the detection limit for refractometric sensors relying on high-Q optical cavities and show that the ultimate classical detection limit is given by min {Δn} ≳ η, with n + iη being the complex refractive index of the material under refractometric investigation. Taking finite Q factors and filling fractions into account, the detection limit declines. As an example we discuss the fundamental limits of silicon-based high-Q resonators, such as photonic crystal resonators, for sensing in a bio-liquid environment, such as a water buffer. In the transparency window (λ ≳ 1100 nm) of silicon the detection limit becomes almost independent on the filling fraction, while in the visible, the detection limit depends strongly on the filling fraction because the silicon absorbs strongly.

Proposal for a prototype of portable μXRF spectrometer

NASA Astrophysics Data System (ADS)

Polese, C.; Dabagov, S. B.; Esposito, A.; Liedl, A.; Hampai, D.; Bartùli, C.; Ferretti, M.

2015-07-01

μXRF is a powerful instrument for non-destructive characterization of materials of cultural interest. At the XLab Frascati Laboratory this technique is already well performed thanks to the polyCO set equipment allowing simultaneous μXRF 2D mapping. However, due to the strict demand for in situ analysis in this particular field, a new portable μXRF spectrometer equipped with a full polycapillary lens conjugated with a transmission anode X-ray tube is proposed. Many cultural objects are characterized by elements (Ag, Sn, etc.) with high energy fluorescence K-lines. Thus, the capability of a full lens to deliver a high energy fraction of X-ray spectrum, in order to excite the fluorescence K-lines of such elements, is tested.

Material Limitations on the Detection Limit in Refractometry

PubMed Central

Skafte-Pedersen, Peder; Nunes, Pedro S.; Xiao, Sanshui; Mortensen, Niels Asger

2009-01-01

We discuss the detection limit for refractometric sensors relying on high-Q optical cavities and show that the ultimate classical detection limit is given by min {Δn} ≳ η, with n + iη being the complex refractive index of the material under refractometric investigation. Taking finite Q factors and filling fractions into account, the detection limit declines. As an example we discuss the fundamental limits of silicon-based high-Q resonators, such as photonic crystal resonators, for sensing in a bio-liquid environment, such as a water buffer. In the transparency window (λ ≳ 1100 nm) of silicon the detection limit becomes almost independent on the filling fraction, while in the visible, the detection limit depends strongly on the filling fraction because the silicon absorbs strongly. PMID:22291513

Electrochemical X-ray fluorescence spectroscopy for trace heavy metal analysis: enhancing X-ray fluorescence detection capabilities by four orders of magnitude.

PubMed

Hutton, Laura A; O'Neil, Glen D; Read, Tania L; Ayres, Zoë J; Newton, Mark E; Macpherson, Julie V

2014-05-06

The development of a novel analytical technique, electrochemical X-ray fluorescence (EC-XRF), is described and applied to the quantitative detection of heavy metals in solution, achieving sub-ppb limits of detection (LOD). In EC-XRF, electrochemical preconcentration of a species of interest onto the target electrode is achieved here by cathodic electrodeposition. Unambiguous elemental identification and quantification of metal concentration is then made using XRF. This simple electrochemical preconcentration step improves the LOD of energy dispersive XRF by over 4 orders of magnitude (for similar sample preparation time scales). Large area free-standing boron doped diamond grown using microwave plasma chemical vapor deposition techniques is found to be ideal as the electrode material for both electrodeposition and XRF due to its wide solvent window, transparency to the XRF beam, and ability to be produced in mechanically robust freestanding thin film form. During electrodeposition it is possible to vary both the deposition potential (Edep) and deposition time (tdep). For the metals Cu(2+) and Pb(2+) the highest detection sensitivities were found for Edep = -1.75 V and tdep (=) 4000 s with LODs of 0.05 and 0.04 ppb achieved, respectively. In mixed Cu(2+)/Pb(2+) solutions, EC-XRF shows that Cu(2+) deposition is unimpeded by Pb(2+), across a broad concentration range, but this is only true for Pb(2+) when both metals are present at low concentrations (10 nM), boding well for trace level measurements. In a dual mixed metal solution, EC-XRF can also be employed to either selectively deposit the metal which has the most positive formal reduction potential, E(0), or exhaustively deplete it from solution, enabling uninhibited detection of the metal with the more negative E(0).

EUTERPE, a small electron storage ring for XRF

NASA Astrophysics Data System (ADS)

Botman, J. I. M.; Mutsaers, P. H. A.; Hagedoorn, H. L.; De Voigt, M. J. A.

1990-04-01

A small-sized electron storage ring is under construction at the Eindhoven University of Technology which will cover the energy range of 15 to 400 MeV. At top energy the characteristic wavelength of the synchrotron radiation spectrum is 8.3 nm for the regular dipole magnets and 1.2 nm corresponding to 1.06 keV for a 10 T wiggler magnet. This will provide useful radiation for X-ray fluorescence (XRF) up to 3.2 keV. Alternatively, photon conversion with a high power CO 2 laser beam of 0.124 eV photons will generate X-rays for XRF with energies ranging from 0.5 to 300 keV, depending on the operating energy of the storage ring. This facility will provide an important extension to the activities of the Eindhoven group on PIXE, RBS and microbeam analysis. A short description of the macnine will be given together with applications and specific examples of the XRF method.

NHEXAS PHASE I ARIZONA STUDY--METALS-XRF IN DUST ANALYTICAL RESULTS

EPA Science Inventory

The Metals-XRF in Dust data set contains X-ray fluorescence (XRF) analytical results for measurements of up to 27 metals in 384 dust samples over 384 households. Samples were taken by collecting dust from the indoor floor areas in the main room and in the bedroom of the primary ...

Application of principal component analysis for improvement of X-ray fluorescence images obtained by polycapillary-based micro-XRF technique

NASA Astrophysics Data System (ADS)

Aida, S.; Matsuno, T.; Hasegawa, T.; Tsuji, K.

2017-07-01

Micro X-ray fluorescence (micro-XRF) analysis is repeated as a means of producing elemental maps. In some cases, however, the XRF images of trace elements that are obtained are not clear due to high background intensity. To solve this problem, we applied principal component analysis (PCA) to XRF spectra. We focused on improving the quality of XRF images by applying PCA. XRF images of the dried residue of standard solution on the glass substrate were taken. The XRF intensities for the dried residue were analyzed before and after PCA. Standard deviations of XRF intensities in the PCA-filtered images were improved, leading to clear contrast of the images. This improvement of the XRF images was effective in cases where the XRF intensity was weak.

PIXE and XRF Analysis of Roman Denarii

NASA Astrophysics Data System (ADS)

Fasano, Cecilia; Raddell, Mark; Manukyan, Khachatur; Stech, Edward; Wiescher, Michael

2017-09-01

A set of Roman Denarii from the republican to the imperial period (140BC-240AD) has been studied using X-ray fluorescent (XRF) scanning and proton induced x-ray emission (PIXE) techniques. XRF and PIXE are commonly used in the study of cultural heritage objects because they are nondestructive. The combination of these two methods is also unique because of the ability to penetrate the sample with a broader spectrum of depths and energies than either could achieve on its own. The coins are from a large span of Roman history and their analysis serves to follow the economic and political change of the era using the relative silver and copper contents in each sample. In addition to analyzing the samples, the study sought to compare these two common analysis techniques and to explore the use of a standard to examine any shortcomings in either of the methods. Data sets were compared and then adjusted to a calibration curve which was created from the analysis of a number of standard solutions. The concentrations of the standard solutions were confirmed using inductively coupled plasma spectroscopy. Through this we were able to assemble results which will progress the basis of understanding of PIXE and XRF techniques as well as increase the wealth of knowledge of Ancient Roman currency.

Effects of Kapton Sample Cell Windows on the Detection Limit of Smectite: Implications for CheMin on the Mars Science Laboratory Mission

NASA Technical Reports Server (NTRS)

Achilles, C. N.; Ming, Douglas W.; Morris, R. V.; Blake, D. F.

2012-01-01

The CheMin instrument on the Mars Science Laboratory (MSL) rover Curiosity is an X-ray diffraction (XRD) and X-ray fluorescence (XRF) instrument capable of providing the mineralogical and chemical compositions of rocks and soils on the surface of Mars. CheMin uses a microfocus X-ray tube with a Co target, transmission geometry, and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D XRD patterns and energy-dispersive X-ray histograms from powdered samples. CheMin has two different window materials used for sample cells -- Mylar and Kapton. Instrument details are provided elsewhere. Fe/Mg-smectite (e.g., nontronite) has been identified in Gale Crater, the MSL future landing site, by CRISM spectra. While large quantities of phyllosilicate minerals will be easily detected by CheMin, it is important to establish detection limits of such phases to understand capabilities and limitations of the instrument. A previous study indicated that the (001) peak of smectite at 15 Ang was detectable in a mixture of 1 wt.% smectite with olivine when Mylar is the window material for the sample cell. Complications arise when Kapton is the window material because Kapton itself also has a diffraction peak near 15 Ang (6.8 deg 2 Theta). This study presents results of mineral mixtures of smectite and olivine to determine smectite detection limits for Kapton sample cells. Because the intensity and position of the smectite (001) peak depends on the hydration state, we also analyzed mixtures with "hydrated" and "dehydrated"h smectite to examine the effects of hydration state on detection limits.

Nondestructive Analysis of Astromaterials by Micro-CT and Micro-XRF Analysis for PET Examination

NASA Technical Reports Server (NTRS)

Zeigler, R. A.; Righter, K.; Allen, C. C.

2013-01-01

An integral part of any sample return mission is the initial description and classification of returned samples by the preliminary examination team (PET). The goal of the PET is to characterize and classify returned samples and make this information available to the larger research community who then conduct more in-depth studies on the samples. The PET tries to minimize the impact their work has on the sample suite, which has in the past limited the PET work to largely visual, nonquantitative measurements (e.g., optical microscopy). More modern techniques can also be utilized by a PET to nondestructively characterize astromaterials in much more rigorous way. Here we discuss our recent investigations into the applications of micro-CT and micro-XRF analyses with Apollo samples and ANSMET meteorites and assess the usefulness of these techniques in future PET. Results: The application of micro computerized tomography (micro-CT) to astromaterials is not a new concept. The technique involves scanning samples with high-energy x-rays and constructing 3-dimensional images of the density of materials within the sample. The technique can routinely measure large samples (up to approx. 2700 cu cm) with a small individual voxel size (approx. 30 cu m), and has the sensitivity to distinguish the major rock forming minerals and identify clast populations within brecciated samples. We have recently run a test sample of a terrestrial breccia with a carbonate matrix and multiple igneous clast lithologies. The test results are promising and we will soon analyze a approx. 600 g piece of Apollo sample 14321 to map out the clast population within the sample. Benchtop micro x-ray fluorescence (micro-XRF) instruments can rapidly scan large areas (approx. 100 sq cm) with a small pixel size (approx. 25 microns) and measure the (semi) quantitative composition of largely unprepared surfaces for all elements between Be and U, often with sensitivity on the order of a approx. 100 ppm. Our recent

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF TECHNOLOGIES FOR MEASURING TRACE ELEMENTS IN SOIL AND SEDIMENT RONTEC PICOTAX XRF ANALYZER

EPA Science Inventory

The Rontec PicoTAX x-ray fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kennedy Athletic, Rec...

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF TECHNOLOGIES FOR MEASURING TRACE ELEMENTS IN SOIL AND SEDIMENT XCALIBUR ELVAX XRF ANALYZER

EPA Science Inventory

The Innov-X XT400 Series (XT400) x-ray fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kenned...

Analysis of heterogeneous gallstones using laser-induced breakdown spectroscopy (LIBS) and wavelength dispersive X-ray fluorescence (WD-XRF).

PubMed

Jaswal, Brij Bir S; Kumar, Vinay; Sharma, Jitendra; Rai, Pradeep K; Gondal, Mohammed A; Gondal, Bilal; Singh, Vivek K

2016-04-01

Laser-induced breakdown spectroscopy (LIBS) is an emerging analytical technique with numerous advantages such as rapidity, multi-elemental analysis, no specific sample preparation requirements, non-destructiveness, and versatility. It has been proven to be a robust elemental analysis tool attracting interest because of being applied to a wide range of materials including biomaterials. In this paper, we have performed spectroscopic studies on gallstones which are heterogeneous in nature using LIBS and wavelength dispersive X-ray fluorescence (WD-XRF) techniques. It has been observed that the presence and relative concentrations of trace elements in different kind of gallstones (cholesterol and pigment gallstones) can easily be determined using LIBS technique. From the experiments carried out on gallstones for trace elemental mapping and detection, it was found that LIBS is a robust tool for such biomedical applications. The stone samples studied in the present paper were classified using the Fourier transform infrared (FTIR) spectroscopy. WD-XRF spectroscopy has been applied for the qualitative and quantitative analysis of major and trace elements present in the gallstone which was compared with the LIBS data. The results obtained in the present paper show interesting prospects for LIBS and WD-XRF to study cholelithiasis better.

In-Situ XRF Measurements in Lunar Surface Exploration Using Apollo Samples as a Standard

NASA Technical Reports Server (NTRS)

Young, Kelsey E.; Evans, C.; Allen, C.; Mosie, A.; Hodges, K. V.

2011-01-01

Samples collected during the Apollo lunar surface missions were sampled and returned to Earth by astronauts with varying degrees of geological experience. The technology used in these EVAs, or extravehicular activities, included nothing more advanced than traditional terrestrial field instruments: rock hammer, scoop, claw tool, and sample bags. 40 years after Apollo, technology is being developed that will allow for a high-resolution geochemical map to be created in the field real-time. Handheld x-ray fluorescence (XRF) technology is one such technology. We use handheld XRF to enable a broad in-situ characterization of a geologic site of interest based on fairly rapid techniques that can be implemented by either an astronaut or a robotic explorer. The handheld XRF instrument we used for this study was the Innov-X Systems Delta XRF spectrometer.

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF TECHNOLOGIES FOR MEASURING TRACE ELEMENTS IN SOIL AND SEDIMENT OXFORD ED2000 XRF ANALYZER

EPA Science Inventory

The Oxford ED2000 x-ray fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kennedy Athletic, Recr...

Characterization of fossil remains using XRF, XPS and XAFS spectroscopies

NASA Astrophysics Data System (ADS)

Zougrou, I. M.; Katsikini, M.; Pinakidou, F.; Brzhezinskaya, M.; Papadopoulou, L.; Vlachos, E.; Tsoukala, E.; Paloura, E. C.

2016-05-01

Synchrotron radiation micro-X-Ray Fluorescence (μ-XRF), X-ray photoelectron (XPS) and X-ray Absorption Fine Structure (XAFS) spectroscopies are applied for the study of paleontological findings. More specifically the costal plate of a gigantic terrestrial turtle Titanochelon bacharidisi and a fossilized coprolite of the cave spotted hyena Crocuta crocuta spelaea are studied. Ca L 2,3-edge NEXAFS and Ca 2p XPS are applied for the identification and quantification of apatite and Ca containing minerals. XRF mapping and XAFS are employed for the study of the spatial distribution and speciation of the minerals related to the deposition environment.

XRF-analysis of fine and ultrafine particles emitted from laser printing devices.

PubMed

Barthel, Mathias; Pedan, Vasilisa; Hahn, Oliver; Rothhardt, Monika; Bresch, Harald; Jann, Oliver; Seeger, Stefan

2011-09-15

In this work, the elemental composition of fine and ultrafine particles emitted by ten different laser printing devices (LPD) is examined. The particle number concentration time series was measured as well as the particle size distributions. In parallel, emitted particles were size-selectively sampled with a cascade impactor and subsequently analyzed by the means of XRF. In order to identify potential sources for the aerosol's elemental composition, materials involved in the printing process such as toner, paper, and structural components of the printer were also analyzed. While the majority of particle emissions from laser printers are known to consist of recondensated semi volatile organic compounds, elemental analysis identifies Si, S, Cl, Ca, Ti, Cr, and Fe as well as traces of Ni and Zn in different size fractions of the aerosols. These elements can mainly be assigned to contributions from toner and paper. The detection of elements that are likely to be present in inorganic compounds is in good agreement with the measurement of nonvolatile particles. Quantitative measurements of solid particles at 400 °C resulted in residues of 1.6 × 10(9) and 1.5 × 10(10) particles per print job, representing fractions of 0.2% and 1.9% of the total number of emitted particles at room temperature. In combination with the XRF results it is concluded that solid inorganic particles contribute to LPD emissions in measurable quantities. Furthermore, for the first time Br was detected in significant concentrations in the aerosol emitted from two LPD. The analysis of several possible sources identified the plastic housings of the fuser units as main sources due to substantial Br concentrations related to brominated flame retardants.

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--METALS/XRF IN DUST ANALYTICAL RESULTS

EPA Science Inventory

The Metals-XRF in Dust data set contains X-ray fluorescence (XRF) analytical results for measurements of up to 27 metals in 91 dust samples over 91 households. Samples were taken by collecting dust from the indoor floor areas in the main room and in the bedroom of the primary re...

Applications of XRF, NAA and low-kV radiographic techniques in the study of body composition and diseased tissue

NASA Astrophysics Data System (ADS)

Bradley, D. A.; Ng, K. H.; Green, S.; Mountford, P. J.; Shukri, A.; Evans, J.

1996-05-01

Members of this group have responded to a number of challenging health issues by attempting to devise sensitive XRF, NAA and low-kV radiographic measurement systems foboth in vivo and in vitro applications. These studies are generally either of toxicological importance, examine potential for diagnosing the presence of disease, or offer effective means for monitoring potentially harmful side-effects of therapy. Particular examples include the in vivo XRF investigation of human skeletal uptake of Pb in working and living environments, in vivo XRF monitoring of elevated levels of Fe in skin (indicating the presence of an undesirable side-effect of the treatment of thalassaemia), in vivo NAA monitoring of elevated levels of Al in bone (indicating an undesirable side-effect of the treatment of chronic renal failure) and in vitro characterization, by means of low-kV imaging, of a range of calcification parameters in healthy and diseased breast tissue. The latter investigation has been conducted in association with an in vitro NAA study of concentrations of trace elements in the same types of tissue. Figures of merit for the various measurement systems have been obtained in terms of minimum detectable levels and concentrations (MDL's and MDC's) and where applicable, image related parameters.

Investigation of gunshot residue patterns using milli-XRF-techniques: first experiences in casework

NASA Astrophysics Data System (ADS)

Schumacher, Rüdiger; Barth, Martin; Neimke, Dieter; Niewöhner, Ludwig

2010-06-01

The investigation of gunshot residue (GSR) patterns for shooting range estimation is usually based on visualizing the lead, copper, or nitrocellulose distributions on targets like fabric or adhesive tape by chemographic color tests. The method usually provides good results but has its drawbacks when it comes to the examination of ammunition containing lead-free primers or bloody clothing. A milli-X-ray fluorescence (m-XRF) spectrometer with a large motorized stage can help to circumvent these problems allowing the acquisition of XRF mappings of relatively large areas (up to 20 x 20 cm) in millimeter resolution within reasonable time (2-10 hours) for almost all elements. First experiences in GSR casework at the Forensic Science Institute of the Bundeskriminalamt (BKA) have shown, that m-XRF is a useful supplementation for conventional methods in shooting ranges estimation, which helps if there are problems in transferring a GSR pattern to secondary targets (e.g. bloody or stained garments) or if there is no suitable color test available for the element of interest. The resulting elemental distributions are a good estimate for the shooting range and can be evaluated by calculating radial distributions or integrated count rates of irregular shaped regions like pieces of human skin which are too small to be investigated with a conventional WD-XRF spectrometer. Beside a mapping mode the milli-XRF offers also point and line scan modes which can also be utilized in gunshot crime investigations as a quick survey tool to identify bullet holes based on the elements present in the wipe ring.

Textural and Mineralogical Analysis of Volcanic Rocks by µ-XRF Mapping.

PubMed

Germinario, Luigi; Cossio, Roberto; Maritan, Lara; Borghi, Alessandro; Mazzoli, Claudio

2016-06-01

In this study, µ-XRF was applied as a novel surface technique for quick acquisition of elemental X-ray maps of rocks, image analysis of which provides quantitative information on texture and rock-forming minerals. Bench-top µ-XRF is cost-effective, fast, and non-destructive, can be applied to both large (up to a few tens of cm) and fragile samples, and yields major and trace element analysis with good sensitivity. Here, X-ray mapping was performed with a resolution of 103.5 µm and spot size of 30 µm over sample areas of about 5×4 cm of Euganean trachyte, a volcanic porphyritic rock from the Euganean Hills (NE Italy) traditionally used in cultural heritage. The relative abundance of phenocrysts and groundmass, as well as the size and shape of the various mineral phases, were obtained from image analysis of the elemental maps. The quantified petrographic features allowed identification of various extraction sites, revealing an objective method for archaeometric provenance studies exploiting µ-XRF imaging.

A novel approach to water polution monitoring by combining ion exchange resin and XRF-scanning technique

NASA Astrophysics Data System (ADS)

Huang, J. J.; Lin, S. C.; Löwemark, L.; Liou, Y. H.; Chang, Q. M.; Chang, T. K.; Wei, K. Y.; Croudace, I. W. C.

2017-12-01

Due to the rapid industrial expansion, environments are subject to irregular fluctuations and spatial distributions in pollutant concentrations. This study proposes to use ion exchange resin accompanied with the XRF-scanning technique to monitor environmental pollution. As a passive sampling sorbent, the use of ion exchange resin provides a rapid, low cost and simple method to detect episodic pollution signals with a high spatial sampling density. In order to digest large quantities of samples, the fast and non-destructive Itrax-XRF core scanner has been introduced to assess elemental concentrations in the resin samples. Although the XRF scanning results are often considered as a semi-quantitative measurement due to possible absorption or scattering caused by the physical variabilities of scanned materials, the use of resin can minimize such influences owing to the standarization of the sample matrix. In this study, 17 lab-prepared standard resin samples were scanned with the Itrax-XRF core scanner (at 100 s exposure time with the Mo-tube) and compared with the absolute elemental concentrations. Six elements generally used in pollution studies (Cr, Mn, Ni, Cu, Zn, and Pb) were selected, and their regression lines and correlation coefficients were determined. In addition, 5 standard resin samples were scanned at different exposure time settings (1 s, 5 s, 15 s, 30 s, 100 s) to address the influence of exposure time on the accuracy of the measurements. The results show that within the test range (from few ppm to thousands ppm), the correlation coefficients are higher than 0.97, even at the shortest exposure time (1 s). Furthermore, a pilot field survey with 30 resin samples has been conducted in a potentially polluted farm area in central Taiwan to demonstrate the feasibility of this novel approach. The polluted hot zones could be identified and the properties and sources of wastewater pollution can therefore be traced over large areas for the purposes of

Elemental analysis of granite by instrumental neutron activation analysis (INAA) and X-ray fluorescence analysis (XRF).

PubMed

El-Taher, A

2012-01-01

The instrumental neutron activation analysis technique (INAA) was used for qualitative and quantitative analysis of granite samples collected from four locations in the Aswan area in South Egypt. The samples were prepared together with their standards and simultaneously irradiated in a neutron flux of 7×10(11)n/cm(2)s in the TRIGA Mainz research reactor. Gamma-ray spectra from an hyper-pure germanium detector were analyzed. The present study provides the basic data of elemental concentrations of granite rocks. The following elements have been determined Na, Mg, K, Fe, Mn, Sc, Cr, Ti, Co, Zn, Ga, Rb, Zr, Nb, Sn, Ba, Cs, La, Ce, Nd, Sm, Eu, Yb, Lu, Hf, Ta, Th and U. The X-ray fluorescence (XRF) was used for comparison and to detect elements, which can be detected only by XRF such as F, S, Cl, Co, Cu, Mo, Ni, Pb, Se and V. The data presented here are our contribution to understanding the elemental composition of the granite rocks. Because there are no existing databases for the elemental analysis of granite, our results are a start to establishing a database for the Egyptian granite. It is hoped that the data presented here will be useful to those dealing with geochemistry, granite chemistry and related fields. Copyright © 2011 Elsevier Ltd. All rights reserved.

Monitoring of WEEE plastics in regards to brominated flame retardants using handheld XRF

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aldrian, Alexia, E-mail: alexia.aldrian@unileoben.ac.at; Ledersteger, Alfred, E-mail: a.ledersteger@saubermacher.at; Pomberger, Roland, E-mail: roland.pomberger@unileoben.ac.at

Highlights: • Specification of an empirical factor for conversion from bromine to PBB and PBDE. • The handheld XRF device was validated for this particular application. • A very large number of over 4600 pieces of monitor housings was analysed. • The recyclable fraction mounts up to 85% for TV but only 53% of PC waste plastics. • A high percentage of pieces with bromine contents of over 50,000 ppm was obtained. - Abstract: This contribution is focused on the on-site determination of the bromine content in waste electrical and electronic equipment (WEEE), in particular waste plastics from television setsmore » (TV) and personal computer monitors (PC) using a handheld X-ray fluorescence (XRF) device. The described approach allows the examination of samples in regards to the compliance with legal specifications for polybrominated biphenyls (PBBs) and polybrominated diphenyl ethers (PBDEs) directly after disassembling and facilitates the sorting out of plastics with high contents of brominated flame retardants (BFRs). In all, over 3000 pieces of black (TV) and 1600 pieces of grey (PC) plastic waste were analysed with handheld XRF technique for this study. Especially noticeable was the high percentage of pieces with a bromine content of over 50,000 ppm for TV (7%) and PC (39%) waste plastics. The applied method was validated by comparing the data of handheld XRF with results obtained by GC–MS. The results showed the expected and sufficiently accurate correlation between these two methods. It is shown that handheld XRF technique is an effective tool for fast monitoring of large volumes of WEEE plastics in regards to BFRs for on-site measurements.« less

[Study on trace elements of lake sediments by ICP-AES and XRF core scanning].

PubMed

Cheng, Ai-Ying; Yu, Jun-Qing; Gao, Chun-Liang; Zhang, Li-Sha; He, Xian-Hu

2013-07-01

It is the first time to study sediment of Toson lake in Qaidam Basin. Trace elements including Cd, Cr, Cu, Zn and Pb in lake sediment were measured by ICP-AES method, studied and optimized from different resolution methods respectively, and finally determined a optimum pretreatment system for sediment of Toson lake, namely, HCl-HNO3-HF-HClO4-H2O2 system in the proportions of 5 : 5 : 5 : 1 : 1 was determined. At the same time, the data measured by XRF core scanning were compared, the use of moisture content correction method was analyzed, and the influence of the moisture content on the scanning method was discussed. The results showed that, compared to the background value, the contents of Cd and Zn were a little higher, the content of Cr, Cu and Pb was within the background value limits. XRF core scanning was controlled by sediment elements as well as water content in sediment to some extent. The results by the two methods showed a significant positive correlation, with the correlation coefficient up to 0.673-0.925, and they have a great comparability.

Monitoring of WEEE plastics in regards to brominated flame retardants using handheld XRF.

PubMed

Aldrian, Alexia; Ledersteger, Alfred; Pomberger, Roland

2015-02-01

This contribution is focused on the on-site determination of the bromine content in waste electrical and electronic equipment (WEEE), in particular waste plastics from television sets (TV) and personal computer monitors (PC) using a handheld X-ray fluorescence (XRF) device. The described approach allows the examination of samples in regards to the compliance with legal specifications for polybrominated biphenyls (PBBs) and polybrominated diphenyl ethers (PBDEs) directly after disassembling and facilitates the sorting out of plastics with high contents of brominated flame retardants (BFRs). In all, over 3000 pieces of black (TV) and 1600 pieces of grey (PC) plastic waste were analysed with handheld XRF technique for this study. Especially noticeable was the high percentage of pieces with a bromine content of over 50,000ppm for TV (7%) and PC (39%) waste plastics. The applied method was validated by comparing the data of handheld XRF with results obtained by GC-MS. The results showed the expected and sufficiently accurate correlation between these two methods. It is shown that handheld XRF technique is an effective tool for fast monitoring of large volumes of WEEE plastics in regards to BFRs for on-site measurements. Copyright © 2014 Elsevier Ltd. All rights reserved.

Limits of detection and decision. Part 4

NASA Astrophysics Data System (ADS)

Voigtman, E.

2008-02-01

Probability density functions (PDFs) have been derived for a number of commonly used limit of detection definitions, including several variants of the Relative Standard Deviation of the Background-Background Equivalent Concentration (RSDB-BEC) method, for a simple linear chemical measurement system (CMS) having homoscedastic, Gaussian measurement noise and using ordinary least squares (OLS) processing. All of these detection limit definitions serve as both decision and detection limits, thereby implicitly resulting in 50% rates of Type 2 errors. It has been demonstrated that these are closely related to Currie decision limits, if the coverage factor, k, is properly defined, and that all of the PDFs are scaled reciprocals of noncentral t variates. All of the detection limits have well-defined upper and lower limits, thereby resulting in finite moments and confidence limits, and the problem of estimating the noncentrality parameter has been addressed. As in Parts 1-3, extensive Monte Carlo simulations were performed and all the simulation results were found to be in excellent agreement with the derived theoretical expressions. Specific recommendations for harmonization of detection limit methodology have also been made.

The holy grail of soil metal contamination site assessment: reducing risk and increasing confidence of decision making using infield portable X-ray Fluorescence (pXRF) technology

NASA Astrophysics Data System (ADS)

Rouillon, M.; Taylor, M. P.; Dong, C.

2016-12-01

This research assesses the advantages of integrating field portable X-ray Fluorescence (pXRF) technology for reducing the risk and increase confidence of decision making for metal-contaminated site assessments. Metal-contaminated sites are often highly heterogeneous and require a high sampling density to accurately characterize the distribution and concentration of contaminants. The current regulatory assessment approaches rely on a small number of samples processed using standard wet-chemistry methods. In New South Wales (NSW), Australia, the current notification trigger for characterizing metal-contaminated sites require the upper 95% confidence interval of the site mean to equal or exceed the relevant guidelines. The method's low `minimum' sampling requirements can misclassify sites due to the heterogeneous nature of soil contamination, leading to inaccurate decision making. To address this issue, we propose integrating infield pXRF analysis with the established sampling method to overcome sampling limitations. This approach increases the minimum sampling resolution and reduces the 95% CI of the site mean. Infield pXRF analysis at contamination hotspots enhances sample resolution efficiently and without the need to return to the site. In this study, the current and proposed pXRF site assessment methods are compared at five heterogeneous metal-contaminated sites by analysing the spatial distribution of contaminants, 95% confidence intervals of site means, and the sampling and analysis uncertainty associated with each method. Finally, an analysis of costs associated with both the current and proposed methods is presented to demonstrate the advantages of incorporating pXRF into metal-contaminated site assessments. The data shows that pXRF integrated site assessments allows for faster, cost-efficient, characterisation of metal-contaminated sites with greater confidence for decision making.

Remote In-Situ Quantitative Mineralogical Analysis Using XRD/XRF

NASA Technical Reports Server (NTRS)

Blake, D. F.; Bish, D.; Vaniman, D.; Chipera, S.; Sarrazin, P.; Collins, S. A.; Elliott, S. T.

2001-01-01

X-Ray Diffraction (XRD) is the most direct and accurate method for determining mineralogy. The CHEMIN XRD/XRF instrument has shown promising results on a variety of mineral and rock samples. Additional information is contained in the original extended abstract.

Fine-resolved XRF geochemistry of bottom fills from Asian lakes

NASA Astrophysics Data System (ADS)

Phedorin (Fedorin), Mikhail

2010-05-01

Over the last fifteen years (1994-2009) several teams from Siberian Branch of Russian Academy of Science have carried out numerous studies of cores of bottom sediments from Asian lakes, to perform regional reconstructions of past climate changes. Within these researches, the method of x-ray fluorescence (XRF) has widely been used to predict downcore distributions of elements; high-resolution XRF scanning of cores has been employed since 1999. Experiments have been performed at XRF facilities of Siberian Synchrotron Center. In this presentation I report (1) ‘know-how's of quantitative processing of experimental fine-scanning XRF data for lacustrine cores, and (2) geochemical signatures of sediments from Asian lakes obtained after XRF fine-scanning of cores. (1) Quantitative prediction of concentrations of elements from fine-scanning XRF data is problematic because of varying water content along scanning profile, as well as due to varying matrix chemistry and sample optical thickness. All these cause varying inter-element influence that changes fluorescence flux through its absorption and/or secondary excitation. To overcome these difficulties we have used an adapted algorithm of fundamental parameters. The mathematical model based on this algorithm accounts for two events of photon/matter interaction. Element concentrations are estimated using reference samples and the internal standard procedure, both with correction of interference effects. The pore water content is inferred from its correlation with the coherent/incoherent scatter intensity ratio. Sediment density is found from water content by a reliable sedimentological law. Normalization to Compton scattering accounts for the irradiated mass of wet sediment controlled by porosity and sampling-related core disturbance. The mathematical model also includes these scattering variations related to lithology, water content, and density of samples. The new method was applied to XRF scans of cores to predict

MapX: 2D XRF for Planetary Exploration - Image Formation and Optic Characterization

DOE PAGES

Sarrazin, P.; Blake, D.; Gailhanou, M.; ...

2018-04-01

Map-X is a planetary instrument concept for 2D X-Ray Fluorescence (XRF) spectroscopy. The instrument is placed directly on the surface of an object and held in a fixed position during the measurement. The formation of XRF images on the CCD detector relies on a multichannel optic configured for 1:1 imaging and can be analyzed through the point spread function (PSF) of the optic. The PSF can be directly measured using a micron-sized monochromatic X-ray source in place of the sample. Such PSF measurements were carried out at the Stanford Synchrotron and are compared with ray tracing simulations. It is shownmore » that artifacts are introduced by the periodicity of the PSF at the channel scale and the proximity of the CCD pixel size and the optic channel size. A strategy of sub-channel random moves was used to cancel out these artifacts and provide a clean experimental PSF directly usable for XRF image deconvolution.« less

MapX: 2D XRF for Planetary Exploration - Image Formation and Optic Characterization

NASA Astrophysics Data System (ADS)

Sarrazin, P.; Blake, D.; Gailhanou, M.; Marchis, F.; Chalumeau, C.; Webb, S.; Walter, P.; Schyns, E.; Thompson, K.; Bristow, T.

2018-04-01

Map-X is a planetary instrument concept for 2D X-Ray Fluorescence (XRF) spectroscopy. The instrument is placed directly on the surface of an object and held in a fixed position during the measurement. The formation of XRF images on the CCD detector relies on a multichannel optic configured for 1:1 imaging and can be analyzed through the point spread function (PSF) of the optic. The PSF can be directly measured using a micron-sized monochromatic X-ray source in place of the sample. Such PSF measurements were carried out at the Stanford Synchrotron and are compared with ray tracing simulations. It is shown that artifacts are introduced by the periodicity of the PSF at the channel scale and the proximity of the CCD pixel size and the optic channel size. A strategy of sub-channel random moves was used to cancel out these artifacts and provide a clean experimental PSF directly usable for XRF image deconvolution.

MapX: 2D XRF for Planetary Exploration - Image Formation and Optic Characterization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sarrazin, P.; Blake, D.; Gailhanou, M.

Map-X is a planetary instrument concept for 2D X-Ray Fluorescence (XRF) spectroscopy. The instrument is placed directly on the surface of an object and held in a fixed position during the measurement. The formation of XRF images on the CCD detector relies on a multichannel optic configured for 1:1 imaging and can be analyzed through the point spread function (PSF) of the optic. The PSF can be directly measured using a micron-sized monochromatic X-ray source in place of the sample. Such PSF measurements were carried out at the Stanford Synchrotron and are compared with ray tracing simulations. It is shownmore » that artifacts are introduced by the periodicity of the PSF at the channel scale and the proximity of the CCD pixel size and the optic channel size. A strategy of sub-channel random moves was used to cancel out these artifacts and provide a clean experimental PSF directly usable for XRF image deconvolution.« less

Portable X-ray fluorescence for the detection of POP-BFRs in waste plastics.

PubMed

Sharkey, Martin; Abdallah, Mohamed Abou-Elwafa; Drage, Daniel S; Harrad, Stuart; Berresheim, Harald

2018-05-17

The purpose of this study was to establish the efficacy of portable X-ray fluorescence (XRF) instrumentation as a screening tool for a variety of end of life plastics which may contain excess amounts of brominated flame retardants (BFRs), in compliance with European Union (EU) and United Nations Environment Programme (UNEP) legislative limits (low POP concentration limits - LPCLs). 555 samples of waste plastics were collected from eight waste and recycling sites in Ireland, including waste electrical and electronic equipment (WEEE), textiles, polyurethane foams (PUFs), and expanded polystyrene foams. Samples were screened for bromine content, in situ using a Niton™ XL3T GOLDD XRF analyser, the results of which were statistically compared to mass spectrometry (MS)-based measurements of polybrominated diphenyl ethers (PBDEs), hexabromocyclododecane (HBCDD) and tetrabromobisphenol-A (TBBP-A) concentrations in the same samples. Regression between XRF and MS for WEEE samples shows that, despite an overall favourable trend, large deviations occur for a cluster of samples indicative of other bromine-based compounds in some samples; even compensating for false-positives due to background interference from electronic components, XRF tends to over-estimate MS-determined BFR concentrations in the 100 to 10,000 mg kg -1 range. Substantial deviations were additionally found between results for PUFs, textiles and polystyrene samples, with the XRF over-estimating BFR concentrations by a factor of up to 1.9; this is likely due to matrix effects influencing XRF measurements. However, expanded (EPS) and extruded polystyrene (XPS) yielded much more reliable estimations of BFR-content due to a dominance of HBCDD in these materials. XRF proved much more reliable as a "pass/fail" screening tool for LPCL compliance (including a prospective LPCL on Deca-BDE based on REACH). Using a conservative threshold of BFR content exceeding legislative limits (710 mg kg -1 bromine

An optical supernova associated with the X-ray flash XRF 060218.

PubMed

Pian, E; Mazzali, P A; Masetti, N; Ferrero, P; Klose, S; Palazzi, E; Ramirez-Ruiz, E; Woosley, S E; Kouveliotou, C; Deng, J; Filippenko, A V; Foley, R J; Fynbo, J P U; Kann, D A; Li, W; Hjorth, J; Nomoto, K; Patat, F; Sauer, D N; Sollerman, J; Vreeswijk, P M; Guenther, E W; Levan, A; O'Brien, P; Tanvir, N R; Wijers, R A M J; Dumas, C; Hainaut, O; Wong, D S; Baade, D; Wang, L; Amati, L; Cappellaro, E; Castro-Tirado, A J; Ellison, S; Frontera, F; Fruchter, A S; Greiner, J; Kawabata, K; Ledoux, C; Maeda, K; Møller, P; Nicastro, L; Rol, E; Starling, R

2006-08-31

Long-duration gamma-ray bursts (GRBs) are associated with type Ic supernovae that are more luminous than average and that eject material at very high velocities. Less-luminous supernovae were not hitherto known to be associated with GRBs, and therefore GRB-supernovae were thought to be rare events. Whether X-ray flashes--analogues of GRBs, but with lower luminosities and fewer gamma-rays--can also be associated with supernovae, and whether they are intrinsically 'weak' events or typical GRBs viewed off the axis of the burst, is unclear. Here we report the optical discovery and follow-up observations of the type Ic supernova SN 2006aj associated with X-ray flash XRF 060218. Supernova 2006aj is intrinsically less luminous than the GRB-supernovae, but more luminous than many supernovae not accompanied by a GRB. The ejecta velocities derived from our spectra are intermediate between these two groups, which is consistent with the weakness of both the GRB output and the supernova radio flux. Our data, combined with radio and X-ray observations, suggest that XRF 060218 is an intrinsically weak and soft event, rather than a classical GRB observed off-axis. This extends the GRB-supernova connection to X-ray flashes and fainter supernovae, implying a common origin. Events such as XRF 060218 are probably more numerous than GRB-supernovae.

Application of Compton-suppressed self-induced XRF to spent nuclear fuel measurement

NASA Astrophysics Data System (ADS)

Park, Se-Hwan; Jo, Kwang Ho; Lee, Seung Kyu; Seo, Hee; Lee, Chaehun; Won, Byung-Hee; Ahn, Seong-Kyu; Ku, Jeong-Hoe

2017-11-01

Self-induced X-ray fluorescence (XRF) is a technique by which plutonium (Pu) content in spent nuclear fuel can be directly quantified. In the present work, this method successfully measured the plutonium/uranium (Pu/U) peak ratio of a pressurized water reactor (PWR)'s spent nuclear fuel at the Korea atomic energy research institute (KAERI)'s post irradiation examination facility (PIEF). In order to reduce the Compton background in the low-energy X-ray region, the Compton suppression system additionally was implemented. By use of this system, the spectrum's background level was reduced by a factor of approximately 2. This work shows that Compton-suppressed selfinduced XRF can be effectively applied to Pu accounting in spent nuclear fuel.

PXRF, μ-XRF, vacuum μ-XRF, and EPMA analysis of Email Champlevé objects present in Belgian museums.

PubMed

Van der Linden, Veerle; Meesdom, Eva; Devos, Annemie; Van Dooren, Rita; Nieuwdorp, Hans; Janssen, Elsje; Balace, Sophie; Vekemans, Bart; Vincze, Laszlo; Janssens, Koen

2011-10-01

The enamel of 20 Email Champlevé objects dating between the 12th and 19th centuries was investigated by means of microscopic and portable X-ray fluorescence analysis (μ-XRF and PXRF). Seven of these objects were microsampled and the fragments were analyzed with electron probe microanalysis (EPMA) and vacuum μ-XRF to obtain quantitative data about the composition of the glass used to produce these enameled objects. As a result of the evolution of the raw materials employed to produce the base glass, three different compositional groups could be discriminated. The first group consisted of soda-lime-silica glass with a sodium source of mineral origin (with low K content) that was opacified by addition of calcium antimonate crystals. This type of glass was only used in objects made in the 12th century. Email Champlevé objects from the beginning of the 13th century onward were enameled with soda-lime-silica glass with a sodium source of vegetal origin. This type of glass, which has a higher potassium content, was opacified with SnO2 crystals. The glass used for 19th century Email Champlevé artifacts was produced with synthetic and purified components resulting in a different chemical composition compared to the other groups. Although the four analytical techniques employed in this study have their own specific characteristics, they were all found to be suitable for classifying the objects into the different chronological categories.

Elemental analysis using ED-XRF and 14C dating of Cuman wall paintings samples

NASA Astrophysics Data System (ADS)

Brocchieri, J.; Sabbarese, C.; Marzaioli, F.; Passariello, I.; Terrasi, F.; De Maio, C.; Ferrara, L.

2018-04-01

The aim of the present research was to analyse pigments and mortars of fresco fragments located at Cuma (Naples, Italy). The ED-XRF technique and 14C dating were used to establish the nature of the pigments and the age of mortars, respectively. ED-XRF results allowed to determine the elemental composition of the pigments that identified the colours and, hence, the historical period of completion. The 14C dating, applied to mortars using a particular preparation, provided results that are in accordance with the archaeological information within the 2σ interval range.

A 3,000-year quantitative drought record derived from XRF element data from a south Texas playa

NASA Astrophysics Data System (ADS)

Livsey, D. N.; Simms, A.; Hangsterfer, A.; Nisbet, R.; DeWitt, R.

2013-12-01

Recent droughts throughout the central United States highlight the need for a better understanding of the past frequency and severity of drought occurrence. Current records of past drought for the south Texas coast are derived from tree-ring data that span approximately the last 900 years before present (BP). In this study we utilize a supervised learning routine to create a transfer function between X-Ray Fluorescence (XRF) derived elemental data from Laguna Salada, Texas core LS10-02 to a locally derived tree-ring drought record. From this transfer function the 900 BP tree-ring drought record was extended to 3,000 BP. The supervised learning routine was trained on the first 100 years of XRF element data and tree-ring drought data to create the transfer function and training data set output. The model was then projected from the XRF elemental data for the next 800 years to create a deployed data set output and to test the transfer function parameters. The coefficients of determination between the model output and observed values are 0.77 and 0.70 for the 100-year training data set and 900-year deployed data set respectively. Given the relatively high coefficients of determination for both the training data set and deployed data set we interpret the model parameters are fairly robust and that a high-resolution drought record can be derived from the XRF element data. These results indicate that XRF element data can be used as a quantitative tool to reconstruct past drought records.

Micro-PIXE and micro-SR-XRF studies for Romanian archaeological gold identification

NASA Astrophysics Data System (ADS)

Constantinescu, B.

2009-04-01

For gold, trace elements are more significant for provenancing archaeological artifacts than the main components: Platinum Group Elements (PGE), Sn, Te, Sb, Hg, Pb, but also high melting point elements, such as Ta and Nb. Several small fragments of native Carpathian gold were studied using micro-PIXE technique at the AGLAE accelerator, Louvre Museum and at the Legnaro AN2000 microbeam facility, and using SR-XRF at BESSY synchrotron. The goal of the study was to identify the trace elements, especially Sn, Sb and Te. At BESSY, the SR-XRF measurements were performed in air by using a 34 keV beam to excite the characteristic X-lines in Sn-Sb-Te region. We found Sn to be present in placers from Valea Arieşului and Valea Pianului, Sb in primary gold from Zlatna, Ruda-Brad, Valea Morii, Runculeţ-Straja and Pb in primary gold from Brǎdişor-Brad, Zlatna, Runculeţ-Straja, Valea Morii, Muşariu-Brad. Ten native gold nuggets and several fragments of objects coming from Visigothic Pietroasa "The Golden Brood Hen with Its Chickens" hoard were analyzed using micro-PIXE technique at the AGLAE accelerator, Louvre Museum, Paris and at the Legnaro AN2000 microbeam facility. We found Te in primary gold from Brǎdişor-Brad, Muşariu-Brad (different samples from BESSY analyzed ones), and Roşia Montanǎ, Sb in primary gold at Bucium-Izbiţa. For Pietroasa hoard, we found Sn in the Oenochoe cup and small fibula, indicating that alluvial gold - probably from Anatolia (Pactolus river) - was used. We also detected Ta inclusions in the large fibula, indicating that Ural Mountains (the only region where Ta and Au minerals are together) gold was (at least partially) used. A spectacular application to nine Dacian gold bracelets (belonging to National History Museum of Romania) authentication is presented. These bracelets look like spirals and are based on the same artistic idea, are centred around the same theme. The number of spiral varies from 6 to 8. When uncoiled, some bracelets

XPS-XRF hybrid metrology enabling FDSOI process

NASA Astrophysics Data System (ADS)

Hossain, Mainul; Subramanian, Ganesh; Triyoso, Dina; Wahl, Jeremy; Mcardle, Timothy; Vaid, Alok; Bello, A. F.; Lee, Wei Ti; Klare, Mark; Kwan, Michael; Pois, Heath; Wang, Ying; Larson, Tom

2016-03-01

Planar fully-depleted silicon-on-insulator (FDSOI) technology potentially offers comparable transistor performance as FinFETs. pFET FDOSI devices are based on a silicon germanium (cSiGe) layer on top of a buried oxide (BOX). Ndoped interfacial layer (IL), high-k (HfO2) layer and the metal gate stacks are then successively built on top of the SiGe layer. In-line metrology is critical in precisely monitoring the thickness and composition of the gate stack and associated underlying layers in order to achieve desired process control. However, any single in-line metrology technique is insufficient to obtain the thickness of IL, high-k, cSiGe layers in addition to Ge% and N-dose in one single measurement. A hybrid approach is therefore needed that combines the capabilities of more than one measurement technique to extract multiple parameters in a given film stack. This paper will discuss the approaches, challenges, and results associated with the first-in-industry implementation of XPS-XRF hybrid metrology for simultaneous detection of high-k thickness, IL thickness, N-dose, cSiGe thickness and %Ge, all in one signal measurement on a FDSOI substrate in a manufacturing fab. Strong correlation to electrical data for one or more of these measured parameters will also be presented, establishing the reliability of this technique.

A Combined XRD/XRF Instrument for Lunar Resource Assessment

NASA Technical Reports Server (NTRS)

Vaniman, D. T.; Bish, D. L.; Chipera, S. J.; Blacic, J. D.

1992-01-01

Robotic surface missions to the Moon should be capable of measuring mineral as well as chemical abundances in regolith samples. Although much is already known about the lunar regolith, our data are far from comprehensive. Most of the regolith samples returned to Earth for analysis had lost the upper surface, or it was intermixed with deeper regolith. This upper surface is the part of the regolith most recently exposed to the solar wind; as such it will be important to resource assessment. In addition, it may be far easier to mine and process the uppermost few centimeters of regolith over a broad area than to engage in deep excavation of a smaller area. The most direct means of analyzing the regolith surface will be by studies in situ. In addition, the analysis of the impact-origin regolith surfaces, the Fe-rich glasses of mare pyroclastic deposits, are of resource interest, but are inadequately known; none of the extensive surface-exposed pyroclastic deposits of the Moon have been systematically sampled, although we know something about such deposits from the Apollo 17 site. Because of the potential importance of pyroclastic deposits, methods to quantify glass as well as mineral abundances will be important to resource evaluation. Combined x ray diffraction (XRD) and x ray fluorescence (XRF) analysis will address many resource characterization problems on the Moon. XRF methods are valuable for obtaining full major-element abundances with high precision. Such data, collected in parallel with quantitative mineralogy, permit unambiguous determination of both mineral and chemical abundances where concentrations are high enough to be of resource grade. Collection of both XRD and XRF data from a single sample provides simultaneous chemical and mineralogic information. These data can be used to correlate quantitative chemistry and mineralogy as a set of simultaneous linear equations, the solution of which can lead to full characterization of the sample. The use of

DELAMINATION AND XRF ANALYSIS OF NIST LEAD IN PAINT FILM STANDARDS

EPA Science Inventory

The objectives of this protocol were to remove the laminate coating from lead paint film standards acquired from NIST by means of surface heating. The average XRF value did not change after removal of the polymer coating suggesting that this protocol is satisfactory for renderin...

Comparison of soil pollution concentrations determined using AAS and portable XRF techniques.

PubMed

Radu, Tanja; Diamond, Dermot

2009-11-15

Past mining activities in the area of Silvermines, Ireland, have resulted in heavily polluted soils. The possibility of spreading pollution to the surrounding areas through dust blow-offs poses a potential threat for the local communities. Conventional environmental soil and dust analysis techniques are very slow and laborious and consequently there is a need for fast and accurate analytical methods, which can provide real-time in situ pollution mapping. Laboratory-based aqua regia acid digestion of the soil samples collected in the area followed by the atomic absorption spectrophotometry (AAS) analysis confirmed very high pollution, especially by Pb, As, Cu, and Zn. In parallel, samples were analyzed using portable X-ray fluorescence radioisotope and miniature tube powered (XRF) NITON instruments and their performance was compared. Overall, the portable XRF instrument gave excellent correlation with the laboratory-based reference AAS method.

A novel XRF method to measure environmental release of copper and zinc from antifouling paints.

PubMed

Ytreberg, Erik; Lagerström, Maria; Holmqvist, Albin; Eklund, Britta; Elwing, Hans; Dahlström, Magnus; Dahl, Peter; Dahlström, Mia

2017-06-01

The release of copper (Cu) and zinc (Zn) from vessels and leisure crafts coated with antifouling paints can pose a threat to water quality in semi-enclosed areas such as harbors and marinas as well as to coastal archipelagos. However, no reliable, practical and low-cost method exists to measure the direct release of metals from antifouling paints. Therefore, the paint industry and regulatory authorities are obliged to use release rate measurements derived from either mathematical models or from laboratory studies. To bridge this gap, we have developed a novel method using a handheld X-Ray Fluorescence spectrometer (XRF) to determine the cumulative release of Cu and Zn from antifouling paints. The results showed a strong linear relationship between XRF K α net intensities and metal concentrations, as determined by ICP-MS. The release of Cu and Zn were determined for coated panels exposed in harbors located in the Baltic Sea and in Kattegat. The field study showed salinity to have a strong impact on the release of Cu, i.e. the release increased with salinity. Contrary, the effect of salinity on Zn was not as evident. As exemplified in this work, the XRF method also makes it possible to identify the governing parameters to the release of Cu and Zn, e.g. salinity and type of paint formulation. Thus, the XRF method can be used to measure environmentally relevant releases of metallic compounds to design more efficient and optimized antifouling coatings. Copyright © 2017 The Authors. Published by Elsevier Ltd.. All rights reserved.

Statistical behavior of ten million experimental detection limits

NASA Astrophysics Data System (ADS)

Voigtman, Edward; Abraham, Kevin T.

2011-02-01

Using a lab-constructed laser-excited fluorimeter, together with bootstrapping methodology, the authors have generated many millions of experimental linear calibration curves for the detection of rhodamine 6G tetrafluoroborate in ethanol solutions. The detection limits computed from them are in excellent agreement with both previously published theory and with comprehensive Monte Carlo computer simulations. Currie decision levels and Currie detection limits, each in the theoretical, chemical content domain, were found to be simply scaled reciprocals of the non-centrality parameter of the non-central t distribution that characterizes univariate linear calibration curves that have homoscedastic, additive Gaussian white noise. Accurate and precise estimates of the theoretical, content domain Currie detection limit for the experimental system, with 5% (each) probabilities of false positives and false negatives, are presented.

Micro-XRF analysis of silver coins from medieval Poland

NASA Astrophysics Data System (ADS)

del Hoyo-Meléndez, Julio M.; Świt, Paweł; Matosz, Marta; Woźniak, Mateusz; Klisińska-Kopacz, Anna; Bratasz, Łukasz

2015-04-01

X-ray fluorescence (XRF) analysis has become a standard method in archaeological science due to its non-invasive and non-destructive nature. This technique has extensively been used for the study of numismatic collections since the data derived from it can be correlated with manufacturing processes, provenance of raw materials, and geographical distribution of ancient mints. A group of 71 silver coins of the first Piasts: Boleslaus the Brave (996-1025) and Mieszko II Lambert (1025-1034) belonging to the collections of the National Museum in Krakow have been characterized using micro-XRF spectrometry. This is the most numerous collection of their coins representing nearly 30% of all known coins from these rulers. The research has focused on evaluating the use of this technique as a screening tool for elemental surface characterization of the alloys. Surveyed coins are mainly constituted by Ag, Cu and Pb along with trace levels of Fe, Ni, Zn, Au, Hg, Bi, and Br. Quantitative analyses have revealed Ag contents in the 81.6-97.5% range for all the evaluated coins. This study had the goal of providing information about the elemental composition of these objects, which will serve to enhance the existing knowledge about geographical and chronological diversification of Polish numismatic collections.

Impact of an external radiation field on handheld XRF measurements for nuclear forensics applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Steeb, Jennifer L.; Mertz, Carol J.; Finck, Martha R.

X-ray fluorescence (XRF) is an attractive technique for nuclear forensics applications. We evaluated a handheld, portable XRF device by applying an external radiation field (10 mR/h to 17 R/h) using two types of radiography sources: a 60Co radiography camera to observe effects from high-energy gamma emissions and an 192Ir radiography camera to observe effects from several low-energy gamma (0.604, 0.468, and 0.317 MeV) and decay daughter x-ray emissions. External radiation tests proved that radiation, in general, has a significant effect on the dead time or background at dose rates over 1 R/hr for both the 192Ir and 60Co sources.

Automatic rectum limit detection by anatomical markers correlation.

PubMed

Namías, R; D'Amato, J P; del Fresno, M; Vénere, M

2014-06-01

Several diseases take place at the end of the digestive system. Many of them can be diagnosed by means of different medical imaging modalities together with computer aided detection (CAD) systems. These CAD systems mainly focus on the complete segmentation of the digestive tube. However, the detection of limits between different sections could provide important information to these systems. In this paper we present an automatic method for detecting the rectum and sigmoid colon limit using a novel global curvature analysis over the centerline of the segmented digestive tube in different imaging modalities. The results are compared with the gold standard rectum upper limit through a validation scheme comprising two different anatomical markers: the third sacral vertebra and the average rectum length. Experimental results in both magnetic resonance imaging (MRI) and computed tomography colonography (CTC) acquisitions show the efficacy of the proposed strategy in automatic detection of rectum limits. The method is intended for application to the rectum segmentation in MRI for geometrical modeling and as contextual information source in virtual colonoscopies and CAD systems. Copyright © 2014 Elsevier Ltd. All rights reserved.

A con-focal setup for micro-XRF experiments using diamond anvil cells

NASA Astrophysics Data System (ADS)

Wilke, Max; Rickers, Karen; Vincze, Laszlo; Schmidt, Christian; Borchert, Manuela; Pascarelli, Sakura

2010-05-01

In this contribution we introduce an experimental setup to perform con-focal micro X-ray fluorescence measurements in situ in samples at high temperatures and pressures in diamond anvil cells (DAC) (e.g. Schmidt et al. 2007). The con-focal arrangement is used to suppress the background in X-ray fluorescence (XRF) spectra that stems from elastic and inelastic scattering of the diamond anvils. The setup is based on a focusing optic in the incident beam that reaches a spot of 5-10 μm and a focusing poly-capillary in front of an energy-dispersive solid-state detector. The detector poly-capillary is designed to work at a very long working distance of 50 mm in order to collect the radiation from the center of the DAC at 90° to the incident beam. The probing volume is defined by the two foci and has a size of ca. 300 μm at 8 keV and 150 μm at 19 keV as measured by scans through thin metal foils. Comparison of XRF spectra acquired with a usual detector collimator and spectra recorded with the detector capillary shows a strong suppression of XRF signal generated outside the probed volume, i.e. XRF from the gasket material and signal from elastic and Compton scattering by the diamond anvils. The ratio of the Zr K-alpha fluorescence peak to the peak of the Compton scattering changes from 0.5 (collimator) to 1.26 (detector capillary) for a ca. 1000 ppm Zr standard solution and an incident beam energy of 20 keV. For a standard solution containing ca. 1000 ppm Hf, the ratio of the L-alpha to the Compton signal increases to 6 using the detector capillary and an incident beam energy of 9.7 keV. Thus, the con-focal setup substantially improves the fluorescence to background ratio. This will result in higher sensitivities for dilute elements in the sample chamber of the DAC. Furthermore, the possibilities of interference of the sample's signal with signal from the sample environment are greatly reduced. In a broader sense, the setup can also be applied to other confined samples

Mineralogical In-situ Investigation of Acid-Sulfate Samples from the Rio Tinto River, Spain, with a Portable XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Sarrazin, P.; Ming, D. W.; Morris, R. V.; Fernandez-Remolar, D.; Amils, R.; Arvidson, R. E.; Blake, D.; Bish, D. L.

2007-01-01

A field campaign was organized in September 2006 by Centro de Astobiologica (Spain) and Washington University (St Louis, USA) for the geological study of the Rio Tinto river bed sediments using a suite of in-situ instruments comprising an ASD reflectance spectrometer, an emission spectrometer, panoramic and close-up color imaging cameras, a life detection system and NASA's CheMin 4 XRD/XRF prototype. The primary objectives of the field campaign were to study the geology of the site and test the potential of the instrument suite in an astrobiological investigation context for future Mars surface robotic missions. The results of the overall campaign will be presented elsewhere. This paper focuses on the results of the XRD/XRF instrument deployment. The specific objectives of the CheMin 4 prototype in Rio Tinto were to 1) characterize the mineralogy of efflorescent salts in their native environments; 2) analyze the mineralogy of salts and oxides from the modern environment to terraces formed earlier as part of the Rio Tinto evaporative system; and 3) map the transition from hematite-dominated terraces to the mixed goethite/salt-bearing terraces where biosignatures are best preserved.

A novel approach to measure elemental concentrations in cation exchange resins using XRF-scanning technique, and its potential in water pollution studies

NASA Astrophysics Data System (ADS)

Huang, Jyh-Jaan; Lin, Sheng-Chi; Löwemark, Ludvig; Liou, Ya-Hsuan; Chang, Queenie; Chang, Tsun-Kuo; Wei, Kuo-Yen; Croudace, Ian W.

2016-04-01

X-ray fluorescence (XRF) core-scanning is a fast, and convenient technique to assess elemental variations for a wide variety of research topics. However, the XRF scanning counts are often considered a semi-quantitative measurement due to possible absorption or scattering caused by down core variability in physical properties. To overcome this problem and extend the applications of XRF-scanning to water pollution studies, we propose to use cation exchange resin (IR-120) as an "elemental carrier", and to analyze the resins using the Itrax-XRF core scanner. The use of resin minimizes the matrix effects during the measurements, and can be employed in the field in great numbers due to its low price. Therefore, the fast, and non-destructive XRF-scanning technique can provide a quick and economical method to analyze environmental pollution via absorption in the resin. Five standard resin samples were scanned by the Itrax-XRF core scanner at different exposure times (1 s, 5 s, 15 s, 30 s, 100 s) to allow the comparisons of scanning counts with the absolute concentrations. The regression lines and correlation coefficients of elements that are generally used in pollution studies (Ca, Ti, Cr, Ni, Cu, Zn, and Pb) were examined for the different exposure times. The result shows that within the test range (from few ppm to thousands ppm), the correlation coefficients are all higher than 0.97, even at the shortest exposure time (1 s). Therefore, we propose to use this method in the field to monitor for example sewage disposal events. The low price of resin, and fast, multi elements and precise XRF-scanning technique provide a viable, cost- and time-effective approach that allows large sample numbers to be processed. In this way, the properties and sources of wastewater pollution can be traced for the purpose of environmental monitoring and environmental forensics.

µ-XANES AND µ-XRF INVESTIGATIONS OF METAL BINDING MECHANISMS IN BIOSOLIDS

EPA Science Inventory

Micro-X-ray fluorescence (µ-XRF) microprobe analysis and micro-X-ray absorption near edge spectroscopy (µ-XANES) were employed to identify Fe and Mn phases and their association with selected toxic elements in two biosolids (limed composted and Nu-Earth) containing low ...

Determination of the chemical properties of residues retained in individual cloud droplets by XRF microprobe at SPring-8

NASA Astrophysics Data System (ADS)

Ma, C.-J.; Tohno, S.; Kasahara, M.; Hayakawa, S.

2004-06-01

To determine the chemical properties of residue retained in individual cloud droplets is primarily important for the understanding of rainout mechanism and aerosol modification in droplet. The sampling of individual cloud droplets were carried out on the summit of Mt. Taiko located in Tango peninsula, Kyoto prefecture, during Asian dust storm event in March of 2002. XRF microprobe system equipped at SPring-8, BL-37XU was applied to the subsequent quantification analysis of ultra trace elements in residues of individual cloud droplets. It was possible to form the replicas of separated individual cloud droplets on the thin collodion film. The two dimensional XRF maps for the residues in individual cloud droplets were clearly drawn by scanning of micro-beam. Also, XRF spectra of trace elements in residues were well resolved. From the XRF spectra for individual residues, the chemical mixed state of residues could be assumed. The chemical forms of Fe (Fe +++) and Zn (Zn +) could be clearly characterized by their K-edge micro-XANES spectra. By comparison of Z/Si mass ratios of residues in cloud droplets and those of the original sands collected in desert areas in China, the aging of ambient dust particles and their in cloud modification were indirectly assumed.

XRF and XANES Data for Kaplan U Paper

EPA Pesticide Factsheets

The dataset contains two XRF images of iron and uranium distribution on plant roots and a database of XANES data used to produce XANES spectra figure for Figure 7 in the published paper.This dataset is associated with the following publication:Kaplan, D., R. Kukkadapu, J. Seaman, B. Arey, A. Dohnalkova, S. Buettner, D. Li, T. Varga, K. Scheckel, and P. Jaffe. Iron Mineralogy and Uranium-Binding Environment in the Rhizosphere of a Wetland Soil. D. Barcelo SCIENCE OF THE TOTAL ENVIRONMENT. Elsevier BV, AMSTERDAM, NETHERLANDS, 569: 53-64, (2016).

Quantitative assessment of historical coastal landfill contamination using in-situ field portable XRF (FPXRF)

NASA Astrophysics Data System (ADS)

O'Shea, Francis; Spencer, Kate; Brasington, James

2014-05-01

Historically, waste was deposited on low value, easily accessible coastal land (e.g. marsh land). Within England and Wales alone, there are over 5000 historical landfills situated within coastal areas at risk of flooding at a 1 in 100 year return period (Environment Agency, 2012). Historical sites were constructed prior to relevant legislation, and have no basal or side wall engineering, and the waste constituents are mostly unknown. In theory, contaminant concentrations should be reduced through natural attenuation as the leachate plume migrates through surrounding fine-grained inter-tidal sediments before reaching receptor waters. However, erosion resulting from rising sea level and increased storm intensity may re-distribute these sediments and release associated contaminants into the estuarine and coastal environment. The diffuse discharge from these sites has not been quantified and this presents a problem for those landfill managers who are required to complete EIAs. An earlier detailed field campaign at Newlands landfill site, on the Thames Estuary, UK identified a sub-surface (~2m depth) contaminant plume extending c. 20 m from the landfill boundary into surrounding fine-grained saltmarsh sediments. These saltmarsh sediments are risk of being eroded releasing their contaminant load to the Thames Estuary. The aims of this work were to; 1) assess whether this plume is representative of other historical landfills with similar characteristics and 2) to develop a rapid screening methodology using field portable XRF that could be used to identify potential risk of other coastal landfill sites. GIS was used to select landfill sites of similar age, hydrological regime and sedimentary setting in the UK, for comparison. Collection of sediment samples and analysis by ICP OES is expensive and time-consuming, therefore cores were extracted and analysed with a Niton Goldd XRF in-situ. Contaminant data were available immediately and the sampling strategy could be adapted

Nitromethane K-9 Detection Limit

DOE Office of Scientific and Technical Information (OSTI.GOV)

Strobel, R; Kury, J

2003-08-29

The Bureau of Alcohol, Tobacco and Firearms (ATF) trains canine/handler teams to detect explosives for government and other agencies worldwide. After completing the training program the teams are tested on an array containing explosives and numerous other samples designed to distract a canine. Passing this test results in a team's certification. These teams can be considered as ''detection instruments'' freshly calibrated just before leaving the ''factory''. Using these teams to examine special experimental arrays immediately following certification can lead to a better understanding of a canine's detection capabilities. Forty-one of these ''detection instruments'' were used in four test series withmore » arrays containing dilute nitromethane-in-water solutions. (The canines had been trained on the amount of nitromethane vapor in equilibrium with the undiluted liquid explosive.) By diluting liquid nitromethane with water, the amount of explosive vapor can be reduced many orders of magnitude to test the lower limit of the canine's nitromethane vapor detection response. The results are presented in this paper.« less

In vivo investigation of a new 109Cd γ-ray induced K-XRF bone lead measurement system

NASA Astrophysics Data System (ADS)

Nie, Huiling; Chettle, David; Luo, Liqiang; O'Meara, Joanne

2006-01-01

A new 109Cd γ-ray induced K-XRF bone lead measurement system using an array of four detectors has been developed. Previous results from Monte Carlo (MC) simulations and experiments with phantoms predicted that it would be about three times more sensitive than the conventional system, albeit using a more active source. A dosimetry study has been performed for this system and it demonstrated that the dose delivered to the measured individuals is acceptable even for 5-year-old children. Approval to apply this system to human studies has been received from the Research Ethics Board. In this study, 20 adult volunteers, 10 male, 10 female, were recruited to have their tibia measured with both the conventional system and the new system. The result confirmed the improvement predicted by the MC simulations and the in vitro measurements. Two other interesting points were discovered from the data. One is that the data from the new system showed a significant positive correlation between age and tibia lead concentration, while the data from the conventional system do not. The other is that 85% of the tibia lead concentrations were under the minimum detection limit when measured by the conventional system, and the proportion reduced to 50% when measured by the new system.

Micro-XRF complemented by x-radiography and digital microscopy imaging for the study of hidden paintings

NASA Astrophysics Data System (ADS)

Gasanova, Svetlana; Hermon, Sorin

2017-07-01

The present study describes a novel approach to the study of hidden by integrating the non-invasive micro-X-Ray Fluorescence spectroscopy, X-radiography and digital microscopy. The case study analysed is a portrait of a male figure discovered under the painting of Ecce Homo, attributed to Titian's studio with an estimated date in the 1550s. The X-radiography images exposed the details of the underpainting, which appeared to be a nearly finished portrait of a standing man, overpainted by the current composition of Ecce Homo at a 180° angle. The microscopy observations of the upper painting's cracks and flaked areas enabled the study of the exposed underlayers in terms of their colour appearance and pigment particles. The subsequent pigment analysis was performed by micro-XRF. Since the described XRF analysis was performed not in scanner mode, the correct selection of the measurement spots for the micro analysis and separation between pigments of the lower and the upper painting was of paramount importance. The described approach for spot selection was based on the results of the preceding X-radiography and digital microscopy tests. The presence of lead white, vermilion, copper green and iron earth in the underlying portrait was confirmed by the multiple point XRF analysis of Pb, Hg, Cu, Fe and Mn lines. The described investigation method proved to be useful in the identification of the pigments of the underlying painting and consequently assisted in the tentative reconstruction of its colour palette. Moreover, the undertaken approach allowed discovering the potential of micro-XRF technique in the study of hidden compositions.

Reducing risk and increasing confidence of decision making at a lower cost: In-situ pXRF assessment of metal-contaminated sites.

PubMed

Rouillon, Marek; Taylor, Mark P; Dong, Chenyin

2017-10-01

This study evaluates the in-situ use of field portable X-ray Fluorescence (pXRF) for metal-contaminated site assessments, and assesses the advantages of increased sampling to reduce risk, and increase confidence of decision making at a lower cost. Five metal-contaminated sites were assessed using both in-situ pXRF and ex-situ inductively coupled plasma mass spectrometry (ICP-MS) analyses at various sampling resolutions. Twenty second in-situ pXRF measurements of Mn, Zn and Pb were corrected using a subset of parallel ICP-MS measurements taken at each site. Field and analytical duplicates revealed sampling as the major contributor (>95% variation) to measurement uncertainties. This study shows that increased sampling led to several benefits including more representative site characterisation, higher soil-metal mapping resolution, reduced uncertainty around the site mean, and reduced sampling uncertainty. Real time pXRF data enabled efficient, on-site decision making for further judgemental sampling, without the need to return to the site. Additionally, in-situ pXRF was more cost effective than the current approach of ex-situ sampling and ICP-MS analysis, even with higher sampling at each site. Lastly, a probabilistic site assessment approach was applied to demonstrate the advantages of integrating estimated measurement uncertainties into site reporting. Copyright © 2017 Elsevier Ltd. All rights reserved.

Nondestructive Analysis of Astromaterials by Micro-CT and Micro-XRF Analysis for PET Examination

NASA Astrophysics Data System (ADS)

Zeigler, R. A.; Righter, K.; Allen, C. C.

2013-09-01

Here we discuss our recent investigations into the applications of micro-CT and micro-XRF analyses with Apollo samples and ANSMET meteorites and assess the usefulness of these techniques in future PET.

Normalizing XRF-scanner data: A cautionary note on the interpretation of high-resolution records from organic-rich lakes

NASA Astrophysics Data System (ADS)

Löwemark, L.; Chen, H.-F.; Yang, T.-N.; Kylander, M.; Yu, E.-F.; Hsu, Y.-W.; Lee, T.-Q.; Song, S.-R.; Jarvis, S.

2011-04-01

X-ray fluorescence (XRF) scanning of unlithified, untreated sediment cores is becoming an increasingly common method used to obtain paleoproxy data from lake records. XRF-scanning is fast and delivers high-resolution records of relative variations in the elemental composition of the sediment. However, lake sediments display extreme variations in their organic matter content, which can vary from just a few percent to well over 50%. As XRF scanners are largely insensitive to organic material in the sediment, increasing levels of organic material effectively dilute those components that can be measured, such as the lithogenic material (the closed-sum effect). Consequently, in sediments with large variations in organic material, the measured variations in an element will to a large extent mirror the changes in organic material. It is therefore necessary to normalize the elements in the lithogenic component of the sediment against a conservative element to allow changes in the input of the elements to be addressed. In this study we show that Al, which is the lightest element that can be measured using the Itrax XRF-scanner, can be used to effectively normalize the elements of the lithogenic fraction of the sediment against variations in organic content. We also show that care must be taken when choosing resolution and exposure time to ensure optimal output from the measurements.

Search times and probability of detection in time-limited search

NASA Astrophysics Data System (ADS)

Wilson, David; Devitt, Nicole; Maurer, Tana

2005-05-01

When modeling the search and target acquisition process, probability of detection as a function of time is important to war games and physical entity simulations. Recent US Army RDECOM CERDEC Night Vision and Electronics Sensor Directorate modeling of search and detection has focused on time-limited search. Developing the relationship between detection probability and time of search as a differential equation is explored. One of the parameters in the current formula for probability of detection in time-limited search corresponds to the mean time to detect in time-unlimited search. However, the mean time to detect in time-limited search is shorter than the mean time to detect in time-unlimited search and the relationship between them is a mathematical relationship between these two mean times. This simple relationship is derived.

Nuclear Fuel Assay through analysis of Uranium L-shell by Hybrid L-edge/XRF Densitometer using a Surrogate Material

NASA Astrophysics Data System (ADS)

Park, Seunghoon; Joung, Sungyeop; Park, Jerry AB(; ), AC(; )

2018-01-01

Assay of L-series of nuclear material solution is useful for determination of amount of nuclear materials and ratio of minor actinide in the materials. The hybrid system of energy dispersive X-ray absorption edge spectrometry, i.e. L-edge densitometry, and X-ray fluorescence spectrometry is one of the analysis methods. The hybrid L-edge/XRF densitometer can be a promising candidate for a portable and compact equipment due to advantage of using low energy X-ray beams without heavy shielding systems and liquid nitrogen cooling compared to hybrid K-edge/XRF densitometer. A prototype of the equipment was evaluated for feasibility of the nuclear material assay using a surrogate material (lead) to avoid radiation effects from nuclear materials. The uncertainty of L-edge and XRF characteristics of the sample material and volume effects was discussed in the article.

Direct identification and analysis of heavy metals in solution (Hg, Cu, Pb, Zn, Ni) by use of in situ electrochemical X-ray fluorescence.

PubMed

O'Neil, Glen D; Newton, Mark E; Macpherson, Julie V

2015-01-01

The development and application of a new methodology, in situ electrochemical X-ray fluorescence (EC-XRF), is described that enables direct identification and quantification of heavy metals in solution. A freestanding film of boron-doped diamond serves as both an X-ray window and the electrode material. The electrode is biased at a suitable driving potential to electroplate metals from solution onto the electrode surface. Simultaneously, X-rays that pass through the back side of the electrode interrogate the time-dependent electrodeposition process by virtue of the XRF signals, which are unique to each metal. In this way it is possible to unambiguously identify which metals are in solution and relate the XRF signal intensity to a concentration of metal species in solution. To increase detection sensitivity and reduce detection times, solution is flown over the electrode surface by use of a wall-jet configuration. Initial studies focused on the in situ detection of Pb(2+), where concentration detection limits of 99 nM were established in this proof-of-concept study (although significantly lower values are anticipated with system refinement). This is more than 3 orders of magnitude lower than that achievable by XRF alone in a flowing solution (0.68 mM). In situ EC-XRF measurements were also carried out on a multimetal solution containing Hg(2+), Pb(2+), Cu(2+), Ni(2+), Zn(2+), and Fe(3+) (all at 10 μM concentration). Identification of five of these metals was possible in one simple measurement. In contrast, while anodic stripping voltammetry (ASV) also revealed five peaks, peak identification was not straightforward, requiring further experiments and prior knowledge of the metals in solution. Time-dependent EC-XRF nucleation data for the five metals, recorded simultaneously, demonstrated similar deposition rates. Studies are now underway to lower detection limits and provide a quantitative understanding of EC-XRF responses in real, multimetal solutions. Finally, the

Laboratory evaluation of a field-portable sealed source X-ray fluorescence spectrometer for determination of metals in air filter samples.

PubMed

Lawryk, Nicholas J; Feng, H Amy; Chen, Bean T

2009-07-01

Recent advances in field-portable X-ray fluorescence (FP XRF) spectrometer technology have made it a potentially valuable screening tool for the industrial hygienist to estimate worker exposures to airborne metals. Although recent studies have shown that FP XRF technology may be better suited for qualitative or semiquantitative analysis of airborne lead in the workplace, these studies have not extensively addressed its ability to measure other elements. This study involved a laboratory-based evaluation of a representative model FP XRF spectrometer to measure elements commonly encountered in workplace settings that may be collected on air sample filter media, including chromium, copper, iron, manganese, nickel, lead, and zinc. The evaluation included assessments of (1) response intensity with respect to location on the probe window, (2) limits of detection for five different filter media, (3) limits of detection as a function of analysis time, and (4) bias, precision, and accuracy estimates. Teflon, polyvinyl chloride, polypropylene, and mixed cellulose ester filter media all had similarly low limits of detection for the set of elements examined. Limits of detection, bias, and precision generally improved with increasing analysis time. Bias, precision, and accuracy estimates generally improved with increasing element concentration. Accuracy estimates met the National Institute for Occupational Safety and Health criterion for nearly all the element and concentration combinations. Based on these results, FP XRF spectrometry shows potential to be useful in the assessment of worker inhalation exposures to other metals in addition to lead.

Development of a versatile XRF scanner for the elemental imaging of paintworks

NASA Astrophysics Data System (ADS)

Ravaud, E.; Pichon, L.; Laval, E.; Gonzalez, V.; Eveno, M.; Calligaro, T.

2016-01-01

Scanning XRF is a powerful elemental imaging technique introduced at the synchrotron that has recently been transposed to laboratory. The growing interest in this technique stems from its ability to collect images reflecting pigment distribution within large areas on artworks by means of their elemental signature. In that sense, scanning XRF appears highly complementary to standard imaging techniques (Visible, UV, IR photography and X-ray radiography). The versatile XRF scanner presented here has been designed and built at the C2RMF in response to specific constraints: transportability, cost-effectiveness and ability to scan large areas within a single working day. The instrument is based on a standard X-ray generator with sub-millimetre collimated beam and a SDD-based spectrometer to collected X-ray spectra. The instrument head is scanned in front of the painting by means of motorised movements to cover an area up to 300 × 300 mm2 with a resolution of 0.5 mm (600 × 600 pixels). The 15-kg head is mounted on a stable photo stand for rapid positioning on paintworks and maintains a free side-access for safety; it can also be attached to a lighter tripod for field measurements. Alignment is achieved with a laser pointer and a micro-camera. With a scanning speed of 5 mm/s and 0.1 s/point, elemental maps are collected in 10 h, i.e. a working day. The X-ray spectra of all pixels are rapidly processed using an open source program to derive elemental maps. To illustrate the capabilities of this instrument, this contribution presents the results obtained on the Belle Ferronnière painted by Leonardo da Vinci (1452-1519) and conserved in the Musée du Louvre, prior to its restoration at the C2RMF.

XRF inductive bead fusion and PLC based control system

NASA Astrophysics Data System (ADS)

Zhu, Jin-hong; Wang, Ying-jie; Shi, Hong-xin; Chen, Qing-ling; Chen, Yu-xi

2009-03-01

In order to ensure high-quality X-ray fluorescence spectrometry (XRF) analysis, an inductive bead fusion machine was developed. The prototype consists of super-audio IGBT induction heating power supply, rotation and swing mechanisms, and programmable logic controller (PLC). The system can realize sequence control, mechanical movement control, output current and temperature control. Experimental results show that the power supply can operate at an ideal quasi-resonant state, in which the expected power output and the required temperature can be achieved for rapid heating and the uniform formation of glass beads respectively.

Reasons of different colors in the ignimbrite lithology: micro-XRF and confocal Raman spectrometry method.

PubMed

Koralay, Tamer; Kadioglu, Yusuf Kagan

2008-03-01

Medium to large volume ignimbrites usually show vertical changes in terms of color, mineral components, texture and geochemistry. Determination of vertical changes in single extensive ignimbrite flow unit is difficult and requires careful studies. Color changes in ignimbrite flow units are very important for earth scientists. This may cause to identify the same ignimbrite series with different definition. Incesu ignimbrite has a wide distribution in the Central Anatolian Volcanic Province (CAVP). It is classified into three levels as lower, middle and upper according to color and welding degree. There is a sharp contact between the lower and middle level. The lower level is dark brown to black in color and the middle level has pinkish red to red color. The present paper focuses on the investigation of color changes between the ignimbrite levels by using micro-XRF and confocal Raman spectrometry. Micro-XRF and Raman spectrometry studies were performed on the polished thin sections of the lower and middle levels with different compositions. These differences were because of the compositional changes of K and slightly Fe elements distribution within the matrix. The dark brown to black color of the lower level was related to the high concentration of the K and Fe relatively to the middle level. Confocal Raman spectrometry investigations exhibited the matrix of the lower level mainly composed of anorthoclase, supporting the results of the micro-XRF.

Energy-Dispersive X-Ray Fluorescence Spectrometry: A Long Overdue Addition to the Chemistry Curriculum

ERIC Educational Resources Information Center

Palmer, Peter T.

2011-01-01

Portable Energy-Dispersive X-Ray Fluorescence (XRF) analyzers have undergone significant improvements over the past decade. Salient advantages of XRF for elemental analysis include minimal sample preparation, multielement analysis capabilities, detection limits in the low parts per million (ppm) range, and analysis times on the order of 1 min.…

USE OF METHOD DETECTION LIMITS IN ENVIRONMENTAL MEASUREMENTS

EPA Science Inventory

Environmental measurements often produce values below the method detection limit (MDL). Because low or zero values may be used in determining compliance with regulatory limits, in determining emission factors (typical concentrations emitted by a given type of source), or in model...

X-Ray Fluorescence (XRF) to identify chemical analysis of minerals in Buton island, SE Sulawesi, Indonesia

NASA Astrophysics Data System (ADS)

Jamaluddin; Darwis, A.; Massinai, M. A.

2018-02-01

Asbuton as natural rock asphalt consists of a granular material; usually limestone or sandstone. In its natural state, it contains bitumen intimately dispersed throughout its mass, while the remainder of the material is a solid mineral matter. This research was conducted in Sorowalio, Buton Regency, Southeast Sulawesi province, Indonesia. This study aims to determine the content and the percentage of minerals contained in the rocks by using X-Ray Fluorescence (XRF). The method of research is a preliminary survey, sampling and laboratory analysis. XRF reports chemical composition, including Si (quartz) and Ca (calcite). The results indicate the content and the percentage of element dominate the rock sample is Fe2O3, MgO, CaO, and SiO2. Research results using XRF show that there are four metal oxide dominant elements. Hematite (Fe2O3) is dominant in all locations of sampling. Magnesium oxide (MgO) has the highest levels found in sample number six and the lowest is in sample number five. Silicates (SiO) has the highest levels at sample number six and the lowest in sample number seven. Calcium oxide (CaO) is dominant in all sampling locations. The sample of asbuton contains 37.90% asphalt, 43.28% carbonate, and18.82% other minerals.

Evaluation of elemental status of ancient human bone samples from Northeastern Hungary dated to the 10th century AD by XRF

NASA Astrophysics Data System (ADS)

János, I.; Szathmáry, L.; Nádas, E.; Béni, A.; Dinya, Z.; Máthé, E.

2011-11-01

The present study is a multielemental analysis of bone samples belonging to skeletal individuals originating from two contemporaneous (10th century AD) cemeteries (Tiszavasvári Nagy-Gyepáros and Nagycserkesz-Nádasibokor sites) in Northeastern Hungary, using the XRF analytical technique. Emitted X-rays were detected in order to determine the elemental composition of bones and to appreciate the possible influence of the burial environment on the elemental content of the human skeletal remains. Lumbar vertebral bodies were used for analysis. Applying the ED(P)XRF technique concentration of the following elements were determined: P, Ca, K, Na, Mg, Al, Cl, Mn, Fe, Zn, Br and Sr. The results indicated post mortem mineral exchange between the burial environment (soil) and bones (e.g. the enhanced levels of Fe and Mn) and referred to diagenetic alteration processes during burials. However, other elements such as Zn, Sr and Br seemed to be accumulated during the past life. On the basis of statistical analysis, clear separation could not be observed between the two excavation sites in their bone elemental concentrations which denoted similar diagenetic influences, environmental conditions. The enhanced levels of Sr might be connected with the past dietary habits, especially consumption of plant food.

In vivo quantification of lead in bone with a portable x-ray fluorescence system--methodology and feasibility.

PubMed

Nie, L H; Sanchez, S; Newton, K; Grodzins, L; Cleveland, R O; Weisskopf, M G

2011-02-07

This study was conducted to investigate the methodology and feasibility of developing a portable x-ray fluorescence (XRF) technology to quantify lead (Pb) in bone in vivo. A portable XRF device was set up and optimal settings of voltage, current, and filter combination for bone lead quantification were selected to achieve the lowest detection limit. The minimum radiation dose delivered to the subject was calculated by Monte Carlo simulations. An ultrasound device was used to measure soft tissue thickness to account for signal attenuation, and an alternative method to obtain soft tissue thickness from the XRF spectrum was developed and shown to be equivalent to the ultrasound measurements (intraclass correlation coefficient, ICC = 0.82). We tested the correlation of in vivo bone lead concentrations between the standard KXRF technology and the portable XRF technology. There was a significant correlation between the bone lead concentrations obtained from the standard KXRF technology and those obtained from the portable XRF technology (ICC = 0.65). The detection limit for the portable XRF device was about 8.4 ppm with 2 mm soft tissue thickness. The entrance skin dose delivered to the human subject was about 13 mSv and the total body effective dose was about 1.5 µSv and should pose minimal radiation risk. In conclusion, portable XRF technology can be used for in vivo bone lead measurement with sensitivity comparable to the KXRF technology and good correlation with KXRF measurements.

Use of small volume cups in XRF analysis of treated wood retention

Treesearch

Rene Stelzer; Adam Taylor; Patricia Lebow

2017-01-01

Efforts are underway in the United States to improve the conformance of commercially-treated wood with the applicable retention standards. As part of an effort to devise a practical method for on-site assessment of within-charge retention variation, we investigated whether small-volume x-ray fluorescence (XRF) sample cups could be used with treated wood. A range of cup...

An Integrated XRF/XRD Instrument for Mars Exobiology and Geology Experiments

NASA Technical Reports Server (NTRS)

Koppel, L. N.; Franco, E. D.; Kerner, J. A.; Fonda, M. L.; Schwartz, D. E.; Marshall, J. R.

1993-01-01

By employing an integrated x-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details characterizing the past and present environment on Mars and those relevant to the possibility of the origin and evolution of life will be acquired. A combined x-ray fluorescence/x-ray diffraction (XRF/XRD) instrument was breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for MESUR and future Mars missions. Among others, primary objectives for the exploration of Mars include the intense study of local areas on Mars to establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance, and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epoches; and to establish the global chemical and physical characteristics of the Martian surface. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment. Preliminary breadboard experiments confirmed the fundamental instrument design approach and measurement performance.

Epidemiologic Evaluation of Measurement Data in the Presence of Detection Limits

PubMed Central

Lubin, Jay H.; Colt, Joanne S.; Camann, David; Davis, Scott; Cerhan, James R.; Severson, Richard K.; Bernstein, Leslie; Hartge, Patricia

2004-01-01

Quantitative measurements of environmental factors greatly improve the quality of epidemiologic studies but can pose challenges because of the presence of upper or lower detection limits or interfering compounds, which do not allow for precise measured values. We consider the regression of an environmental measurement (dependent variable) on several covariates (independent variables). Various strategies are commonly employed to impute values for interval-measured data, including assignment of one-half the detection limit to nondetected values or of “fill-in” values randomly selected from an appropriate distribution. On the basis of a limited simulation study, we found that the former approach can be biased unless the percentage of measurements below detection limits is small (5–10%). The fill-in approach generally produces unbiased parameter estimates but may produce biased variance estimates and thereby distort inference when 30% or more of the data are below detection limits. Truncated data methods (e.g., Tobit regression) and multiple imputation offer two unbiased approaches for analyzing measurement data with detection limits. If interest resides solely on regression parameters, then Tobit regression can be used. If individualized values for measurements below detection limits are needed for additional analysis, such as relative risk regression or graphical display, then multiple imputation produces unbiased estimates and nominal confidence intervals unless the proportion of missing data is extreme. We illustrate various approaches using measurements of pesticide residues in carpet dust in control subjects from a case–control study of non-Hodgkin lymphoma. PMID:15579415

Stochastic fluctuations and the detectability limit of network communities.

PubMed

Floretta, Lucio; Liechti, Jonas; Flammini, Alessandro; De Los Rios, Paolo

2013-12-01

We have analyzed the detectability limits of network communities in the framework of the popular Girvan and Newman benchmark. By carefully taking into account the inevitable stochastic fluctuations that affect the construction of each and every instance of the benchmark, we come to the conclusion that the native, putative partition of the network is completely lost even before the in-degree/out-degree ratio becomes equal to that of a structureless Erdös-Rényi network. We develop a simple iterative scheme, analytically well described by an infinite branching process, to provide an estimate of the true detectability limit. Using various algorithms based on modularity optimization, we show that all of them behave (semiquantitatively) in the same way, with the same functional form of the detectability threshold as a function of the network parameters. Because the same behavior has also been found by further modularity-optimization methods and for methods based on different heuristics implementations, we conclude that indeed a correct definition of the detectability limit must take into account the stochastic fluctuations of the network construction.

Rapid screening of heavy metals and trace elements in environmental samples using portable X-ray fluorescence spectrometer, A comparative study

PubMed Central

McComb, Jacqueline Q.; Rogers, Christian; Han, Fengxiang X.; Tchounwou, Paul B.

2014-01-01

With industrialization, great amounts of trace elements and heavy metals have been excavated and released on the surface of the earth and dissipated into the environments. Rapid screening technology for detecting major and trace elements as well as heavy metals in variety of environmental samples is most desired. The objectives of this study were to determine the detection limits, accuracy, repeatability and efficiency of a X-ray fluorescence spectrometer (Niton XRF analyzer) in comparison with the traditional analytical methods, inductively coupled plasma optical emission spectrometer (ICP-OES) and inductively coupled plasma optical emission spectrometer (ICP-MS) in screening of major and trace elements of environmental samples including estuary soils and sediments, contaminated soils, and biological samples. XRF is a fast and non-destructive method in measuring the total concentration of multi--elements simultaneously. Contrary to ICP-OES and ICP-MS, XRF analyzer is characterized by the limited preparation required for solid samples, non-destructive analysis, increased total speed and high throughout, the decreased production of hazardous waste and the low running costs as well as multi-elemental determination and portability in the fields. The current comparative study demonstrates that XRF is a good rapid non-destructive method for contaminated soils, sediments and biological samples containing higher concentrations of major and trace elements. Unfortunately, XRF does not have sensitive detection limits of most major and trace elements as ICP-OES or ICP-MS but it may serve as a rapid screening tool for locating hot spots of uncontaminated field soils and sediments. PMID:25861136

Combined Survey Format (CSF) Archaeogeophysical (Metal Detecting, Radiometrics and Resistivity) and Archaeochemical (XRF) Investigations of the 19th Century La Hacienda Y Presidio of Babocomari Military Site in Arizona

NASA Astrophysics Data System (ADS)

Lundin, R. J.; Aydin, N.; Brackett, C.

2007-05-01

Recent archaeological investigations of Historic Era Mexican and Anglo-American and Prehistoric and Protohistoric Hohokam and Sobaipuri culture sites on the Babacomari Land Grant near Sierra Vista Arizona by Carothers Environmental, LLC (CE), Wondjina Research Institute (WRI) and DMG Four Corners Research (FCR) led to the discovery of two major 19th Century military sites that were known from the literature but had not been scientifically investigated. It was decided by WRI and BABACOMARI RANCH that this project was ideal for an experimental cooperative training program for archaeologists and geologists from the anthropology and geology departments of UA, ASU, NAU, PC, and members of AAS, AAHS, AAC, THS and USFS personnel in the use of the new CSF archaeogeophysical, archaeochemical and airbourne remote sensing technologies and field techniques that have just been recently introduced in the US. WRI, CE and Statistical Research Inc. (SRI) conducted CSF VLF Metal Detecting, Radiometrics and Resistivity studies and portable X-Ray Fluorescence (XRF) archaeochemical studies. The results will be presented along with suggestions as to use of these technologies in CSF studies.

Detection limit used for early warning in public health surveillance.

PubMed

Kobari, Tsuyoshi; Iwaki, Kazuo; Nagashima, Tomomi; Ishii, Fumiyoshi; Hayashi, Yuzuru; Yajima, Takehiko

2009-06-01

A theory of detection limit, developed in analytical chemistry, is applied to public health surveillance to detect an outbreak of national emergencies such as natural disaster and bioterrorism. In this investigation, the influenza epidemic around the Tokyo area from 2003 to 2006 is taken as a model of normal and large-scale epidemics. The detection limit of the normal epidemic is used as a threshold with a specified level of significance to identify a sign of the abnormal epidemic among the daily variation in anti-influenza drug sales at community pharmacies. While auto-correlation of data is often an obstacle to an unbiased estimator of standard deviation involved in the detection limit, the analytical theory (FUMI) can successfully treat the auto-correlation of the drug sales in the same way as the auto-correlation appearing as 1/f noise in many analytical instruments.

Comparison of PIXE and XRF analysis of airborne particulate matter samples collected on Teflon and quartz fibre filters

NASA Astrophysics Data System (ADS)

Chiari, M.; Yubero, E.; Calzolai, G.; Lucarelli, F.; Crespo, J.; Galindo, N.; Nicolás, J. F.; Giannoni, M.; Nava, S.

2018-02-01

Within the framework of research projects focusing on the sampling and analysis of airborne particulate matter, Particle Induced X-ray Emission (PIXE) and Energy Dispersive X-ray Fluorescence (ED-XRF) techniques are routinely used in many laboratories throughout the world to determine the elemental concentration of the particulate matter samples. In this work an inter-laboratory comparison of the results obtained from analysing several samples (collected on both Teflon and quartz fibre filters) using both techniques is presented. The samples were analysed by PIXE (in Florence, at the 3 MV Tandetron accelerator of INFN-LABEC laboratory) and by XRF (in Elche, using the ARL Quant'X EDXRF spectrometer with specific conditions optimized for specific groups of elements). The results from the two sets of measurements are in good agreement for all the analysed samples, thus validating the use of the ARL Quant'X EDXRF spectrometer and the selected measurement protocol for the analysis of aerosol samples. Moreover, thanks to the comparison of PIXE and XRF results on Teflon and quartz fibre filters, possible self-absorption effects due to the penetration of the aerosol particles inside the quartz fibre-filters were quantified.

The limit of detection for explosives in spectroscopic differential reflectometry

NASA Astrophysics Data System (ADS)

Dubroca, Thierry; Vishwanathan, Karthik; Hummel, Rolf E.

2011-05-01

In the wake of recent terrorist attacks, such as the 2008 Mumbai hotel explosion or the December 25th 2009 "underwear bomber", our group has developed a technique (US patent #7368292) to apply differential reflection spectroscopy to detect traces of explosives. Briefly, light (200-500 nm) is shone on a surface such as a piece of luggage at an airport. Upon reflection, the light is collected with a spectrometer combined with a CCD camera. A computer processes the data and produces in turn a differential reflection spectrum involving two adjacent areas of the surface. This differential technique is highly sensitive and provides spectroscopic data of explosives. As an example, 2,4,6, trinitrotoluene (TNT) displays strong and distinct features in differential reflectograms near 420 nm. Similar, but distinctly different features are observed for other explosives. One of the most important criteria for explosive detection techniques is the limit of detection. This limit is defined as the amount of explosive material necessary to produce a signal to noise ratio of three. We present here, a method to evaluate the limit of detection of our technique. Finally, we present our sample preparation method and experimental set-up specifically developed to measure the limit of detection for our technology. This results in a limit ranging from 100 nano-grams to 50 micro-grams depending on the method and the set-up parameters used, such as the detector-sample distance.

A compact small-beam XRF instrument for in-situ analysis of objects of historical and/or artistic value

NASA Astrophysics Data System (ADS)

Vittiglio, G.; Janssens, K.; Vekemans, B.; Adams, F.; Oost, A.

1999-11-01

The analytical characteristics, possibilities and limitations of a compact and easily transportable small-beam XRF instrument are described. The instrument consists of a compact, mini-focus Mo X-ray tube that is collimated to produce a sub-mm beam and a peltier-cooled PIN diode detector. Relative MDLs in highly scattering matrices are situated in the 10-100-ppm range; for metallic matrices featuring strong matrix lines, the MDLs of the instrument are approximately a factor 2 higher. Since only a small irradiation area is required, a simple micro-polishing technique that may be performed in situ in combination with the measurements is shown to be effective for the determination of the bulk composition of corroded bronze objects. As an example, a series of Egyptian bronze objects date from XXII nd Egyptian Dynasty (ca. 1090 BC) to the Roman era (30 BC to 640 AD) was analyzed in order to contribute to the very limited database on Cu-alloy compositions from this period.

In vivo evaluation of Fe in human skin employing X-Ray Fluorescence Methodology (XRF)

NASA Astrophysics Data System (ADS)

Estevam, M.; Appoloni, C. R.

2007-02-01

Recent technological improvements allow the method of in vivo XRF to provide useful sensibility for diagnostics or monitoring in biomedical applications. In cases of hereditary sanguine disorders as the β-thalassaemia or a genetic disorder like Haemochromatosis, there is a high concentration of elements as Fe, Zn and Cu in the skin and internal organs, due to the treatment of those abnormalities or due to the own dysfunction caused by the disease. The levels of Fe related to the patient bearers of the β-thalassaemia are determined, at the moment, measuring a protein in the sanguine current, called ferritin. The monitoring of the protein is ineffective in several situations, such as when the patient suffers any disturbance of health. Nowadays, the main forms of measuring the levels of those metals through hepatic storage are the biopsy of the liver, that is invasive and potentially dangerous, presenting a rate of mortality of 0.1%, and by means of magnetic susceptibilities that employs a quantum superconductor, which is highly expensive and there are only three main world centers with this equipment This work investigates the use of a Si PIN-diode detector and a 238Pu source (13 and 17keV; 13%; 95.2mCi; 86y) for the measurement of Fe skin levels compatible with those associated to the disease β-thalassaemia. XRF spectra were analyzed using a set of AXIL-WinQXAS programs elaborated and disseminated by the IAEA. The determination coefficient of the calibration model (sensitivity curve) was 0.97. Measurements on skin phantoms containing concentrations of Fe in the range from 10 to 150 parts per million (ppm), indicate that we are able to detect Fe at levels of the order of 15ppm, using monitoring periods of 50 seconds and skin entrance dose less than 10 mSv, The literature reports skin Fe levels from 15.0 to 60.0 ppm in normal persons and from 70 to 150 ppm in thalassaemics patients. So, the employed methodology allows the measurement of the skin Fe concentration.

Detection of colloidal silver chloride near solubility limit

NASA Astrophysics Data System (ADS)

Putri, K. Y.; Adawiah, R.

2018-03-01

Detection of nanoparticles in solution has been made possible by several means; one of them is laser-induced breakdown detection (LIBD). LIBD is able to distinguish colloids of various sizes and concentrations. This technique has been used in several solubility studies. In this study, the formation of colloids in a mixed system of silver nitrate and sodium chloride was observed by acoustic LIBD. Silver chloride has low solubility limit, therefore LIBD measurement is appropriate. Silver and chloride solutions with equal concentrations, set at below and above the solubility of silver chloride as the expected solid product, were mixed and the resulting colloids were observed. The result of LIBD measurement showed that larger particles were present as more silver and chloride introduced. However, once the concentrations exceeded the solubility limit of silver chloride, the detected particle size seemed to be decreasing, hence suggested the occurrence of coprecipitation process. This phenomenon indicated that the ability of LIBD to detect even small changes in colloid amounts might be a useful tool in study on formation and stability of colloids, i.e. to confirm whether nanoparticles synthesis has been successfully performed and whether the system is stable or not.

Composition and microstructure of MTA and Aureoseal Plus: XRF, EDS, XRD and FESEM evaluation.

PubMed

Cianconi, L; Palopoli, P; Campanella, V; Mancini, M

2016-12-01

The aim of this study was to determine the chemical composition and the phases' microstructure of Aureoseal Plus (OGNA, Italy) and ProRoot MTA (Dentsply Tulsa Dental, USA) and to compare their characteristics. Study Design: Comparing Aureoseal Plus and ProRoot MTA microstructure by means of several analyses type. The chemical analysis of the two cements was assessed following the UNI EN ISO 196-2 norm. X-Ray fluorescence (XRF) was used to determine the element composition. The crystalline structure was analysed quantitatively using x-ray diffraction (XRD). Powders morphology was evaluated using a scanning electron microscope (SEM) with backscattering detectors, and a field emission scanning electron microscope (FESEM). Elemental analysis was performed by energy dispersive x-ray analysis (EDS). The semi-quantitative XRF analysis showed the presence of heavy metal oxides in both cements. The XRD spectra of the two cements reported the presence of dicalcium silicate, tricalcium silicate, tricalcium aluminate, tetracalcium aluminoferrite, bismuth oxide and gypsum. SEM analysis showed that ProRoot MTA powder is less coarse and more homogeneous than Aureoseal. Both powders are formed by particles of different shapes: round, prismatic and oblong. The EDS analysis showed that some ProRoot MTA particles, differently from Aureoseal, contain Ca, Si, Al and Fe. Oblong particles in ProRoot and Aureoseal are rich of bismuth. The strong interest in developing new Portland cement-based endodontic sealers will create materials with increased handling characteristics and physicochemical properties. A thorough investigation on two cement powders was carried out by using XRF, XRD, SEM and EDS analysis. To date there was a lack of studies on Aureoseal Plus. This cement is similar in composition to ProRoot MTA. Despite that it has distinctive elements that could improve its characteristics, resulting in a good alternative to MTA.

XRF-measured bone lead (Pb) as a biomarker for Pb exposure and toxicity among children diagnosed with Pb poisoning.

PubMed

Specht, Aaron J; Lin, Yanfen; Weisskopf, Marc; Yan, Chonghuai; Hu, Howard; Xu, Jian; Nie, Linda H

2016-01-01

Childhood lead (Pb) poisoning remains a global issue, especially in industrial areas. In this study, 115 children with average age 5.7 years were recruited as either patient diagnosed with Pb poisoning or controls at Xinhua Hospital in China. The subjects' bone Pb was measured with a K-shell X-ray fluorescence (KXRF) and a portable X-ray fluorescence (XRF) system. A significant correlation between KXRF bone Pb and blood Pb and portable XRF and KXRF measurements were observed. The half-life of blood-lead was calculated to be 9.96 ± 3.92 d. Our results indicate that bone is a useful biomarker for Pb in children.

True detection limits in an experimental linearly heteroscedastic system.. Part 2

NASA Astrophysics Data System (ADS)

Voigtman, Edward; Abraham, Kevin T.

2011-11-01

Despite much different processing of the experimental fluorescence detection data presented in Part 1, essentially the same estimates were obtained for the true theoretical Currie decision levels ( YC and XC) and true Currie detection limits ( YD and XD). The obtained experimental values, for 5% probability of false positives and 5% probability of false negatives, were YC = 56.0 mV, YD = 125. mV, XC = 0.132 μg/mL and XD = 0.293 μg/mL. For 5% probability of false positives and 1% probability of false negatives, the obtained detection limits were YD = 158 . mV and XD = 0.371 μg/mL. Furthermore, by using bootstrapping methodology on the experimental data for the standards and the analytical blank, it was possible to validate previously published experimental domain expressions for the decision levels ( yC and xC) and detection limits ( yD and xD). This was demonstrated by testing the generated decision levels and detection limits for their performance in regard to false positives and false negatives. In every case, the obtained numbers of false negatives and false positives were as specified a priori.

Calculation of the detection limit in radiation measurements with systematic uncertainties

NASA Astrophysics Data System (ADS)

Kirkpatrick, J. M.; Russ, W.; Venkataraman, R.; Young, B. M.

2015-06-01

The detection limit (LD) or Minimum Detectable Activity (MDA) is an a priori evaluation of assay sensitivity intended to quantify the suitability of an instrument or measurement arrangement for the needs of a given application. Traditional approaches as pioneered by Currie rely on Gaussian approximations to yield simple, closed-form solutions, and neglect the effects of systematic uncertainties in the instrument calibration. These approximations are applicable over a wide range of applications, but are of limited use in low-count applications, when high confidence values are required, or when systematic uncertainties are significant. One proposed modification to the Currie formulation attempts account for systematic uncertainties within a Gaussian framework. We have previously shown that this approach results in an approximation formula that works best only for small values of the relative systematic uncertainty, for which the modification of Currie's method is the least necessary, and that it significantly overestimates the detection limit or gives infinite or otherwise non-physical results for larger systematic uncertainties where such a correction would be the most useful. We have developed an alternative approach for calculating detection limits based on realistic statistical modeling of the counting distributions which accurately represents statistical and systematic uncertainties. Instead of a closed form solution, numerical and iterative methods are used to evaluate the result. Accurate detection limits can be obtained by this method for the general case.

In-situ and elementally resolved determination of the thickness uniformity of multi-ply films by confocal micro XRF.

PubMed

Peng, Song; Liu, Zhiguo; Sun, Tianxi; Wang, Guangfu; Ma, Yongzhong; Ding, Xunliang

2014-08-01

Confocal micro X-ray fluorescence (CM-XRF) with quasi-monochromatic excitation based on polycapillary X-ray optics was used to measure the thickness of multi-ply films. The relative errors of measuring an Fe film with a thickness of 16.3 μm and a Cu film with a thickness of 24.5 μm were 7.3% and 0.4%, respectively. The non-destructive and in-situ measurement of the thickness and uniformity of multi-ply films of Cu, Fe and Ni on a silicon surface was performed. CM-XRF was convenient in in-situ and elementally resolved analysis of the thickness of multi-ply films without a cumbersome theoretical correction model. Copyright © 2014 Elsevier Ltd. All rights reserved.

Nondestructive Analysis of Apollo Samples by Micro-CT and Micro-XRF Analysis: A PET Style Examination

NASA Technical Reports Server (NTRS)

Zeigler, Ryan A.

2014-01-01

An integral part of any sample return mission is the initial description and classification of returned samples by the preliminary examination team (PET). The goal of a PET is to characterize and classify the returned samples, making this information available to the general research community who can then conduct more in-depth studies on the samples. A PET strives to minimize the impact their work has on the sample suite, which often limits the PET work to largely visual measurements and observations like optical microscopy. More modern techniques can also be utilized by future PET to nondestructively characterize astromaterials in a more rigorous way. Here we present our recent analyses of Apollo samples 14321 and 14305 by micro-CT and micro-XRF (respectively), assess the potential for discovery of "new" Apollo samples for scientific study, and evaluate the usefulness of these techniques in future PET efforts.

Estimating the resolution limit of the map equation in community detection

NASA Astrophysics Data System (ADS)

Kawamoto, Tatsuro; Rosvall, Martin

2015-01-01

A community detection algorithm is considered to have a resolution limit if the scale of the smallest modules that can be resolved depends on the size of the analyzed subnetwork. The resolution limit is known to prevent some community detection algorithms from accurately identifying the modular structure of a network. In fact, any global objective function for measuring the quality of a two-level assignment of nodes into modules must have some sort of resolution limit or an external resolution parameter. However, it is yet unknown how the resolution limit affects the so-called map equation, which is known to be an efficient objective function for community detection. We derive an analytical estimate and conclude that the resolution limit of the map equation is set by the total number of links between modules instead of the total number of links in the full network as for modularity. This mechanism makes the resolution limit much less restrictive for the map equation than for modularity; in practice, it is orders of magnitudes smaller. Furthermore, we argue that the effect of the resolution limit often results from shoehorning multilevel modular structures into two-level descriptions. As we show, the hierarchical map equation effectively eliminates the resolution limit for networks with nested multilevel modular structures.

Using Nondestructive Portable X-ray Fluorescence Spectrometers on Stone, Ceramics, Metals, and Other Materials in Museums: Advantages and Limitations.

PubMed

Tykot, Robert H

2016-01-01

Elemental analysis is a fundamental method of analysis on archaeological materials to address their overall composition or identify the source of their geological components, yet having access to instrumentation, its often destructive nature, and the time and cost of analyses have limited the number and/or size of archaeological artifacts tested. The development of portable X-ray fluorescence (pXRF) instruments over the past decade, however, has allowed nondestructive analyses to be conducted in museums around the world, on virtually any size artifact, producing data for up to several hundred samples per day. Major issues have been raised, however, about the sensitivity, precision, and accuracy of these devices, and the limitation of performing surface analysis on potentially heterogeneous objects. The advantages and limitations of pXRF are discussed here regarding archaeological studies of obsidian, ceramics, metals, bone, and painted materials. © The Author(s) 2015.

Shot noise limited detection of OH using the technique of laser induced fluorescence

NASA Technical Reports Server (NTRS)

Bakalyar, D. M.; Davis, L. I., Jr.; Guo, C.; James, J. V.; Kakos, S.; Morris, P. T.; Wang, C. C.

1984-01-01

Nearly shot-noise limited detection of OH using the technique of laser-induced fluorescence is reported. A LIDAR configuration is used to excite fluorescence in a large volume and a narrow-bandwidth interference filter provides spectral discrimination. This arrangement alleviates the effect of ozone interference and facilitates image processing at relatively close distances. The detection limit is determined mainly by the shot-noise of the solar background. Ground-based measurements in Dearborn indicate a detection limit of better than 1 x 10 to the 6th power OH/cubic cm over a forty-minute acquisition period. Under favorable conditions, a comparable detection limit was also observed for airborne measurements.

Shot noise limited detection of OH using the technique of laser-induced fluorescence

NASA Technical Reports Server (NTRS)

Bakalyar, D. M.; Davis, L. I., Jr.; Guo, C.; James, J. V.; Wang, C. C.; Kakos, S.; Morris, P. T.

1984-01-01

Nearly shot-noise limited detection of OH using the technique of laser-induced fluorescence is reported. A LIDAR configuration is used to excite fluoresence in a large volume and a narrow-bandwidth interference filter provides spectral discrimination. This arrangement alleviates the effect of ozone interference and facilitates image processing at relatively close distances. The detection limit is determined mainly by the short-noise of the solar background. Ground-based measurements in Dearborn indicate a detection limit of better than 1 x 10 to the 6th power OH/cubic cm over a forty-minute acquisition period. Under favorable conditions, a comparable detection limit was also observed for airborne measurements.

Tandem transmission/reflection mode XRD instrument including XRF for in situ measurement of Martian rocks and soils

NASA Astrophysics Data System (ADS)

Delhez, Robert; Van der Gaast, S. J.; Wielders, Arno; de Boer, J. L.; Helmholdt, R. B.; van Mechelen, J.; Reiss, C.; Woning, L.; Schenk, H.

2003-02-01

The mineralogy of the surface material of Mars is the key to disclose its present and past life and climates. Clay mineral species, carbonates, and ice (water and CO2) are and/or contain their witnesses. X-ray powder diffraction (XRPD) is the most powerful analytical method to identify and quantitatively characterize minerals in complex mixtures. This paper discusses the development of a working model of an instrument consisting of a reflection mode diffractometer and a transmission mode CCD-XRPD instrument, combined with an XRF module. The CCD-XRD/XRF instrument is analogous to the instrument for Mars missions developed by Sarrazin et al. (1998). This part of the tandem instrument enables "quick and dirty" analysis of powdered (!) matter to monitor semi-quantitatively the presence of clay minerals as a group, carbonates, and ices and yields semi-quantitative chemical information from X-ray fluorescence (XRF). The reflection mode instrument (i) enables in-situ measurements of rocks and soils and quantitative information on the compounds identified, (ii) has a high resolution and reveals large spacings for accurate identification, in particular of clay mineral species, and (iii) the shape of the line profiles observed reveals the kind and approximate amounts of lattice imperfections present. It will be shown that the information obtained with the reflection mode diffractometer is crucial for finding signs of life and changes in the climate on Mars. Obviously this instrument can also be used for other extra-terrestrial research.

Limits of detection and decision. Part 3

NASA Astrophysics Data System (ADS)

Voigtman, E.

2008-02-01

It has been shown that the MARLAP (Multi-Agency Radiological Laboratory Analytical Protocols) for estimating the Currie detection limit, which is based on 'critical values of the non-centrality parameter of the non-central t distribution', is intrinsically biased, even if no calibration curve or regression is used. This completed the refutation of the method, begun in Part 2. With the field cleared of obstructions, the true theory underlying Currie's limits of decision, detection and quantification, as they apply in a simple linear chemical measurement system (CMS) having heteroscedastic, Gaussian measurement noise and using weighted least squares (WLS) processing, was then derived. Extensive Monte Carlo simulations were performed, on 900 million independent calibration curves, for linear, "hockey stick" and quadratic noise precision models (NPMs). With errorless NPM parameters, all the simulation results were found to be in excellent agreement with the derived theoretical expressions. Even with as much as 30% noise on all of the relevant NPM parameters, the worst absolute errors in rates of false positives and false negatives, was only 0.3%.

Of Detection Limits and Effective Mitigation: The Use of Infrared Cameras for Methane Leak Detection

NASA Astrophysics Data System (ADS)

Ravikumar, A. P.; Wang, J.; McGuire, M.; Bell, C.; Brandt, A. R.

2017-12-01

Mitigating methane emissions, a short-lived and potent greenhouse gas, is critical to limiting global temperature rise to two degree Celsius as outlined in the Paris Agreement. A major source of anthropogenic methane emissions in the United States is the oil and gas sector. To this effect, state and federal governments have recommended the use of optical gas imaging systems in periodic leak detection and repair (LDAR) surveys to detect for fugitive emissions or leaks. The most commonly used optical gas imaging systems (OGI) are infrared cameras. In this work, we systematically evaluate the limits of infrared (IR) camera based OGI system for use in methane leak detection programs. We analyze the effect of various parameters that influence the minimum detectable leak rates of infrared cameras. Blind leak detection tests were carried out at the Department of Energy's MONITOR natural gas test-facility in Fort Collins, CO. Leak sources included natural gas wellheads, separators, and tanks. With an EPA mandated 60 g/hr leak detection threshold for IR cameras, we test leak rates ranging from 4 g/hr to over 350 g/hr at imaging distances between 5 ft and 70 ft from the leak source. We perform these experiments over the course of a week, encompassing a wide range of wind and weather conditions. Using repeated measurements at a given leak rate and imaging distance, we generate detection probability curves as a function of leak-size for various imaging distances, and measurement conditions. In addition, we estimate the median detection threshold - leak-size at which the probability of detection is 50% - under various scenarios to reduce uncertainty in mitigation effectiveness. Preliminary analysis shows that the median detection threshold varies from 3 g/hr at an imaging distance of 5 ft to over 150 g/hr at 50 ft (ambient temperature: 80 F, winds < 4 m/s). Results from this study can be directly used to improve OGI based LDAR protocols and reduce uncertainty in estimated

Targeted Analyte Detection by Standard Addition Improves Detection Limits in MALDI Mass Spectrometry

PubMed Central

Eshghi, Shadi Toghi; Li, Xingde; Zhang, Hui

2014-01-01

Matrix-assisted laser desorption/ionization has proven an effective tool for fast and accurate determination of many molecules. However, the detector sensitivity and chemical noise compromise the detection of many invaluable low-abundance molecules from biological and clinical samples. To challenge this limitation, we developed a targeted analyte detection (TAD) technique. In TAD, the target analyte is selectively elevated by spiking a known amount of that analyte into the sample, thereby raising its concentration above the noise level, where we take advantage of the improved sensitivity to detect the presence of the endogenous analyte in the sample. We assessed TAD on three peptides in simple and complex background solutions with various exogenous analyte concentrations in two MALDI matrices. TAD successfully improved the limit of detection (LOD) of target analytes when the target peptides were added to the sample in a concentration close to optimum concentration. The optimum exogenous concentration was estimated through a quantitative method to be approximately equal to the original LOD for each target. Also, we showed that TAD could achieve LOD improvements on an average of 3-fold in a simple and 2-fold in a complex sample. TAD provides a straightforward assay to improve the LOD of generic target analytes without the need for costly hardware modifications. PMID:22877355

Detection limits of antimicrobials in ewe milk by delvotest photometric measurements.

PubMed

Althaus, R L; Torres, A; Montero, A; Balasch, S; Molina, M P

2003-02-01

The Delvotest method detection limits per manufacturer's instructions at a fixed reading time of 3 h for 24 antimicrobial agents were determined in ewe milk by photometric measurement. For each drug, eight concentrations were tested on 20 ewe milk samples from individual ewes. Detection limits, determined by means of logistic regression models, were (microg/kg): 3, amoxycillin; 2, ampicillin; 18, cloxacillin; 1, penicillin "G"; 34, cefadroxil; 430, cephalosporin "C"; 40, cephalexin; 20, cefoperazone; 33, Ceftiofur; 18, cefuroxime; 6100, streptomycin; 1200, gentamycin; 2600, neomycin; 830, erythromycin; 100, tylosin; 180, doxycycline; 320, oxytetracycline; 590, tetracycline; 88, sulfadiazine; 44, sulfamethoxazole; 140, sulfametoxypyridazine; 48, sulfaquinoxaline; 12,000, chloramphenicol; and 290, trimethoprim. Whereas the beta-lactam antibiotics, sulphonamides, and tylosin were detected by Delvotest method at levels equal to those of maximum residue limits, its sensitivity needs to be enhanced to detect aminoglycosides, tetracyclines, streptomycin, chloramphenicol, and trimethoprim residues in ewe milk or to develop an integrated residue detection system for ewe milk with different sensitive microorganisms for each group of antiinfectious agents.

True detection limits in an experimental linearly heteroscedastic system. Part 1

NASA Astrophysics Data System (ADS)

Voigtman, Edward; Abraham, Kevin T.

2011-11-01

Using a lab-constructed laser-excited filter fluorimeter deliberately designed to exhibit linearly heteroscedastic, additive Gaussian noise, it has been shown that accurate estimates may be made of the true theoretical Currie decision levels ( YC and XC) and true Currie detection limits ( YD and XD) for the detection of rhodamine 6 G tetrafluoroborate in ethanol. The obtained experimental values, for 5% probability of false positives and 5% probability of false negatives, were YC = 56.1 mV, YD = 125. mV, XC = 0.132 μg /mL and XD = 0.294 μg /mL. For 5% probability of false positives and 1% probability of false negatives, the obtained detection limits were YD = 158. mV and XD = 0.372 μg /mL. These decision levels and corresponding detection limits were shown to pass the ultimate test: they resulted in observed probabilities of false positives and false negatives that were statistically equivalent to the a priori specified values.

Leonardo da Vinci's drapery studies: characterization of lead white pigments by µ-XRD and 2D scanning XRF

NASA Astrophysics Data System (ADS)

Gonzalez, Victor; Calligaro, Thomas; Pichon, Laurent; Wallez, Gilles; Mottin, Bruno

2015-11-01

This work focuses on the composition and microstructure of the lead white pigment employed in a set of paintworks, using a combination of µ-XRD and 2D scanning XRF, directly applied on five drapery studies attributed to Leonardo da Vinci (1452-1519) and conserved in the Département des Arts Graphiques, Musée du Louvre and in the Musée des Beaux- Arts de Rennes. Trace elements present in the composition as well as in the lead white highlights were imaged by 2D scanning XRF. Mineral phases were determined in a fully noninvasive way using a special µ-XRD diffractometer. Phase proportions were estimated by Rietveld refinement. The analytical results obtained will contribute to differentiate lead white qualities and to highlight the artist's technique.

Theoretical detection limit of PIXE analysis using 20 MeV proton beams

NASA Astrophysics Data System (ADS)

Ishii, Keizo; Hitomi, Keitaro

2018-02-01

Particle-induced X-ray emission (PIXE) analysis is usually performed using proton beams with energies in the range 2∼3 MeV because at these energies, the detection limit is low. The detection limit of PIXE analysis depends on the X-ray production cross-section, the continuous background of the PIXE spectrum and the experimental parameters such as the beam currents and the solid angle and detector efficiency of X-ray detector. Though the continuous background increases as the projectile energy increases, the cross-section of the X-ray increases as well. Therefore, the detection limit of high energy proton PIXE is not expected to increase significantly. We calculated the cross sections of continuous X-rays produced in several bremsstrahlung processes and estimated the detection limit of a 20 MeV proton PIXE analysis by modelling the Compton tail of the γ-rays produced in the nuclear reactions, and the escape effect on the secondary electron bremsstrahlung. We found that the Compton tail does not affect the detection limit when a thin X-ray detector is used, but the secondary electron bremsstrahlung escape effect does have an impact. We also confirmed that the detection limit of the PIXE analysis, when used with 4 μm polyethylene backing film and an integrated beam current of 1 μC, is 0.4∼2.0 ppm for proton energies in the range 10∼30 MeV and elements with Z = 16-90. This result demonstrates the usefulness of several 10 MeV cyclotrons for performing PIXE analysis. Cyclotrons with these properties are currently installed in positron emission tomography (PET) centers.

In vivo evaluation of Fe in human skin employing X-Ray Fluorescence Methodology (XRF)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Estevam, M.; Appoloni, C. R.

2007-02-12

Recent technological improvements allow the method of in vivo XRF to provide useful sensibility for diagnostics or monitoring in biomedical applications. In cases of hereditary sanguine disorders as the {beta}-thalassaemia or a genetic disorder like Haemochromatosis, there is a high concentration of elements as Fe, Zn and Cu in the skin and internal organs, due to the treatment of those abnormalities or due to the own dysfunction caused by the disease. The levels of Fe related to the patient bearers of the {beta}-thalassaemia are determined, at the moment, measuring a protein in the sanguine current, called ferritin. The monitoring ofmore » the protein is ineffective in several situations, such as when the patient suffers any disturbance of health. Nowadays, the main forms of measuring the levels of those metals through hepatic storage are the biopsy of the liver, that is invasive and potentially dangerous, presenting a rate of mortality of 0.1%, and by means of magnetic susceptibilities that employs a quantum superconductor, which is highly expensive and there are only three main world centers with this equipment This work investigates the use of a Si PIN-diode detector and a 238Pu source (13 and 17keV; 13%; 95.2mCi; 86y) for the measurement of Fe skin levels compatible with those associated to the disease {beta}-thalassaemia. XRF spectra were analyzed using a set of AXIL-WinQXAS programs elaborated and disseminated by the IAEA. The determination coefficient of the calibration model (sensitivity curve) was 0.97. Measurements on skin phantoms containing concentrations of Fe in the range from 10 to 150 parts per million (ppm), indicate that we are able to detect Fe at levels of the order of 15ppm, using monitoring periods of 50 seconds and skin entrance dose less than 10 mSv, The literature reports skin Fe levels from 15.0 to 60.0 ppm in normal persons and from 70 to 150 ppm in thalassaemics patients. So, the employed methodology allows the measurement of the skin

Evaluation of a new optic-enabled portable X-ray fluorescence spectrometry instrument for measuring toxic metals/metalloids in consumer goods and cultural products

NASA Astrophysics Data System (ADS)

Guimarães, Diana; Praamsma, Meredith L.; Parsons, Patrick J.

2016-08-01

X-ray fluorescence spectrometry (XRF) is a rapid, non-destructive multi-elemental analytical technique used for determining elemental contents ranging from percent down to the μg/g level. Although detection limits are much higher for XRF compared to other laboratory-based methods, such as inductively coupled plasma mass spectrometry (ICP-MS), ICP-optical emission spectrometry (OES) and atomic absorption spectrometry (AAS), its portability and ease of use make it a valuable tool, especially for field-based studies. A growing necessity to monitor human exposure to toxic metals and metalloids in consumer goods, cultural products, foods and other sample types while performing the analysis in situ has led to several important developments in portable XRF technology. In this study, a new portable XRF analyzer based on the use of doubly curved crystal optics (HD Mobile®) was evaluated for detecting toxic elements in foods, medicines, cosmetics and spices used in many Asian communities. Two models of the HD Mobile® (a pre-production and a final production unit) were investigated. Performance parameters including accuracy, precision and detection limits were characterized in a laboratory setting using certified reference materials (CRMs) and standard solutions. Bias estimates for key elements of public health significance such as As, Cd, Hg and Pb ranged from - 10% to 11% for the pre-production, and - 14% to 16% for the final production model. Five archived public health samples including herbal medicine products, ethnic spices and cosmetic products were analyzed using both XRF instruments. There was good agreement between the pre-production and final production models for the four key elements, such that the data were judged to be fit-for-purpose for the majority of samples analyzed. Detection of the four key elements of interest using the HD Mobile® was confirmed using archived samples for which ICP-OES data were available based on digested sample materials. The HD

Micro-XRF for In Situ Geological Exploration of Other Planets

NASA Technical Reports Server (NTRS)

Wade, Lawrence A.; Hodyss, Robert P.; Allwood, Abigail C.; Gao, Ning; Kozaczek, Kris

2013-01-01

In situ analysis of rock chemistry is a fundamental tool for exploration of planets. To meet this need, a high-spatial-resolution micro x-ray fluorescence (Micro-XRF) instrument was developed that is capable of determining the elemental composition of rocks (elements Na U) with 100 microns spatial resolution, thus providing insight to the composition of features as small as sand grains and individual laminae. The resulting excitation beam is of sufficient intensity that high signal-to-noise punctual spectra are acquired in seconds to a few minutes using an Amptek Silicon Drift Detector (SDD). The instrument features a tightly focused x-ray tube and HVPS developed by Moxtek that provides up to 200 micro-A at 10 to 50 keV, with a custom polycapillary optic developed by XOS Inc. and integrated into a breadboard Micro-XRF (see figure). The total mass of the complete breadboard instrument is 2.76 kg, including mounting hardware, mounting plate, camera, laser, etc. A flight version of this instrument would require less than 5W nominal power and 1.5 kg mass. The instrument includes an Amptek SDD that draws 2.5 W and has a resolution of 135 to 155 eV FWHM at 5.9 keV. It weighs 180 g, including the preamplifier, digital pulse processor, multichannel analyzer, detector and preamp power supplies, and packaging. Rock samples are positioned relative to the instrument by a three-axis arm whose position is controlled by closed-loop translators (mimicking the robotic arm of a rover). The distance from the source to the detector is calculated from the position of a focused laser beam on the sample as imaged by the camera. The instrument enables quick scans of major elements in only 1 second, and rapid acquisition (30 s) of data with excellent signal-to-noise and energy resolution for trace element analysis

Censoring: a new approach for detection limits in total-reflection X-ray fluorescence

NASA Astrophysics Data System (ADS)

Pajek, M.; Kubala-Kukuś, A.; Braziewicz, J.

2004-08-01

It is shown that the detection limits in the total-reflection X-ray fluorescence (TXRF), which restrict quantification of very low concentrations of trace elements in the samples, can be accounted for using the statistical concept of censoring. We demonstrate that the incomplete TXRF measurements containing the so-called "nondetects", i.e. the non-measured concentrations falling below the detection limits and represented by the estimated detection limit values, can be viewed as the left random-censored data, which can be further analyzed using the Kaplan-Meier (KM) method correcting for nondetects. Within this approach, which uses the Kaplan-Meier product-limit estimator to obtain the cumulative distribution function corrected for the nondetects, the mean value and median of the detection limit censored concentrations can be estimated in a non-parametric way. The Monte Carlo simulations performed show that the Kaplan-Meier approach yields highly accurate estimates for the mean and median concentrations, being within a few percent with respect to the simulated, uncensored data. This means that the uncertainties of KM estimated mean value and median are limited in fact only by the number of studied samples and not by the applied correction procedure for nondetects itself. On the other hand, it is observed that, in case when the concentration of a given element is not measured in all the samples, simple approaches to estimate a mean concentration value from the data yield erroneous, systematically biased results. The discussed random-left censoring approach was applied to analyze the TXRF detection-limit-censored concentration measurements of trace elements in biomedical samples. We emphasize that the Kaplan-Meier approach allows one to estimate the mean concentrations being substantially below the mean level of detection limits. Consequently, this approach gives a new access to lower the effective detection limits for TXRF method, which is of prime interest for

Non-matrix Matched Glass Disk Calibration Standards Improve XRF Micronutrient Analysis of Wheat Grain across Five Laboratories in India

PubMed Central

Guild, Georgia E.; Stangoulis, James C. R.

2016-01-01

Within the HarvestPlus program there are many collaborators currently using X-Ray Fluorescence (XRF) spectroscopy to measure Fe and Zn in their target crops. In India, five HarvestPlus wheat collaborators have laboratories that conduct this analysis and their throughput has increased significantly. The benefits of using XRF are its ease of use, minimal sample preparation and high throughput analysis. The lack of commercially available calibration standards has led to a need for alternative calibration arrangements for many of the instruments. Consequently, the majority of instruments have either been installed with an electronic transfer of an original grain calibration set developed by a preferred lab, or a locally supplied calibration. Unfortunately, neither of these methods has been entirely successful. The electronic transfer is unable to account for small variations between the instruments, whereas the use of a locally provided calibration set is heavily reliant on the accuracy of the reference analysis method, which is particularly difficult to achieve when analyzing low levels of micronutrient. Consequently, we have developed a calibration method that uses non-matrix matched glass disks. Here we present the validation of this method and show this calibration approach can improve the reproducibility and accuracy of whole grain wheat analysis on 5 different XRF instruments across the HarvestPlus breeding program. PMID:27375644

Sniper detection using infrared camera: technical possibilities and limitations

NASA Astrophysics Data System (ADS)

Kastek, M.; Dulski, R.; Trzaskawka, P.; Bieszczad, G.

2010-04-01

The paper discusses technical possibilities to build an effective system for sniper detection using infrared cameras. Descriptions of phenomena which make it possible to detect sniper activities in infrared spectra as well as analysis of physical limitations were performed. Cooled and uncooled detectors were considered. Three phases of sniper activities were taken into consideration: before, during and after the shot. On the basis of experimental data the parameters defining the target were determined which are essential in assessing the capability of infrared camera to detect sniper activity. A sniper body and muzzle flash were analyzed as targets. The simulation of detection ranges was done for the assumed scenario of sniper detection task. The infrared sniper detection system was discussed, capable of fulfilling the requirements. The discussion of the results of analysis and simulations was finally presented.

Nondestructive 3D confocal laser imaging with deconvolution of seven whole stardust tracks with complementary XRF and quantitative analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Greenberg, M.; Ebel, D.S.

2009-03-19

We present a nondestructive 3D system for analysis of whole Stardust tracks, using a combination of Laser Confocal Scanning Microscopy and synchrotron XRF. 3D deconvolution is used for optical corrections, and results of quantitative analyses of several tracks are presented. The Stardust mission to comet Wild 2 trapped many cometary and ISM particles in aerogel, leaving behind 'tracks' of melted silica aerogel on both sides of the collector. Collected particles and their tracks range in size from submicron to millimeter scale. Interstellar dust collected on the obverse of the aerogel collector is thought to have an average track length ofmore » {approx}15 {micro}m. It has been our goal to perform a total non-destructive 3D textural and XRF chemical analysis on both types of tracks. To that end, we use a combination of Laser Confocal Scanning Microscopy (LCSM) and X Ray Florescence (XRF) spectrometry. Utilized properly, the combination of 3D optical data and chemical data provides total nondestructive characterization of full tracks, prior to flattening or other destructive analysis methods. Our LCSM techniques allow imaging at 0.075 {micro}m/pixel, without the use of oil-based lenses. A full textural analysis on track No.82 is presented here as well as analysis of 6 additional tracks contained within 3 keystones (No.128, No.129 and No.140). We present a method of removing the axial distortion inherent in LCSM images, by means of a computational 3D Deconvolution algorithm, and present some preliminary experiments with computed point spread functions. The combination of 3D LCSM data and XRF data provides invaluable information, while preserving the integrity of the samples for further analysis. It is imperative that these samples, the first extraterrestrial solids returned since the Apollo era, be fully mapped nondestructively in 3D, to preserve the maximum amount of information prior to other, destructive analysis.« less

Detectability limit and uncertainty considerations for laser induced fluorescence spectroscopy in flames

NASA Technical Reports Server (NTRS)

Daily, J. W.

1978-01-01

Laser induced fluorescence spectroscopy of flames is discussed, and derived uncertainty relations are used to calculate detectability limits due to statistical errors. Interferences due to Rayleigh scattering from molecules as well as Mie scattering and incandescence from particles have been examined for their effect on detectability limits. Fluorescence trapping is studied, and some methods for reducing the effect are considered. Fluorescence trapping places an upper limit on the number density of the fluorescing species that can be measured without signal loss.

Detection limit of a VCO based detection chain dedicated to particles recognition and tracking

NASA Astrophysics Data System (ADS)

Coulié, K.; Rahajandraibe, W.; Aziza, H.; Micolau, G.; Vauché, R.

2018-01-01

A particle detection chain based on CMOS-SOI VCO circuit is presented. The solution is used for the recognition and the tracking of a given particle at circuit level. TCAD simulation of the detector has been performed on a 3×3 matrix of diodes based detector for particles recognition and tracking. The current response of the detector has been used for a case study in order to determine the ability of the chain to recognize an alpha particle crossing a 3×3 detection cell. The detection limit of the proposed solution is investigated and discussed in this paper.

Identification of New Lithic Clasts in Lunar Breccia 14305 by Micro-CT and Micro-XRF Analysis

NASA Technical Reports Server (NTRS)

Zeigler, Ryan A.; Carpenter, Paul K.; Jolliff, Bradley L.

2014-01-01

From 1969 to 1972, Apollo astronauts collected 382 kg of rocks, soils, and core samples from six locations on the surface of the Moon. The samples were initially characterized, largely by binocular examination, in a custom-built facility at Johnson Space Center (JSC), and the samples have been curated at JSC ever since. Despite over 40 years of study, demand for samples remains high (500 subsamples per year are allocated to scientists around the world), particularly for plutonic (e.g., anorthosites, norites, etc.) and evolved (e.g., granites, KREEP basalts) lithologies. The reason for the prolonged interest is that as new scientists and new techniques examine the samples, our understanding of how the Moon, Earth, and other inner Solar System bodies formed and evolved continues to grow. Scientists continually clamor for new samples to test their emerging hypotheses. Although all of the large Apollo samples that are igneous rocks have been classified, many Apollo samples are complex polymict breccias that have previously yielded large (cm-sized) igneous clasts. In this work we present the initial efforts to use the non-destructive techniques of micro-computed tomography (micro-CT) and micro x-ray fluorescence (micro-XRF) to identify large lithic clasts in Apollo 14 polymict breccia sample 14305. The sample in this study is 14305,483, a 150 g slab of regolith breccia 14305 measuring 10x6x2 cm (Figure 1a). The sample was scanned at the University of Texas High-Resolution X-ray CT Facility on an Xradia MicroXCT scanner. Two adjacent overlapping volumes were acquired at 49.2 micrometer resolution and stitched together, resulting in 1766 slices. Each volume was acquired at 100 kV accelerating voltage and 98 mA beam current with a 1 mm CaF2 filter, with 2161 views gathered over 360deg at 3 seconds acquisition time per view. Micro-XRF analyses were done at Washington University in St. Louis, Missouri on an EDAX Orbis PC micro-XRF instrument. Multiple scans were made at 40 k

The metamorphosis of supernova SN 2008D/XRF 080109: a link between supernovae and GRBs/hypernovae.

PubMed

Mazzali, Paolo A; Valenti, Stefano; Della Valle, Massimo; Chincarini, Guido; Sauer, Daniel N; Benetti, Stefano; Pian, Elena; Piran, Tsvi; D'Elia, Valerio; Elias-Rosa, Nancy; Margutti, Raffaella; Pasotti, Francesco; Antonelli, L Angelo; Bufano, Filomena; Campana, Sergio; Cappellaro, Enrico; Covino, Stefano; D'Avanzo, Paolo; Fiore, Fabrizio; Fugazza, Dino; Gilmozzi, Roberto; Hunter, Deborah; Maguire, Kate; Maiorano, Elisabetta; Marziani, Paola; Masetti, Nicola; Mirabel, Felix; Navasardyan, Hripsime; Nomoto, Ken'ichi; Palazzi, Eliana; Pastorello, Andrea; Panagia, Nino; Pellizza, L J; Sari, Re'em; Smartt, Stephen; Tagliaferri, Gianpiero; Tanaka, Masaomi; Taubenberger, Stefan; Tominaga, Nozomu; Trundle, Carrie; Turatto, Massimo

2008-08-29

The only supernovae (SNe) to show gamma-ray bursts (GRBs) or early x-ray emission thus far are overenergetic, broad-lined type Ic SNe (hypernovae, HNe). Recently, SN 2008D has shown several unusual features: (i) weak x-ray flash (XRF), (ii) an early, narrow optical peak, (iii) disappearance of the broad lines typical of SN Ic HNe, and (iv) development of helium lines as in SNe Ib. Detailed analysis shows that SN 2008D was not a normal supernova: Its explosion energy (E approximately 6x10(51) erg) and ejected mass [ approximately 7 times the mass of the Sun (M(middle dot in circle))] are intermediate between normal SNe Ibc and HNe. We conclude that SN 2008D was originally a approximately 30 M(middle dot in circle) star. When it collapsed, a black hole formed and a weak, mildly relativistic jet was produced, which caused the XRF. SN 2008D is probably among the weakest explosions that produce relativistic jets. Inner engine activity appears to be present whenever massive stars collapse to black holes.

A Review of the Handheld X-Ray Fluorescence Spectrometer as a Tool for Field Geologic Investigations on Earth and in Planetary Surface Exploration

NASA Technical Reports Server (NTRS)

Young, Kelsey E.; Evans, Cynthia A.; Hodges, Kip V.; Bleacher, Jacob E.; Graff, Trevor G.

2016-01-01

X-ray fluorescence (XRF) spectroscopy is a well-established and commonly used technique in obtaining diagnostic compositional data on geological samples. Recently, developments in X-ray tube and detector technologies have resulted in miniaturized, field-portable instruments that enable new applications both in and out of standard laboratory settings. These applications, however, have not been extensively applied to geologic field campaigns. This study investigates the feasibility of using developing handheld XRF (hXRF) technology to enhance terrestrial field geology, with potential applications in planetary surface exploration missions. We demonstrate that the hXRF is quite stable, providing reliable and accurate data continuously over a several year period. Additionally, sample preparation is proved to have a marked effect on the strategy for collecting and assimilating hXRF data. While the hXRF is capable of obtaining data that are comparable to laboratory XRF analysis for several geologically-important elements (such as Si, Ca, Ti, and K), the instrument is unable to detect other elements (such as Mg and Na) reliably. While this limits the use of the hXRF, especially when compared to laboratory XRF techniques, the hXRF is still capable of providing the field user with significantly improved contextual awareness of a field site, and more work is needed to fully evaluate the potential of this instrument in more complex geologic environments.

On the Determination of Uncertainty and Limit of Detection in Label-Free Biosensors.

PubMed

Lavín, Álvaro; Vicente, Jesús de; Holgado, Miguel; Laguna, María F; Casquel, Rafael; Santamaría, Beatriz; Maigler, María Victoria; Hernández, Ana L; Ramírez, Yolanda

2018-06-26

A significant amount of noteworthy articles reviewing different label-free biosensors are being published in the last years. Most of the times, the comparison among the different biosensors is limited by the procedure used of calculating the limit of detection and the measurement uncertainty. This article clarifies and establishes a simple procedure to determine the calibration function and the uncertainty of the concentration measured at any point of the measuring interval of a generic label-free biosensor. The value of the limit of detection arises naturally from this model as the limit at which uncertainty tends when the concentration tends to zero. The need to provide additional information, such as the measurement interval and its linearity, among others, on the analytical systems and biosensor in addition to the detection limit is pointed out. Finally, the model is applied to curves that are typically obtained in immunoassays and a discussion is made on the application validity of the model and its limitations.

Prediction of the limit of detection of an optical resonant reflection biosensor.

PubMed

Hong, Jongcheol; Kim, Kyung-Hyun; Shin, Jae-Heon; Huh, Chul; Sung, Gun Yong

2007-07-09

A prediction of the limit of detection of an optical resonant reflection biosensor is presented. An optical resonant reflection biosensor using a guided-mode resonance filter is one of the most promising label-free optical immunosensors due to a sharp reflectance peak and a high sensitivity to the changes of optical path length. We have simulated this type of biosensor using rigorous coupled wave theory to calculate the limit of detection of the thickness of the target protein layer. Theoretically, our biosensor has an estimated ability to detect thickness change approximately the size of typical antigen proteins. We have also investigated the effects of the absorption and divergence of the incident light on the detection ability of the biosensor.

Analytical possibilities of different X-ray fluorescence systems for determination of trace elements in aqueous samples pre-concentrated with carbon nanotubes

NASA Astrophysics Data System (ADS)

Marguí, E.; Zawisza, B.; Skorek, R.; Theato, T.; Queralt, I.; Hidalgo, M.; Sitko, R.

2013-10-01

This study was aimed to achieve improved instrumental sensitivity and detection limits for multielement determination of V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Se, Pb and Cd in liquid samples by using different X-ray fluorescence (XRF) configurations (a benchtop energy-dispersive X-ray fluorescence spectrometer, a benchtop polarised energy-dispersive X-ray fluorescence spectrometer and a wavelength-dispersive X-ray fluorescence spectrometer). The preconcentration of metals from liquid solutions consisted on a solid-phase extraction using carbon nanotubes (CNTs) as solid sorbents. After the extraction step, the aqueous sample was filtered and CNTs with the absorbed elements were collected onto a filter paper which was directly analyzed by XRF. The calculated detection limits in all cases were in the low ng mL- 1 range. Nevertheless, results obtained indicate the benefits, in terms of sensitivity, of using polarized X-ray sources using different secondary targets in comparison to conventional XRF systems, above all if Cd determination is required. The developed methodologies, using the aforementioned equipments, have been applied for multielement determination in water samples from an industrial area of Poland.

Synchrotron radiation based STXM analysis and micro-XRF mapping of differential expression of extracellular thiol groups by Acidithiobacillus ferrooxidans grown on Fe(2+) and S(0).

PubMed

Xia, Jin-Lan; Liu, Hong-Chang; Nie, Zhen-Yuan; Peng, An-An; Zhen, Xiang-Jun; Yang, Yun; Zhang, Xiu-Li

2013-09-01

The differential expression of extracellular thiol groups by Acidithiobacillus ferrooxidans grown on substrates Fe(2+) and S(0) was investigated by using synchrotron radiation based scanning transmission X-ray microscopy (STXM) imaging and microbeam X-ray fluorescence (μ-XRF) mapping. The extracellular thiol groups (SH) were first alkylated by iodoacetic acid forming Protein-SCH2COOH and then the P-SCH2COOH was marked by calcium ions forming P-SCH2COOCa. The STXM imaging and μ-XRF mapping of SH were based on analysis of SCH2COO-bonded Ca(2+). The results indicated that the thiol group content of A. ferrooxidans grown on S(0) is 3.88 times to that on Fe(2+). Combined with selective labeling of SH by Ca(2+), the STXM imaging and μ-XRF mapping provided an in situ and rapid analysis of differential expression of extracellular thiol groups. © 2013.

Nonparametric rank regression for analyzing water quality concentration data with multiple detection limits.

PubMed

Fu, Liya; Wang, You-Gan

2011-02-15

Environmental data usually include measurements, such as water quality data, which fall below detection limits, because of limitations of the instruments or of certain analytical methods used. The fact that some responses are not detected needs to be properly taken into account in statistical analysis of such data. However, it is well-known that it is challenging to analyze a data set with detection limits, and we often have to rely on the traditional parametric methods or simple imputation methods. Distributional assumptions can lead to biased inference and justification of distributions is often not possible when the data are correlated and there is a large proportion of data below detection limits. The extent of bias is usually unknown. To draw valid conclusions and hence provide useful advice for environmental management authorities, it is essential to develop and apply an appropriate statistical methodology. This paper proposes rank-based procedures for analyzing non-normally distributed data collected at different sites over a period of time in the presence of multiple detection limits. To take account of temporal correlations within each site, we propose an optimal linear combination of estimating functions and apply the induced smoothing method to reduce the computational burden. Finally, we apply the proposed method to the water quality data collected at Susquehanna River Basin in United States of America, which clearly demonstrates the advantages of the rank regression models.

Innovative instrumentation for mineralogical and elemental analyses of solid extraterrestrial surfaces: The Backscatter Moessbauer Spectrometer/X Ray Fluorescence analyzer (BaMS/XRF)

NASA Technical Reports Server (NTRS)

Shelfer, T. D.; Morris, Richard V.; Nguyen, T.; Agresti, D. G.; Wills, E. L.

1994-01-01

We have developed a four-detector research-grade backscatter Moessbauer spectrometer (BaMS) instrument with low resolution x-ray fluorescence analysis (XRF) capability. A flight-qualified instrument based on this design would be suitable for use on missions to the surfaces of solid solar-system objects (Moon, Mars, asteroids, etc.). Target specifications for the flight instrument are as follows: mass less than 500 g; volumes less than 300 cu cm; and power less than 2 W. The BaMS/XRF instrument would provide data on the oxidation state of iron and its distribution among iron-bearing mineralogies and elemental composition information. This data is a primary concern for the characterization of extraterrestrial surface materials.

LIMITATIONS ON THE USES OF MULTIMEDIA EXPOSURE MEASUREMENTS FOR MULTIPATHWAY EXPOSURE ASSESSMENT - PART I: HANDLING OBSERVATIONS BELOW DETECTION LIMITS

EPA Science Inventory

Multimedia data from two probability-based exposure studies were investigated in terms of how censoring of non-detects affected estimation of population parameters and associations. Appropriate methods for handling censored below-detection-limit (BDL) values in this context were...

Electroadsorption-assisted direct determination of trace arsenic without interference using transmission X-ray fluorescence spectroscopy.

PubMed

Jiang, Tian-Jia; Guo, Zheng; Liu, Jin-Huai; Huang, Xing-Jiu

2015-08-18

An analytical technique based on electroadsorption and transmission X-ray fluorescence (XRF) for the quantitative determination of arsenic in aqueous solution with ppb-level limits of detection (LOD) is proposed. The approach uses electroadsorption to enhance the sensitivity and LOD of the arsenic XRF response. Amine-functionalized carbonaceous microspheres (NH2-CMSs) are found to be the ideal materials for both the quantitative adsorption of arsenic and XRF analysis due to the basic amine sites on the surface and their noninterference in the XRF spectrum. In electroadsorptive X-ray fluorescence (EA-XRF), arsenic is preconcentrated by a conventional three-electrode system with a positive electricity field around the adsorbents. Then, the quantification of arsenic on the adsorbents is achieved using XRF. The electroadsorption preconcentration can realize the fast transfer of arsenic from the solution to the adsorbents and improve the LOD of conventional XRF compared with directly determining arsenic solution by XRF alone. The sensitivity of 0.09 cnt ppb(-1) is obtained without the interferences from coexisted metal ions in the determination of arsenic, and the LOD is found to be 7 ppb, which is lower than the arsenic guideline value of 10 ppb given by the World Health Organization (WHO). These results demonstrated that XRF coupled with electroadsorption was able to determine trace arsenic in real water sample.

Cyclostratigraphic analysis of the Middle to lower Upper Ordovician Postolonnec Formation in the Armorican Massif (France): integrating pXRF, gammay-ray and lithological data

NASA Astrophysics Data System (ADS)

Sinnesael, Matthias; Loi, Alfredo; Dabard, Marie-Pierre; Vandenbroucke, Thijs; Claeys, Philippe

2017-04-01

The Middle to lower Upper Ordovician sections of the Crozon Peninsula area (Postolonnec Formation, Armorican Massif, western France) show multi-order eustatic sea-level changes (Dabard et al., 2015). The sections are characterized by siliciclastic facies, which were deposited in tidal to storm-dominated shelf environments. Dabard et al. (2015) analysed the facies, their stacking patterns, and gamma-ray data and applied backstripping to identify subsidence and several orders of sea-level change. The main stratigraphic constraints are coming from (chitinozoan) biostratigraphy. The 3th to 5th orders changes are hypothesized to correspond to various frequencies related to astronomical forcing. This study investigates the potential added value of portable X-Ray Fluorescence (pXRF) and the application of spectral analyses. High-resolution (cm-scale) non-destructive pXRF and natural gamma-ray measurements were carried out on 14 m of section that was equally logged on a cm resolution. The pXRF measurements on the surface of the outcrops are compared with earlier results of wavelength dispersive XRF spectrometry and ICP-MS. The potassium records of the pXRF and gamma-ray logs are comparable and essentially reflect lithological variations (i.e., between mudstone and coarse sandstones). Other reliably measured elements also reflected lithological aspects such as clay-sandstone alternations (e.g. K, Rb, Ti), placer locations (Zr, Ce, Ti) and potentially clay mineralogy and condensation horizons (Ni, Zn, Co, Mn). Spectral analyses of the various proxies (lithology, natural gamma-ray and pXRF) are compared with each other. Both the new high-resolution data (14 m of section) as well as the published low-resolution data (which span almost 400 m of Darriwilian-Sandbian) were analyzed. The study reveals strong indications for the imprint of obliquity, precession and eccentricity. Obtaining age constraints, in addition to the existing biostratigraphical framework is a challenge in

Long term fine aerosol analysis by XRF and PIXE techniques in the city of Rijeka, Croatia

NASA Astrophysics Data System (ADS)

Ivošević, Tatjana; Orlić, Ivica; Radović, Iva Bogdanović

2015-11-01

The results of a long term, multi elemental XRF and PIXE analysis of fine aerosol pollution in the city of Rijeka, Croatia, are reported for the first time. The samples were collected during a seven months period (6th Aug 2013-28th Feb 2014) on thin stretched Teflon filters and analyzed by energy dispersive X-ray fluorescence (EDXRF) at the Laboratory for Elemental Micro-Analysis (LEMA), University of Rijeka and by Particle Induced X-ray Emission (PIXE) using 1.6 MeV protons at the Laboratory for Ion Beam Interactions (LIBI), Ruđer Bošković Institute, Zagreb. The newly developed micro-XRF system at LEMA provided results for 19 elements in the range from Si to Pb. The PIXE at the LIBI provided information for the same elements as well for the light elements such as Na, Mg and Al. Black carbon was determined with the Laser Integrated Plate Method (LIPM). The results were statistically evaluated by means of the positive matrix factorization (PMF). The seven major pollution sources were identified together with their relative contributions, these are: secondary sulfates, road traffic, smoke, road dust, sea spray, ship emissions and soil dust.

Non-destructive geochemical analysis and element mapping using bench-top μ-XRF: applications and uses for geoscience problems

NASA Astrophysics Data System (ADS)

Flude, Stephanie; Haschke, Michael; Tagle, Roald; Storey, Michael

2013-04-01

X-Ray Fluorescence (XRF) has long been used to provide valuable geochemical analysis of bulk rock samples in geological studies. However, it is a destructive technique, requiring samples to be homogenised by grinding to a fine powder and formed into a compacted pellet, or fused glass disk and the resulting sample has to be completely flat for reliable analysis. Until recently, non-destructive, high spatial resolution µ- XRF analysis was possible only at specialised Synchrotron radiation facilities, where high excitation beam energies are possible and specialised X-ray focussing optical systems are available. Recently, a number of bench-top µ-XRF systems have become available, allowing easy, rapid and non-destructive geochemical analysis of various materials. We present a number of examples of how the new bench-top M4 Tornado µ-XRF system, developed by Bruker Nano, can be used to provide valuable geochemical information on geological samples. Both quantitative and qualitative (in the form of X-Ray area-maps) data can be quickly and easily acquired for a wide range of elements (as light as Na, using a vacuum), with minimal sample preparation, using an X-Ray spot size as low as 25 µm. Large specimens up to 30 cm and 5 kg in weight can be analysed due to the large sample chamber, allowing non-destructive characterisation of rare or valuable materials. This technique is particularly useful in characterising heterogeneous samples, such as drill cores, sedimentary and pyroclastic rocks containing a variety of clasts, lavas sourced from mixed and mingled magmas, mineralised samples and fossils. An obvious application is the ability to produce element maps or line-scans of minerals, allowing zoning of major and trace elements to be identified and thus informing on crystallisation histories. An application of particular interest to 40Ar/39Ar geochronologists is the ability to screen and assess the purity of mineral separates, or to characterise polished slabs for

Measurements of Strontium Levels in Human Bone In Vivo Using Portable X-ray Fluorescence (XRF).

PubMed

Specht, Aaron J; Mostafaei, Farshad; Lin, Yanfen; Xu, Jian; Nie, Linda H

2017-08-01

Measurement of bone strontium (Sr) is vital to determining the effectiveness of Sr supplementation, which is commonly used for the treatment of osteoporosis. Previous technology uses radioisotope sources and bulky equipment to measure bone Sr. This study demonstrates the effectiveness of portable X-ray fluorescence (XRF) for bone Sr measurement and validates it using data from a population of 238 children. We identified correlations between bone Sr and age in our participants.

A comparison of portable XRF and ICP-OES analysis for lead on air filter samples from a lead ore concentrator mill and a lead-acid battery recycler.

PubMed

Harper, Martin; Pacolay, Bruce; Hintz, Patrick; Andrew, Michael E

2006-03-01

, which encompassed the permissible exposure limit of 150 mg m(-3) enforced in the USA by the Mine Safety and Health Administration (MSHA). Linear regression on the results from most samplers gave almost 1 ratio 1 correlations without additional correction, indicating an absence of matrix effects from the presence of iron and zinc in the samples. An approximately 10% negative bias was found for the slope of the Button sampler regression, in line with other studies, but it did not significantly affect the accuracy as all XRF results from this sampler were within 20% of the corresponding ICP values. As in previous studies, the best results were obtained with the GSP sampler using the average of three readings, with all XRF results within 20% of the corresponding ICP values and a slope close to 1 (0.99). Greater than 95% of XRF results were within 20% of the corresponding ICP values for the closed-face 37 mm cassette using the OSHA algorithm, and the IOM sampler using a sample area of 3.46 cm2. As in previous studies, considerable material was found on the interior walls of all samplers that possess an internal surface for deposition, at approximately the same proportion for all samplers. At the lead-acid battery recycler all five samplers in their optimal configurations gave good correlations (r2 > 0.92) between the two analytical methods over the entire range of found lead mass, which included the permissible exposure limit enforced in the USA by the Occupational Safety and Health Administration (OSHA). Linear regression on the results from most samplers gave almost 1 ratio 1 correlations (except for the Button sampler), indicating an absence of matrix effects from the presence of the smaller quantities of the other metals in the samples. A negative bias was found for the slope of the button sampler regression, in line with other studies. Even though very high concentrations of lead were encountered (up to almost 6 mg m(-3)) no saturation of the detector was observed. Most

Trace element profiles in modern horse molar enamel as tracers of seasonality: Evidence from micro-XRF, LA-ICP-MS and stable isotope analysis

NASA Astrophysics Data System (ADS)

de Winter, Niels; Goderis, Steven; van Malderen, Stijn; Vanhaecke, Frank; Claeys, Philippe

2016-04-01

A combination of laboratory micro-X-ray Fluorescence (μXRF) and stable carbon and oxygen isotope analysis shows that trace element profiles from modern horse molars reveal a seasonal pattern that co-varies with seasonality in the oxygen isotope records of enamel carbonate from the same teeth. A combination of six cheek teeth (premolars and molars) from the same individual yields a seasonal isotope and trace element record of approximately three years recorded during the growth of the molars. This record shows that reproducible measurements of various trace element ratios (e.g., Sr/Ca, Zn/Ca, Fe/Ca, K/Ca and S/Ca) lag the seasonal pattern in oxygen isotope records by 2-3 months. Laser Ablation-ICP-Mass Spectrometry (LA-ICP-MS) analysis on a cross-section of the first molar of the same individual is compared to the bench-top tube-excitation μXRF results to test the robustness of the measurements and to compare both methods. Furthermore, trace element (e.g. Sr, Zn, Mg & Ba) profiles perpendicular to the growth direction of the same tooth, as well as profiles parallel to the growth direction are measured with LA-ICP-MS and μXRF to study the internal distribution of trace element ratios in two dimensions. Results of this extensive complementary line-scanning procedure shows the robustness of state of the art laboratory micro-XRF scanning for the measurement of trace elements in bioapatite. The comparison highlights the advantages and disadvantages of both methods for trace element analysis and illustrates their complementarity. Results of internal variation within the teeth shed light on the origins of trace elements in mammal teeth and their potential use for paleo-environmental reconstruction.

Using Instruments as Applied Science, Multipurpose Tools During Human Exploration: An XRD/XRF Demonstration Strategy for the Deep Space Gateway

NASA Astrophysics Data System (ADS)

Bleacher, J. E.; Gendreau, K.; Arzoumanian, Z.; Young, K. E.; McAdam, A.

2018-02-01

Science instruments to be used during human exploration should be designed to serve as multipurpose tools that are of use throughout a mission. Here we discuss a multipurpose tool approach to using contact XRD/XRF onboard the Deep Space Gateway.

An adaptive confidence limit for periodic non-steady conditions fault detection

NASA Astrophysics Data System (ADS)

Wang, Tianzhen; Wu, Hao; Ni, Mengqi; Zhang, Milu; Dong, Jingjing; Benbouzid, Mohamed El Hachemi; Hu, Xiong

2016-05-01

System monitoring has become a major concern in batch process due to the fact that failure rate in non-steady conditions is much higher than in steady ones. A series of approaches based on PCA have already solved problems such as data dimensionality reduction, multivariable decorrelation, and processing non-changing signal. However, if the data follows non-Gaussian distribution or the variables contain some signal changes, the above approaches are not applicable. To deal with these concerns and to enhance performance in multiperiod data processing, this paper proposes a fault detection method using adaptive confidence limit (ACL) in periodic non-steady conditions. The proposed ACL method achieves four main enhancements: Longitudinal-Standardization could convert non-Gaussian sampling data to Gaussian ones; the multiperiod PCA algorithm could reduce dimensionality, remove correlation, and improve the monitoring accuracy; the adaptive confidence limit could detect faults under non-steady conditions; the fault sections determination procedure could select the appropriate parameter of the adaptive confidence limit. The achieved result analysis clearly shows that the proposed ACL method is superior to other fault detection approaches under periodic non-steady conditions.

Gold nanoparticle-based low limit of detection Love wave biosensor for carcinoembryonic antigens.

PubMed

Li, Shuangming; Wan, Ying; Su, Yan; Fan, Chunhai; Bhethanabotla, Venkat R

2017-09-15

In this work, a Love wave biosensing platform is described for detecting cancer-related biomarker carcinoembryonic antigen (CEA). An ST 90°-X quartz Love wave device with a layer of SiO 2 waveguide was combined with gold nanoparticles (Au NPs) to amplify the mass loading effect of the acoustic wave sensor to achieve a limit of detection of 37pg/mL. The strategy involves modifying the Au NPs with anti-CEA antibody conjugates to form nanoprobes in a sandwich immunoassay. The unamplified detection limit of the Love wave biosensor is 9.4ng/mL. This 2-3 order of magnitude reduction in the limit of detection brings the SAW platform into the range useful for clinical diagnosis. Measurement electronics and microfluidics are easily constructed for acoustic wave biosensors, such as the Love wave device described here, allowing for robust platforms for point of care applications for cancer biomarkers in general. Copyright © 2017 Elsevier B.V. All rights reserved.

Strategies and limitations for fluorescence detection of XAFS at high flux beamlines

DOE PAGES

Heald, Steve M.

2015-02-17

The issue of detecting the XAFS signal from dilute samples is discussed in detail with the aim of making best use of high flux beamlines that provide up to 10 13 photons -1. Various detection methods are compared, including filters with slits, solid state detectors, crystal analyzers and combinations of these. These comparisons rely on simulations that use experimentally determined parameters. It is found that inelastic scattering places a fundamental limit on detection, and that it is important to take proper account of the polarization dependence of the signals. The combination of a filter–slit system with a solid state detectormore » is a promising approach. With an optimized system good performance can be obtained even if the total count rate is limited to 10 7 Hz. Detection schemes with better energy resolution can help at the largest dilutions if their collection efficiency and count rate limits can be improved.« less

Strategies and limitations for fluorescence detection of XAFS at high flux beamlines

PubMed Central

Heald, Steve M.

2015-01-01

The issue of detecting the XAFS signal from dilute samples is discussed in detail with the aim of making best use of high flux beamlines that provide up to 1013 photons s−1. Various detection methods are compared, including filters with slits, solid state detectors, crystal analyzers and combinations of these. These comparisons rely on simulations that use experimentally determined parameters. It is found that inelastic scattering places a fundamental limit on detection, and that it is important to take proper account of the polarization dependence of the signals. The combination of a filter–slit system with a solid state detector is a promising approach. With an optimized system good performance can be obtained even if the total count rate is limited to 107 Hz. Detection schemes with better energy resolution can help at the largest dilutions if their collection efficiency and count rate limits can be improved. PMID:25723945

Limit of detection of 15{sub N} by gas-chromatography atomic emission detection: Optimization using an experimental design

DOE Office of Scientific and Technical Information (OSTI.GOV)

Deruaz, D.; Bannier, A.; Pionchon, C.

1995-08-01

This paper deals with the optimal conditions for the detection of {sup 15}N determined using a four-factor experimental design from [2{sup 13}C,-1,3 {sup 15}N] caffeine measured with an atomic emission detector (AED) coupled to gas chromatography (GC). Owing to the capability of a photodiodes array, AED can simultaneously detect several elements using their specific emission lines within a wavelength range of 50 nm. So, the emissions of {sup 15}N and {sup 14}N are simultaneously detected at 420.17 nm and 421.46 nm respectively. Four independent experimental factors were tested (1) helium flow rate (plasma gas); (2) methane pressure (reactant gas); (3)more » oxygen pressure; (4) hydrogen pressure. It has been shown that these four gases had a significant influence on the analytical response of {sup 15}N. The linearity of the detection was determined using {sup 15}N amounts ranging from 1.52 pg to 19 ng under the optimal conditions obtained from the experimental design. The limit of detection was studied using different methods. The limits of detection of {sup 15}N was 1.9 pg/s according to the IUPAC method (International-Union of Pure and Applied Chemistry). The method proposed by Quimby and Sullivan gave a value of 2.3 pg/s and that of Oppenheimer gave a limit of 29 pg/s. For each determination, and internal standard: 1-isobutyl-3.7 dimethylxanthine was used. The results clearly demonstrate that GC AED is sensitive and selective enough to detect and measure {sup 15}N-labelled molecules after gas chromatographic separation.« less

Method for improving the limit of detection in a data signal

DOEpatents

Synovec, Robert E.; Yueng, Edward S.

1989-10-17

A method for improving the limit of detection for a data set in which experimental noise is uncorrelated along a given abscissa and an analytical signal is correlated to the abscissa, the steps comprising collecting the data set, converting the data set into a data signal including an analytical portion and the experimental noise portion, designating and adjusting a baseline of the data signal to center the experimental noise numerically about a zero reference, and integrating the data signal preserving the corresponding information for each point of the data signal. The steps of the method produce an enhanced integrated data signal which improves the limit of detection of the data signal.

Étude comparative des techniques d'analyse par fluorescence X à dispersion d'énergie (ED-XRF) et à dispersion de longueur d'onde (WD-XRF), et par spectrométrie d'émission atomique à source plasma couplée par induction (ICP-AES)

NASA Astrophysics Data System (ADS)

Rahmani, A.; Benyaïch, F.; Bounakhla, M.; Bilal, E.; Moutte, J.; Gruffat, J. J.; Zahry, F.

2004-11-01

Dans ce travail, nous présentons une étude comparative des techniques d'analyse par fluorescence X à dispersion d'énergie (ED-XRF) et à dispersion de longueur d'onde (WD-XRF), et par spectrométrie d'émission atomique à source plasma couplée par induction (ICP-AES). Les résultats de la calibration des spectromètres à dispersion d'énergie, à excitation par sources radioactives (55Fe, 109Cd et 241Am) et à excitation secondaire (cible secondaire Mo et Cu) du Centre National pour l'Energie, les Sciences et les Techniques Nucléaires (CNESTEN, Rabat, Maroc) sur des échantillons étalons de références de l'Agence International de l'Energie Atomique (AIEA) et du Community Bureau of Référence (BCR) ont été comparés aux résultats d'analyse des mêmes échantillons étalons par la spectrométrie X à dispersion de longueur d'onde (WD-XRF) et par spectrométrie d'émission atomique à source plasma couplé par induction (ICP-AES) au département GENERIC du centre SPIN à l'Ecole des Mines de Saint-Etienne (France). Les trois techniques d'analyse utilisées donnent des résultats comparables pour le dosage des éléments majeurs, alors que pour les traces on note des déviations importantes à cause des effets de matrice qui sont difficiles à corriger dans le cas de la fluorescence X.

METHODS OF DEALING WITH VALUES BELOW THE LIMIT OF DETECTION USING SAS

EPA Science Inventory

Due to limitations of chemical analysis procedures, small concentrations cannot be precisely measured. These concentrations are said to be below the limit of detection (LOD). In statistical analyses, these values are often censored and substituted with a constant value, such ...

Method for improving the limit of detection in a data signal

DOEpatents

Synovec, R.E.; Yueng, E.S.

1989-10-17

Disclosed is a method for improving the limit of detection for a data set in which experimental noise is uncorrelated along a given abscissa and an analytical signal is correlated to the abscissa, the steps comprising collecting the data set, converting the data set into a data signal including an analytical portion and the experimental noise portion, designating and adjusting a baseline of the data signal to center the experimental noise numerically about a zero reference, and integrating the data signal preserving the corresponding information for each point of the data signal. The steps of the method produce an enhanced integrated data signal which improves the limit of detection of the data signal. 8 figs.

Signal detection evidence for limited capacity in visual search

PubMed Central

Fencsik, David E.; Flusberg, Stephen J.; Horowitz, Todd S.; Wolfe, Jeremy M.

2014-01-01

The nature of capacity limits (if any) in visual search has been a topic of controversy for decades. In 30 years of work, researchers have attempted to distinguish between two broad classes of visual search models. Attention-limited models have proposed two stages of perceptual processing: an unlimited-capacity preattentive stage, and a limited-capacity selective attention stage. Conversely, noise-limited models have proposed a single, unlimited-capacity perceptual processing stage, with decision processes influenced only by stochastic noise. Here, we use signal detection methods to test a strong prediction of attention-limited models. In standard attention-limited models, performance of some searches (feature searches) should only be limited by a preattentive stage. Other search tasks (e.g., spatial configuration search for a “2” among “5”s) should be additionally limited by an attentional bottleneck. We equated average accuracies for a feature and a spatial configuration search over set sizes of 1–8 for briefly presented stimuli. The strong prediction of attention-limited models is that, given overall equivalence in performance, accuracy should be better on the spatial configuration search than on the feature search for set size 1, and worse for set size 8. We confirm this crossover interaction and show that it is problematic for at least one class of one-stage decision models. PMID:21901574

XRF Core Scanning of Igneous Rocks: a Case Study of IODP Expeditions 367/368 Lava Flows, South China Sea

NASA Astrophysics Data System (ADS)

Höfig, T. W.; LeVay, B.; Stock, J. M.; Sun, Z.; Klaus, A.; Jian, Z.; Larsen, H. C.; Alvarez Zarikian, C. A.

2017-12-01

For three decades, X-ray fluorescence core scanning (XRF-CS) has been widely applied to split sediment cores to obtain continuous data sets of element intensities, serving as chemical proxies for paleoceanography and paleoclimate studies. In contrast, there is no record published on igneous rock cores. This study utilizes a remarkably consistent recovery of lava flows from the South China Sea (SCS), intersected during International Ocean Discovery Program (IODP) Expeditions 367/368, to gain preliminary insights into the chemical inventory of a volcanic suite. At IODP Site U1500, a drilled interval of 150 m, starting at 1379.1 meters below seafloor, yielded 115 m of intercalated fine-grained massive, sheet, and pillow lava flows of basaltic modal composition, consisting of aphyric to highly plagioclase-phyric rocks. The pillow lavas feature numerous well-preserved chilled and glassy margins. The whole succession of lavas is overall slightly to moderately altered and notably fresh in parts. The present XRF data, obtained from a third-generation energy dispersive Avaatech® core scanner at a step size of 2 cm, suggest the existence of two chemically distinct lava suites. The bottom six lava flows (in total 40 m thick) show low intensities of both Cr and Ti (e.g., Ti: 7000-8500 counts), while the upper 11 flows reflect higher concentrations of Cr and Ti (e.g., Ti: 8200-9500 counts). A massive flow, which marks the chemical transition, represents the top of the low-Cr and -Ti lava suite. The compositional change from low-Cr-Ti to high-Cr-Ti lavas reflects a clear temporal magmatic evolution of this submarine SCS volcanism, which is characterized by generally constant Fe/Mn ratios. Thus, this trend may be explained by a change to less fractionated and/or less contaminated lavas over time. On a smaller scale, the XRF-CS also enabled mapping of the compositional variations of crosscutting veins with depth as well as the transition from glassy margins to the micro- to

Naturally occurring levels of elements in fishes as determined by PIXE and XRF methods

NASA Astrophysics Data System (ADS)

Tallandini, L.; Giacobini, F.; Turchetto, M.; Galassini, S.; Liu, Q. X.; Shao, H. R.; Moschini, G.; Moro, R.; Gialanella, G.; Ghermandi, G.; Cecchi, R.; Injuk, J.; Valković, V.

1989-04-01

Naturally occurring levels of S, Cl, K, Ca, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Br, Sb, Sr and Pb were measured in the gills, liver and muscles of fishes ( Zosterisessor ophiocephalus Pall) in the northwestern region of the Adriatic Sea. The overall performance of PIXE and XRF methods was tested by the analysis of standard reference materials. The mean concentration values for elements were calculated from the distribution of experimentally determined concentration values. The obtained data are discussed in the framework of metal metabolism and toxicology.

Pigment analysis by Raman microscopy and portable X-ray fluorescence (pXRF) of thirteenth to fourteenth century illuminations and cuttings from Bologna

PubMed Central

Clark, Robin J. H.; Jones, Richard; Gibbs, Robert

2016-01-01

Non-destructive pigment analysis by Raman microscopy (RM) and portable X-ray fluorescence (pXRF) has been carried out on some Bolognese illuminations and cuttings chosen to represent the beginnings, evolution and height of Bolognese illuminated manuscript production. Dating to the thirteenth and fourteenth centuries and held in a private collection, the study provides evidence for the pigments generally used in this period. The results, which are compared with those obtained for other north Italian artwork, show the developments in usage of artistic materials and technique. Also addressed in this study is an examination of the respective roles of RM and pXRF analysis in this area of technical art history. This article is part of the themed issue ‘Raman spectroscopy in art and archaeology’. PMID:27799427

Temporary implementation and testing of a confocal SR- μXRF system for bone analysis at the X-ray Fluorescence beamline at Elettra

NASA Astrophysics Data System (ADS)

Perneczky, L.; Rauwolf, M.; Ingerle, D.; Eichert, D.; Brigidi, F.; Jark, W.; Bjeoumikhova, S.; Pepponi, G.; Wobrauschek, P.; Streli, C.; Turyanskaya, A.

2018-07-01

The confocal μXRF spectrometer of Atominstitut (ATI) was transported and set up at the X-ray Fluorescence beamline at Elettra - Sincrotrone Trieste. It was successfully adjusted to the incoming beam (9.2 keV). Test measurements on a free-standing Cu wire were performed to determine the size of the focused micro-beam (non-confocal mode, 56 × 35 μm2) and the size of the confocal volume (confocal mode, 41 × 24 × 34 μm2) for the Cu-K α emission. In order to test the setup's capabilities, two areas on different human bone samples were measured in confocal scanning mode. For one of the samples the comparison with a previous μ XRF measurement, obtained with a low power X-ray tube in the lab, is presented.

Re-evaluation of groundwater monitoring data for glyphosate and bentazone by taking detection limits into account.

PubMed

Hansen, Claus Toni; Ritz, Christian; Gerhard, Daniel; Jensen, Jens Erik; Streibig, Jens Carl

2015-12-01

Current regulatory assessment of pesticide contamination of Danish groundwater is exclusively based on samples with pesticide concentrations above detection limit. Here we demonstrate that a realistic quantification of pesticide contamination requires the inclusion of "non-detect" samples i.e. samples with concentrations below the detection limit, as left-censored observations. The median calculated pesticide concentrations are shown to be reduced 10(4) to 10(5) fold for two representative herbicides (glyphosate and bentazone) relative to the median concentrations based upon observations above detection limits alone. Copyright © 2015 Elsevier B.V. All rights reserved.

METHODS OF DEALING WITH VALUES BELOW THE LIMIT OF DETECTION USING SAS

EPA Science Inventory

Due to limitations of chemical analysis procedures, small values cannot be precisely measured. These values are said to be below the limit of detection (LOD). In statistical analyses, these values are often censored and substituted with a constant value, such as half the LOD,...

Identification of green pigments from fragments of Roman mural paintings of three Roman sites from north of Germania Superior

NASA Astrophysics Data System (ADS)

Debastiani, Rafaela; Simon, Rolf; Goettlicher, Joerg; Heissler, Stefan; Steininger, Ralph; Batchelor, David; Fiederle, Michael; Baumbach, Tilo

2016-10-01

Roman mural green pigment painting fragments from three Roman sites in the north of the Roman province Germania Superior: Koblenz Stadtwald Remstecken (KOSR), Weißenthurm " Am guten Mann" (WEIS) and Mendig Lungenkärchen (MELU), dating from second and third centuries AD were analyzed. The experiments were performed nondestructively using synchrotron-based scanning macro-X-ray fluorescence (SR-MA-XRF), synchrotron-based scanning micro-X-ray fluorescence (SR-μ-XRF), synchrotron-based X-ray diffraction (SR-XRD) and Raman spectroscopy. Correlation between SR-MA-XRF, SR-μ-XRF elemental map distributions and optical images of scanned areas was mainly found for the elements Ca, Fe and K. With XRF, Fe and K were identified correlated with green pigment, but in samples from two sites, Mendig Lungenkärchen and Weißenthurm " Am guten Mann", also Cu was detected in minor concentration. The results of SR-XRD and Raman spectroscopy were limited to one sample from Weißenthurm " Am guten Mann". In this sample, green earth and calcium carbonate were identified by SR-XRD and, additionally, malachite by Raman spectroscopy.

Global limits and interference patterns in dark matter direct detection

DOE Office of Scientific and Technical Information (OSTI.GOV)

Catena, Riccardo; Gondolo, Paolo

2015-08-13

We compare the general effective theory of one-body dark matter nucleon interactions to current direct detection experiments in a global multidimensional statistical analysis. We derive exclusion limits on the 28 isoscalar and isovector coupling constants of the theory, and show that current data place interesting constraints on dark matter-nucleon interaction operators usually neglected in this context. We characterize the interference patterns that can arise in dark matter direct detection from pairs of dark matter-nucleon interaction operators, or from isoscalar and isovector components of the same operator. We find that commonly neglected destructive interference effects weaken standard direct detection exclusion limitsmore » by up to one order of magnitude in the coupling constants.« less

Global limits and interference patterns in dark matter direct detection

DOE Office of Scientific and Technical Information (OSTI.GOV)

Catena, Riccardo; Gondolo, Paolo, E-mail: riccardo.catena@theorie.physik.uni-goettingen.de, E-mail: paolo.gondolo@utah.edu

2015-08-01

We compare the general effective theory of one-body dark matter nucleon interactions to current direct detection experiments in a global multidimensional statistical analysis. We derive exclusion limits on the 28 isoscalar and isovector coupling constants of the theory, and show that current data place interesting constraints on dark matter-nucleon interaction operators usually neglected in this context. We characterize the interference patterns that can arise in dark matter direct detection from pairs of dark matter-nucleon interaction operators, or from isoscalar and isovector components of the same operator. We find that commonly neglected destructive interference effects weaken standard direct detection exclusion limitsmore » by up to one order of magnitude in the coupling constants.« less

Tin accumulation in spermatozoa of the rats exposed to tributyltin chloride by synchrotron radiation X-ray fluorescence (SR-XRF) analysis with microprobe

NASA Astrophysics Data System (ADS)

Homma-Takeda, S.; Nishimura, Y.; Terada, Y.; Ueno, S.; Watanabe, Y.; Yukawa, M.

2005-04-01

Organotin compounds are widely used in industry and its environmental contamination by these compounds has recently become a concern. It is known that they act as endocrine disruptors but details of the dynamics of Sn in reproductive organs are still unknown. In the present study, we attempted to determine Sn distribution in the testis of rats exposed to tributyltin chloride (TBTC) by inductively coupled argon plasma-mass spectrometry (ICP-MS) for microdissectioned seminiferous tubules and cell-selective metal determination of synchrotron radiation X-ray florescence (SR-XRF) analysis. TBTC was orally administered to rats at a dose of 45 μmol/kg per day for 3 days. One day later, Sn was detected in the microdissectioned seminiferous tubules at a level approximately equivalent to that in the testis. Significant stage-specificity of Sn accumulation was not observed in the experimental model. Sn was also detected in spermatozoa at the stage VIII seminiferous tubule, which are the final step of spermatogenesis in the testis. These data indicate that Sn accumulates in germ cells as well as in spermatozoa in a short period of TBTC exposure.

pXRF analyses of Louise Herreshoff's paintings in relation to CdS and other pigment degradation issues

NASA Astrophysics Data System (ADS)

Uffelman, Erich S.; Hobbs, Patricia A.; Barisas, Derek A. G.; Mass, Jennifer L.

2013-04-01

Portable X-ray Fluorescence Spectrometry (pXRF) was used to survey 33 works in Washington and Lee University's collection of Louise Herreshoff's paintings. This work was done both to support a condition assessment of the paintings and their pigments and to determine which paintings might be appropriate for further study in the context of ongoing key synchrotron research into the degradation mechanisms of cadmium sulfide yellow pigment (CdS).

Immuno-analysis of microparticles: probing at the limits of detection

PubMed Central

Latham, Sharissa L.; Tiberti, Natalia; Gokoolparsadh, Naveena; Holdaway, Karen; Olivier Couraud, Pierre; Grau, Georges E. R.; Combes, Valery

2015-01-01

Microparticle (MP) research is clouded by debate regarding the accuracy and validity of flow cytometry (FCM) as an analytical methodology, as it is influenced by many variables including the pre-analytical conditions, instruments physical capabilities and detection parameters. This study utilises a simplistic in vitro system for generating MP, and through comparative analysis with immuno-electron microscopy (Immuno-EM) assesses the strengths and limitations of probe selection and high-sensitivity FCM. Of the markers examined, MP were most specifically labelled with phosphatidylserine ligands, annexin V and lactadherin, although only ~60% MP are PS positive. Whilst these two ligands detect comparable absolute MP numbers, they interact with the same population in distinct manners; annexin V binding is enhanced on TNF induced MP. CD105 and CD54 expression were, as expected, consistent and enhanced following TNF activation respectively. Their labelling however accounted for as few as 30–40% of MP. The greatest discrepancies between FCM and I-EM were observed in the population solely labelled for the surface antigen. These findings demonstrate that despite significant improvements in resolution, high-sensitivity FCM remains limited in detecting small-size MP expressing low antigen levels. This study highlights factors to consider when selecting endothelial MP probes, as well as interpreting and representing data. PMID:26553743

Elemental classification of the tusks of dugong (Dugong dugong) by HH-XRF analysis and comparison with other species

NASA Astrophysics Data System (ADS)

Nganvongpanit, Korakot; Buddhachat, Kittisak; Piboon, Promporn; Euppayo, Thippaporn; Kaewmong, Patcharaporn; Cherdsukjai, Phaothep; Kittiwatanawong, Kongkiat; Thitaram, Chatchote

2017-04-01

The elemental composition was investigated and applied for identifying the sex and habitat of dugongs, in addition to distinguishing dugong tusks and teeth from other animal wildlife materials such as Asian elephant (Elephas maximus) tusks and tiger (Panthera tigris tigris) canine teeth. A total of 43 dugong tusks, 60 dugong teeth, 40 dolphin teeth, 1 whale tooth, 40 Asian elephant tusks and 20 tiger canine teeth were included in the study. Elemental analyses were conducted using a handheld X-ray fluorescence analyzer (HH-XRF). There was no significant difference in the elemental composition of male and female dugong tusks, whereas the overall accuracy for identifying habitat (the Andaman Sea and the Gulf of Thailand) was high (88.1%). Dolphin teeth were able to be correctly predicted 100% of the time. Furthermore, we demonstrated a discrepancy in elemental composition among dugong tusks, Asian elephant tusks and tiger canine teeth, and provided a high correct prediction rate among these species of 98.2%. Here, we demonstrate the feasible use of HH-XRF for preliminary species classification and habitat determination prior to using more advanced techniques such as molecular biology.

Targeted analyte detection by standard addition improves detection limits in matrix-assisted laser desorption/ionization mass spectrometry.

PubMed

Toghi Eshghi, Shadi; Li, Xingde; Zhang, Hui

2012-09-18

Matrix-assisted laser desorption/ionization (MALDI) has proven an effective tool for fast and accurate determination of many molecules. However, the detector sensitivity and chemical noise compromise the detection of many invaluable low-abundance molecules from biological and clinical samples. To challenge this limitation, we developed a targeted analyte detection (TAD) technique. In TAD, the target analyte is selectively elevated by spiking a known amount of that analyte into the sample, thereby raising its concentration above the noise level, where we take advantage of the improved sensitivity to detect the presence of the endogenous analyte in the sample. We assessed TAD on three peptides in simple and complex background solutions with various exogenous analyte concentrations in two MALDI matrices. TAD successfully improved the limit of detection (LOD) of target analytes when the target peptides were added to the sample in a concentration close to optimum concentration. The optimum exogenous concentration was estimated through a quantitative method to be approximately equal to the original LOD for each target. Also, we showed that TAD could achieve LOD improvements on an average of 3-fold in a simple and 2-fold in a complex sample. TAD provides a straightforward assay to improve the LOD of generic target analytes without the need for costly hardware modifications.

100-OL-1 Operable Unit Pilot Study: XRF Evaluation of Select Pre-Hanford Orchards

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bunn, Amoret L.; Fritz, Brad G.; Pulsipher, Brent A.

Prior to the acquisition of land by the U.S. Department of War in February 1943 and the creation of the Hanford Site, the land along the Columbia River was home to over 1000 people. Farming and orchard operations by both homesteaders and commercial organizations were prevalent. Orchard activities and the associated application of lead arsenate pesticide ceased in 1943, when residents were moved from the Hanford Site at the beginning of the Manhattan Project. Today, the residues from historical application of lead arsenate pesticide persist in some locations on the Hanford Site. In 2012, the U.S. Department of Energy, U.S.more » Environmental Protection Agency, and Washington State Department of Ecology established the 100-OL-1 Operable Unit (OU) through the Hanford Federal Facility Agreement and Consent Order, known as the Tri-Party Agreement. The pre-Hanford orchard lands identified as the 100-OL-1 OU are located south of the Columbia River and east of the present-day Vernita Bridge, and extend southeast to the former Hanford townsite. The discontinuous orchard lands within 100-OL-1 OU are approximately 20 km2 (5000 ac). A pilot study was conducted to support the approval of the remedial investigation/feasibility study work plan to evaluate the 100-OL-1 OU. This pilot study evaluated the use of a field portable X-ray fluorescence (XRF) analyzer for evaluating lead and arsenic concentrations on the soil surface as an indicator of lead arsenate pesticide residues in the OU. The objectives of the pilot study included evaluating a field portable XRF analyzer as the analytical method for decision making, estimating the nature and extent of lead and arsenic in surface soils in four decision units, evaluating the results for the purpose of optimizing the sampling approach implemented in the remedial investigation, and collecting information to improve the cost estimate and planning the cultural resources review for sampling activities in the remedial investigation

Detection limit for rate fluctuations in inhomogeneous Poisson processes

NASA Astrophysics Data System (ADS)

Shintani, Toshiaki; Shinomoto, Shigeru

2012-04-01

Estimations of an underlying rate from data points are inevitably disturbed by the irregular occurrence of events. Proper estimation methods are designed to avoid overfitting by discounting the irregular occurrence of data, and to determine a constant rate from irregular data derived from a constant probability distribution. However, it can occur that rapid or small fluctuations in the underlying density are undetectable when the data are sparse. For an estimation method, the maximum degree of undetectable rate fluctuations is uniquely determined as a phase transition, when considering an infinitely long series of events drawn from a fluctuating density. In this study, we analytically examine an optimized histogram and a Bayesian rate estimator with respect to their detectability of rate fluctuation, and determine whether their detectable-undetectable phase transition points are given by an identical formula defining a degree of fluctuation in an underlying rate. In addition, we numerically examine the variational Bayes hidden Markov model in its detectability of rate fluctuation, and determine whether the numerically obtained transition point is comparable to those of the other two methods. Such consistency among these three principled methods suggests the presence of a theoretical limit for detecting rate fluctuations.

Detection limit for rate fluctuations in inhomogeneous Poisson processes.

PubMed

Shintani, Toshiaki; Shinomoto, Shigeru

2012-04-01

Estimations of an underlying rate from data points are inevitably disturbed by the irregular occurrence of events. Proper estimation methods are designed to avoid overfitting by discounting the irregular occurrence of data, and to determine a constant rate from irregular data derived from a constant probability distribution. However, it can occur that rapid or small fluctuations in the underlying density are undetectable when the data are sparse. For an estimation method, the maximum degree of undetectable rate fluctuations is uniquely determined as a phase transition, when considering an infinitely long series of events drawn from a fluctuating density. In this study, we analytically examine an optimized histogram and a Bayesian rate estimator with respect to their detectability of rate fluctuation, and determine whether their detectable-undetectable phase transition points are given by an identical formula defining a degree of fluctuation in an underlying rate. In addition, we numerically examine the variational Bayes hidden Markov model in its detectability of rate fluctuation, and determine whether the numerically obtained transition point is comparable to those of the other two methods. Such consistency among these three principled methods suggests the presence of a theoretical limit for detecting rate fluctuations.

Gold Provenance Studies for Romanian Archaeological Objects Using Micro-SR-XRF

NASA Astrophysics Data System (ADS)

Vasilescu, Angela; Constantinescu, Bogdan; Bugoi, Roxana; Radtke, Martin; Reinholz, Uwe; Simon, Rolf

2010-04-01

Studies by Synchrotron Radiation—X-Ray Fluorescence (SR-XRF) for the search of the presence of trace elements like Sb, Sn, Te and Pb in archaeological metallic objects found on the territory of Romania—old coins and Bronze Age jewelry, aimed to determine the provenance of the gold used in their manufacture. The results are compared with the detailed elemental composition of alluvial or primary gold samples, obtained by the same technique. This work attempted to establish the origin of the gold used for the mint of two different types of koson coins. We found that the kosons with monogram are made of refined gold, while the one used for the kosons without monogram is mainly alluvial. The gold used in the manufacture of the Calarasi Vulchitrun-type disk and the Tauteu hair ring is also of alluvial origin.

Ultrafast scene detection and recognition with limited visual information

PubMed Central

Hagmann, Carl Erick; Potter, Mary C.

2016-01-01

Humans can detect target color pictures of scenes depicting concepts like picnic or harbor in sequences of six or twelve pictures presented as briefly as 13 ms, even when the target is named after the sequence (Potter, Wyble, Hagmann, & McCourt, 2014). Such rapid detection suggests that feedforward processing alone enabled detection without recurrent cortical feedback. There is debate about whether coarse, global, low spatial frequencies (LSFs) provide predictive information to high cortical levels through the rapid magnocellular (M) projection of the visual path, enabling top-down prediction of possible object identities. To test the “Fast M” hypothesis, we compared detection of a named target across five stimulus conditions: unaltered color, blurred color, grayscale, thresholded monochrome, and LSF pictures. The pictures were presented for 13–80 ms in six-picture rapid serial visual presentation (RSVP) sequences. Blurred, monochrome, and LSF pictures were detected less accurately than normal color or grayscale pictures. When the target was named before the sequence, all picture types except LSF resulted in above-chance detection at all durations. Crucially, when the name was given only after the sequence, performance dropped and the monochrome and LSF pictures (but not the blurred pictures) were at or near chance. Thus, without advance information, monochrome and LSF pictures were rarely understood. The results offer only limited support for the Fast M hypothesis, suggesting instead that feedforward processing is able to activate conceptual representations without complementary reentrant processing. PMID:28255263

The use of XRF core scanner technique to identify anthropogenic chronological markers for dating recent sediments and for mapping and estimating the quantity of contaminated sediments in different fjord settings in western Norway

NASA Astrophysics Data System (ADS)

Haflidason, H.; Thorsen, L.; Soldal, O. L.

2016-12-01

Following the initiation of the industrial revolution in Norway at the early 1900´s many of the heavy industrial factories established at that time were located in inner fjord systems of western Norway. The advantage was an easy access to cheap electricity, but the main disadvantage has been that the pollution from this industrial activity has been transported into fjord systems where the circulation of the water masses has been fairly limited leading to a high concentration of heavy metals in the fjord basin sediments. The recently developed non-destructive X-ray Fluorescence (XRF) core scanning technique offers new possibilities to obtain near-continuous records of bulk element composition in marine records. This new analytical geochemical method can measure the bulk element content directly from the surface sediment archives within a period of seconds and with a resolution up to 200 microns. By applying this method on rapidly deposited sediments one can reconstruct a continuous record of carbonate content on a sub-decadal to annual scale. This kind of high-resolution records can also be compared directly with historical and instrumental records from the same area. This offers new possibilities to identify in an effective way the geochemical anomalies in the sediment column and estimate the variability of the industrially produced elements as e.g. Cu, Zn and Pb and their distribution and thickness/quantity in fjord basin sediments. Examples will be presented demonstrating the close linkage between the industrial production history and the entrance of these elements in the fjord sediments. Identification of these elements offers an excellent opportunity to date the recent marine sediments using these elements as an event spike and also to reconstruct the history of pollution in these fjord basin sediments. As the precision of the XRF element detection is high the time of full recovery to natural conditions of the basin sediments, after close down of these

Confirmation of the E(sup src)(sub Peak)-E(sub iso) (Amati) relation from the x-ray flash XRF 050416A observed by the Swift burst alert telescope

NASA Technical Reports Server (NTRS)

Sakamoti, T.; Barbier, L.; Barthelmy, S. D.; Cummings, J. R.; Fenimore, E. E.; Gehrels, N.; Hullinger, D.; Krimm, H. A.; Markwardt, C. B.

2006-01-01

We report Swift Burst Alert Telescope (BAT) observations of the X-ray flash (XRF) XRF 050416A. The fluence ratio between the 15-25 and 25-50 keV energy bands of this event is 1.5, thus making it the softest gamma-ray burst (GRB) observed by BAT so far. The spectrum is well fitted by a Band function with E(sup obs)(sub peak) of 15.0(sup +2.3)(sub -2.7) keV. Assuming the redshift of the host galaxy (z = 0.6535), the isotropic equivalent radiated energy E(sub iso) and the peak energy at the GRB rest frame (E(sup src)(sub peak)) of XRF 050416A are not only consistent with the correlation found by Amati et al. and extended to XRFs by Sakamoto et al. but also fill in the gap of this relation around the 30-80 keV range of E(sup src)(sub peak). This result tightens the validity of the E(sup src)(sub Peak)-E(sup src)(sub peak) relation from XRFs to GRBs. We also find that the jet break time estimated using the empirical relation between E(sup src)(sub peak) and the collimation corrected energy E(sub gamma), is inconsistent with the afterglow observation by the Swift X-Ray Telescope. This could be due to the extra external shock emission overlaid around the jet break time or to the nonexistence of a jet break feature for XRFs, which might be a further challenge for GRB jet emission models and XRF/GRB unification scenarios.

Failure Detecting Method of Fault Current Limiter System with Rectifier

NASA Astrophysics Data System (ADS)

Tokuda, Noriaki; Matsubara, Yoshio; Asano, Masakuni; Ohkuma, Takeshi; Sato, Yoshibumi; Takahashi, Yoshihisa

A fault current limiter (FCL) is extensively needed to suppress fault current, particularly required for trunk power systems connecting high-voltage transmission lines, such as 500kV class power system which constitutes the nucleus of the electric power system. We proposed a new type FCL system (rectifier type FCL), consisting of solid-state diodes, DC reactor and bypass AC reactor, and demonstrated the excellent performances of this FCL by developing the small 6.6kV and 66kV model. It is important to detect the failure of power devices used in the rectifier under the normal operating condition, for keeping the excellent reliability of the power system. In this paper, we have proposed a new failure detecting method of power devices most suitable for the rectifier type FCL. This failure detecting system is simple and compact. We have adapted the proposed system to the 66kV prototype single-phase model and successfully demonstrated to detect the failure of power devices.

The detection limits of antimicrobial agents in cow's milk by a simple Yoghurt Culture Test.

PubMed

Mohsenzadeh, M; Bahrainipour, A

2008-09-15

The aim of this study was to study performance of Yoghurt Culture Test (YCT) in the detection of antimicrobial residues in milk. For this purpose, the sensitivity of YCT for 15 antibiotics were determined. For each drug, 8 concentrations were tested. The detection limits of YCT at 2.5 h and 4 h incubation were determined (microg kg(-1)): 15 and 37.5, penicillin G; 4 and 5, ampicillin; 5 and 7.5, amoxycillin; 100 and 200, cephalexin; 80 and 100, cefazoline; 100 and 200, oxytetracycline; 500 and 100, chlortetracycline; 100 and 200, tetracycline; 150 and 200, doxycycline; 200 and 400, sulphadimidine; 500 and 1000, gentamycin; 1000 and 1500, spectinomycin; 400 and 500, erythromycin; 50 and 100, tylosin; 5000 and 10000, chloramphenicol. The YCT detection limits at 2.5 h incubation for ampicillin, cephalexin, tetracycline, oxytetracycline and tylosin are similar to those obtained as Maximum Residue Limit (MRL) according to Regulation 2377/90 EEC as set out by the European Union. In addition the detection limits of YCT for some antibiotics were lower than some of microbial inhibitor test.

Theoretical modeling of a portable x-ray tube based KXRF system to measure lead in bone.

PubMed

Specht, Aaron J; Weisskopf, Marc G; Nie, Linda Huiling

2017-03-01

K-shell x-ray fluorescence (KXRF) techniques have been used to identify health effects resulting from exposure to metals for decades, but the equipment is bulky and requires significant maintenance and licensing procedures. A portable x-ray fluorescence (XRF) device was developed to overcome these disadvantages, but introduced a measurement dependency on soft tissue thickness. With recent advances to detector technology, an XRF device utilizing the advantages of both systems should be feasible. In this study, we used Monte Carlo simulations to test the feasibility of an XRF device with a high-energy x-ray tube and detector operable at room temperature. We first validated the use of Monte Carlo N-particle transport code (MCNP) for x-ray tube simulations, and found good agreement between experimental and simulated results. Then, we optimized x-ray tube settings and found the detection limit of the high-energy x-ray tube based XRF device for bone lead measurements to be 6.91 µg g -1 bone mineral using a cadmium zinc telluride detector. In conclusion, this study validated the use of MCNP in simulations of x-ray tube physics and XRF applications, and demonstrated the feasibility of a high-energy x-ray tube based XRF for metal exposure assessment.

Theoretical modeling of a portable x-ray tube based KXRF system to measure lead in bone

PubMed Central

Specht, Aaron J; Weisskopf, Marc G; Nie, Linda Huiling

2017-01-01

Objective K-shell x-ray fluorescence (KXRF) techniques have been used to identify health effects resulting from exposure to metals for decades, but the equipment is bulky and requires significant maintenance and licensing procedures. A portable x-ray fluorescence (XRF) device was developed to overcome these disadvantages, but introduced a measurement dependency on soft tissue thickness. With recent advances to detector technology, an XRF device utilizing the advantages of both systems should be feasible. Approach In this study, we used Monte Carlo simulations to test the feasibility of an XRF device with a high-energy x-ray tube and detector operable at room temperature. Main Results We first validated the use of Monte Carlo N-particle transport code (MCNP) for x-ray tube simulations, and found good agreement between experimental and simulated results. Then, we optimized x-ray tube settings and found the detection limit of the high-energy x-ray tube based XRF device for bone lead measurements to be 6.91 μg g−1 bone mineral using a cadmium zinc telluride detector. Significance In conclusion, this study validated the use of MCNP in simulations of x-ray tube physics and XRF applications, and demonstrated the feasibility of a high-energy x-ray tube based XRF for metal exposure assessment. PMID:28169835

Attentional Capacity Limits Gap Detection during Concurrent Sound Segregation.

PubMed

Leung, Ada W S; Jolicoeur, Pierre; Alain, Claude

2015-11-01

Detecting a brief silent interval (i.e., a gap) is more difficult when listeners perceive two concurrent sounds rather than one in a sound containing a mistuned harmonic in otherwise in-tune harmonics. This impairment in gap detection may reflect the interaction of low-level encoding or the division of attention between two sound objects, both of which could interfere with signal detection. To distinguish between these two alternatives, we compared ERPs during active and passive listening with complex harmonic tones that could include a gap, a mistuned harmonic, both features, or neither. During active listening, participants indicated whether they heard a gap irrespective of mistuning. During passive listening, participants watched a subtitled muted movie of their choice while the same sounds were presented. Gap detection was impaired when the complex sounds included a mistuned harmonic that popped out as a separate object. The ERP analysis revealed an early gap-related activity that was little affected by mistuning during the active or passive listening condition. However, during active listening, there was a marked decrease in the late positive wave that was thought to index attention and response-related processes. These results suggest that the limitation in detecting the gap is related to attentional processing, possibly divided attention induced by the concurrent sound objects, rather than deficits in preattentional sensory encoding.

Combining markers with and without the limit of detection

PubMed Central

Dong, Ting; Liu, Catherine Chunling; Petricoin, Emanuel F.; Tang, Liansheng Larry

2014-01-01

In this paper, we consider the combination of markers with and without the limit of detection (LOD). LOD is often encountered when measuring proteomic markers. Because of the limited detecting ability of an equipment or instrument, it is difficult to measure markers at a relatively low level. Suppose that after some monotonic transformation, the marker values approximately follow multivariate normal distributions. We propose to estimate distribution parameters while taking the LOD into account, and then combine markers using the results from the linear discriminant analysis. Our simulation results show that the ROC curve parameter estimates generated from the proposed method are much closer to the truth than simply using the linear discriminant analysis to combine markers without considering the LOD. In addition, we propose a procedure to select and combine a subset of markers when many candidate markers are available. The procedure based on the correlation among markers is different from a common understanding that a subset of the most accurate markers should be selected for the combination. The simulation studies show that the accuracy of a combined marker can be largely impacted by the correlation of marker measurements. Our methods are applied to a protein pathway dataset to combine proteomic biomarkers to distinguish cancer patients from non-cancer patients. PMID:24132938

Field-portable-XRF reveals the ubiquity of antimony in plastic consumer products.

PubMed

Turner, Andrew; Filella, Montserrat

2017-04-15

Very little systematic information exists on the occurrence and concentrations of antimony (Sb) in consumer products. In this study, a Niton XL3t field-portable-X-ray fluorescence (FP-XRF) spectrometer was deployed in situ and in the laboratory to provide quantitative information on Sb dissipated in plastic items and fixtures (including rubber, textile and foamed materials) from the domestic, school, vehicular and office settings. The metalloid was detected in 18% of over 800 measurements performed, with concentrations ranging from about 60 to 60,000μgg -1 . The highest concentrations were encountered in white, electronic casings and in association with similar concentrations of Br, consistent with the use of antimony oxides (e.g. Sb 2 O 3 ) as synergistic flame retardants. Concentrations above 1000μgg -1 , and with or without Br, were also encountered in paints, piping and hosing, adhesives, whiteboards, Christmas decorations, Lego blocks, document carriers, garden furniture, upholstered products and interior panels of private motor vehicles. Lower concentrations of Sb were encountered in a wide variety of items but its presence (without Br) in food tray packaging, single-use drinks bottles, straws and small toys were of greatest concern from a human health perspective. While the latter observations are consistent with the use of antimony compounds as catalysts in the production of polyethylene terephthalate, co-association of Sb and Br in many products not requiring flame retardancy suggests that electronic casings are widely recycled. Further research is required into the mobility of Sb when dissipated in new, recycled and aged polymeric materials. Copyright © 2017 Elsevier B.V. All rights reserved.

XRF, μ-XRD and μ-spectroscopic techniques for revealing the composition and structure of paint layers on polychrome sculptures after multiple restorations.

PubMed

Franquelo, M L; Duran, A; Castaing, J; Arquillo, D; Perez-Rodriguez, J L

2012-01-30

This paper presents the novel application of recently developed analytical techniques to the study of paint layers on sculptures that have been restored/repainted several times across centuries. Analyses were performed using portable XRF, μ-XRD and μ-Raman instruments. Other techniques, such as optical microscopy, SEM-EDX and μ-FTIR, were also used. Pigments and other materials including vermilion, minium, red lac, ivory black, lead white, barium white, zinc white (zincite), titanium white (rutile and anatase), lithopone, gold and brass were detected. Pigments from both ancient and modern times were found due to the different restorations/repaintings carried out. μ-Raman was very useful to characterise some pigments that were difficult to determine by μ-XRD. In some cases, pigments identification was only possible by combining results from the different analytical techniques used in this work. This work is the first article devoted to the study of sculpture cross-section samples using laboratory-made μ-XRD systems. Copyright © 2011 Elsevier B.V. All rights reserved.

Detection limits for nanoparticles in solution with classical turbidity spectra

NASA Astrophysics Data System (ADS)

Le Blevennec, G.

2013-09-01

Detection of nanoparticles in solution is required to manage safety and environmental problems. Spectral transmission turbidity method has now been known for a long time. It is derived from the Mie Theory and can be applied to any number of spheres, randomly distributed and separated by large distance compared to wavelength. Here, we describe a method for determination of size, distribution and concentration of nanoparticles in solution using UV-Vis transmission measurements. The method combines Mie and Beer Lambert computation integrated in a best fit approximation. In a first step, a validation of the approach is completed on silver nanoparticles solution. Verification of results is realized with Transmission Electronic Microscopy measurements for size distribution and an Inductively Coupled Plasma Mass Spectrometry for concentration. In view of the good agreement obtained, a second step of work focuses on how to manage the concentration to be the most accurate on the size distribution. Those efficient conditions are determined by simple computation. As we are dealing with nanoparticles, one of the key points is to know what the size limits reachable are with that kind of approach based on classical electromagnetism. In taking into account the transmission spectrometer accuracy limit we determine for several types of materials, metals, dielectrics, semiconductors the particle size limit detectable by such a turbidity method. These surprising results are situated at the quantum physics frontier.

Thermal Infrared Spectral Band Detection Limits for Unidentified Surface Materials

NASA Technical Reports Server (NTRS)

Kirkland, Laurel E.; Herr, Kenneth C.; Salisbury, John W.

2001-01-01

Infrared emission spectra recorded by airborne or satellite spectrometers can be searched for spectral features to determine the composition of rocks on planetary surfaces. Surface materials are identified by detections of characteristic spectral bands. We show how to define whether to accept an observed spectral feature as a detection when the target material is unknown. We also use remotely sensed spectra measured by the Thermal Emission Spectrometer (TES) and the Spatially Enhanced Broadband Array Spectrograph System to illustrate the importance of instrument parameters and surface properties on band detection limits and how the variation in signal-to-noise ratio with wavelength affects the bands that are most detectable for a given instrument. The spectrometer's sampling interval, spectral resolution, signal-to-noise ratio as a function of wavelength, and the sample's surface properties influence whether the instrument can detect a spectral feature exhibited by a material. As an example, in the 6-13 micrometer wavelength region, massive carbonates exhibit two bands: a very strong, broad feature at approximately 6.5 micrometers and a less intense, sharper band at approximately 11.25 micrometers. Although the 6.5-micrometer band is stronger and broader in laboratory-measured spectra, the 11.25-micrometer band will cause a more detectable feature in TES spectra.

Man vs. Machine: A Junior-level Laboratory Exercise Comparing Human and Instrumental Detection Limits

ERIC Educational Resources Information Center

Elias, Ryan J.; Hopfer, Helene; Hofstaedter, Amanda N.; Hayes, John E.

2017-01-01

The human nose is a very sensitive detector and is able to detect potent aroma compounds down to low ng/L levels. These levels are often below detection limits of analytical instrumentation. The following laboratory exercise is designed to compare instrumental and human methods for the detection of volatile odor active compounds. Reference…

Evaluation of portable Raman spectroscopy and handheld X-ray fluorescence analysis (hXRF) for the direct analysis of glyptics

NASA Astrophysics Data System (ADS)

Lauwers, D.; Candeias, A.; Coccato, A.; Mirao, J.; Moens, L.; Vandenabeele, P.

2016-03-01

In archaeometry, the advantages of a combined use of Raman spectroscopy and X-ray fluorescence spectroscopy are extensively discussed for applications such as the analysis of paintings, manuscripts, pottery, etc. Here, we demonstrate for the first time the advantage of using both techniques for analysing glyptics. These engraved gemstones or glass materials were originally used as stamps, to identify the owner, for instance on letters, but also on wine vessels. For this research, a set of 64 glyptics (42 Roman glass specimens and 22 modern ones), belonging to the collection of the museum 'Quinta das Cruzes' in Funchal (Madeira, Portugal), was analysed with portable Raman spectroscopy and handheld X-ray fluorescence (hXRF). These techniques were also used to confirm the gemological identification of these precious objects and can give extra information about the glass composition. Raman spectroscopy identifies the molecular composition as well as on the crystalline phases present. On the other hand, hXRF results show that the antique Roman glass samples are characterised with low Pb and Sn levels and that the modern specimens can be discriminated in two groups: lead-based and non-lead-based ones.

Evaluation of portable Raman spectroscopy and handheld X-ray fluorescence analysis (hXRF) for the direct analysis of glyptics.

PubMed

Lauwers, D; Candeias, A; Coccato, A; Mirao, J; Moens, L; Vandenabeele, P

2016-03-15

In archaeometry, the advantages of a combined use of Raman spectroscopy and X-ray fluorescence spectroscopy are extensively discussed for applications such as the analysis of paintings, manuscripts, pottery, etc. Here, we demonstrate for the first time the advantage of using both techniques for analysing glyptics. These engraved gemstones or glass materials were originally used as stamps, to identify the owner, for instance on letters, but also on wine vessels. For this research, a set of 64 glyptics (42 Roman glass specimens and 22 modern ones), belonging to the collection of the museum 'Quinta das Cruzes' in Funchal (Madeira, Portugal), was analysed with portable Raman spectroscopy and handheld X-ray fluorescence (hXRF). These techniques were also used to confirm the gemological identification of these precious objects and can give extra information about the glass composition. Raman spectroscopy identifies the molecular composition as well as on the crystalline phases present. On the other hand, hXRF results show that the antique Roman glass samples are characterised with low Pb and Sn levels and that the modern specimens can be discriminated in two groups: lead-based and non-lead-based ones. Copyright © 2015 Elsevier B.V. All rights reserved.

Calculation of the detection limits for radionuclides identified in gamma-ray spectra based on post-processing peak analysis results.

PubMed

Korun, M; Vodenik, B; Zorko, B

2018-03-01

A new method for calculating the detection limits of gamma-ray spectrometry measurements is presented. The method is applicable for gamma-ray emitters, irrespective of the influences of the peaked background, the origin of the background and the overlap with other peaks. It offers the opportunity for multi-gamma-ray emitters to calculate the common detection limit, corresponding to more peaks. The detection limit is calculated by approximating the dependence of the uncertainty in the indication on its value with a second-order polynomial. In this approach the relation between the input quantities and the detection limit are described by an explicit expression and can be easy investigated. The detection limit is calculated from the data usually provided by the reports of peak-analyzing programs: the peak areas and their uncertainties. As a result, the need to use individual channel contents for calculating the detection limit is bypassed. Copyright © 2017 Elsevier Ltd. All rights reserved.

Gold Provenance Studies for Romanian Archaeological Objects Using Micro-SR-XRF

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vasilescu, Angela; Constantinescu, Bogdan; Bugoi, Roxana

2010-04-06

Studies by Synchrotron Radiation--X-Ray Fluorescence (SR-XRF) for the search of the presence of trace elements like Sb, Sn, Te and Pb in archaeological metallic objects found on the territory of Romania--old coins and Bronze Age jewelry, aimed to determine the provenance of the gold used in their manufacture. The results are compared with the detailed elemental composition of alluvial or primary gold samples, obtained by the same technique. This work attempted to establish the origin of the gold used for the mint of two different types of koson coins. We found that the kosons with monogram are made of refinedmore » gold, while the one used for the kosons without monogram is mainly alluvial. The gold used in the manufacture of the Calarasi Vulchitrun-type disk and the Tauteu hair ring is also of alluvial origin.« less

Determination of target detection limits in hyperspectral data using band selection and dimensionality reduction

NASA Astrophysics Data System (ADS)

Gross, W.; Boehler, J.; Twizer, K.; Kedem, B.; Lenz, A.; Kneubuehler, M.; Wellig, P.; Oechslin, R.; Schilling, H.; Rotman, S.; Middelmann, W.

2016-10-01

Hyperspectral remote sensing data can be used for civil and military applications to robustly detect and classify target objects. High spectral resolution of hyperspectral data can compensate for the comparatively low spatial resolution, which allows for detection and classification of small targets, even below image resolution. Hyperspectral data sets are prone to considerable spectral redundancy, affecting and limiting data processing and algorithm performance. As a consequence, data reduction strategies become increasingly important, especially in view of near-real-time data analysis. The goal of this paper is to analyze different strategies for hyperspectral band selection algorithms and their effect on subpixel classification for different target and background materials. Airborne hyperspectral data is used in combination with linear target simulation procedures to create a representative amount of target-to-background ratios for evaluation of detection limits. Data from two different airborne hyperspectral sensors, AISA Eagle and Hawk, are used to evaluate transferability of band selection when using different sensors. The same target objects were recorded to compare the calculated detection limits. To determine subpixel classification results, pure pixels from the target materials are extracted and used to simulate mixed pixels with selected background materials. Target signatures are linearly combined with different background materials in varying ratios. The commonly used classification algorithms Adaptive Coherence Estimator (ACE) is used to compare the detection limit for the original data with several band selection and data reduction strategies. The evaluation of the classification results is done by assuming a fixed false alarm ratio and calculating the mean target-to-background ratio of correctly detected pixels. The results allow drawing conclusions about specific band combinations for certain target and background combinations. Additionally

Process monitoring and control with CHEMIN, a miniaturized CCD-based instrument for simultaneous XRD/XRF analysis

NASA Astrophysics Data System (ADS)

Vaniman, David T.; Bish, D.; Guthrie, G.; Chipera, S.; Blake, David E.; Collins, S. Andy; Elliott, S. T.; Sarrazin, P.

1999-10-01

There is a large variety of mining and manufacturing operations where process monitoring and control can benefit from on-site analysis of both chemical and mineralogic constituents. CHEMIN is a CCD-based instrument capable of both X-ray fluorescence (XRF; chemical) and X-ray diffraction (XRD; mineralogic) analysis. Monitoring and control with an instrument like CHEMIN can be applied to feedstocks, intermediate materials, and final products to optimize production. Examples include control of cement feedstock, of ore for smelting, and of minerals that pose inhalation hazards in the workplace. The combined XRD/XRF capability of CHEMIN can be used wherever a desired commodity is associated with unwanted constituents that may be similar in chemistry or structure but not both (e.g., Ca in both gypsum and feldspar, where only the gypsum is desired to make wallboard). In the mining industry, CHEMIN can determine mineral abundances on the spot and enable more economical mining by providing the means to assay when is being mined, quickly and frequently, at minimal cost. In manufacturing, CHEMIN could be used to spot-check the chemical composition and crystalline makeup of a product at any stage of production. Analysis by CHEMIN can be used as feedback in manufacturing processes where rates of heating, process temperature, mixture of feedstocks, and other variables must be adjusted in real time to correct structure and/or chemistry of the product (e.g., prevention of periclase and alkali sulfate coproduction in cement manufacture).

Comparison of field portable measurements of ultrafine TiO2: X-ray fluorescence, laser-induced breakdown spectroscopy, and Fourier-transform infrared spectroscopy.

PubMed

LeBouf, Ryan F; Miller, Arthur L; Stipe, Christopher; Brown, Jonathan; Murphy, Nate; Stefaniak, Aleksandr B

2013-06-01

Laboratory measurements of ultrafine titanium dioxide (TiO2) particulate matter loaded on filters were made using three field portable methods (X-ray fluorescence (XRF), laser-induced breakdown spectroscopy (LIBS), and Fourier-transform infrared (FTIR) spectroscopy) to assess their potential for determining end-of-shift exposure. Ultrafine TiO2 particles were aerosolized and collected onto 37 mm polycarbonate track-etched (PCTE) filters in the range of 3 to 578 μg titanium (Ti). Limit of detection (LOD), limit of quantification (LOQ), and calibration fit were determined for each measurement method. The LOD's were 11.8, 0.032, and 108 μg Ti per filter, for XRF, LIBS, and FTIR, respectively and the LOQ's were 39.2, 0.11, and 361 μg Ti per filter, respectively. The XRF calibration curve was linear over the widest dynamic range, up to the maximum loading tested (578 μg Ti per filter). LIBS was more sensitive but, due to the sample preparation method, the highest loaded filter measurable was 252 μg Ti per filter. XRF and LIBS had good predictability measured by regressing the predicted mass to the gravimetric mass on the filter. XRF and LIBS produced overestimations of 4% and 2%, respectively, with coefficients of determination (R(2)) of 0.995 and 0.998. FTIR measurements were less dependable due to interference from the PCTE filter media and overestimated mass by 2% with an R(2) of 0.831.

In vitro bioassays for detecting dioxin-like activity--application potentials and limits of detection, a review.

PubMed

Eichbaum, Kathrin; Brinkmann, Markus; Buchinger, Sebastian; Reifferscheid, Georg; Hecker, Markus; Giesy, John P; Engwall, Magnus; van Bavel, Bert; Hollert, Henner

2014-07-15

Use of in vitro assays as screening tool to characterize contamination of a variety of environmental matrices has become an increasingly popular and powerful toolbox in the field of environmental toxicology. While bioassays cannot entirely substitute analytical methods such as gas chromatography-mass spectrometry (GC-MS), the increasing improvement of cell lines and standardization of bioassay procedures enhance their utility as bioanalytical pre-screening tests prior to more targeted chemical analytical investigations. Dioxin-receptor-based assays provide a holistic characterization of exposure to dioxin-like compounds (DLCs) by integrating their overall toxic potential, including potentials of unknown DLCs not detectable via e.g. GC-MS. Hence, they provide important additional information with respect to environmental risk assessment of DLCs. This review summarizes different in vitro bioassay applications for detection of DLCs and considers the comparability of bioassay and chemical analytically derived toxicity equivalents (TEQs) of different approaches and various matrices. These range from complex samples such as sediments through single reference to compound mixtures. A summary of bioassay derived detection limits (LODs) showed a number of current bioassays to be equally sensitive as chemical methodologies, but moreover revealed that most of the bioanalytical studies conducted to date did not report their LODs, which represents a limitation with regard to low potency samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Predictive inference for best linear combination of biomarkers subject to limits of detection.

PubMed

Coolen-Maturi, Tahani

2017-08-15

Measuring the accuracy of diagnostic tests is crucial in many application areas including medicine, machine learning and credit scoring. The receiver operating characteristic (ROC) curve is a useful tool to assess the ability of a diagnostic test to discriminate between two classes or groups. In practice, multiple diagnostic tests or biomarkers are combined to improve diagnostic accuracy. Often, biomarker measurements are undetectable either below or above the so-called limits of detection (LoD). In this paper, nonparametric predictive inference (NPI) for best linear combination of two or more biomarkers subject to limits of detection is presented. NPI is a frequentist statistical method that is explicitly aimed at using few modelling assumptions, enabled through the use of lower and upper probabilities to quantify uncertainty. The NPI lower and upper bounds for the ROC curve subject to limits of detection are derived, where the objective function to maximize is the area under the ROC curve. In addition, the paper discusses the effect of restriction on the linear combination's coefficients on the analysis. Examples are provided to illustrate the proposed method. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

The feasibility of in vivo detection of lanthanum using a 241Am K x-ray fluorescence system.

PubMed

Nguyen, Joanna; Keldani, Zaid; Da Silva, Eric; Pejović-Milić, Ana; Gräfe, James L

2017-08-21

Lanthanum (La) is commonly used in phosphate binders in the form of lanthanum carbonate in patients with end-stage kidney disease undergoing hemodialysis treatments. With this administration, there is the potential for La storage in the body with bone being the main site of concern. However, the long-term effects of residual La in the body on bone health are not yet known. In this work, we investigate the feasibility of using a K x-ray fluorescence (K-XRF) spectroscopy system to measure bone La in vivo. A series of hydroxyapatite (HAp) bone mineral phantoms were created to represent human bone. A 1.09 GBq 241 Am source was used to excite the HAp phantoms doped with various known concentrations of La placed in a 90° geometry relative to the photon source and high-purity germanium (HPGe) detector. For a detector live time of 2000 s, the minimum detection limit was calculated to be 1.7 µg La g -1 Ca or 0.7 µg La g -1 HAp and is comparable to previously reported in vivo bone La concentrations. The technique developed in this study shows promising results and provides an alternative method to invasive biopsy sampling techniques to monitor the accumulation of bone La. To the best of our knowledge, this is the first reported work that seeks to non-invasively measure bone La via in vivo XRF.

Synchrotron-based ν-XRF mapping and μ-FTIR microscopy enable to look into the fate and effects of tattoo pigments in human skin.

PubMed

Schreiver, Ines; Hesse, Bernhard; Seim, Christian; Castillo-Michel, Hiram; Villanova, Julie; Laux, Peter; Dreiack, Nadine; Penning, Randolf; Tucoulou, Remi; Cotte, Marine; Luch, Andreas

2017-09-12

The increasing prevalence of tattoos provoked safety concerns with respect to particle distribution and effects inside the human body. We used skin and lymphatic tissues from human corpses to address local biokinetics by means of synchrotron X-ray fluorescence (XRF) techniques at both the micro (μ) and nano (ν) scale. Additional advanced mass spectrometry-based methodology enabled to demonstrate simultaneous transport of organic pigments, heavy metals and titanium dioxide from skin to regional lymph nodes. Among these compounds, organic pigments displayed the broadest size range with smallest species preferentially reaching the lymph nodes. Using synchrotron μ-FTIR analysis we were also able to detect ultrastructural changes of the tissue adjacent to tattoo particles through altered amide I α-helix to β-sheet protein ratios and elevated lipid contents. Altogether we report strong evidence for both migration and long-term deposition of toxic elements and tattoo pigments as well as for conformational alterations of biomolecules that likely contribute to cutaneous inflammation and other adversities upon tattooing.

40 CFR Appendix B to Part 136 - Definition and Procedure for the Determination of the Method Detection Limit-Revision 1.11

Code of Federal Regulations, 2010 CFR

2010-07-01

... calculated method detection limit. To insure that the estimate of the method detection limit is a good...) where: MDL = the method detection limit t(n-1,1- α=.99) = the students' t value appropriate for a 99... Determination of the Method Detection Limit-Revision 1.11 B Appendix B to Part 136 Protection of Environment...

2D-3D μXRF elemental mapping of archeological samples

NASA Astrophysics Data System (ADS)

Hampai, D.; Liedl, A.; Cappuccio, G.; Capitolo, E.; Iannarelli, M.; Massussi, M.; Tucci, S.; Sardella, R.; Sciancalepore, A.; Polese, C.; Dabagov, S. B.

2017-07-01

Recently opened for users at LNF XLab-Frascati a μ XRF station, named "Rainbow X-ray" - RXR, has been optimized for most of X-ray analytical research fields. The basic principle of the station is in the use of various geometrical combinations of polycapillary optics for X-ray beam shaping (focusing/collimation) at specially designed laboratory unit. In this work we have presented the results of archaeological studies on the artifacts of Paleolithic period and Iron Age (9th century BC to the midway of the 8th BC). The elemental analysis of these artifacts has been first performed by compact laboratory setup. Superficial (2D) and bulk (3D) micro-fluorescence mapping provides useful informations for the geologists in order to identify the possible artifacts provenience and origin. The results presented in this work are a part of wider anthropological/archeological investigations aimed at the understanding of social and economical relations of prehistorical communities.

µ-XRF Studies on the Colour Brilliance in Ancient Wool Carpets

PubMed Central

Meyer, Markus; Borca, Camelia N.; Huthwelker, Thomas; Bieber, Manfred; Meßlinger, Karl; Fink, Rainer H.

2017-01-01

Many handmade ancient and recent oriental wool carpets show outstanding brilliance and persistence of colour that is not achieved by common industrial dyeing procedures. Anthropologists have suggested the influence of wool fermentation prior to dyeing as key technique to achieve the high dyeing quality. By means of μ-XRF elemental mapping of mordant metals we corroborate this view and show a deep and homogenous penetration of colourants into fermented wool fibres. Furthermore we are able to apply this technique and prove that the fermentation process for ancient specimens cannot be investigated by standard methods due to the lack of intact cuticle layers. This finding suggests a broad range of further investigations that will contribute to a deeper understanding of the development of traditional dyeing techniques. Spectroscopic studies add information on the oxidation states of the metal ions within the respective mordant-dye-complexes and suggest a partial charge transfer as basis for a significant colour change when Fe mordants are used. PMID:29109824

Radiometric Short-Term Fourier Transform analysis of photonic Doppler velocimetry recordings and detectivity limit

NASA Astrophysics Data System (ADS)

Prudhomme, G.; Berthe, L.; Bénier, J.; Bozier, O.; Mercier, P.

2017-01-01

Photonic Doppler Velocimetry is a plug-and-play and versatile diagnostic used in dynamic physic experiments to measure velocities. When signals are analyzed using a Short-Time Fourier Transform, multiple velocities can be distinguished: for example, the velocities of moving particle-cloud appear on spectrograms. In order to estimate the back-scattering fluxes of target, we propose an original approach "PDV Radiometric analysis" resulting in an expression of time-velocity spectrograms coded in power units. Experiments involving micron-sized particles raise the issue of detection limit; particle-size limit is very difficult to evaluate. From the quantification of noise sources, we derive an estimation of the spectrogram noise leading to a detectivity limit, which may be compared to the fraction of the incoming power which has been back-scattered by the particle and then collected by the probe. This fraction increases with their size. At last, some results from laser-shock accelerated particles using two different PDV systems are compared: it shows the improvement of detectivity with respect to the Effective Number of Bits (ENOB) of the digitizer.

Iron pentacarbonyl detection limits in the cigarette smoke matrix using FT-IR spectroscopy

NASA Astrophysics Data System (ADS)

Parrish, Milton E.; Plunkett, Susan E.; Harward, Charles N.

2005-11-01

Endogenous metals present in tobacco from agricultural practices have been purported to generate metal carbonyls in cigarette smoke. Transition metal catalysts, such as iron oxide, have been investigated for the reduction of carbon monoxide (CO) in cigarette smoke. These studies motivated the development of an analytical method to determine if iron pentacarbonyl [Fe(CO) 5] is present in mainstream smoke from cigarette models having cigarette paper made with iron oxide. An FT-IR puff-by-puff method was developed and the detection limit was determined using two primary reference spectra from different sources to estimate the amount of Fe(CO) 5 present in a high-pressure steel cylinder of CO. We do not detect Fe(CO) 5 in a single 35 mL puff from reference cigarettes or from those cigarette models having cigarette paper made with iron oxide, with a 30-ppbV limit of detection (LOD). Also, it was shown that a filter containing activated carbon would remove Fe(CO) 5.

Energy-dispersive X-ray fluorescence systems as analytical tool for assessment of contaminated soils.

PubMed

Vanhoof, Chris; Corthouts, Valère; Tirez, Kristof

2004-04-01

To determine the heavy metal content in soil samples at contaminated locations, a static and time consuming procedure is used in most cases. Soil samples are collected and analyzed in the laboratory at high quality and high analytical costs. The demand by government and consultants for a more dynamic approach and by customers requiring performances in which analyses are performed in the field with immediate feedback of the analytical results, is growing. Especially during the follow-up of remediation projects or during the determination of the sampling strategy, field analyses are advisable. For this purpose four types of ED-XRF systems, ranging from portable up to high performance laboratory systems, have been evaluated. The evaluation criteria are based on the performance characteristics for all the ED-XRF systems such as limit of detection, accuracy and the measurement uncertainty on one hand, and also the influence of the sample pretreatment on the obtained results on the other hand. The study proved that the field portable system and the bench top system, placed in a mobile van, can be applied as field techniques, resulting in semi-quantitative analytical results. A limited homogenization of the analyzed sample significantly increases the representativeness of the soil sample. The ED-XRF systems can be differentiated by their limits of detection which are a factor of 10 to 20 higher for the portable system. The accuracy of the results and the measurement uncertainty also improved using the bench top system. Therefore, the selection criteria for applicability of both field systems are based on the required detection level and also the required accuracy of the results.

Metals in boat paint fragments from slipways, repair facilities and abandoned vessels: an evaluation using field portable XRF.

PubMed

Turner, Andrew; Comber, Sean; Rees, Aldous B; Gkiokas, Dimitrios; Solman, Kevin

2015-01-01

Paint flaking off abandoned vessels or generated during boat repair is hazardous to human health and wildlife. In this study, a means of screening paint fragments using a field portable-X-ray fluorescence (FP-XRF) spectrometer is described. The technique is capable of delivering rapid, surficial measurements of Ba, Cu, Pb and Zn down to concentrations less than 150 μg g(-1), and Sn and Cr to concentrations of a few hundred μg g(-1). Application of the technique to fragments collected from slipways, yards, hardstandings, abandoned boats and ships undergoing maintenance throughout the EU reveal highly variable concentrations of metals among samples from the same environment or from the same region of a given boat; in many cases, variability is also evident in different areas or on different surfaces of the same fragment. Of particular concern are elevated concentrations of substances that have been restricted or banned (e.g. Sn, an indicator of organotin, and up to concentrations of 40,000 μg g(-1), and Pb up to concentrations of 200,000 μg g(-1)). Although FP-XRF can rapidly screen samples whose composition and origin are unknown and can assist in instantaneous decision making, a full risk assessment will rely on additional analyses of the precise species (including organo-forms) of the metals present. Copyright © 2014 Elsevier B.V. All rights reserved.

Pots, plates and provenance: sourcing Indian coarse wares from Mleiha using X-ray fluorescence (XRF) spectrometry analysis

NASA Astrophysics Data System (ADS)

Reddy, A.; Attaelmanan, A. G.; Mouton, M.

2012-07-01

The identification of more than 25% of the pottery sherds from the late PIR.D period (ca. 2nd - mid. 3rd c. AD) assemblage from the recently excavated building H at Mleiha as Indian is based on form and fabric, but using only visual assessment. Petrographic analysis of the fabrics can provide more precise indicators of the geographical origin of the wares. In this study, a total of 21 sherds from various key sites in Western India were compared with 7 different 'Indian' coarse-ware vessels sampled at Mleiha using X-ray fluorescence (XRF) spectrometry. The analyses were conducted on powdered samples collected from the core of each sherd. Each sample was irradiated for 1000 seconds using a 1.2 mm diameter X-ray beam. The resulting spectra were used for quantification of the X-ray intensity and elemental concentration. Levels of correlation in the elemental ratios of the sherds were statistically tested using an F-test as well as a Chi-test. Initial review of the XRF results indicates that the Maharashtra and Gujarat regions of India are probable source areas for at least two of the types of wares. Collection of additional samples from these areas and other regions of India, and further statistical analysis through methods such as Principal Component Analysis will help to isolate groups of wares from India and correlate them with types of vessels imported into the Oman peninsula in antiquity.

Gravitational wave detection using laser interferometry beyond the standard quantum limit

NASA Astrophysics Data System (ADS)

Heurs, M.

2018-05-01

Interferometric gravitational wave detectors (such as advanced LIGO) employ high-power solid-state lasers to maximize their detection sensitivity and hence their reach into the universe. These sophisticated light sources are ultra-stabilized with regard to output power, emission frequency and beam geometry; this is crucial to obtain low detector noise. However, even when all laser noise is reduced as far as technically possible, unavoidable quantum noise of the laser still remains. This is a consequence of the Heisenberg Uncertainty Principle, the basis of quantum mechanics: in this case, it is fundamentally impossible to simultaneously reduce both the phase noise and the amplitude noise of a laser to arbitrarily low levels. This fact manifests in the detector noise budget as two distinct noise sources-photon shot noise and quantum radiation pressure noise-which together form a lower boundary for current-day gravitational wave detector sensitivities, the standard quantum limit of interferometry. To overcome this limit, various techniques are being proposed, among them different uses of non-classical light and alternative interferometer topologies. This article explains how quantum noise enters and manifests in an interferometric gravitational wave detector, and gives an overview of some of the schemes proposed to overcome this seemingly fundamental limitation, all aimed at the goal of higher gravitational wave event detection rates. This article is part of a discussion meeting issue `The promises of gravitational-wave astronomy'.

Portable X-ray diffractometer equipped with XRF for archaeometry

NASA Astrophysics Data System (ADS)

Uda, M.; Ishizaki, A.; Satoh, R.; Okada, K.; Nakajima, Y.; Yamashita, D.; Ohashi, K.; Sakuraba, Y.; Shimono, A.; Kojima, D.

2005-09-01

A portable X-ray diffractometer equipped with an X-ray fluorescence spectrometer was improved so as to get a diffraction pattern and a fluorescence spectrum simultaneously in air from one and the same small area on a specimen. Here, diffraction experiments were performed in two modes, i.e. an angle rotation mode and an energy dispersive mode. In the latter a diffraction pattern and a fluorescence spectrum were simultaneously recorded in a short time, 100 s or less, on one display. The diffractometer was tested in the field to confirm its performance. Targets chosen for this purpose were a bronze mirror from the Eastern Han Dynasty (25-220), and a stupa and its pedestal which are part of the painted statue of "Tamonten holding a stupa" from the Heian Period (794-1192), enshrined in the Engyouji temple founded in 996. The bronze mirror was identified as a product of the Han Dynasty from its chemical composition and the existence of the δ phase in the Cu-Sn alloy. The stupa and its pedestal were decorated with gold powder and gold leaf, respectively. From the XRF data of the pedestal, the underlying layer of gold leaf seems to have been painted with emerald green.

Maia Mapper: high definition XRF imaging in the lab

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ryan, Chris G.; Kirkham, R.; Moorhead, G. F.

Here, Maia Mapper is a laboratory μXRF mapping system for efficient elemental imaging of drill core sections serving minerals research and industrial applications. It targets intermediate spatial scales, with imaging of up to ~80 M pixels over a 500×150 mm 2 sample area. It brings together (i) the Maia detector and imaging system, with its large solid-angle, event-mode operation, millisecond pixel transit times in fly-scan mode and real-time spectral deconvolution and imaging, (ii) the high brightness MetalJet D2 liquid metal micro-focus X-ray source from Excillum, and (iii) an efficient XOS polycapillary lens with a flux gain ~15,900 at 21 keVmore » into a ~32 μm focus, and (iv) a sample scanning stage engineered for standard drill-core sections. Count-rates up to ~3 M/s are observed on drill core samples with low dead-time up to ~1.5%. Automated scans are executed in sequence with display of deconvoluted element component images accumulated in real-time in the Maia detector. Application images on drill core and polished rock slabs illustrate Maia Mapper capabilities as part of the analytical workflow of the Advanced Resource Characterisation Facility, which spans spatial dimensions from ore deposit to atomic scales.« less

Maia Mapper: high definition XRF imaging in the lab

DOE PAGES

Ryan, Chris G.; Kirkham, R.; Moorhead, G. F.; ...

2018-03-13

Here, Maia Mapper is a laboratory μXRF mapping system for efficient elemental imaging of drill core sections serving minerals research and industrial applications. It targets intermediate spatial scales, with imaging of up to ~80 M pixels over a 500×150 mm 2 sample area. It brings together (i) the Maia detector and imaging system, with its large solid-angle, event-mode operation, millisecond pixel transit times in fly-scan mode and real-time spectral deconvolution and imaging, (ii) the high brightness MetalJet D2 liquid metal micro-focus X-ray source from Excillum, and (iii) an efficient XOS polycapillary lens with a flux gain ~15,900 at 21 keVmore » into a ~32 μm focus, and (iv) a sample scanning stage engineered for standard drill-core sections. Count-rates up to ~3 M/s are observed on drill core samples with low dead-time up to ~1.5%. Automated scans are executed in sequence with display of deconvoluted element component images accumulated in real-time in the Maia detector. Application images on drill core and polished rock slabs illustrate Maia Mapper capabilities as part of the analytical workflow of the Advanced Resource Characterisation Facility, which spans spatial dimensions from ore deposit to atomic scales.« less

Maia Mapper: high definition XRF imaging in the lab

NASA Astrophysics Data System (ADS)

Ryan, C. G.; Kirkham, R.; Moorhead, G. F.; Parry, D.; Jensen, M.; Faulks, A.; Hogan, S.; Dunn, P. A.; Dodanwela, R.; Fisher, L. A.; Pearce, M.; Siddons, D. P.; Kuczewski, A.; Lundström, U.; Trolliet, A.; Gao, N.

2018-03-01

Maia Mapper is a laboratory μXRF mapping system for efficient elemental imaging of drill core sections serving minerals research and industrial applications. It targets intermediate spatial scales, with imaging of up to ~80 M pixels over a 500×150 mm2 sample area. It brings together (i) the Maia detector and imaging system, with its large solid-angle, event-mode operation, millisecond pixel transit times in fly-scan mode and real-time spectral deconvolution and imaging, (ii) the high brightness MetalJet D2 liquid metal micro-focus X-ray source from Excillum, and (iii) an efficient XOS polycapillary lens with a flux gain ~15,900 at 21 keV into a ~32 μm focus, and (iv) a sample scanning stage engineered for standard drill-core sections. Count-rates up to ~3 M/s are observed on drill core samples with low dead-time up to ~1.5%. Automated scans are executed in sequence with display of deconvoluted element component images accumulated in real-time in the Maia detector. Application images on drill core and polished rock slabs illustrate Maia Mapper capabilities as part of the analytical workflow of the Advanced Resource Characterisation Facility, which spans spatial dimensions from ore deposit to atomic scales.

Inclusivity, exclusivity and limit of detection of commercially available real-time PCR assays for the detection of Salmonella.

PubMed

Margot, H; Stephan, R; Guarino, S; Jagadeesan, B; Chilton, D; O'Mahony, E; Iversen, C

2013-08-01

The traditional cultural detection of Salmonella spp. is both time- and labour-intensive. Salmonella is often a release criterion for the food industry and time to result is therefore an important factor. Storage of finished products and raw materials can be costly and may adversely impact available shelf-life. The application of real-time PCR for the detection of Salmonella spp. in food samples enables a potential time-saving of up to four days. The advancement of real-time PCR coupled with the development of commercially available systems in different formats has made this technology accessible for laboratories in an industrial environment. Ideally these systems are reliable and rapid as well as easy to use. The current study represents a comparative evaluation of seven commercial real-time PCR systems for the detection of Salmonella. Forty-nine target and twenty-nine non-target strains were included in the study to assess inclusivity and exclusivity. The limit of detection for each of the method was determined in four different food products. All systems evaluated were able to correctly identify the 49 Salmonella strains. Nevertheless, false positive results (Citrobacter spp.) were obtained with four of the seven systems. In milk powder and bouillon powder, the limit of detection was similar for all systems, suggesting a minimal matrix effect with these samples. Conversely, for black tea and cocoa powder some systems were prone to inhibition from matrix components. Up to 100% of the samples were inhibited using the proprietary extracts but inhibition could be reduced considerably by application of a DNA clean-up kit. Copyright © 2013 Elsevier B.V. All rights reserved.

Assessment of target detection limits in hyperspectral data

NASA Astrophysics Data System (ADS)

Gross, W.; Boehler, J.; Schilling, H.; Middelmann, W.; Weyermann, J.; Wellig, P.; Oechslin, R.; Kneubuehler, M.

2015-10-01

Hyperspectral remote sensing data can be used for civil and military applications to detect and classify target objects that cannot be reliably separated using broadband sensors. The comparably low spatial resolution is compensated by the fact that small targets, even below image resolution, can still be classified. The goal of this paper is to determine the target size to spatial resolution ratio for successful classification of different target and background materials. Airborne hyperspectral data is used to simulate data with known mixture ratios and to estimate the detection threshold for given false alarm rates. The data was collected in July 2014 over Greding, Germany, using airborne aisaEAGLE and aisaHAWK hyperspectral sensors. On the ground, various target materials were placed on natural background. The targets were four quadratic molton patches with an edge length of 7 meters in the colors black, white, grey and green. Also, two different types of polyethylene (camouflage nets) with an edge length of approximately 5.5 meters were deployed. Synthetic data is generated from the original data using spectral mixtures. Target signatures are linearly combined with different background materials in specific ratios. The simulated mixtures are appended to the original data and the target areas are removed for evaluation. Commonly used classification algorithms, e.g. Matched Filtering, Adaptive Cosine Estimator are used to determine the detection limit. Fixed false alarm rates are employed to find and analyze certain regions where false alarms usually occur first. A combination of 18 targets and 12 backgrounds is analyzed for three VNIR and two SWIR data sets of the same area.

XRF map identification problems based on a PDE electrodeposition model

NASA Astrophysics Data System (ADS)

Sgura, Ivonne; Bozzini, Benedetto

2017-04-01

In this paper we focus on the following map identification problem (MIP): given a morphochemical reaction-diffusion (RD) PDE system modeling an electrodepostion process, we look for a time t *, belonging to the transient dynamics and a set of parameters \\mathbf{p} , such that the PDE solution, for the morphology h≤ft(x,y,{{t}\\ast};\\mathbf{p}\\right) and for the chemistry θ ≤ft(x,y,{{t}\\ast};\\mathbf{p}\\right) approximates a given experimental map M *. Towards this aim, we introduce a numerical algorithm using singular value decomposition (SVD) and Frobenius norm to give a measure of error distance between experimental maps for h and θ and simulated solutions of the RD-PDE system on a fixed time integration interval. The technique proposed allows quantitative use of microspectroscopy images, such as XRF maps. Specifically, in this work we have modelled the morphology and manganese distributions of nanostructured components of innovative batteries and we have followed their changes resulting from ageing under operating conditions. The availability of quantitative information on space-time evolution of active materials in terms of model parameters will allow dramatic improvements in knowledge-based optimization of battery fabrication and operation.

A fuel-limited isothermal DNA machine for the sensitive detection of cellular deoxyribonucleoside triphosphates.

PubMed

Dong, Jiantong; Wu, Tongbo; Xiao, Yu; Xu, Lei; Fang, Simin; Zhao, Meiping

2016-09-29

A fuel-limited isothermal DNA machine has been built for the sensitive fluorescence detection of cellular deoxyribonucleoside triphosphates (dNTPs) at the fmol level, which greatly reduces the required sample cell number. Upon the input of the limiting target dNTP, the machine runs automatically at 37 °C without the need for higher temperature.

Gravitational wave detection using laser interferometry beyond the standard quantum limit.

PubMed

Heurs, M

2018-05-28

Interferometric gravitational wave detectors (such as advanced LIGO) employ high-power solid-state lasers to maximize their detection sensitivity and hence their reach into the universe. These sophisticated light sources are ultra-stabilized with regard to output power, emission frequency and beam geometry; this is crucial to obtain low detector noise. However, even when all laser noise is reduced as far as technically possible, unavoidable quantum noise of the laser still remains. This is a consequence of the Heisenberg Uncertainty Principle, the basis of quantum mechanics: in this case, it is fundamentally impossible to simultaneously reduce both the phase noise and the amplitude noise of a laser to arbitrarily low levels. This fact manifests in the detector noise budget as two distinct noise sources-photon shot noise and quantum radiation pressure noise-which together form a lower boundary for current-day gravitational wave detector sensitivities, the standard quantum limit of interferometry. To overcome this limit, various techniques are being proposed, among them different uses of non-classical light and alternative interferometer topologies. This article explains how quantum noise enters and manifests in an interferometric gravitational wave detector, and gives an overview of some of the schemes proposed to overcome this seemingly fundamental limitation, all aimed at the goal of higher gravitational wave event detection rates.This article is part of a discussion meeting issue 'The promises of gravitational-wave astronomy'. © 2018 The Author(s).

Detection of PLGA-based nanoparticles at a single-cell level by synchrotron radiation FTIR spectromicroscopy and correlation with X-ray fluorescence microscopy

PubMed Central

Pascolo, Lorella; Bortot, Barbara; Benseny-Cases, Nuria; Gianoncelli, Alessandra; Tosi, Giovanni; Ruozi, Barbara; Rizzardi, Clara; De Martino, Eleonora; Vandelli, Maria Angela; Severini, Giovanni Maria

2014-01-01

Poly-lactide-co-glycolide (PLGA) is one of the few polymers approved by the US Food and Drug Administration as a carrier for drug administration in humans; therefore, it is one of the most used materials in the formulation of polymeric nanoparticles (NPs) for therapeutic purposes. Because the cellular uptake of polymeric NPs is a hot topic in the nanomedicine field, the development of techniques able to ensure incontrovertible evidence of the presence of NPs in the cells plays a key role in gaining understanding of their therapeutic potential. On the strength of this premise, this article aims to evaluate the application of synchrotron radiation-based Fourier transform infrared spectroscopy (SR-FTIR) spectromicroscopy and SR X-ray fluorescence (SR-XRF) microscopy in the study of the in vitro interaction of PLGA NPs with cells. To reach this goal, we used PLGA NPs, sized around 200 nm and loaded with superparamagnetic iron oxide NPs (PLGA-IO-NPs; Fe3O4; size, 10–15 nm). After exposing human mesothelial (MeT5A) cells to PLGA-IO-NPs (0.1 mg/mL), the cells were analyzed after fixation both by SR-FTIR spectromicroscopy and SR-XRF microscopy setups. SR-FTIR-SM enabled the detection of PLGA NPs at single-cell level, allowing polymer detection inside the biological matrix by the characteristic band in the 1,700–2,000 cm−1 region. The precise PLGA IR-signature (1,750 cm−1 centered pick) also was clearly evident within an area of high amide density. SR-XRF microscopy performed on the same cells investigated under SR-FTIR microscopy allowed us to put in evidence the Fe presence in the cells and to emphasize the intracellular localization of the PLGA-IO-NPs. These findings suggest that SR-FTIR and SR-XRF techniques could be two valuable tools to follow the PLGA NPs’ fate in in vitro studies on cell cultures. PMID:24944512

X-ray fluorescence for quantification of lead and strontium in vivo

NASA Astrophysics Data System (ADS)

Specht, Aaron James

Lead (Pb) is a toxicant well known for its effects on almost every organ system in the body. Pb use in industry has declined since removal of Pb from gasoline, but many developing countries still have significant use of Pb. Exposure to Pb has been linked with diseases causing neurodegeneration and thus have lasting effects long after the initial exposure. Another metal, strontium (Sr), has been linked with bone disease in particular situations and shown to have uses in treating osteoporosis as a supplement. However, there are no studies of the effects of Sr using a meaningful biomarker. The most commonly used biomarkers for Pb and Sr exposures are blood Pb and Sr; however, blood tests are unable to identify long-term exposure levels due to the short half-life of these metals in blood. Bone stores of Pb and Sr have a half-life of years to decades and serve as a biomarker of long-term exposure. X-ray fluorescence has been used to measure bone Pb and Sr. However, current systems have limitations with radioisotope sources, bulky equipment, and long measurement times. A portable XRF device capable of measurement of bone Pb and Sr, overcomes the limitation of the current systems and has been developed in this work. The detection limit of the portable XRF for bone Pb and Sr was found to be 11 ppm and 5 ppm respectively at 5 mm of skin thickness. The portable XRF will have limitations of measurement based on an individual's skin thickness. The device was calibrated using standard phantoms and validated with in-lab samples, which demonstrated good agreement between KXRF and portable XRF measurements with strong correlations between goat bone, cadaver bone, and phantom measurements. In a population study of Pb poisoned children the portable XRF was further validated and a significant correlation between KXRF measured bone Pb and portable XRF measured bone Pb was identified; however, the device had limitations based on anatomical differences unaccounted for in children from

Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

2004-01-01

A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

Trace element analysis by EPMA in geosciences: detection limit, precision and accuracy

NASA Astrophysics Data System (ADS)

Batanova, V. G.; Sobolev, A. V.; Magnin, V.

2018-01-01

Use of the electron probe microanalyser (EPMA) for trace element analysis has increased over the last decade, mainly because of improved stability of spectrometers and the electron column when operated at high probe current; development of new large-area crystal monochromators and ultra-high count rate spectrometers; full integration of energy-dispersive / wavelength-dispersive X-ray spectrometry (EDS/WDS) signals; and the development of powerful software packages. For phases that are stable under a dense electron beam, the detection limit and precision can be decreased to the ppm level by using high acceleration voltage and beam current combined with long counting time. Data on 10 elements (Na, Al, P, Ca, Ti, Cr, Mn, Co, Ni, Zn) in olivine obtained on a JEOL JXA-8230 microprobe with tungsten filament show that the detection limit decreases proportionally to the square root of counting time and probe current. For all elements equal or heavier than phosphorus (Z = 15), the detection limit decreases with increasing accelerating voltage. The analytical precision for minor and trace elements analysed in olivine at 25 kV accelerating voltage and 900 nA beam current is 4 - 18 ppm (2 standard deviations of repeated measurements of the olivine reference sample) and is similar to the detection limit of corresponding elements. To analyse trace elements accurately requires careful estimation of background, and consideration of sample damage under the beam and secondary fluorescence from phase boundaries. The development and use of matrix reference samples with well-characterised trace elements of interest is important for monitoring and improving of the accuracy. An evaluation of the accuracy of trace element analyses in olivine has been made by comparing EPMA data for new reference samples with data obtained by different in-situ and bulk analytical methods in six different laboratories worldwide. For all elements, the measured concentrations in the olivine reference sample

Trace Metal Variations Detected by Using Continuous XRF Core Scanning: Preliminary Results on Redox-sensitive Elements in East Sea, Korea

NASA Astrophysics Data System (ADS)

Cho, J. H.; Shin, D. H.; Kim, J. K.; Hyun, S.; Jang, S.; Kum, B. C.; Yoo, K. C.; Moh, T. J.

2017-12-01

The cruise of R/V ISABU focused on the detailed geological, geochemical and paleoceanographical investigations in the East Sea. The purpose of this cruise was the use of technically sophisticated Giant Piston Corer (GPC, OSIL) as well as the recovery of the longest piston core (20.7 m, ISA-16ESUB-2B) ever recorded in KIOST with a high resolution of stratigraphic sedimentary layer. The Late Pleistocene to the Holocene sediments in the Ulleung Basin are characterized by several volcanic tephra layers with alternations of fine light and dark clayey layers, reflecting variability in the paleoenvironment. Based on the previous researches and AMS results, we determine the ages of sedimentary layers from three tephra layers, 1.86 mbsf (U-Oki, 10.7 ka), 3.31 mbsf (AT, 29.4 ka), 11.67 mbsf (Aso-4, 88.0 ka) and 17.09 mbsf (Aso-3, 133.0 ka) respectively. Sediment textures are identified as hemipelagic mud, bioturbated mud and laminated mud with tephra layers. The sedimentation rates of each intervals are 0.174 m/kyr (present to U-Oki), 0.078 m/kyr (U-Oki to AT), 0.143 m/kyr (AT to Aso-4) and 0.120 m/kyr (Aso-4 to Aso-3) respectively. Sensitivity of XRF core scanner was obtained by establishing equivalences between peak areas. Element concentrations are analyzed by traditional techniques such as ICP-MS, ICP-OES. The Ca/Fe ratio reflects carbonate content and ISA-16ESUB-2B core shows strong correlation to sedimentary horizons. Sr/Ca ratio has good correlation with sedimentary units. Enhanced Sr contents indicates strong surface ocean production. Br/Cl ratio are high peak during MIS 5.5. Br content implies generally high organic rich sediments.

Assessment of Occupational Exposure to Manganese and Other Metals in Welding Fumes by Portable X-ray Fluorescence Spectrometer

PubMed Central

Laohaudomchok, Wisanti; Cavallari, Jennifer M.; Fang, Shona C.; Lin, Xihong; Herrick, Robert F.; Christiani, David C.; Weisskopf, Marc G.

2011-01-01

Elemental analysis of welding fume samples can be done using several laboratory-based techniques. However, portable measurement techniques could offer several advantages. In this study, we sought to determine whether the portable X-ray fluorescence spectrometer (XRF) is suitable for analysis of five metals (manganese, iron, zinc, copper, and chromium) on 37-mm polytetrafluoroethylene filters. Using this filter fitted on a cyclone in line with a personal pump, gravimetric samples were collected from a group of boilermakers exposed to welding fumes. We assessed the assumption of uniform deposition of these metals on the filters, and the relationships between measurement results of each metal obtained from traditional laboratory-based XRF and the portable XRF. For all five metals of interest, repeated measurements with the portable XRF at the same filter area showed good consistency (reliability ratios are equal or close to 1.0 for almost all metals). The portable XRF readings taken from three different areas of each filter were not significantly different (p-values = 0.77 to 0.98). This suggested that the metal rich PM2.5 deposits uniformly on the samples collected using this gravimetric method. For comparison of the two XRFs, the results from the portable XRF were well correlated and highly predictive of those from the laboratory XRF. The Spearman correlation coefficients were from 0.325 for chromium, to 0.995 for manganese and 0.998 for iron. The mean differences as a percent of the mean laboratory XRF readings were also small (<5%) for manganese, iron, and copper. The differences were greater for zinc and chromium, which were present at very low amounts in our samples and below the limits of detection of the portable XRF for many of the samples. These five metals were moderately to strongly correlated with the total fine particle fraction on filters (Spearman ρ = 0.41 for zinc to 0.97 for iron). Such strong correlations and comparable results suggested that the

Assessment of occupational exposure to manganese and other metals in welding fumes by portable X-ray fluorescence spectrometer.

PubMed

Laohaudomchok, Wisanti; Cavallari, Jennifer M; Fang, Shona C; Lin, Xihong; Herrick, Robert F; Christiani, David C; Weisskopf, Marc G

2010-08-01

Elemental analysis of welding fume samples can be done using several laboratory-based techniques. However, portable measurement techniques could offer several advantages. In this study, we sought to determine whether the portable X-ray fluorescence spectrometer (XRF) is suitable for analysis of five metals (manganese, iron, zinc, copper, and chromium) on 37-mm polytetrafluoroethylene filters. Using this filter fitted on a cyclone in line with a personal pump, gravimetric samples were collected from a group of boilermakers exposed to welding fumes. We assessed the assumption of uniform deposition of these metals on the filters, and the relationships between measurement results of each metal obtained from traditional laboratory-based XRF and the portable XRF. For all five metals of interest, repeated measurements with the portable XRF at the same filter area showed good consistency (reliability ratios are equal or close to 1.0 for almost all metals). The portable XRF readings taken from three different areas of each filter were not significantly different (p-values = 0.77 to 0.98). This suggested that the metal rich PM(2.5) deposits uniformly on the samples collected using this gravimetric method. For comparison of the two XRFs, the results from the portable XRF were well correlated and highly predictive of those from the laboratory XRF. The Spearman correlation coefficients were from 0.325 for chromium, to 0.995 for manganese and 0.998 for iron. The mean differences as a percent of the mean laboratory XRF readings were also small (<5%) for manganese, iron, and copper. The differences were greater for zinc and chromium, which were present at very low amounts in our samples and below the limits of detection of the portable XRF for many of the samples. These five metals were moderately to strongly correlated with the total fine particle fraction on filters (Spearman rho = 0.41 for zinc to 0.97 for iron). Such strong correlations and comparable results suggested that

Finite-size analysis of the detectability limit of the stochastic block model

NASA Astrophysics Data System (ADS)

Young, Jean-Gabriel; Desrosiers, Patrick; Hébert-Dufresne, Laurent; Laurence, Edward; Dubé, Louis J.

2017-06-01

It has been shown in recent years that the stochastic block model is sometimes undetectable in the sparse limit, i.e., that no algorithm can identify a partition correlated with the partition used to generate an instance, if the instance is sparse enough and infinitely large. In this contribution, we treat the finite case explicitly, using arguments drawn from information theory and statistics. We give a necessary condition for finite-size detectability in the general SBM. We then distinguish the concept of average detectability from the concept of instance-by-instance detectability and give explicit formulas for both definitions. Using these formulas, we prove that there exist large equivalence classes of parameters, where widely different network ensembles are equally detectable with respect to our definitions of detectability. In an extensive case study, we investigate the finite-size detectability of a simplified variant of the SBM, which encompasses a number of important models as special cases. These models include the symmetric SBM, the planted coloring model, and more exotic SBMs not previously studied. We conclude with three appendices, where we study the interplay of noise and detectability, establish a connection between our information-theoretic approach and random matrix theory, and provide proofs of some of the more technical results.

Astrobiological Significance of Definitive Mineralogical Analysis of Martian Surface Samples Using the CheMin XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Feldman, S. M.; Blake, D. F.; Sarrazin, P.; Bish, D. L.; Chipera, S. J.; Vaniman, D. T.; Collins, S.

2004-01-01

The search for evidence of habitability, or of extant or extinct life on Mars, will initially be a search for evidence of past or present conditions supportive of life. The three key requirements for the emergence of life are thought to be liquid water; a suitable energy source; and chemical building blocks. CheMin is a miniaturized XRD/XRF (X-Ray diffraction / X-ray fluorescence) instrument which has been developed for definitive mineralogic analysis of soils and rocks on the Martian surface. The CheMin instrument can provide information that is highly relevant to each of these habitability requirements as summarized below.

Signal averaging limitations in heterodyne- and direct-detection laser remote sensing measurements

NASA Technical Reports Server (NTRS)

Menyuk, N.; Killinger, D. K.; Menyuk, C. R.

1983-01-01

The improvement in measurement uncertainty brought about by the averaging of increasing numbers of pulse return signals in both heterodyne- and direct-detection lidar systems is investigated. A theoretical analysis is presented which shows the standard deviation of the mean measurement to decrease as the inverse square root of the number of measurements, except in the presence of temporal correlation. Experimental measurements based on a dual-hybrid-TEA CO2 laser differential absorption lidar system are reported which demonstrate that the actual reduction in the standard deviation of the mean in both heterodyne- and direct-detection systems is much slower than the inverse square-root dependence predicted for uncorrelated signals, but is in agreement with predictions in the event of temporal correlation. Results thus favor the use of direct detection at relatively short range where the lower limit of the standard deviation of the mean is about 2 percent, but advantages of heterodyne detection at longer ranges are noted.

Detection limits of the strip test and PCR for genetically modified corn in Brazil.

PubMed

Nascimento, V E; Von Pinho, É V R; Von Pinho, R G; do Nascimento, A D

2012-08-16

Brazilian legislation establishes a labeling limit for products that contain more than 1% material from genetically modified organisms (GMOs). We assessed the sensitivity of the lateral flow strip test in detection of the GMO corn varieties Bt11 and MON810 and the specificity and sensitivity of PCR techniques for their detection. For the strip test, the GMO seeds were mixed with conventional seeds at levels of 0.2, 0.4 and 0.8% for Bt11, and 0.4, 0.8 and 1.6% for MON810. Three different methodologies were assessed and whole seeds, their endosperm and embryonic axis were used. For the PCR technique, the GMO seeds of each of the two varieties were mixed with conventional seeds at levels of 20, 10, 5, 2, 1, and 0.5%. The seeds were ground and the DNA extracted. For detection of the GMO material, specific primers were used for MON810 and Bt11 and maize zein as an endogenous control. The sensitivity of the strip test varied for both maize varieties and methodologies. The test was positive for Bt11 only at 0.8%, in contrast with the detection limit of 0.4% indicated by the manufacturer. In the multiplex PCR, the primers proved to be specific for the different varieties. These varieties were detected in samples with one GMO seed in 100. Thus, this technique proved to be efficient in detecting contaminations equal to or greater than 1%.

Laser spectrum detection methods for substance of Mars surface

NASA Astrophysics Data System (ADS)

Zhang, Dan; Xue, Bin; Zhao, Yi-yi

2014-11-01

The chemical element and mineral rock's abundance and distribution are the basic material of planetary geology evolution research [1], hence preterit detection for composition of Mars surface substance contains both elements sorts and mineral ingredients. This article introduced new ways to detect Mars elements and mineral components, Laser Induced Breakdown Spectroscopy (LIBS) and Raman Spectroscopy (RS) which have distinct advantages, such as work over a long distance, detect rapidly, accuratly and nondestructively. LIBS and RS both use laser excitation to shoot the substance of Mars exciting new wavelengths. The techniques of LIBS and RS in laboratory are mature, besides the technique of LIBS is being used in MSL (Chemcam) now and RS will be used in ExoMars. Comparing LIBS and RS's detection results with XRF and APXS, Mossbauer spectrometer, these existed Mars surface material detection instruments,and the Infrared spectrometer, Mid-IR, they have more accurate detection results. So LIBS and RS are competent for Mars surface substance detection instead of X-ray spectrometer and Mossbauer spectrometer which were already used in 'Viking 1' and 'Opportunity'. Only accurate detection results about Mars surface substance can lead to scientist's right analysis in inversing geological evolution of the planet.

Experimental Study of the Detection Limit in Dual-Gate Biosensors Using Ultrathin Silicon Transistors

DOE PAGES

Wu, Ting; Alharbi, Abdullah; You, Kai-Dyi; ...

2017-06-21

Dual-gate field-effect biosensors (bioFETs) with asymmetric gate capacitances were shown to surpass the Nernst limit of 59 mV/pH. However, previous studies have conflicting findings on the effect of the capacitive amplification scheme on the sensor detection limit, which is inversely proportional to the signal-to-noise ratio (SNR). In this paper, we present a systematic experimental investigation of the SNR using ultrathin silicon transistors. Our sensors operate at low voltage and feature asymmetric front and back oxide capacitances with asymmetry factors of 1.4 and 2.3. We demonstrate that in the dual-gate configuration, the response of our bioFETs to the pH change increasesmore » proportional to the asymmetry factor and indeed exceeds the Nernst limit. Further, our results reveal that the noise amplitude also increases in proportion to the asymmetry factor. We establish that the commensurate increase of the noise amplitude originates from the intrinsic low-frequency characteristic of the sensor noise, dominated by number fluctuation. Finally, these findings suggest that this capacitive signal amplification scheme does not improve the intrinsic detection limit of the dual-gate biosensors.« less

Experimental Study of the Detection Limit in Dual-Gate Biosensors Using Ultrathin Silicon Transistors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Ting; Alharbi, Abdullah; You, Kai-Dyi

Dual-gate field-effect biosensors (bioFETs) with asymmetric gate capacitances were shown to surpass the Nernst limit of 59 mV/pH. However, previous studies have conflicting findings on the effect of the capacitive amplification scheme on the sensor detection limit, which is inversely proportional to the signal-to-noise ratio (SNR). In this paper, we present a systematic experimental investigation of the SNR using ultrathin silicon transistors. Our sensors operate at low voltage and feature asymmetric front and back oxide capacitances with asymmetry factors of 1.4 and 2.3. We demonstrate that in the dual-gate configuration, the response of our bioFETs to the pH change increasesmore » proportional to the asymmetry factor and indeed exceeds the Nernst limit. Further, our results reveal that the noise amplitude also increases in proportion to the asymmetry factor. We establish that the commensurate increase of the noise amplitude originates from the intrinsic low-frequency characteristic of the sensor noise, dominated by number fluctuation. Finally, these findings suggest that this capacitive signal amplification scheme does not improve the intrinsic detection limit of the dual-gate biosensors.« less

Experimental Study of the Detection Limit in Dual-Gate Biosensors Using Ultrathin Silicon Transistors.

PubMed

Wu, Ting; Alharbi, Abdullah; You, Kai-Dyi; Kisslinger, Kim; Stach, Eric A; Shahrjerdi, Davood

2017-07-25

Dual-gate field-effect biosensors (bioFETs) with asymmetric gate capacitances were shown to surpass the Nernst limit of 59 mV/pH. However, previous studies have conflicting findings on the effect of the capacitive amplification scheme on the sensor detection limit, which is inversely proportional to the signal-to-noise ratio (SNR). Here, we present a systematic experimental investigation of the SNR using ultrathin silicon transistors. Our sensors operate at low voltage and feature asymmetric front and back oxide capacitances with asymmetry factors of 1.4 and 2.3. We demonstrate that in the dual-gate configuration, the response of our bioFETs to the pH change increases proportional to the asymmetry factor and indeed exceeds the Nernst limit. Further, our results reveal that the noise amplitude also increases in proportion to the asymmetry factor. We establish that the commensurate increase of the noise amplitude originates from the intrinsic low-frequency characteristic of the sensor noise, dominated by number fluctuation. These findings suggest that this capacitive signal amplification scheme does not improve the intrinsic detection limit of the dual-gate biosensors.

Evaluation of a single-item screening question to detect limited health literacy in peritoneal dialysis patients.

PubMed

Jain, Deepika; Sheth, Heena; Bender, Filitsa H; Weisbord, Steven D; Green, Jamie A

2014-01-01

Studies have shown that a single-item question might be useful in identifying patients with limited health literacy. However, the utility of the approach has not been studied in patients receiving maintenance peritoneal dialysis (PD). We assessed health literacy in a cohort of 31 PD patients by administering the Rapid Estimate of Adult Literacy in Medicine (REALM) and a single-item health literacy (SHL) screening question "How confident are you filling out medical forms by yourself?" (Extremely, Quite a bit, Somewhat, A little bit, or Not at all). To determine the accuracy of the single-item question for detecting limited health literacy, we performed sensitivity and specificity analyses of the SHL and plotted the area under the receiver operating characteristic (AUROC) curve using the REALM as a reference standard. Using a cut-off of "Somewhat" or less confident, the sensitivity of the SHL for detecting limited health literacy was 80%, and the specificity was 88%. The positive likelihood ratio was 6.9. The SHL had an AUROC of 0.79 (95% confidence interval: 0.52 to 1.00). Our results show that the SHL could be effective in detecting limited health literacy in PD patients.

First direct detection limits on sub-GeV dark matter from XENON10.

PubMed

Essig, Rouven; Manalaysay, Aaron; Mardon, Jeremy; Sorensen, Peter; Volansky, Tomer

2012-07-13

The first direct detection limits on dark matter in the MeV to GeV mass range are presented, using XENON10 data. Such light dark matter can scatter with electrons, causing ionization of atoms in a detector target material and leading to single- or few-electron events. We use 15  kg day of data acquired in 2006 to set limits on the dark-matter-electron scattering cross section. The strongest bound is obtained at 100 MeV where σ(e)<3×10(-38)  cm2 at 90% C.L., while dark-matter masses between 20 MeV and 1 GeV are bounded by σ(e)<10(-37)  cm2 at 90% C.L. This analysis provides a first proof of principle that direct detection experiments can be sensitive to dark-matter candidates with masses well below the GeV scale.

Power-limited low-thrust trajectory optimization with operation point detection

NASA Astrophysics Data System (ADS)

Chi, Zhemin; Li, Haiyang; Jiang, Fanghua; Li, Junfeng

2018-06-01

The power-limited solar electric propulsion system is considered more practical in mission design. An accurate mathematical model of the propulsion system, based on experimental data of the power generation system, is used in this paper. An indirect method is used to deal with the time-optimal and fuel-optimal control problems, in which the solar electric propulsion system is described using a finite number of operation points, which are characterized by different pairs of thruster input power. In order to guarantee the integral accuracy for the discrete power-limited problem, a power operation detection technique is embedded in the fourth-order Runge-Kutta algorithm with fixed step. Moreover, the logarithmic homotopy method and normalization technique are employed to overcome the difficulties caused by using indirect methods. Three numerical simulations with actual propulsion systems are given to substantiate the feasibility and efficiency of the proposed method.

100-OL-1 Operable Unit Field Portable X-Ray Fluorescence (XRF) Analyzer Pilot Study Plans

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bunn, Amoret L.; Fritz, Brad G.; Wellman, Dawn M.

A pilot study is being conducted to support the approval of the Remedial Investigation/Feasibility Study (RI/FS) Work Plan to evaluate the 100-OL-1 Operable Unit (OU) pre-Hanford orchard lands. Based on comments received by the U.S. Environmental Protection Agency (EPA) and Washington State Department of Ecology, the pilot study will evaluate the use of field portable X-ray fluorescence (XRF) spectrometry measurements for evaluating lead and arsenic concentrations on the soil surface as an indicator of past use of lead arsenate pesticide residue in the OU. The work will be performed in the field during the summer of 2014, and assist inmore » the planning for the characterization activities in the RI/FS.« less

STATISTICAL METHODS FOR ENVIRONMENTAL APPLICATIONS USING DATA SETS WITH BELOW DETECTION LIMIT OBSERVATIONS AS INCORPORTED IN PROUCL 4.0

EPA Science Inventory

Nondetect (ND) or below detection limit (BDL) results cannot be measured accurately, and, therefore, are reported as less than certain detection limit (DL) values. However, since the presence of some contaminants (e.g., dioxin) in environmental media may pose a threat to human he...

Detection limit of intragenic deletions with targeted array comparative genomic hybridization

PubMed Central

2013-01-01

Background Pathogenic mutations range from single nucleotide changes to deletions or duplications that encompass a single exon to several genes. The use of gene-centric high-density array comparative genomic hybridization (aCGH) has revolutionized the detection of intragenic copy number variations. We implemented an exon-centric design of high-resolution aCGH to detect single- and multi-exon deletions and duplications in a large set of genes using the OGT 60 K and 180 K arrays. Here we describe the molecular characterization and breakpoint mapping of deletions at the smaller end of the detectable range in several genes using aCGH. Results The method initially implemented to detect single to multiple exon deletions, was able to detect deletions much smaller than anticipated. The selected deletions we describe vary in size, ranging from over 2 kb to as small as 12 base pairs. The smallest of these deletions are only detectable after careful manual review during data analysis. Suspected deletions smaller than the detection size for which the method was optimized, were rigorously followed up and confirmed with PCR-based investigations to uncover the true detection size limit of intragenic deletions with this technology. False-positive deletion calls often demonstrated single nucleotide changes or an insertion causing lower hybridization of probes demonstrating the sensitivity of aCGH. Conclusions With optimizing aCGH design and careful review process, aCGH can uncover intragenic deletions as small as dozen bases. These data provide insight that will help optimize probe coverage in array design and illustrate the true assay sensitivity. Mapping of the breakpoints confirms smaller deletions and contributes to the understanding of the mechanism behind these events. Our knowledge of the mutation spectra of several genes can be expected to change as previously unrecognized intragenic deletions are uncovered. PMID:24304607

Quantification of zinc-porphyrin in dry-cured ham products by spectroscopic methods Comparison of absorption, fluorescence and X-ray fluorescence spectroscopy.

PubMed

Laursen, Kristoffer; Adamsen, Christina E; Laursen, Jens; Olsen, Karsten; Møller, Jens K S

2008-03-01

Zinc-protoporphyrin (Zn-pp), which has been identified as the major pigment in certain dry-cured meat products, was extracted with acetone/water (75%) and isolated from the following meat products: Parma ham, Iberian ham and dry-cured ham with added nitrite. The quantification of Zn-pp by electron absorption, fluorescence and X-ray fluorescence (XRF) spectroscopy was compared (concentration range used [Zn-pp]=0.8-9.7μM). All three hams were found to contain Zn-pp, and the results show no significant difference among the content of Zn-pp quantified by fluorescence, absorbance and X-ray fluorescence spectroscopy for Parma ham and Iberian ham. All three methods can be used for quantification of Zn-pp in acetone/water extracts of different ham types if the content is higher than 1.0ppm. For dry-cured ham with added nitrite, XRF was not applicable due to the low content of Zn-pp (<0.1ppm). In addition, XRF spectroscopy provides further information regarding other trace elements and can therefore be advantageous in this aspect. This study also focused on XRF determination of Fe in the extracts and as no detectable Fe was found in the three types of ham extracts investigated (limit of detection; Fe⩽1.8ppm), it allows the conclusion that iron containing pigments, e.g., heme, do not contribute to the noticeable red colour observed in some of the extracts.

Destructive versus non-destructive methods for geochemical analyses of ceramic artifacts: comparison of portable XRF and ICP-MS data on Bronze Age ceramics from Failaka Island (Kuwait) and Bahrain

NASA Astrophysics Data System (ADS)

Stremtan, Ciprian; Ashkanani, Hasan; Tykot, Robert H.

2013-04-01

The study of bi-phase (i.e. matrix and clasts) geochemical composition of ceramic artifacts is a very powerful tool in fingerprinting the raw materials used by ancient manufacturers (clay sources, tempering materials, coloring agents, etc.), as well as in understanding the physical parameters of the manufacturing techniques. Reliable datasets often require the deployment of destructive techniques that will irremediably damage the artifact. Recent advances in portable X-ray fluorescence instrumentation (pXRF) allow for quick measurements of a range of chemical elements that not too long ago were available only through complicated and often destructive means of analytical chemistry (instrumental neutron activation analysis - INAA, inductively coupled plasma mass spectrometry - ICP-MS, direct coupled plasma-optical emission spectroscopy - DCP-OES etc.). In this contribution we present a comparison of datasets acquired by means of pXRF, DCP-OES, and ICP-MS on Bronze Age ceramics from Failaka Island (Kuwait) and Bahrain. The samples chosen for this study are fine grained, with very well sorted mineral components, and lack any visible organic material fragments. The sample preparation for ICP-MS and DCP-OES analyses was carried out on powdered samples, by using LiBO2 flux fusion and Ge (for the DCP-OES) and In (for ICP-MS) were used as internal standards. The measurements were calibrated against certified reference materials ranging from shales to rhyolites (SGR-1, SDo-1, JA-2, and JR-1) and performed at Univerity of South Florida's Center for Geochemical Analyses. The analytical errors for major elements was smaller than 5 %, while for selected trace elements the error was usually smaller than 3 %. The same set of elements was measured on the same samples at University of South Florida's Anthropology Department using a pXRF device equipped with obsidian filter. Each sample was measured three times and the values were averaged. Two certified reference materials (NIST-612

In vivo X-ray fluorescence of lead in bone: review and current issues.

PubMed Central

Todd, A C; Chettle, D R

1994-01-01

Bone lead measurements can assess long-term lead dosimetry because the residence time of lead in bone is long. Bone lead measurements thus complement blood and plasma lead measurements, which reflect more short-term exposure. Although the noninvasive, in vivo measurement of lead in bone by X-ray fluorescence (XRF) has been under development since the 1970s, its use is still largely confined to research institutions. There are three principal methods used that vary both in the how lead X-rays are fluoresced and in which lead X-rays are fluoresced. Several groups have reported the independent development of in vivo measurement systems, the majority adopting the 109Cd K XRF method because of its advantages: a robust measurement, a lower detection limit (compared to 57Co K XRF), and a lower effective (radiation) dose (compared to L XRF) when calculated according to the most recent guidelines. These advantages, and the subsequent widespread adoption of the 109Cd method, are primarily consequences of the physics principles of the technique. This paper presents an explanation of the principles of XRF, a description of the practical measurement systems, a review of the human bone lead studies performed to date; and a discussion of some issues surrounding future application of the methods. Images p172-a PMID:8033846

ARE WE THERE YET? TIME TO DETECTION OF NANOHERTZ GRAVITATIONAL WAVES BASED ON PULSAR-TIMING ARRAY LIMITS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taylor, S. R.; Vallisneri, M.; Ellis, J. A.

2016-03-01

Decade-long timing observations of arrays of millisecond pulsars have placed highly constraining upper limits on the amplitude of the nanohertz gravitational-wave stochastic signal from the mergers of supermassive black hole binaries (∼10{sup −15} strain at f = 1 yr{sup −1}). These limits suggest that binary merger rates have been overestimated, or that environmental influences from nuclear gas or stars accelerate orbital decay, reducing the gravitational-wave signal at the lowest, most sensitive frequencies. This prompts the question whether nanohertz gravitational waves (GWs) are likely to be detected in the near future. In this Letter, we answer this question quantitatively using simple statistical estimates,more » deriving the range of true signal amplitudes that are compatible with current upper limits, and computing expected detection probabilities as a function of observation time. We conclude that small arrays consisting of the pulsars with the least timing noise, which yield the tightest upper limits, have discouraging prospects of making a detection in the next two decades. By contrast, we find large arrays are crucial to detection because the quadrupolar spatial correlations induced by GWs can be well sampled by many pulsar pairs. Indeed, timing programs that monitor a large and expanding set of pulsars have an ∼80% probability of detecting GWs within the next 10 years, under assumptions on merger rates and environmental influences ranging from optimistic to conservative. Even in the extreme case where 90% of binaries stall before merger and environmental coupling effects diminish low-frequency gravitational-wave power, detection is delayed by at most a few years.« less

Improvements of low-detection-limit filter-free fluorescence sensor developed by charge accumulation operation

NASA Astrophysics Data System (ADS)

Tanaka, Kiyotsugu; Choi, Yong Joon; Moriwaki, Yu; Hizawa, Takeshi; Iwata, Tatsuya; Dasai, Fumihiro; Kimura, Yasuyuki; Takahashi, Kazuhiro; Sawada, Kazuaki

2017-04-01

We developed a low-detection-limit filter-free fluorescence sensor by a charge accumulation technique. For charge accumulation, a floating diffusion amplifier (FDA), which included a floating diffusion capacitor, a transfer gate, and a source follower circuit, was used. To integrate CMOS circuits with the filter-free fluorescence sensor, we adopted a triple-well process to isolate transistors from the sensor on a single chip. We detected 0.1 nW fluorescence under the illumination of excitation light by 1.5 ms accumulation, which was one order of magnitude greater than that of a previous current detection sensor.

Experimental demonstration of direct L-shell x-ray fluorescence imaging of gold nanoparticles using a benchtop x-ray source.

PubMed

Manohar, Nivedh; Reynoso, Francisco J; Cho, Sang Hyun

2013-08-01

To develop a proof-of-principle L-shell x-ray fluorescence (XRF) imaging system that locates and quantifies sparse concentrations of gold nanoparticles (GNPs) using a benchtop polychromatic x-ray source and a silicon (Si)-PIN diode x-ray detector system. 12-mm-diameter water-filled cylindrical tubes with GNP concentrations of 20, 10, 5, 0.5, 0.05, 0.005, and 0 mg∕cm3 served as calibration phantoms. An imaging phantom was created using the same cylindrical tube but filled with tissue-equivalent gel containing structures mimicking a GNP-loaded blood vessel and approximately 1 cm3 tumor. Phantoms were irradiated by a 3-mm-diameter pencil-beam of 62 kVp x-rays filtered by 1 mm aluminum. Fluorescence∕scatter photons from phantoms were detected at 90° with respect to the beam direction using a Si-PIN detector placed behind a 2.5-mm-diameter lead collimator. The imaging phantom was translated horizontally and vertically in 0.3-mm steps to image a 6 mm×15 mm region of interest (ROI). For each phantom, the net L-shell XRF signal from GNPs was extracted from background, and then corrected for detection efficiency and in-phantom attenuation using a fluorescence-to-scatter normalization algorithm. XRF measurements with calibration phantoms provided a calibration curve showing a linear relationship between corrected XRF signal and GNP mass per imaged voxel. Using the calibration curve, the detection limit (at the 95% confidence level) of the current experimental setup was estimated to be a GNP mass of 0.35 μg per imaged voxel (1.73×10(-2) cm3). A 2D XRF map of the ROI was also successfully generated, reasonably matching the known spatial distribution as well as showing the local variation of GNP concentrations. L-shell XRF imaging can be a highly sensitive tool that has the capability of simultaneously imaging the spatial distribution and determining the local concentration of GNPs presented on the order of parts-per-million level within subcentimeter-sized ex vivo

Experimental demonstration of direct L-shell x-ray fluorescence imaging of gold nanoparticles using a benchtop x-ray source

PubMed Central

Manohar, Nivedh; Reynoso, Francisco J.; Cho, Sang Hyun

2013-01-01

Purpose: To develop a proof-of-principle L-shell x-ray fluorescence (XRF) imaging system that locates and quantifies sparse concentrations of gold nanoparticles (GNPs) using a benchtop polychromatic x-ray source and a silicon (Si)-PIN diode x-ray detector system. Methods: 12-mm-diameter water-filled cylindrical tubes with GNP concentrations of 20, 10, 5, 0.5, 0.05, 0.005, and 0 mg/cm3 served as calibration phantoms. An imaging phantom was created using the same cylindrical tube but filled with tissue-equivalent gel containing structures mimicking a GNP-loaded blood vessel and approximately 1 cm3 tumor. Phantoms were irradiated by a 3-mm-diameter pencil-beam of 62 kVp x-rays filtered by 1 mm aluminum. Fluorescence/scatter photons from phantoms were detected at 90° with respect to the beam direction using a Si-PIN detector placed behind a 2.5-mm-diameter lead collimator. The imaging phantom was translated horizontally and vertically in 0.3-mm steps to image a 6 mm × 15 mm region of interest (ROI). For each phantom, the net L-shell XRF signal from GNPs was extracted from background, and then corrected for detection efficiency and in-phantom attenuation using a fluorescence-to-scatter normalization algorithm. Results: XRF measurements with calibration phantoms provided a calibration curve showing a linear relationship between corrected XRF signal and GNP mass per imaged voxel. Using the calibration curve, the detection limit (at the 95% confidence level) of the current experimental setup was estimated to be a GNP mass of 0.35 μg per imaged voxel (1.73 × 10−2 cm3). A 2D XRF map of the ROI was also successfully generated, reasonably matching the known spatial distribution as well as showing the local variation of GNP concentrations. Conclusions:L-shell XRF imaging can be a highly sensitive tool that has the capability of simultaneously imaging the spatial distribution and determining the local concentration of GNPs presented on the order of parts-per-million level

Procedures for determination of detection limits: application to high-performance liquid chromatography analysis of fat-soluble vitamins in human serum.

PubMed

Browne, Richard W; Whitcomb, Brian W

2010-07-01

Problems in the analysis of laboratory data commonly arise in epidemiologic studies in which biomarkers subject to lower detection thresholds are used. Various thresholds exist including limit of detection (LOD), limit of quantification (LOQ), and limit of blank (LOB). Choosing appropriate strategies for dealing with data affected by such limits relies on proper understanding of the nature of the detection limit and its determination. In this paper, we demonstrate experimental and statistical procedures generally used for estimating different detection limits according to standard procedures in the context of analysis of fat-soluble vitamins and micronutrients in human serum. Fat-soluble vitamins and micronutrients were analyzed by high-performance liquid chromatography with diode array detection. A simulated serum matrix blank was repeatedly analyzed for determination of LOB parametrically by using the observed blank distribution as well as nonparametrically by using ranks. The LOD was determined by combining information regarding the LOB with data from repeated analysis of standard reference materials (SRMs), diluted to low levels; from LOB to 2-3 times LOB. The LOQ was determined experimentally by plotting the observed relative standard deviation (RSD) of SRM replicates compared with the concentration, where the LOQ is the concentration at an RSD of 20%. Experimental approaches and example statistical procedures are given for determination of LOB, LOD, and LOQ. These quantities are reported for each measured analyte. For many analyses, there is considerable information available below the LOQ. Epidemiologic studies must understand the nature of these detection limits and how they have been estimated for appropriate treatment of affected data.

High resolution HH-XRF scanning and XRD modelling as a tool in sedimentological analysis - A case study from the Enreca-3 core, Bach Long Vi Island, Vietnam

NASA Astrophysics Data System (ADS)

Rizzi, Malgorzata; Hemmingsen Schovsbo, Niels; Korte, Christoph; Bryld Wessel Fyhn, Michael

2017-04-01

To improve the understanding and interpretation of the depositional environment of a late Oligocene lacustrine organic rich oil-prone source rock succession, 2464 hand held (HH)-XRF measurements were made systematically on the 500 m long, continuous core from the fully cored Enreca-3 well. This core, drilled on the remote Bach Long Vi Island, northern Gulf of Tonkin, offshore Vietnam, represents a deep lake succession alternating between lacustrine pelagic dominated sediments interrupted by hyperpycnal turbidites, high density turbidites and debris flows [1, 2]. From a combined HH-XRF-XRD data set, multivariate data analysis and regression models are used to type the rock and to predict the XRD mineral composition based on HH-XRF composition. The rock types and the modelled mineral composition highlight the geochemical variations of the sediment and allows for direct comparison with sedimentological processes and facies changes. The modeling also depicts the cyclic alteration of rock types that are present on many different scales ranging from centimeters to hundreds of meters [1, 2]. The sedimentological and geochemical variations observed throughout the cored section reflects fluctuating paleoclimate, tectonism and hinterland condition controlling the depositional setting, which may provide a deeper understanding of the deposition of this and similar Paleogene syn-rift succession in the South China Sea region. It allows furthermore the development of a more generalized depositional model relevant for other deep-lacustrine syn-rift basins. [1] Petersen et al. (2014) Journal of Petroleum Geology, 37: 373-389. [2] Hovikoski et al. (2016) Journal of Sedimentary Research, 86(8): 982-1007.

Definitive Mineralogical Analysis of Mars Analog Rocks Using the CheMin XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Blake, D. F.; Sarrazin, P.; Bish, D. L.; Feldman, S.; Chipera, S. J.; Vaniman, D. T.; Collins, S.

2004-01-01

Mineral identification is a critical component of Mars Astrobiological missions. Chemical or elemental data alone are not definitive because a single elemental or chemical composition or even a single bonding type can represent a range of substances or mineral assemblages. Minerals are defined as unique structural and compositional phases that occur naturally. There are about 15,000 minerals that have been described on Earth, all uniquely identifiable via diffraction methods. There are likely many minerals yet undiscovered on Earth, and likewise on Mars. If an unknown phase is identified on Mars, it can be fully characterized by structural (X-ray Diffraction, XRD) and elemental analysis (X-ray Fluorescence, XRF) without recourse to other data because XRD relies on the principles of atomic arrangement for its determinations. XRD is the principal means of identification and characterization of minerals on Earth.

Portable X-ray fluorescence spectroscopy as a rapid screening technique for analysis of TiO2 and ZnO in sunscreens.

PubMed

Bairi, Venu Gopal; Lim, Jin-Hee; Quevedo, Ivan R; Mudalige, Thilak K; Linder, Sean W

2016-02-01

This investigation reports a rapid and simple screening technique for the quantification of titanium and zinc in commercial sunscreens using portable X-ray fluorescence spectroscopy (pXRF). A highly evolved technique, inductively coupled plasma-mass spectroscopy (ICP-MS) was chosen as a comparative technique to pXRF, and a good correlation (r 2 > 0.995) with acceptable variations (≤25%) in results between both techniques was observed. Analytical figures of merit such as detection limit, quantitation limit, and linear range of the method are reported for the pXRF technique. This method has a good linearity (r 2 > 0.995) for the analysis of titanium (Ti) in the range of 0.4-14.23 wt%, and zinc (Zn) in the range of 1.0-23.90 wt%. However, most commercial sunscreens contain organic ingredients, and these ingredients are known to cause matrix effects. The development of appropriate matrix matched working standards to obtain the calibration curve was found to be a major challenge for the pXRF measurements. In this study, we have overcome the matrix effect by using metal-free commercial sunscreens as a dispersing media for the preparation of working standards. An easy extension of this unique methodology for preparing working standards in different matrices was also reported. This method is simple, rapid, and cost-effective and, in comparison to conventional techniques (e.g., ICP-MS), did not generate toxic wastes during sample analysis.

Portable X-ray fluorescence spectroscopy as a rapid screening technique for analysis of TiO2 and ZnO in sunscreens

NASA Astrophysics Data System (ADS)

Bairi, Venu Gopal; Lim, Jin-Hee; Quevedo, Ivan R.; Mudalige, Thilak K.; Linder, Sean W.

2016-02-01

This investigation reports a rapid and simple screening technique for the quantification of titanium and zinc in commercial sunscreens using portable X-ray fluorescence spectroscopy (pXRF). A highly evolved technique, inductively coupled plasma-mass spectroscopy (ICP-MS) was chosen as a comparative technique to pXRF, and a good correlation (r2 > 0.995) with acceptable variations (≤ 25%) in results between both techniques was observed. Analytical figures of merit such as detection limit, quantitation limit, and linear range of the method are reported for the pXRF technique. This method has a good linearity (r2 > 0.995) for the analysis of titanium (Ti) in the range of 0.4-14.23 wt%, and zinc (Zn) in the range of 1.0-23.90 wt%. However, most commercial sunscreens contain organic ingredients, and these ingredients are known to cause matrix effects. The development of appropriate matrix matched working standards to obtain the calibration curve was found to be a major challenge for the pXRF measurements. In this study, we have overcome the matrix effect by using metal-free commercial sunscreens as a dispersing media for the preparation of working standards. An easy extension of this unique methodology for preparing working standards in different matrices was also reported. This method is simple, rapid, and cost-effective and, in comparison to conventional techniques (e.g., ICP-MS), did not generate toxic wastes during sample analysis.

The limit of detection in scintigraphic imaging with I-131 in patients with differentiated thyroid carcinoma

NASA Astrophysics Data System (ADS)

Hänscheid, H.; Lassmann, M.; Buck, A. K.; Reiners, C.; Verburg, F. A.

2014-05-01

Radioiodine scintigraphy influences staging and treatment in patients with differentiated thyroid carcinoma. The limit of detection for fractional uptake in an iodine avid focus in a scintigraphic image was determined from the number of lesion net counts and the count density of the tissue background. The count statistics were used to calculate the diagnostic activity required to elevate the signal from a lesion with a given uptake significantly above a homogeneous background with randomly distributed counts per area. The dependences of the minimal uptake and the minimal size of lesions visible in a scan on several parameters of influence were determined by linking the typical biokinetics observed in iodine avid tissue to the lesion mass and to the absorbed dose received in a radioiodine therapy. The detection limits for fractional uptake in a neck lesion of a typical patient are about 0.001% after therapy with 7000 MBq, 0.01% for activities typically administered in diagnostic assessments (74-185 MBq), and 0.1% after the administration of 10 MBq I-131. Lesions at the limit of detection in a diagnostic scan with biokinetics eligible for radioiodine therapy are small with diameters of a few millimeters. Increasing the diagnostic activity by a factor of 4 reduces the diameter of visible lesions by 25% or about 1 mm. Several other determinants have a comparable or higher influence on the limit of detection than the administered activity; most important are the biokinetics in both blood pool and target tissue and the time of measurement. A generally valid recommendation for the timing of the scan is impossible as the time of the highest probability to detect iodine avid tissue depends on the administered activity as well as on the biokinetics in the lesion and background in the individual patient.

STATISTICS OF GAMMA-RAY POINT SOURCES BELOW THE FERMI DETECTION LIMIT

DOE Office of Scientific and Technical Information (OSTI.GOV)

Malyshev, Dmitry; Hogg, David W., E-mail: dm137@nyu.edu

2011-09-10

An analytic relation between the statistics of photons in pixels and the number counts of multi-photon point sources is used to constrain the distribution of gamma-ray point sources below the Fermi detection limit at energies above 1 GeV and at latitudes below and above 30 deg. The derived source-count distribution is consistent with the distribution found by the Fermi Collaboration based on the first Fermi point-source catalog. In particular, we find that the contribution of resolved and unresolved active galactic nuclei (AGNs) to the total gamma-ray flux is below 20%-25%. In the best-fit model, the AGN-like point-source fraction is 17%more » {+-} 2%. Using the fact that the Galactic emission varies across the sky while the extragalactic diffuse emission is isotropic, we put a lower limit of 51% on Galactic diffuse emission and an upper limit of 32% on the contribution from extragalactic weak sources, such as star-forming galaxies. Possible systematic uncertainties are discussed.« less

Trace elemental analysis of school chalk using energy dispersive X-ray florescence spectroscopy (ED-XRF)

NASA Astrophysics Data System (ADS)

Maruthi, Y. A.; Das, N. Lakshmana; Ramprasad, S.; Ram, S. S.; Sudarshan, M.

2015-08-01

The present studies focus the quantitative analysis of elements in school chalk to ensure the safety of its use. The elements like Calcium (Ca), Aluminum (Al), Iron (Fe), Silicon (Si) and Chromium (Cr) were analyzed from settled chalk dust samples collected from five classrooms (CD-1) and also from another set of unused chalk samples collected from local market (CD-2) using Energy Dispersive X-Ray florescence(ED-XRF) spectroscopy. Presence of these elements in significant concentrations in school chalk confirmed that, it is an irritant and occupational hazard. It is suggested to use protective equipments like filtered mask for mouth, nose and chalk holders. This study also suggested using the advanced mode of techniques like Digital boards, marker boards and power point presentations to mitigate the occupational hazard for classroom chalk

Detection Limits for Spectro-fluorometry: A Case Study in the Region of Finstersee, Canton Zug, Northern Switzerland

NASA Astrophysics Data System (ADS)

Otz, M. H.; Otz, H. K.; Keller, P.

2002-05-01

Synthetic fluorescent dyes, applied below the visual detection limit (< 0.1 mg/L), have been used as tracers of ground water flow paths since the beginning of the 1950s. Since 1965, we have used spectro-fluorometers with photomultipliers to measure low concentrations of fluorescent dyes in ground water in Switzerland. In collaboration with the Engineering Geology Department of the ETH, we have separated uranine at 0.1 ng/L and Na-naphtionate at 1 ng/L from background fluorescence of spring water in the Finstersee region. These values are 10-100 times lower than postulated detection limits in the literature. The use of low dye concentrations prevents a study region from being contaminated by increased background levels due to remnant dye within the aquifer, thereby leaving the region available for future dye tracing studies. Lower detection limits also can solve particular hydraulic problems where conventional methods fail and enhance the possibility for using artificial dyes in environmentally sensitive aquifer settings.

Application of portable X-ray fluorescence spectrometry in environmental investigation of heavy metal-contaminated sites and comparison with laboratory analysis

NASA Astrophysics Data System (ADS)

Ding, Liang; Wang, Shui; Cai, Bingjie; Zhang, Mancheng; Qu, Changsheng

2018-02-01

In this study, portable X-ray fluorescence spectrometry (pXRF) was used to measure the heavy metal contents of As, Cu, Cr, Ni, Pb and Zn in the soils of heavy metal-contaminated sites. The precision, accuracy and system errors of pXRF were evaluated and compared with traditional laboratory methods to examine the suitability of in situ pXRF. The results show that the pXRF analysis achieved satisfactory accuracy and precision in measuring As, Cr, Cu, Ni, Pb, and Zn in soils, and meets the requirements of the relevant detection technology specifications. For the certified reference soil samples, the pXRF results of As, Cr, Cu, Ni, Pb, and Zn show good linear relationships and coefficients of determination with the values measured using the reference analysis methods; with the exception of Ni, all the measured values were within the 95% confidence level. In the soil samples, the coefficients of determination between Cu, Zn, Pb, and Ni concentrations measured laboratory pXRF and the values measured with laboratory analysis all reach 0.9, showing a good linear relationship; however, there were large deviations between methods for Cr and As. This study provides reference data and scientific support for rapid detection of heavy metals in soils using pXRF in site investigation, which can better guide the practical application of pXRF.

Detection limits for real-time source water monitoring using indigenous freshwater microalgae

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rodriguez Jr, Miguel; Greenbaum, Elias

This research identified toxin detection limits using the variable fluorescence of naturally occurring microalgae in source drinking water for five chemical toxins with different molecular structures and modes of toxicity. The five chemicals investigated were atrazine, Diuron, paraquat, methyl parathion, and potassium cyanide. Absolute threshold sensitivities of the algae for detection of the toxins in unmodified source drinking water were measured. Differential kinetics between the rate of action of the toxins and natural changes in algal physiology, such as diurnal photoinhibition, are significant enough that effects of the toxin can be detected and distinguished from the natural variance. This ismore » true even for physiologically impaired algae where diminished photosynthetic capacity may arise from uncontrollable external factors such as nutrient starvation. Photoinhibition induced by high levels of solar radiation is a predictable and reversible phenomenon that can be dealt with using a period of dark adaption of 30 minutes or more.« less

Detection limits of Legionella pneumophila in environmental samples after co-culture with Acanthamoeba polyphaga

PubMed Central

2013-01-01

Background The efficiency of recovery and the detection limit of Legionella after co-culture with Acanthamoeba polyphaga are not known and so far no investigations have been carried out to determine the efficiency of the recovery of Legionella spp. by co-culture and compare it with that of conventional culturing methods. This study aimed to assess the detection limits of co-culture compared to culture for Legionella pneumophila in compost and air samples. Compost and air samples were spiked with known concentrations of L. pneumophila. Direct culturing and co-culture with amoebae were used in parallel to isolate L. pneumophila and recovery standard curves for both methods were produced for each sample. Results The co-culture proved to be more sensitive than the reference method, detecting 102-103 L. pneumophila cells in 1 g of spiked compost or 1 m3 of spiked air, as compared to 105-106 cells in 1 g of spiked compost and 1 m3 of spiked air. Conclusions Co-culture with amoebae is a useful, sensitive and reliable technique to enrich L. pneumophila in environmental samples that contain only low amounts of bacterial cells. PMID:23442526

Sample-morphology effects on x-ray photoelectron peak intensities. II. Estimation of detection limits for thin-film materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Powell, Cedric J., E-mail: cedric.powell@nist.gov; Werner, Wolfgang S. M.; Smekal, Werner

2014-09-01

The authors show that the National Institute of Standards and Technology database for the simulation of electron spectra for surface analysis (SESSA) can be used to determine detection limits for thin-film materials such as a thin film on a substrate or buried at varying depths in another material for common x-ray photoelectron spectroscopy (XPS) measurement conditions. Illustrative simulations were made for a W film on or in a Ru matrix and for a Ru film on or in a W matrix. In the former case, the thickness of a W film at a given depth in the Ru matrix wasmore » varied so that the intensity of the W 4d{sub 5/2} peak was essentially the same as that for a homogeneous RuW{sub 0.001} alloy. Similarly, the thickness of a Ru film at a selected depth in the W matrix was varied so that the intensity of the Ru 3p{sub 3/2} peak matched that from a homogeneous WRu{sub 0.01} alloy. These film thicknesses correspond to the detection limits of each minor component for measurement conditions where the detection limits for a homogeneous sample varied between 0.1 at. % (for the RuW{sub 0.001} alloy) and 1 at. % (for the WRu{sub 0.01} alloy). SESSA can be similarly used to convert estimates of XPS detection limits for a minor species in a homogeneous solid to the corresponding XPS detection limits for that species as a thin film on or buried in the chosen solid.« less

System for detecting and limiting electrical ground faults within electrical devices

DOEpatents

Gaubatz, Donald C.

1990-01-01

An electrical ground fault detection and limitation system for employment with a nuclear reactor utilizing a liquid metal coolant. Elongate electromagnetic pumps submerged within the liquid metal coolant and electrical support equipment experiencing an insulation breakdown occasion the development of electrical ground fault current. Without some form of detection and control, these currents may build to damaging power levels to expose the pump drive components to liquid metal coolant such as sodium with resultant undesirable secondary effects. Such electrical ground fault currents are detected and controlled through the employment of an isolated power input to the pumps and with the use of a ground fault control conductor providing a direct return path from the affected components to the power source. By incorporating a resistance arrangement with the ground fault control conductor, the amount of fault current permitted to flow may be regulated to the extent that the reactor may remain in operation until maintenance may be performed, notwithstanding the existence of the fault. Monitors such as synchronous demodulators may be employed to identify and evaluate fault currents for each phase of a polyphase power, and control input to the submerged pump and associated support equipment.

Studies on bronze pre-monetary signs found in Dobroudja using XRF and micro-PIXE

NASA Astrophysics Data System (ADS)

Constantinescu, B.; Cristea-Stan, D.; Talmatchi, G.; Ceccato, D.

2016-03-01

We performed compositional analyses on 180 Scythian-type arrowheads and pre-monetary signs using XRF method and on 60 small fragments of such items (approx. 100 microns diameter), sampling being performed on previously corrosion-cleaned areas on their surface, using micro-PIXE. The items are found in Dobroudja, Istros-Histria region. The most relevant for numismatists result is that for each finding place the same type of alloy was used both for fighting arrowheads and for pre-monetary signs. Our analyses revealed three types of alloys: Cu-Sn-Pb ("normal" bronze), Cu-Sn-Mn-Pb and Cu-Sn-Sb-Pb. The presence of antimony suggests the use of fahlore-type poly-metals deposits, most probably from Caucasus Mountains. The problem of ancient bronze containing manganese is more complicated; an explanation could be the use of manganese oxides as flux necessary to smelt oxidized ores.

Visualizing the 17th century underpainting in Portrait of an Old Man by Rembrandt van Rijn using synchrotron-based scanning macro-XRF

NASA Astrophysics Data System (ADS)

Alfeld, Matthias; Siddons, D. Peter; Janssens, Koen; Dik, Joris; Woll, Arthur; Kirkham, Robin; van de Wetering, Ernst

2013-04-01

In 17th century Old Master Paintings, the underpainting generally refers to the first sketch of a composition. The underpainting is applied to a prepared ground using a monochrome, brown oil paint to roughly indicate light, shade and contours. So far, methods to visualize the underpainting—other than in localized cross-sections—have been very limited. Neither infrared reflectography nor neutron induced autoradiography have proven to be practical, adequate visualization tools. Thus, although of fundamental interest in the understanding of a painting's genesis, the underpainting has virtually escaped all imaging efforts. In this contribution we will show that 17th century underpainting may consist of a highly heterogeneous mixture of pigments, including copper pigments. We suggest that this brown pigment mixture is actually the recycled left-over of a palette scraping. With copper as the heaviest exclusive elemental component, we will hence show in a case study on a Portrait of an Old Man attributed to Rembrandt van Rijn how scanning macro-XRF can be used to efficiently visualize the underpainting below the surface painting and how this information can contribute to the discussion of the painting's authenticity.

Comparison of detection limit in fiber-based conventional, amplified, and gain-clamped cavity ring-down techniques

NASA Astrophysics Data System (ADS)

Sharma, K.; Abdul Khudus, M. I. M.; Alam, S. U.; Bhattacharya, S.; Venkitesh, D.; Brambilla, G.

2018-01-01

Relative performance and detection limit of conventional, amplified, and gain-clamped cavity ring-down techniques (CRDT) in all-fiber configurations are compared experimentally for the first time. Refractive index measurement using evanescent field in tapered fibers is used as a benchmark for the comparison. The systematic optimization of a nested-loop configuration in gain-clamped CRDT is also discussed, which is crucial for achieving a constant gain in a CRDT experiment. It is found that even though conventional CRDT has the lowest standard error in ring-down time (Δτ), the value of ring-down time (τ) is very small, thus leading to poor detection limit. Amplified CRDT provides an improvement in τ, albeit with two orders of magnitude higher Δτ due to amplifier noise. The nested-loop configuration in gain-clamped CRDT helps in reducing Δτ by an order of magnitude as compared to amplified CRDT whilst retaining the improvement in τ. A detection limit of 1 . 03 × 10-4 RIU at refractive index of 1.322 with a 3 mm long and 4.5 μm diameter tapered fiber is demonstrated with the gain-clamped CRDT.

Detection limits of organic compounds achievable with intense, short-pulse lasers.

PubMed

Miles, Jordan; De Camillis, Simone; Alexander, Grace; Hamilton, Kathryn; Kelly, Thomas J; Costello, John T; Zepf, Matthew; Williams, Ian D; Greenwood, Jason B

2015-06-21

Many organic molecules have strong absorption bands which can be accessed by ultraviolet short pulse lasers to produce efficient ionization. This resonant multiphoton ionization scheme has already been exploited as an ionization source in time-of-flight mass spectrometers used for environmental trace analysis. In the present work we quantify the ultimate potential of this technique by measuring absolute ion yields produced from the interaction of 267 nm femtosecond laser pulses with the organic molecules indole and toluene, and gases Xe, N2 and O2. Using multiphoton ionization cross sections extracted from these results, we show that the laser pulse parameters required for real-time detection of aromatic molecules at concentrations of one part per trillion in air and a limit of detection of a few attomoles are achievable with presently available commercial laser systems. The potential applications for the analysis of human breath, blood and tissue samples are discussed.

Flexible Modeling of Survival Data with Covariates Subject to Detection Limits via Multiple Imputation.

PubMed

Bernhardt, Paul W; Wang, Huixia Judy; Zhang, Daowen

2014-01-01

Models for survival data generally assume that covariates are fully observed. However, in medical studies it is not uncommon for biomarkers to be censored at known detection limits. A computationally-efficient multiple imputation procedure for modeling survival data with covariates subject to detection limits is proposed. This procedure is developed in the context of an accelerated failure time model with a flexible seminonparametric error distribution. The consistency and asymptotic normality of the multiple imputation estimator are established and a consistent variance estimator is provided. An iterative version of the proposed multiple imputation algorithm that approximates the EM algorithm for maximum likelihood is also suggested. Simulation studies demonstrate that the proposed multiple imputation methods work well while alternative methods lead to estimates that are either biased or more variable. The proposed methods are applied to analyze the dataset from a recently-conducted GenIMS study.

Evaluation on the detection limit of blood hemoglobin using photolepthysmography based on path-length optimization

NASA Astrophysics Data System (ADS)

Sun, Di; Guo, Chao; Zhang, Ziyang; Han, Tongshuai; Liu, Jin

2016-10-01

The blood hemoglobin concentration's (BHC) measurement using Photoplethysmography (PPG), which gets blood absorption to near infrared light from the instantaneous pulse of transmitted light intensity, has not been applied to the clinical use due to the non-enough precision. The main challenge might be caused of the non-enough stable pulse signal when it's very weak and it often varies in different human bodies or in the same body with different physiological states. We evaluated the detection limit of BHC using PPG as the measurement precision level, which can be considered as a best precision result because we got the relative stable subject's pulse signals recorded by using a spectrometer with high signal-to-noise ratio (SNR) level, which is about 30000:1 in short term. Moreover, we optimized the used pathlength using the theory based on optimum pathlength to get a better sensitivity to the absorption variation in blood. The best detection limit was evaluated as about 1 g/L for BHC, and the best SNR of pulse for in vivo measurement was about 2000:1 at 1130 and 1250 nm. Meanwhile, we conclude that the SNR of pulse signal should be better than 400:1 when the required detection limit is set to 5 g/L. Our result would be a good reference to the BHC measurement to get a desired BHC measurement precision of real application.

ED-XRF spectrometry-based comparative inorganic profile of leaf-derived in vitro calli and in vivo leaf samples of Phyllanthus amarus Schum. & Thonn.--a hepatoprotective herb.

PubMed

Nayak, P; Behera, P R; Thirunavoukkarasu, M; Chand, P K

2011-03-01

The Energy Dispersive X-ray Fluorescence (ED-XRF) set-up incorporating a molybdenum secondary exciter was used for quantitative determination of major and minor elements in leaves of in vivo grown medicinal herb Phyllanthus amarus vis-á-vis its leaf-derived in vitro callus culture. The elements such as K, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Se, Rb, Sr and Pb were identified, quantified and compared between both the sources. Experimental results revealed that, compared to the naturally grown herb, in vitro leaf-derived callus cultures were more efficient in accumulating inorganic elements, especially trace elements, which are essential for growth and development and more importantly for prevention and cure of diseases. This investigation on a medicinal plant species is the first of its kind to have used the ED-XRF technique to demonstrate a comparative account of the elemental profile of in vitro callus cultures with their in vivo donor in order to explore the possibility of exploiting the former as a viable alternative and a renewable source of phytochemicals. Copyright © 2010 Elsevier Ltd. All rights reserved.

Modeling of a Single-Notch Microfiber Coupler for High-Sensitivity and Low Detection-Limit Refractive Index Sensing.

PubMed

Zhang, Jiali; Shi, Lei; Zhu, Song; Xu, Xinbiao; Zhang, Xinliang

2016-05-11

A highly sensitive refractive index sensor with low detection limit based on an asymmetric optical microfiber coupler is proposed. It is composed of a silica optical microfiber and an As₂Se₃ optical microfiber. Due to the asymmetry of the microfiber materials, a single-notch transmission spectrum is demonstrated by the large refractive index difference between the two optical microfibers. Compared with the symmetric coupler, the bandwidth of the asymmetric structure is over one order of magnitude narrower than that of the former. Therefore, the asymmetric optical microfiber coupler based sensor can reach over one order of magnitude smaller detection limit, which is defined as the minimal detectable refractive index change caused by the surrounding analyte. With the advantage of large evanescent field, the results also show that a sensitivity of up to 3212 nm per refractive index unit with a bandwidth of 12 nm is achieved with the asymmetric optical microfiber coupler. Furthermore, a maximum sensitivity of 4549 nm per refractive index unit can be reached while the radii of the silica optical microfiber and As₂Se₃ optical microfiber are 0.5 μm and a 0.128 μm, respectively. This sensor component may have important potential for low detection-limit physical and biochemical sensing applications.

Statistical Methods for Generalized Linear Models with Covariates Subject to Detection Limits.

PubMed

Bernhardt, Paul W; Wang, Huixia J; Zhang, Daowen

2015-05-01

Censored observations are a common occurrence in biomedical data sets. Although a large amount of research has been devoted to estimation and inference for data with censored responses, very little research has focused on proper statistical procedures when predictors are censored. In this paper, we consider statistical methods for dealing with multiple predictors subject to detection limits within the context of generalized linear models. We investigate and adapt several conventional methods and develop a new multiple imputation approach for analyzing data sets with predictors censored due to detection limits. We establish the consistency and asymptotic normality of the proposed multiple imputation estimator and suggest a computationally simple and consistent variance estimator. We also demonstrate that the conditional mean imputation method often leads to inconsistent estimates in generalized linear models, while several other methods are either computationally intensive or lead to parameter estimates that are biased or more variable compared to the proposed multiple imputation estimator. In an extensive simulation study, we assess the bias and variability of different approaches within the context of a logistic regression model and compare variance estimation methods for the proposed multiple imputation estimator. Lastly, we apply several methods to analyze the data set from a recently-conducted GenIMS study.

Analysis of sculptures using XRF and X-ray radiography

NASA Astrophysics Data System (ADS)

Calza, C.; Oliveira, D. F.; Freitas, R. P.; Rocha, H. S.; Nascimento, J. R.; Lopes, R. T.

2015-11-01

This work reports the analysis of two sacred images on polychrome wood using X-ray Radiography and Energy Dispersive X-Ray Fluorescence. The first case is the analysis of a sculpture portraying Saint Sebastian, the patron saint of Rio de Janeiro, which is considered the second most ancient sacred image of Brazil. This sculpture was made in Portugal and was transported to Brazil by Estácio Sá, founder of the city of Rio de Janeiro, in 1565. Nowadays, it is located on the main altar of the Church of Capuchin Friars. The second case is the analysis of a sculpture representing Our Lady of Conception, which is located in the D. João VI Museum (EBA/UFRJ, Rio de Janeiro). The objective of these analyses was to evaluate the general conditions of the sculptures, identifying possible problems and internal damages, areas that revealed signs of previous retouchings and the materials and pigments employed by the artists, in order to assist its restoration procedures. EDXRF measurements were carried out with a portable system, developed at the Nuclear Instrumentation Laboratory, consisting of a Si-PIN XR-100CR detector from Amptek and an Oxford TF3005 X-ray tube with W anode. An X-ray source, a CR System GE CR50P and IP detectors were used to perform the radiographs. The XRF analysis of the sculptures identified the original pigments in both cases and the radiographic images revealed details of the manufacture; restored regions; extensive use of lead white; presence of cracks on the wood; use of nails and spikes, etc.

Spatially resolved XRF, XAFS, XRD, STXM and IR investigation of a natural U-rich clay

NASA Astrophysics Data System (ADS)

Denecke, M. A.; Michel, P.; Schäfer, T.; Huber, F.; Rickers, K.; Rothe, J.; Dardenne, K.; Brendebach, B.; Vitova, T.; Elie, M.

2009-11-01

Combined spatially resolved hard X-ray μ-XRF and μ-XAFS studies using an X-ray beam with micrometer dimensions at the INE-Beamline for actinide research at ANKA and Beamline L at HASYLAB with those from scanning transmission soft X-ray microscopy (STXM) and synchrotron-based Fourier transform infrared microspectroscopy (μ-FTIR) recorded with beam spots in the nanometer range are used to study a U-rich clay originating from Autunian shales in the Permian Lodève Basin (France). This argillaceous formation is a natural U deposit associated with organic matter (bitumen). Results allow us to differentiate between possible mechanisms leading to U enrichment: likely U immobilization via reaction with organic material associated with clay mineral. Such investigations support development of reliable assessment of the long term radiological safety for proposed nuclear waste disposal sites.

Trace elemental analysis of school chalk using energy dispersive X-ray florescence spectroscopy (ED-XRF)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maruthi, Y. A., E-mail: ymjournal2014@gmail.com; Das, N. Lakshmana, E-mail: nldas9@gmail.com; Ramprasad, S., E-mail: ramprasadsurakala@gmail.com

The present studies focus the quantitative analysis of elements in school chalk to ensure the safety of its use. The elements like Calcium (Ca), Aluminum (Al), Iron (Fe), Silicon (Si) and Chromium (Cr) were analyzed from settled chalk dust samples collected from five classrooms (CD-1) and also from another set of unused chalk samples collected from local market (CD-2) using Energy Dispersive X-Ray florescence(ED-XRF) spectroscopy. Presence of these elements in significant concentrations in school chalk confirmed that, it is an irritant and occupational hazard. It is suggested to use protective equipments like filtered mask for mouth, nose and chalk holders.more » This study also suggested using the advanced mode of techniques like Digital boards, marker boards and power point presentations to mitigate the occupational hazard for classroom chalk.« less

Electron density of Rhizophora spp. wood using Compton scattering technique at 15.77, 17.48 and 22.16 keV XRF energies

NASA Astrophysics Data System (ADS)

Shakhreet, B. Z.; Bauk, S.; Shukri, A.

2015-02-01

Compton (incoherently) scattered photons which are directly proportional to the electron density of the scatterer, have been employed in characterizing Rhizophora spp. as breast tissue equivalent. X-ray fluorescent scattered incoherently from Rhizophora spp. sample was measured using Si-PIN detector and three XRF energy values 15.77, 17.48 and 22.16 keV. This study is aimed at providing electron density information in support of the introduction of new tissue substitute materials for mammography phantoms.

Change in Localizations of Arsenic in Rice Grains After Cooking with High Arsenic Waters - µXRF and XANES studies

NASA Astrophysics Data System (ADS)

Datta, S.; Ryan, B.; Kumar, N.; Bortz, T.; Bolen, Z. T.

2016-12-01

Threats of Arsenic (As) through food uptake, via consumption of rice, is a potential pathway that presents a concern not only for the millions of inhabitants who reside in river valleys and irrigate their soil with contaminated water, but the global rice market as well. This study focuses on high As rice from India and Bangladesh grown in such soils, and the effect of boiling rice with As-contaminated water in preparation for dietary intake. Husked and unhusked rice grains were boiled with >500 µg/L As-bearing water from the field to simulate local cooking methods. The resulting cooked water was analyzed using iCAP low limit detection via ICP-MS to understand the changes in dissolved elemental concentrations before and after cooking, and HPLC was introduced to measure for changes in As speciation in the waters. Using spectroscopic methods such as µXRF mapping associated with µXANES, distribution/localization and speciation changes of As in rice grains were identified. Further, with Linear Combination Fitting (LCF) of XANES spectra utilizing relevant reference compounds (As-S, AsIII, AsV, MMA and DMA), organic and inorganic As species were able to be mapped within rice grains. The results for uncooked/raw grains showed that predominantly As-S combined with AsIII and AsV accounted for 90% of speciation in most samples, localized in areas such as the outer aleurone layer. When analyzing cooked rice grains, the speciation appears to be an unidentified As species while the best LCF shows between 63-93% of As as MMA. Arsenic was found less localized throughout the cooked grains but rather heterogeneously distributed when compared to the uncooked/raw samples. The analyses of boiled/cooked water resulted in a significant decrease in dissolved As post-cooking (90%), but a subsequent increase in elements such as K, La, Li, Mo, Na, Ni, and Zr was observed; As-V was shown to be the main in-As species in the cooked water. The impact that this study portrays is consuming rice

An interlaboratory comparison study on the measurement of elements in PM10

NASA Astrophysics Data System (ADS)

Yatkin, Sinan; Belis, Claudio A.; Gerboles, Michel; Calzolai, Giulia; Lucarelli, Franco; Cavalli, Fabrizia; Trzepla, Krystyna

2016-01-01

An inter-laboratory comparison study was conducted to measure elemental loadings on PM10 samples, collected in Ispra, a regional background/rural site in Italy, using three different XRF (X-ray Fluorescence) methods, namely Epsilon 5 by linear calibration, Quant'X by the standardless analysis, and PIXE (Particle Induced X-ray Emission) with linear calibration. A subset of samples was also analyzed by ICP-MS (Inductively Coupled Plasma-Mass Spectrometry). Several metrics including method detection limits (MDLs), precision, bias from a NIST standard reference material (SRM 2783) quoted values, relative absolute difference, orthogonal regression and the ratio of the absolute difference between the methods to claimed uncertainty were used to compare the laboratories. The MDLs were found to be comparable for many elements. Precision estimates were less than 10% for the majority of the elements. Absolute biases from SRM 2783 remained less than 20% for the majority of certified elements. The regression results of PM10 samples showed that the three XRF laboratories measured very similar mass loadings for S, K, Ti, Mn, Fe, Cu, Br, Sr and Pb with slopes within 20% of unity. The ICP-MS results confirmed the agreement and discrepancies between XRF laboratories for Al, K, Ca, Ti, V, Cu, Sr and Pb. The ICP-MS results are inconsistent with the XRF laboratories for Fe and Zn. The absolute differences between the XRF laboratories generally remained within their claimed uncertainties, showing a pattern generally consistent with the orthogonal regression results.

Picomolar detection limits with current-polarized Pb2+ ion-selective membranes.

PubMed

Pergel, E; Gyurcsányi, R E; Tóth, K; Lindner, E

2001-09-01

Minor ion fluxes across ion-selective membranes bias submicromolar activity measurements with conventional ion-selective electrodes. When ion fluxes are balanced, the lower limit of detection is expected to be dramatically improved. As proof of principle, the flux of lead ions across an ETH 5435 ionophore-based lead-selective membrane was gradually compensated by applying a few nanoamperes of galvanostatic current. When the opposite ion fluxes were matched, and the undesirable leaching of primary ions was eliminated, Nernstian response down to 3 x 10(-12) M was achieved.

Detection limit of Mycobacterium chimaera in water samples for monitoring medical device safety: insights from a pilot experimental series.

PubMed

Schreiber, P W; Köhler, N; Cervera, R; Hasse, B; Sax, H; Keller, P M

2018-07-01

A growing number of Mycobacterium chimaera infections after cardiosurgery have been reported by several countries. These potentially fatal infections were traced back to contaminated heater-cooler devices (HCDs), which use water as a heat transfer medium. Aerosolization of water contaminated with M. chimaera from HCDs enables airborne transmission to patients undergoing open chest surgery. Infection control teams test HCD water samples for mycobacterial growth to guide preventive measures. The detection limit of M. chimaera in water samples, however, has not previously been investigated. To determine the detection limit of M. chimaera in water samples using laboratory-based serial dilution tests. An M. chimaera strain representative of the international cardiosurgery-associated M. chimaera outbreak was used to generate a logarithmic dilution series. Two different water volumes, 50 and 1000mL, were inoculated, and, after identical processing (centrifugation, decantation, and decontamination), seeded on mycobacteria growth indicator tube (MGIT) and Middlebrook 7H11 solid media. MGIT consistently showed a lower detection limit than 7H11 solid media, corresponding to a detection limit of ≥1.44 × 10 4 cfu/mL for 50mL and ≥2.4cfu/mL for 1000mL water samples. Solid media failed to detect M. chimaera in 50mL water samples. Depending on water volume and culture method, major differences exist in the detection limit of M. chimaera. In terms of sensitivity, 1000mL water samples in MGIT media performed best. Our results have important implications for infection prevention and control strategies in mitigation of the M. chimaera outbreak and healthcare water safety in general. Copyright © 2017 The Author(s). Published by Elsevier Ltd.. All rights reserved.

From nature to MEMS: towards the detection-limit of crickets' hair sensors

NASA Astrophysics Data System (ADS)

Dagamseh, A. M. K.

2013-05-01

Crickets use highly sensitive mechanoreceptor hairs to detect approaching spiders. The high sensitivity of these hairs enables perceiving tiny air-movements which are only just distinguishable from noise. This forms our source of inspiration to design sensitive arrays made of artificial hair sensors for flow pattern observation i.e. Flow camera. The realization of such high-sensitive hair sensor requires designs with low thermo-mechanical noise to match the detection-limit of crickets' hairs. Here we investigate the damping factor in our artificial hair-sensor using different models as it is the source of the thermo-mechanical noise in MEMS structures. The results show that the damping factor estimated in air is in the range of 10-12 N.m/rad.s-1 which translates into a 52 μm/s threshold flow velocity.

Batch Fabrication of Ultrasensitive Carbon Nanotube Hydrogen Sensors with Sub-ppm Detection Limit.

PubMed

Xiao, Mengmeng; Liang, Shibo; Han, Jie; Zhong, Donglai; Liu, Jingxia; Zhang, Zhiyong; Peng, Lianmao

2018-04-27

Carbon nanotube (CNT) has been considered as an ideal channel material for building highly sensitive gas sensors. However, the reported H 2 sensors based on CNT always suffered from the low sensitivity or low production. We developed the technology to massively fabricate ultra-highly sensitive H 2 sensors based on solution derived CNT network through comprehensive optimization of the CNT material, device structure, and fabrication process. In the H 2 sensors, high semiconducting purity solution-derived CNT film sorted by poly[9-(1-octylonoyl)-9 H-carbazole-2,7-diyl](PCz) is used as the main channel, which is decorated with Pd nanoparticles as functionalization for capturing H 2 . Meanwhile, Ti contacts are used to form a Schottky barrier for enhancing transferred charge-induced resistance change, and then a response of resistance change by 3 orders of magnitude is achieved at room temperature under the concentration of ∼311 ppm with a very fast response time of approximately 7 s and a detection limit of 890 ppb, which is the highest response to date for CNT H 2 sensors and the very first time to show the sub-ppm detection for H 2 at room temperature. Furthermore, the detection limit concentration can be improved to 89 ppb at 100 °C. The batch fabrication of CNT film H 2 sensors with ultra-high sensitivity and high uniformity is ready to promote CNT devices to application for the first time in some specialized field.

Characterization of Archaeological Sediments Using Fourier Transform Infrared (FT-IR) and Portable X-ray Fluorescence (pXRF): An Application to Formative Period Pyro-Industrial Sites in Pacific Coastal Southern Chiapas, Mexico.

PubMed

Neff, Hector; Bigney, Scott J; Sakai, Sachiko; Burger, Paul R; Garfin, Timothy; George, Richard G; Culleton, Brendan J; Kennett, Douglas J

2016-01-01

Archaeological sediments from mounds within the mangrove zone of far-southern Pacific coastal Chiapas, Mexico, are characterized in order to test the hypothesis that specialized pyro-technological activities of the region's prehistoric inhabitants (salt and ceramic production) created the accumulations visible today. Fourier transform infrared spectroscopy (FT-IR) is used to characterize sediment mineralogy, while portable X-ray fluorescence (pXRF) is used to determine elemental concentrations. Elemental characterization of natural sediments by both instrumental neutron activation analysis (INAA) and pXRF also contribute to understanding of processes that created the archaeological deposits. Radiocarbon dates combined with typological analysis of ceramics indicate that pyro-industrial activity in the mangrove zone peaked during the Late Formative and Terminal Formative periods, when population and monumental activity on the coastal plain and piedmont were also at their peaks. © The Author(s) 2015.

Photonic crystal enhanced fluorescence using a quartz substrate to reduce limits of detection

PubMed Central

Pokhriyal, Anusha; Lu, Meng; Chaudhery, Vikram; Huang, Cheng-Sheng; Schulz, Stephen; Cunningham, Brian T.

2010-01-01

A Photonic Crystal (PC) surface fabricated upon a quartz substrate using nanoimprint lithography has been demonstrated to enhance light emission from fluorescent molecules in close proximity to the PC surface. Quartz was selected for its low autofluorescence characteristics compared to polymer-based PCs, improving the detection sensitivity and signal-to-noise ratio (SNR) of PC Enhanced Fluorescence (PCEF). Nanoimprint lithography enables economical fabrication of the subwavelength PCEF surface structure over entire 1x3 in2 quartz slides. The demonstrated PCEF surface supports a transverse magnetic (TM) resonant mode at a wavelength of λ = 632.8 nm and an incident angle of θ = 11°, which amplifies the electric field magnitude experienced by surface-bound fluorophores. Meanwhile, another TM mode at a wavelength of λ = 690 nm and incident angle of θ = 0° efficiently directs the fluorescent emission toward the detection optics. An enhancement factor as high as 7500 × was achieved for the detection of LD-700 dye spin-coated upon the PC, compared to detecting the same material on an unpatterned glass surface. The detection of spotted Alexa-647 labeled polypeptide on the PC exhibits a 330 × SNR improvement. Using dose-response characterization of deposited fluorophore-tagged protein spots, the PCEF surface demonstrated a 140 × lower limit of detection compared to a conventional glass substrate. PMID:21164826

Accounting for Limited Detection Efficiency and Localization Precision in Cluster Analysis in Single Molecule Localization Microscopy

PubMed Central

Shivanandan, Arun; Unnikrishnan, Jayakrishnan; Radenovic, Aleksandra

2015-01-01

Single Molecule Localization Microscopy techniques like PhotoActivated Localization Microscopy, with their sub-diffraction limit spatial resolution, have been popularly used to characterize the spatial organization of membrane proteins, by means of quantitative cluster analysis. However, such quantitative studies remain challenged by the techniques’ inherent sources of errors such as a limited detection efficiency of less than 60%, due to incomplete photo-conversion, and a limited localization precision in the range of 10 – 30nm, varying across the detected molecules, mainly depending on the number of photons collected from each. We provide analytical methods to estimate the effect of these errors in cluster analysis and to correct for them. These methods, based on the Ripley’s L(r) – r or Pair Correlation Function popularly used by the community, can facilitate potentially breakthrough results in quantitative biology by providing a more accurate and precise quantification of protein spatial organization. PMID:25794150

Elemental composition study of heavy metal (Ni, Cu, Zn) in riverbank soil by electrokinetic-assisted phytoremediation using XRF and SEM/EDX

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jamari, Suhailly; Embong, Zaidi; Bakar, Ismail

Electrokinetic (EK)-assisted phytoremediation is one of the methods that have a big potential in enhancing the ability of plant uptake in soils remediation process. This research was conducted to investigate the difference in elemental composition concentration of riverbank soil and the change of pH between pre- and post-phytoremediation under the following condition: 1) control or as-receive sample; 2) Dieffenbachia spp plant with EK system (a pair of EK electrodes connected to a direct current (DC) power supply). After the electrodes were connected to a magnitude of 6V/cm{sup −1} electric field for 4 hours/day, the soil and plant samples were analyzedmore » using and X-ray Fluorescence Spectrometer (XRF) and Scanning Electron Microscope / Energy Dispersive X-ray Spectroscopy (SEM/EDX). The SEM/EDX analysis showed that concentration of elemental composition (Ni, Cu and Zn) in post-phytoremediation plant powder samples had increase while elemental concentrations in the post-phytoremediation soil samples were decreased. XRF analysis presented a variation in soil elemental composition concentration from anode to cathode where the concentration near anode region increased while decreased near the cathode region. A significant changes in soil pH were obtained where the soil pH increase in cathode region while decrease in anode region. The results reveal that the assistance of EK in phytoremediation process has increase the efficiency of plant uptake.« less

Limits of linearity and detection for some drugs of abuse.

PubMed

Needleman, S B; Romberg, R W

1990-01-01

The limits of linearity (LOL) and detection (LOD) are important factors in establishing the reliability of an analytical procedure for accurately assaying drug concentrations in urine specimens. Multiple analyses of analyte over an extended range of concentrations provide a measure of the ability of the analytical procedure to correctly identify known quantities of drug in a biofluid matrix. Each of the seven drugs of abuse gives linear analytical responses from concentrations at or near their LOD to concentrations several-fold higher than those generally encountered in the drug screening laboratory. The upper LOL exceeds the Department of Navy (DON) cutoff values by factors of approximately 2 to 160. The LOD varies from 0.4 to 5.0% of the DON cutoff value for each drug. The limit of quantitation (LOQ) is calculated as the LOD + 7 SD. The range for LOL is greater for drugs analyzed with deuterated internal standards compared with those using conventional internal standards. For THC acid, cocaine, PCP, and morphine, LOLs are 8 to 160-fold greater than the defined cutoff concentrations. For the other drugs, the LOL's are only 2 to 4-fold greater than the defined cutoff concentrations.

Diamond-based electrochemical aptasensor realizing a femtomolar detection limit of bisphenol A.

PubMed

Ma, Yibo; Liu, Junsong; Li, Hongdong

2017-06-15

In this study, we designed and fabricated an electrochemical impedance aptasensor based on Au nanoparticles (Au-NPs) coated boron-doped diamond (BDD) modified with aptamers, and 6-mercapto-1-hexanol (MCH) for the detection of bisphenol A (BPA). The constructed BPA aptasensor exhibits good linearity from 1.0×10 -14 to 1.0×10 -9 molL -1 . The detection limitation of 7.2×10 -15 molL -1 was achieved, which can be attributed to the synergistic effect of combining BDD with Au-NPs, aptamers, and MCH. The examine results of BPA traces in Tris-HCl buffer and in milk, UV spectra of aptamer/BPA and interference test revealed that the novel aptasensors are of high sensitivity, specificity, stability and repeatability, which could be promising in practical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

The Fast Evolution of SN 2010bh Associated with XRF 100316D

NASA Technical Reports Server (NTRS)

Olivares E., F.; Greiner, J.; Schady, P.; Rau, A.; Klose, S.; Kruhler, T.; Afonso, P. M. J.; Updike, A. C.; Nardini, M.; Filgas, R.;

Detection, Size, Measurement, and Structural Analysis Limits for the 2MASS, UKIDSS-LAS, and VISTA VIKING Surveys

NASA Astrophysics Data System (ADS)

Andrews, Stephen K.; Kelvin, Lee S.; Driver, Simon P.; Robotham, Aaron S. G.

2014-01-01

The 2MASS, UKIDSS-LAS, and VISTA VIKING surveys have all now observed the GAMA 9hr region in the Ks band. Here we compare the detection rates, photometry, basic size measurements, and single-component GALFIT structural measurements for a sample of 37 591 galaxies. We explore the sensitivity limits where the data agree for a variety of issues including: detection, star-galaxy separation, photometric measurements, size and ellipticity measurements, and Sérsic measurements. We find that 2MASS fails to detect at least 20% of the galaxy population within all magnitude bins, however for those that are detected we find photometry is robust (± 0.2 mag) to 14.7 AB mag and star-galaxy separation to 14.8 AB mag. For UKIDSS-LAS we find incompleteness starts to enter at a flux limit of 18.9 AB mag, star-galaxy separation is robust to 16.3 AB mag, and structural measurements are robust to 17.7 AB mag. VISTA VIKING data are complete to approximately 20.0 AB mag and structural measurements appear robust to 18.8 AB mag.

Direct Detection Electron Energy-Loss Spectroscopy: A Method to Push the Limits of Resolution and Sensitivity.

PubMed

Hart, James L; Lang, Andrew C; Leff, Asher C; Longo, Paolo; Trevor, Colin; Twesten, Ray D; Taheri, Mitra L

2017-08-15

In many cases, electron counting with direct detection sensors offers improved resolution, lower noise, and higher pixel density compared to conventional, indirect detection sensors for electron microscopy applications. Direct detection technology has previously been utilized, with great success, for imaging and diffraction, but potential advantages for spectroscopy remain unexplored. Here we compare the performance of a direct detection sensor operated in counting mode and an indirect detection sensor (scintillator/fiber-optic/CCD) for electron energy-loss spectroscopy. Clear improvements in measured detective quantum efficiency and combined energy resolution/energy field-of-view are offered by counting mode direct detection, showing promise for efficient spectrum imaging, low-dose mapping of beam-sensitive specimens, trace element analysis, and time-resolved spectroscopy. Despite the limited counting rate imposed by the readout electronics, we show that both core-loss and low-loss spectral acquisition are practical. These developments will benefit biologists, chemists, physicists, and materials scientists alike.

Na, Mg, Ni and Cs distribution and speciation after long-term alteration of a simulated nuclear waste glass: A micro-XAS/XRF/XRD and wet chemical study

NASA Astrophysics Data System (ADS)

Curti, Enzo; Dähn, Rainer; Farges, François; Vespa, Marika

2009-04-01

trioctahedral Mg-clay minerals. Alternative models assuming other elements (Ni, Al, Fe) in addition to Mg in the second shell could not be fitted successfully. Aqueous concentration data were used to calculate the speciation of the leaching solutions. Saturation index (SI) calculations indicate undersaturation with respect to NiCO 3 and NiSO 4·7H 2O, but oversaturation with respect to β-Ni(OH) 2. The latter result is probably due to the omission of Ni borate and Ni silicate complexes in the speciation calculations, for which formation constants are not available. With the help of estimation techniques, we could infer that such complexes would dominate the Ni speciation and consequently reduce the SI below the saturation of β-Ni(OH) 2. The μ-XRF maps show that Cs is uniformly distributed in the MW glass, since no region with high Cs concentration could be detected. The Cs L III-edge μ-XAS spectra were all very similar independently of the degree of alteration, indicating similar coordination environments of Cs in the core regions of the glass as well as in the secondary clays. These spectra largely differ from that measured for pollucite (a potential secondary Cs-phase in altered glasses) implying that the coordination environments of Cs in the MW glass and in pollucite are fundamentally different. The present study shows that μ-XRF and μ-XAS are essential tools in determining the fate and the retention mechanisms of radionuclides released from nuclear waste during aqueous alteration. Our spectroscopic analyses allowed us to exclude formation of specific Ni and Cs secondary solids (e.g. nepouite, β-Ni(OH) 2, pollucite) during the aqueous alteration. Ni and Cs are instead distributed as trace elements in the alteration phases formed by major elements during the leaching process. Our results imply that solid solution and/or adsorption equilibria, rather than pure phase solubility equilibria, are the adequate chemical models to determine Ni and Cs aqueous concentrations in

Optimizing detector geometry for trace element mapping by X-ray fluorescence

DOE PAGES

Sun, Yue; Gleber, Sophie -Charlotte; Jacobsen, Chris; ...

2015-01-01

We report that trace metals play critical roles in a variety of systems, ranging from cells to photovoltaics. X-Ray Fluorescence (XRF) microscopy using X-ray excitation provides one of the highest sensitivities available for imaging the distribution of trace metals at sub-100 nm resolution. With the growing availability and increasing performance of synchrotron light source based instruments and X-ray nanofocusing optics, and with improvements in energy-dispersive XRF detectors, what are the factors that limit trace element detectability? To address this question, we describe an analytical model for the total signal incident on XRF detectors with various geometries, including the spectral responsemore » of energy dispersive detectors. This model agrees well with experimentally recorded X-ray fluorescence spectra, and involves much shorter calculation times than with Monte Carlo simulations. With such a model, one can estimate the signal when a trace element is illuminated with an X-ray beam, and when just the surrounding non-fluorescent material is illuminated. From this signal difference, a contrast parameter can be calculated and this can in turn be used to calculate the signal-to-noise ratio (S/N) for detecting a certain elemental concentration. We apply this model to the detection of trace amounts of zinc in biological materials, and to the detection of small quantities of arsenic in semiconductors. In conclusion, we conclude that increased detector collection solid angle is (nearly) always advantageous even when considering the scattered signal. However, given the choice between a smaller detector at 90° to the beam versus a larger detector at 180° (in a backscatter-like geometry), the 90° detector is better for trace element detection in thick samples, while the larger detector in 180° geometry is better suited to trace element detection in thin samples.« less

Optimizing detector geometry for trace element mapping by X-ray fluorescence.

PubMed

Sun, Yue; Gleber, Sophie-Charlotte; Jacobsen, Chris; Kirz, Janos; Vogt, Stefan

2015-05-01

Trace metals play critical roles in a variety of systems, ranging from cells to photovoltaics. X-Ray Fluorescence (XRF) microscopy using X-ray excitation provides one of the highest sensitivities available for imaging the distribution of trace metals at sub-100 nm resolution. With the growing availability and increasing performance of synchrotron light source based instruments and X-ray nanofocusing optics, and with improvements in energy-dispersive XRF detectors, what are the factors that limit trace element detectability? To address this question, we describe an analytical model for the total signal incident on XRF detectors with various geometries, including the spectral response of energy dispersive detectors. This model agrees well with experimentally recorded X-ray fluorescence spectra, and involves much shorter calculation times than with Monte Carlo simulations. With such a model, one can estimate the signal when a trace element is illuminated with an X-ray beam, and when just the surrounding non-fluorescent material is illuminated. From this signal difference, a contrast parameter can be calculated and this can in turn be used to calculate the signal-to-noise ratio (S/N) for detecting a certain elemental concentration. We apply this model to the detection of trace amounts of zinc in biological materials, and to the detection of small quantities of arsenic in semiconductors. We conclude that increased detector collection solid angle is (nearly) always advantageous even when considering the scattered signal. However, given the choice between a smaller detector at 90° to the beam versus a larger detector at 180° (in a backscatter-like geometry), the 90° detector is better for trace element detection in thick samples, while the larger detector in 180° geometry is better suited to trace element detection in thin samples. Copyright © 2015. Published by Elsevier B.V.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sun, Yue; Gleber, Sophie-Charlotte; Jacobsen, Chris

Trace metals play critical roles in a variety of systems, ranging from cells to photovoltaics. X-Ray Fluorescence (XRF) microscopy using X-ray excitation provides one of the highest sensitivities available for imaging the distribution of trace metals at sub-100 nm resolution. With the growing availability and increasing performance of synchrotron light source based instruments and X-ray nanofocusing optics, and with improvements in energy-dispersive XRF detectors, what are the factors that limit trace element detectability? To address this question, we describe an analytical model for the total signal incident on XRF detectors with various geometries, including the spectral response of energy dispersivemore » detectors. This model agrees well with experimentally recorded X-ray fluorescence spectra, and involves much shorter calculation times than with Monte Carlo simulations. With such a model, one can estimate the signal when a trace element is illuminated with an X-ray beam, and when just the surrounding non-fluorescent material is illuminated. From this signal difference, a contrast parameter can be calculated and this can in turn be used to calculate the signal-to-noise ratio (S/N) for detecting a certain elemental concentration. We apply this model to the detection of trace amounts of zinc in biological materials, and to the detection of small quantities of arsenic in semiconductors. We conclude that increased detector collection solid angle is (nearly) always advantageous even when considering the scattered signal. However, given the choice between a smaller detector at 90° to the beam versus a larger detector at 180° (in a backscatter-like geometry), the 90° detector is better for trace element detection in thick samples, while the larger detector in 180° geometry is better suited to trace element detection in thin samples.« less

Optimizing detector geometry for trace element mapping by X-ray fluorescence

PubMed Central

Sun, Yue; Gleber, Sophie-Charlotte; Jacobsen, Chris; Kirz, Janos; Vogt, Stefan

2016-01-01

Trace metals play critical roles in a variety of systems, ranging from cells to photovoltaics. X-Ray Fluorescence (XRF) microscopy using X-ray excitation provides one of the highest sensitivities available for imaging the distribution of trace metals at sub-100 nm resolution. With the growing availability and increasing performance of synchrotron light source based instruments and X-ray nanofocusing optics, and with improvements in energy-dispersive XRF detectors, what are the factors that limit trace element detectability? To address this question, we describe an analytical model for the total signal incident on XRF detectors with various geometries, including the spectral response of energy dispersive detectors. This model agrees well with experimentally recorded X-ray fluorescence spectra, and involves much shorter calculation times than with Monte Carlo simulations. With such a model, one can estimate the signal when a trace element is illuminated with an X-ray beam, and when just the surrounding non-fluorescent material is illuminated. From this signal difference, a contrast parameter can be calculated and this can in turn be used to calculate the signal-to-noise ratio (S/N) for detecting a certain elemental concentration. We apply this model to the detection of trace amounts of zinc in biological materials, and to the detection of small quantities of arsenic in semiconductors. We conclude that increased detector collection solid angle is (nearly) always advantageous even when considering the scattered signal. However, given the choice between a smaller detector at 90° to the beam versus a larger detector at 180° (in a backscatter-like geometry), the 90° detector is better for trace element detection in thick samples, while the larger detector in 180° geometry is better suited to trace element detection in thin samples. PMID:25600825

Optimizing detector geometry for trace element mapping by X-ray fluorescence

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sun, Yue; Gleber, Sophie-Charlotte; Jacobsen, Chris

Trace metals play critical roles in a variety of systems, ranging from cells to photovoltaics. X-Ray Fluorescence (XRF) microscopy using X-ray excitation provides one of the highest sensitivities available for imaging the distribution of trace metals at sub-100 nm resolution. With the growing availability and increasing performance of synchrotron light source based instruments and X-ray nanofocusing optics, and with improvements in energy-dispersive XRF detectors, what are the factors that limit trace element detectability? To address this question, we describe an analytical model for the total signal incident on XRF detectors with various geometries, including the spectral response of energy dispersivemore » detectors. This model agrees well with experimentally recorded X-ray fluorescence spectra, and involves much shorter calculation times than with Monte Carlo simulations. With such a model, one can estimate the signal when a trace element is illuminated with an X-ray beam, and when just the surrounding non-fluorescent material is illuminated. From this signal difference, a contrast parameter can be calculated and this can in turn be used to calculate the signal-to-noise ratio (S/N) for detecting a certain elemental concentration. We apply this model to the detection of trace amounts of zinc in biological materials, and to the detection of small quantities of arsenic in semiconductors. We conclude that increased detector collection solid angle is (nearly) always advantageous even when considering the scattered signal. However, given the choice between a smaller detector at 90° to the beam versus a larger detector at 180° (in a backscatter-like geometry), the 90° detector is better for trace element detection in thick samples, while the larger detector in 180° geometry is better suited to trace element detection in thin samples.« less

Optimizing detector geometry for trace element mapping by X-ray fluorescence

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sun, Yue; Gleber, Sophie -Charlotte; Jacobsen, Chris

We report that trace metals play critical roles in a variety of systems, ranging from cells to photovoltaics. X-Ray Fluorescence (XRF) microscopy using X-ray excitation provides one of the highest sensitivities available for imaging the distribution of trace metals at sub-100 nm resolution. With the growing availability and increasing performance of synchrotron light source based instruments and X-ray nanofocusing optics, and with improvements in energy-dispersive XRF detectors, what are the factors that limit trace element detectability? To address this question, we describe an analytical model for the total signal incident on XRF detectors with various geometries, including the spectral responsemore » of energy dispersive detectors. This model agrees well with experimentally recorded X-ray fluorescence spectra, and involves much shorter calculation times than with Monte Carlo simulations. With such a model, one can estimate the signal when a trace element is illuminated with an X-ray beam, and when just the surrounding non-fluorescent material is illuminated. From this signal difference, a contrast parameter can be calculated and this can in turn be used to calculate the signal-to-noise ratio (S/N) for detecting a certain elemental concentration. We apply this model to the detection of trace amounts of zinc in biological materials, and to the detection of small quantities of arsenic in semiconductors. In conclusion, we conclude that increased detector collection solid angle is (nearly) always advantageous even when considering the scattered signal. However, given the choice between a smaller detector at 90° to the beam versus a larger detector at 180° (in a backscatter-like geometry), the 90° detector is better for trace element detection in thick samples, while the larger detector in 180° geometry is better suited to trace element detection in thin samples.« less

Statistical analysis of water-quality data containing multiple detection limits: S-language software for regression on order statistics

USGS Publications Warehouse

Lee, L.; Helsel, D.

2005-01-01

Trace contaminants in water, including metals and organics, often are measured at sufficiently low concentrations to be reported only as values below the instrument detection limit. Interpretation of these "less thans" is complicated when multiple detection limits occur. Statistical methods for multiply censored, or multiple-detection limit, datasets have been developed for medical and industrial statistics, and can be employed to estimate summary statistics or model the distributions of trace-level environmental data. We describe S-language-based software tools that perform robust linear regression on order statistics (ROS). The ROS method has been evaluated as one of the most reliable procedures for developing summary statistics of multiply censored data. It is applicable to any dataset that has 0 to 80% of its values censored. These tools are a part of a software library, or add-on package, for the R environment for statistical computing. This library can be used to generate ROS models and associated summary statistics, plot modeled distributions, and predict exceedance probabilities of water-quality standards. ?? 2005 Elsevier Ltd. All rights reserved.

Micro-Raman spectroscopy and μ-XRF in the investigation of ancient glass beads from the archaeological sites, eastern Taiwan

NASA Astrophysics Data System (ADS)

San Liou, Ying; Liu, Yi Chang

2017-04-01

Ancient glass beads with different colors, shapes, and stylistics unearthed from the archaeological sites of eastern Taiwan, dating back to approximately 1850-310 BP, have been investigated. It is generally known that glass bead is alien to invade into Taiwan along with metal ware, glass, agate, etc. since the Metal Age of Taiwan. Nevertheless, souring provenance and trade routes still remain controversial. Micro-Raman spectroscopy and μ-XRF have been applied on fifty-six ancient glass beads to reveal the mineralogical and chemical compositions and to help decipher the raw materials used and souring provenance. Micro-Raman measurements indicate the presence of hematite, zincite, siderite, sphalerite, lead tin yellow type II, quartz, feldspar, anatase, rutite, ankerite, graphite, calcite, etc. Among them, hematite, zincite, siderite, sphalerite, lead tin yellow type II, and rutile were found to be colorants/opacifiers. Moreover, crystalline phases such as lead tin yellow type II (PbSn1-xSixO3), zincite (ZnO), tricalcium diphosphate (Ca2(PO4)2), sphalerite ((Zn, Fe)S) and ankerite (Ca(Fe, Mg, Mn)(CO3)2) were detected in ancient glass beads unearthed from Taiwan for the first time. The chemical results obtained by μXRF show SiO2, Al2O3, Na2O, K2O, MgO, CaO, and PbO as the most abundant oxides. Na2O, K2O, Al2O3, MgO, and PbO could be the main/minor fluxes and colorants. In general, results of mineralogical and chemical analyses are compatible. According to chemical results, ancient glass beads can be classified as mineral soda alumina glass (m-Na-Al glass), soda plant ash glass (v-Na-Ca glass), lead silicate glass, and some less well known types. Mineral soda alumina and soda plant ash glass beads, as well as lead silicate glass beads are generally believed to be the distinct phases of production and exchange in Southeast Asia and China, respectively. In terms of chronology of glass bead, beads excavated from sites of 1850-930 BP are mineral soda alumina glass (m

Role of XRF in the restoration of a prominent architectural monument at the site of Mleiha

NASA Astrophysics Data System (ADS)

Yousif, Eisa; Attaelmanan, Atta

2012-07-01

The fort at Mleiha is one of the most well known archaeological sites of its period (3rd c. BC to 3rd c. AD) in the United Arab Emirates and has provided much valuable information. The period of its construction and use coincided with the Parthian period, during which there were extensive commercial contacts between the UAE and Mediterranean cities, Egypt, Mesopotamia, Southwest Iran, Pakistan, East Africa, and the southern Arabian Peninsula. It was restored using local materials, and traditional construction methods. The objective of this study was to utilize XRF techniques for the identification of the elemental composition of building material used to construct an archaeological fort, and to compare it to composition of the restoration material. Results of the study show strong correlation between the original fort building material and those used for restoration.

ROBUST ESTIMATION OF MEAN AND VARIANCE USING ENVIRONMENTAL DATA SETS WITH BELOW DETECTION LIMIT OBSERVATIONS

EPA Science Inventory

Scientists, especially environmental scientists often encounter trace level concentrations that are typically reported as less than a certain limit of detection, L. Type 1, left-censored data arise when certain low values lying below L are ignored or unknown as they cannot be mea...

WE-H-206-01: Photoacoustic Tomography: Multiscale Imaging From Organelles to Patients by Ultrasonically Beating the Optical Diffusion Limit

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, L.

Lihong V. Wang: Photoacoustic tomography (PAT), combining non-ionizing optical and ultrasonic waves via the photoacoustic effect, provides in vivo multiscale functional, metabolic, and molecular imaging. Broad applications include imaging of the breast, brain, skin, esophagus, colon, vascular system, and lymphatic system in humans or animals. Light offers rich contrast but does not penetrate biological tissue in straight paths as x-rays do. Consequently, high-resolution pure optical imaging (e.g., confocal microscopy, two-photon microscopy, and optical coherence tomography) is limited to penetration within the optical diffusion limit (∼1 mm in the skin). Ultrasonic imaging, on the contrary, provides fine spatial resolution but suffersmore » from both poor contrast in early-stage tumors and strong speckle artifacts. In PAT, pulsed laser light penetrates tissue and generates a small but rapid temperature rise, which induces emission of ultrasonic waves due to thermoelastic expansion. The ultrasonic waves, orders of magnitude less scattering than optical waves, are then detected to form high-resolution images of optical absorption at depths up to 7 cm, conquering the optical diffusion limit. PAT is the only modality capable of imaging across the length scales of organelles, cells, tissues, and organs (up to whole-body small animals) with consistent contrast. This rapidly growing technology promises to enable multiscale biological research and accelerate translation from microscopic laboratory discoveries to macroscopic clinical practice. PAT may also hold the key to label-free early detection of cancer by in vivo quantification of hypermetabolism, the quintessential hallmark of malignancy. Learning Objectives: To understand the contrast mechanism of PAT To understand the multiscale applications of PAT Benjamin M. W. Tsui: Multi-modality molecular imaging instrumentation and techniques have been major developments in small animal imaging that has contributed

Detection of Stimulus Displacements Across Saccades is Capacity-Limited and Biased in Favor of the Saccade Target

PubMed Central

Irwin, David E.; Robinson, Maria M.

2015-01-01

Retinal image displacements caused by saccadic eye movements are generally unnoticed. Recent theories have proposed that perceptual stability across saccades depends on a local evaluation process centered on the saccade target object rather than on remapping and evaluating the positions of all objects in a display. In three experiments, we examined whether objects other than the saccade target also influence perceptual stability by measuring displacement detection thresholds across saccades for saccade targets and a variable number of non-saccade objects. We found that the positions of multiple objects are maintained across saccades, but with variable precision, with the saccade target object having priority in the perception of displacement, most likely because it is the focus of attention before the saccade and resides near the fovea after the saccade. The perception of displacement of objects that are not the saccade target is affected by acuity limitations, attentional limitations, and limitations on memory capacity. Unlike previous studies that have found that a postsaccadic blank improves the detection of displacement direction across saccades, we found that postsaccadic blanking hurt the detection of displacement per se by increasing false alarms. Overall, our results are consistent with the hypothesis that visual working memory underlies the perception of stability across saccades. PMID:26640430

Eye movements during change detection: implications for search constraints, memory limitations, and scanning strategies.

PubMed

Zelinsky, G J

2001-02-01

Search, memory, and strategy constraints on change detection were analyzed in terms of oculomotor variables. Observers viewed a repeating sequence of three displays (Scene 1-->Mask-->Scene 2-->Mask...) and indicated the presence-absence of a changing object between Scenes 1 and 2. Scenes depicted real-world objects arranged on a surface. Manipulations included set size (one, three, or nine items) and the orientation of the changing objects (similar or different). Eye movements increased with the number of potentially changing objects in the scene, with this set size effect suggesting a relationship between change detection and search. A preferential fixation analysis determined that memory constraints are better described by the operation comparing the pre- and postchange objects than as a capacity limitation, and a scanpath analysis revealed a change detection strategy relying on the peripheral encoding and comparison of display items. These findings support a signal-in-noise interpretation of change detection in which the signal varies with the similarity of the changing objects and the noise is determined by the distractor objects and scene background.

A new large solid angle multi-element silicon drift detector system for low energy X-ray fluorescence spectroscopy

NASA Astrophysics Data System (ADS)

Bufon, J.; Schillani, S.; Altissimo, M.; Bellutti, P.; Bertuccio, G.; Billè, F.; Borghes, R.; Borghi, G.; Cautero, G.; Cirrincione, D.; Fabiani, S.; Ficorella, F.; Gandola, M.; Gianoncelli, A.; Giuressi, D.; Kourousias, G.; Mele, F.; Menk, R. H.; Picciotto, A.; Rachevski, A.; Rashevskaya, I.; Sammartini, M.; Stolfa, A.; Zampa, G.; Zampa, N.; Zorzi, N.; Vacchi, A.

2018-03-01

Low-energy X-ray fluorescence (LEXRF) is an essential tool for bio-related research of organic samples, whose composition is dominated by light elements. Working at energies below 2 keV and being able to detect fluorescence photons of lightweight elements such as carbon (277 eV) is still a challenge, since it requires in-vacuum operations to avoid in-air photon absorption. Moreover, the detectors must have a thin entrance window and collect photons at an angle of incidence near 90 degrees to minimize the absorption by the protective coating. Considering the low fluorescence yield of light elements, it is important to cover a substantial part of the solid angle detecting ideally all emitted X-ray fluorescence (XRF) photons. Furthermore, the energy resolution of the detection system should be close to the Fano limit in order to discriminate elements whose XRF emission lines are often very close within the energy spectra. To ensure all these features, a system consisting of four monolithic multi-element silicon drift detectors was developed. The use of four separate detector units allows optimizing the incidence angle on all the sensor elements. The multi-element approach in turn provides a lower leakage current on each anode, which, in combination with ultra-low noise preamplifiers, is necessary to achieve an energy resolution close to the Fano limit. The potential of the new detection system and its applicability for typical LEXRF applications has been proved on the Elettra TwinMic beamline.

An accurate and inexpensive color-based assay for detecting severe anemia in a limited-resource setting

PubMed Central

McGann, Patrick T.; Tyburski, Erika A.; de Oliveira, Vysolela; Santos, Brigida; Ware, Russell E.; Lam, Wilbur A.

2016-01-01

Severe anemia is an important cause of morbidity and mortality among children in resource-poor settings, but laboratory diagnostics are often limited in these locations. To address this need, we developed a simple, inexpensive, and color-based point-of-care (POC) assay to detect severe anemia. The purpose of this study was to evaluate the accuracy of this novel POC assay to detect moderate and severe anemia in a limited-resource setting. The study was a cross-sectional study conducted on children with sickle cell anemia in Luanda, Angola. The hemoglobin concentrations obtained by the POC assay were compared to reference values measured by a calibrated automated hematology analyzer. A total of 86 samples were analyzed (mean hemoglobin concentration 6.6 g/dL). There was a strong correlation between the hemoglobin concentrations obtained by the POC assay and reference values obtained from an automated hematology analyzer (r=0.88, P<0.0001). The POC assay demonstrated excellent reproducibility (r=0.93, P<0.0001) and the reagents appeared to be durable in a tropical setting (r=0.93, P<0.0001). For the detection of severe anemia that may require blood transfusion (hemoglobin <5 g/dL), the POC assay had sensitivity of 88.9% and specificity of 98.7%. These data demonstrate that an inexpensive (<$0.25 USD) POC assay accurately estimates low hemoglobin concentrations and has the potential to become a transformational diagnostic tool for severe anemia in limited-resource settings. PMID:26317494

Landed XRD/XRF analysis of prime targets in the search for past or present Martian life.

PubMed

Vaniman, D; Bish, D; Blake, D; Elliott, S T; Sarrazin, P; Collins, S A; Chipera, S

1998-12-25

Mars landers seeking evidence for past or present life will be guided by information from orbital mapping and from previous surface exploration. Several target options have been proposed, including sites that may harbor extant life and sites most likely to preserve evidence of past life These sites have specific mineralogic characteristics. Extant life might be gathered around the sinters and associated mineral deposits of rare active fumaroles, or held within brine pockets and inclusions in a few evaporite-mineral deposits. Possibilities for fossilization include deltaic and lake-bottom sediments of once-flooded craters, sinters formed by ancient hot-spring deposits, and the carbonate deposits associated with some evaporite systems. However, the highly varied mineralogy of fossil occurrences on Earth leads to the inference that Mars, an equally complex planet, could host a broad variety of potential fossilizing deposits. The abundance of volcanic systems on Mars and evidence for close associations between volcanism and water release suggest possibilities of organism entrapment and mineralization in volcaniclastic deposits, as found in some instances on Earth. Thus the targets being considered for exploration include a wide variety of unique deposits that would be characterized by silica or various nonsilicate minerals. Beyond these "special" deposits and in the most general case, an ability to distinguish mineralized from uncemented volcanic detritus may be the key to success in finding possible fossil-bearing authigenic mineralogies. A prototype miniaturized X ray diffraction/X ray fluorescence (XRD/XRF) instrument has been evaluated with silica, carbonate, and sulfate minerals and with a basalt, to examine the capabilities of this tool in mineralogic and petrologic exploration for exobiological goals. This instrument. CHEMIN (chemical and mineralogical analyzer), is based on an innovative low-power X ray tube, transmission geometry, and CCD collection and

Qualitative Contrast between Knowledge-Limited Mixed-State and Variable-Resources Models of Visual Change Detection

ERIC Educational Resources Information Center

Nosofsky, Robert M.; Donkin, Chris

2016-01-01

We report an experiment designed to provide a qualitative contrast between knowledge-limited versions of mixed-state and variable-resources (VR) models of visual change detection. The key data pattern is that observers often respond "same" on big-change trials, while simultaneously being able to discriminate between same and small-change…

Applications of Nanomaterials Based on Magnetite and Mesoporous Silica on the Selective Detection of Zinc Ion in Live Cell Imaging.

PubMed

Erami, Roghayeh Sadeghi; Ovejero, Karina; Meghdadi, Soraia; Filice, Marco; Amirnasr, Mehdi; Rodríguez-Diéguez, Antonio; De La Orden, María Ulagares; Gómez-Ruiz, Santiago

2018-06-14

Functionalized magnetite nanoparticles (FMNPs) and functionalized mesoporous silica nanoparticles (FMSNs) were synthesized by the conjugation of magnetite and mesoporous silica with the small and fluorogenic benzothiazole ligand, that is, 2(2-hydroxyphenyl)benzothiazole ( hpbtz ). The synthesized fluorescent nanoparticles were characterized by FTIR, XRD, XRF, 13 C CP MAS NMR, BET, and TEM. The photophysical behavior of FMNPs and FMSNs in ethanol was studied using fluorescence spectroscopy. The modification of magnetite and silica scaffolds with the highly fluorescent benzothiazole ligand enabled the nanoparticles to be used as selective and sensitive optical probes for zinc ion detection. Moreover, the presence of hpbtz in FMNPs and FMSNs induced efficient cell viability and zinc ion uptake, with desirable signaling in the normal human kidney epithelial (Hek293) cell line. The significant viability of FMNPs and FMSNs (80% and 92%, respectively) indicates a potential applicability of these nanoparticles as in vitro imaging agents. The calculated limit of detections (LODs) were found to be 2.53 × 10 −6 and 2.55 × 10 −6 M for Fe₃O₄-H@hpbtz and MSN-Et₃N-IPTMS-hpbtz-f1, respectively. FMSNs showed more pronounced zinc signaling relative to FMNPs, as a result of the more efficient penetration into the cells.

Combined use of FORS, XRF and Raman spectroscopy in the study of mural paintings in the Aosta Valley (Italy).

PubMed

Appolonia, Lorenzo; Vaudan, Davide; Chatel, Valentina; Aceto, Maurizio; Mirti, Piero

2009-12-01

Mural paintings which decorate the external façade and the internal apsidal wall of a chapel dedicated to St. Maxime and located at Challand St. Victor in the Aosta Valley (Italy) have been analysed with a combined approach involving high-resolution fibre-optic reflectance spectroscopy (FORS), X-ray fluorescence (XRF) spectrometry and Raman spectroscopy. The paintings are attributed to Giacomino from Ivrea, a painter active around the mid-fifteenth century. In order to characterise the palette used by the painter and to yield information useful to restorers, the cited techniques were used either in situ with portable instruments and in laboratory, working on micro samples withdrawn from paintings. The global analytical approach, though not entirely non-invasive, can indeed be considered non-destructive as multiple analyses, including SEM-EDX, could be carried out on the micro samples, exploiting the features of each technique. On the basis of the information obtained, the palette was found to be composed of typical fresco pigments such as calcite, azurite, malachite, vermilion, red and yellow ochres. A particular situation was noted for black pigments since the presence of graphite, rather than wood or lamp carbon, was found, possibly related to the presence of graphite deposits in the Aosta Valley. Furthermore, the presence of smalt superimposed to azurite in areas showing evidence of repainting was detected, suggesting that paintings were subjected to retouching at a relatively early stage after the original execution. Finally, the presence of tin foils, used to decorate haloes of Evangelists, was ascertained.

Determination of Detection Limits and Quantitation Limits for Compounds in a Database of GC/MS by FUMI Theory

PubMed Central

Nakashima, Shinya; Hayashi, Yuzuru

2016-01-01

The aim of this paper is to propose a stochastic method for estimating the detection limits (DLs) and quantitation limits (QLs) of compounds registered in a database of a GC/MS system and prove its validity with experiments. The approach described in ISO 11843 Part 7 is adopted here as an estimation means of DL and QL, and the decafluorotriphenylphosphine (DFTPP) tuning and retention time locking are carried out for adjusting the system. Coupled with the data obtained from the system adjustment experiments, the information (noise and signal of chromatograms and calibration curves) stored in the database is used for the stochastic estimation, dispensing with the repetition measurements. Of sixty-six pesticides, the DL values obtained by the ISO method were compared with those from the statistical approach and the correlation between them was observed to be excellent with the correlation coefficient of 0.865. The accuracy of the method proposed was also examined and concluded to be satisfactory as well. The samples used are commercial products of pesticides mixtures and the uncertainty from sample preparation processes is not taken into account. PMID:27162706

Enhancement of laser-induced breakdown spectroscopy (LIBS) Detection limit using a low-pressure and short-pulse laser-induced plasma process.

PubMed

Wang, Zhen Zhen; Deguchi, Yoshihiro; Kuwahara, Masakazu; Yan, Jun Jie; Liu, Ji Ping

2013-11-01

Laser-induced breakdown spectroscopy (LIBS) technology is an appealing technique compared with many other types of elemental analysis because of the fast response, high sensitivity, real-time, and noncontact features. One of the challenging targets of LIBS is the enhancement of the detection limit. In this study, the detection limit of gas-phase LIBS analysis has been improved by controlling the pressure and laser pulse width. In order to verify this method, low-pressure gas plasma was induced using nanosecond and picosecond lasers. The method was applied to the detection of Hg. The emission intensity ratio of the Hg atom to NO (IHg/INO) was analyzed to evaluate the LIBS detection limit because the NO emission (interference signal) was formed during the plasma generation and cooling process of N2 and O2 in the air. It was demonstrated that the enhancement of IHg/INO arose by decreasing the pressure to a few kilopascals, and the IHg/INO of the picosecond breakdown was always much higher than that of the nanosecond breakdown at low buffer gas pressure. Enhancement of IHg/INO increased more than 10 times at 700 Pa using picosecond laser with 35 ps pulse width. The detection limit was enhanced to 0.03 ppm (parts per million). We also saw that the spectra from the center and edge parts of plasma showed different features. Comparing the central spectra with the edge spectra, IHg/INO of the edge spectra was higher than that of the central spectra using the picosecond laser breakdown process.

Nanoparticle size detection limits by single particle ICP-MS for 40 elements.

PubMed

Lee, Sungyun; Bi, Xiangyu; Reed, Robert B; Ranville, James F; Herckes, Pierre; Westerhoff, Paul

2014-09-02

The quantification and characterization of natural, engineered, and incidental nano- to micro-size particles are beneficial to assessing a nanomaterial's performance in manufacturing, their fate and transport in the environment, and their potential risk to human health. Single particle inductively coupled plasma mass spectrometry (spICP-MS) can sensitively quantify the amount and size distribution of metallic nanoparticles suspended in aqueous matrices. To accurately obtain the nanoparticle size distribution, it is critical to have knowledge of the size detection limit (denoted as Dmin) using spICP-MS for a wide range of elements (other than a few available assessed ones) that have been or will be synthesized into engineered nanoparticles. Herein is described a method to estimate the size detection limit using spICP-MS and then apply it to nanoparticles composed of 40 different elements. The calculated Dmin values correspond well for a few of the elements with their detectable sizes that are available in the literature. Assuming each nanoparticle sample is composed of one element, Dmin values vary substantially among the 40 elements: Ta, U, Ir, Rh, Th, Ce, and Hf showed the lowest Dmin values, ≤10 nm; Bi, W, In, Pb, Pt, Ag, Au, Tl, Pd, Y, Ru, Cd, and Sb had Dmin in the range of 11-20 nm; Dmin values of Co, Sr, Sn, Zr, Ba, Te, Mo, Ni, V, Cu, Cr, Mg, Zn, Fe, Al, Li, and Ti were located at 21-80 nm; and Se, Ca, and Si showed high Dmin values, greater than 200 nm. A range of parameters that influence the Dmin, such as instrument sensitivity, nanoparticle density, and background noise, is demonstrated. It is observed that, when the background noise is low, the instrument sensitivity and nanoparticle density dominate the Dmin significantly. Approaches for reducing the Dmin, e.g., collision cell technology (CCT) and analyte isotope selection, are also discussed. To validate the Dmin estimation approach, size distributions for three engineered nanoparticle samples were

A Shadowing Problem in the Detection of Overlapping Communities: Lifting the Resolution Limit through a Cascading Procedure

PubMed Central

Young, Jean-Gabriel; Allard, Antoine; Hébert-Dufresne, Laurent; Dubé, Louis J.

2015-01-01

Community detection is the process of assigning nodes and links in significant communities (e.g. clusters, function modules) and its development has led to a better understanding of complex networks. When applied to sizable networks, we argue that most detection algorithms correctly identify prominent communities, but fail to do so across multiple scales. As a result, a significant fraction of the network is left uncharted. We show that this problem stems from larger or denser communities overshadowing smaller or sparser ones, and that this effect accounts for most of the undetected communities and unassigned links. We propose a generic cascading approach to community detection that circumvents the problem. Using real and artificial network datasets with three widely used community detection algorithms, we show how a simple cascading procedure allows for the detection of the missing communities. This work highlights a new detection limit of community structure, and we hope that our approach can inspire better community detection algorithms. PMID:26461919

Detection of radioactive particles offshore by γ-ray spectrometry Part I: Monte Carlo assessment of detection depth limits

NASA Astrophysics Data System (ADS)

Maučec, M.; de Meijer, R. J.; Rigollet, C.; Hendriks, P. H. G. M.; Jones, D. G.

2004-06-01

A joint research project between the British Geological Survey and Nuclear Geophysics Division of the Kernfysisch Versneller Instituut, Groningen, the Netherlands, was commissioned by the United Kingdom Atomic Energy Authority to establish the efficiency of a towed seabed γ-ray spectrometer for the detection of 137Cs-containing radioactive particles offshore Dounreay, Scotland. Using the MCNP code, a comprehensive Monte Carlo feasibility study was carried out to model various combinations of geological matrices, particle burial depth and lateral displacement, source activity and detector material. To validate the sampling and absolute normalisation procedures of MCNP for geometries including multiple (natural and induced) heterogeneous sources in environmental monitoring, a benchmark experiment was conducted. The study demonstrates the ability of seabed γ-ray spectrometry to locate radioactive particles offshore and to distinguish between γ count rate increases due to particles from those due to enhanced natural radioactivity. The information presented in this study will be beneficial for estimation of the inventory of 137Cs particles and their activity distribution and for the recovery of particles from the sea floor. In this paper, the Monte Carlo assessment of the detection limits is presented. The estimation of the required towing speed and acquisition times and their application to radioactive particle detection and discrimination offshore formed a supplementary part of this study.

A novel dNTP-limited PCR and HRM assay to detect Williams-Beuren syndrome.

PubMed

Zhang, Lichen; Zhang, Xiaoqing; You, Guoling; Yu, Yongguo; Fu, Qihua

2018-06-01

Williams-Beuren syndrome (WBS) is caused by a microdeletion of chromosome arm 7q11.23. A rapid and inexpensive genotyping method to detect microdeletion on 7q11.23 needs to be developed for the diagnosis of WBS. This study describes the development of a new type of molecular diagnosis method to detect microdeletion on 7q11.23 based upon high-resolution melting (HRM). Four genes on 7q11.23 were selected as the target genes for the deletion genotyping. dNTP-limited duplex PCR was used to amplify the reference gene, CFTR, and one of the four genes respectively on 7q11.23. An HRM assay was performed on the PCR products, and the height ratio of the negative derivative peaks between the target gene and reference gene was employed to analyze the copy number variation of the target region. A new genotyping method for detecting 7q11.23 deletion was developed based upon dNTP-limited PCR and HRM, which cost only 96 min. Samples from 15 WBS patients and 12 healthy individuals were genotyped by this method in a blinded fashion, and the sensitivity and specificity was 100% (95% CI, 0.80-1, and 95% CI, 0.75-1, respectively) which was proved by CytoScan HD array. The HRM assay we developed is an rapid, inexpensive, and highly accurate method for genotyping 7q11.23 deletion. It is potentially useful in the clinical diagnosis of WBS. Copyright © 2018 Elsevier B.V. All rights reserved.

Investigation of detection limits for solutes in water measured by laser raman spectrometry

USGS Publications Warehouse

Goldberg, M.C.

1977-01-01

The influence of experimental parameters on detection sensitivity was determined for laser Raman analysis of dissolved solutes in water. Individual solutions of nitrate, sulfate, carbonate, bicarbonate, monohydrogen phosphate, dihydrogen phosphate, acetate ion, and acetic acid were measured. An equation is derived which expresses the signal-to-noise ratio in terms of solute concentration, measurement time, spectral slit width, laser power fluctuations, and solvent background intensity. Laser beam intensity fluctuations at the sample and solvent background intensity are the most important limiting factors.

Resolving colocalization of bacteria and metal(loid)s on plant root surfaces by combining fluorescence in situ hybridization (FISH) with multiple-energy micro-focused X-ray fluorescence (ME μXRF).

PubMed

Honeker, Linnea K; Root, Robert A; Chorover, Jon; Maier, Raina M

2016-12-01

Metal(loid)-contamination of the environment due to anthropogenic activities is a global problem. Understanding the fate of contaminants requires elucidation of biotic and abiotic factors that influence metal(loid) speciation from molecular to field scales. Improved methods are needed to assess micro-scale processes, such as those occurring at biogeochemical interfaces between plant tissues, microbial cells, and metal(loid)s. Here we present an advanced method that combines fluorescence in situ hybridization (FISH) with synchrotron-based multiple-energy micro-focused X-ray fluorescence microprobe imaging (ME μXRF) to examine colocalization of bacteria and metal(loid)s on root surfaces of plants used to phytostabilize metalliferous mine tailings. Bacteria were visualized on a small root section using SytoBC nucleic acid stain and FISH probes targeting the domain Bacteria and a specific group (Alphaproteobacteria, Gammaproteobacteria, or Actinobacteria). The same root region was then analyzed for elemental distribution and metal(loid) speciation of As and Fe using ME μXRF. The FISH and ME μXRF images were aligned using ImageJ software to correlate microbiological and geochemical results. Results from quantitative analysis of colocalization show a significantly higher fraction of As colocalized with Fe-oxide plaques on the root surfaces (fraction of overlap 0.49±0.19) than to bacteria (0.072±0.052) (p<0.05). Of the bacteria that colocalized with metal(loid)s, Actinobacteria, known for their metal tolerance, had a higher correlation with both As and Fe than Alphaproteobacteria or Gammaproteobacteria. This method demonstrates how coupling these micro-techniques can expand our understanding of micro-scale interactions between roots, metal(loid)s and microbes, information that should lead to improved mechanistic models of metal(loid) speciation and fate. Copyright © 2016 Elsevier B.V. All rights reserved.

Efficacy of a lead based paint XRF analyzer and a commercially available colorimetric lead test kit as qualitative field tools for determining presence of lead in religious powders.

PubMed

Shah, Manthan P; Shendell, Derek G; Meng, Qingyu; Ohman-Strickland, Pamela; Halperin, William

2018-04-23

The performances of a portable X-Ray Fluorescence (XRF) lead paint analyzer (RMD LPA-1, Protec Instrument Corp., Waltham, MA) and a commercially available colorimetric lead test kit (First Alert Lead Test Kit, eAccess Solutions, Inc., Palatine, IL) were evaluated for use by local or state health departments as potential cost-effective rapid analysis or "spot test" field techniques for tentative identification of lead content in sindoor powders. For both field-sampling methods, sensitivity, specificity and predictive values varied widely for samples containing <300,000 μg/g lead. For samples containing ≥300,000 μg/g lead, the aforementioned metrics were 100% (however, the CIs had a wide range). In addition, both field sampling methods showed clear, consistent positive readings only for samples containing ≥300,000 μg/g lead. Even samples with lead content as high as 5,110 μg/g were not positively identified by either field analysis technique. The results of this study suggest the XRF analyzer and colorimetric lead test kit cannot be used as a rapid field test for sindoor by health department inspectors.

Use of tourmaline as a potential petrogenetic indicator in the determination of host magma: CRS, XRD and PED-XRF methods

NASA Astrophysics Data System (ADS)

Gullu, Bahattin; Kadioglu, Yusuf Kagan

2017-08-01

Tourmaline defines a group of complex borosilicate forms as accessory mineral in igneous and metamorphic rocks and they act an important role in the interpretation of the chemical composition changes of the composition of the host fluid of the magma. The variety of tourmaline can be identified by using optical microscopy, X-Ray Diffraction (XRD) and by determining its chemical composition through Polarized Energy Dispersive X-Ray Fluorescence (PED-XRF) methods. However, microscopic investigations and XRD analyses are not quite adequate for detailed determination of tourmaline sub-groups. In addition, the use of chemical composition of tourmaline as a strict indicator of geochemical processes might be a misleading method. In this study, variable tourmaline crystals were collected from three different pegmatitic occurrences in Behrekdag, Yozgat and Karakaya granitic bodies of Central Anatolia to identify their chemical properties through Confocal Raman Spectroscopy (CRS), PED-XRF and XRD analyses. The confocal Raman spectrometry of collected tourmalines from the Behrekdag, Yozgat and Karakaya granites are in the compositions of schorl, schorl and elbaite respectively. The dominant compositional groups of these tourmalines are in the form of schorl. Raman shift values of tourmalines revealed four bands centered at almost 1050, 750, 400 and 300 cm- 1. The first group of the band arises from SiO stretching, the second from Bsbnd O stretching and the other two belong to bending modes of Osbnd Bsbnd O and Bsbnd Osbnd Al with symmetrical deformation of Sisbnd Osbnd Si. The strongest spectra near 360 cm- 1 should belong to the bonding of Alsbnd O. As a result, the confocal Raman studies are more sensitive for identification of tourmaline subgroup compositions and have a quite important in the explaining source of the magma.

Use of tourmaline as a potential petrogenetic indicator in the determination of host magma: CRS, XRD and PED-XRF methods.

PubMed

Gullu, Bahattin; Kadioglu, Yusuf Kagan

2017-08-05

Tourmaline defines a group of complex borosilicate forms as accessory mineral in igneous and metamorphic rocks and they act an important role in the interpretation of the chemical composition changes of the composition of the host fluid of the magma. The variety of tourmaline can be identified by using optical microscopy, X-Ray Diffraction (XRD) and by determining its chemical composition through Polarized Energy Dispersive X-Ray Fluorescence (PED-XRF) methods. However, microscopic investigations and XRD analyses are not quite adequate for detailed determination of tourmaline sub-groups. In addition, the use of chemical composition of tourmaline as a strict indicator of geochemical processes might be a misleading method. In this study, variable tourmaline crystals were collected from three different pegmatitic occurrences in Behrekdag, Yozgat and Karakaya granitic bodies of Central Anatolia to identify their chemical properties through Confocal Raman Spectroscopy (CRS), PED-XRF and XRD analyses. The confocal Raman spectrometry of collected tourmalines from the Behrekdag, Yozgat and Karakaya granites are in the compositions of schorl, schorl and elbaite respectively. The dominant compositional groups of these tourmalines are in the form of schorl. Raman shift values of tourmalines revealed four bands centered at almost 1050, 750, 400 and 300cm -1 . The first group of the band arises from SiO stretching, the second from BO stretching and the other two belong to bending modes of OBO and BOAl with symmetrical deformation of SiOSi. The strongest spectra near 360cm -1 should belong to the bonding of AlO. As a result, the confocal Raman studies are more sensitive for identification of tourmaline subgroup compositions and have a quite important in the explaining source of the magma. Copyright © 2017 Elsevier B.V. All rights reserved.

A Spectacular Radio Flare from XRF 050416a at 40 Days and Implications for the Nature of X-Ray Flashes

NASA Technical Reports Server (NTRS)

Soderberg, A. M.; Nakar, E.; Cenko, S. B.; Cameron, P. B.; Frail, D. A.; Kulkarni, S. R.; Fox, D. B.; Berger, E.; Gal-Yam, A.; Moon, D-S.;

Comparison of detection limits in environmental analysis--is it possible? An approach on quality assurance in the lower working range by verification.

PubMed

Geiss, S; Einax, J W

2001-07-01

Detection limit, reporting limit and limit of quantitation are analytical parameters which describe the power of analytical methods. These parameters are used for internal quality assurance and externally for competing, especially in the case of trace analysis in environmental compartments. The wide variety of possibilities for computing or obtaining these measures in literature and in legislative rules makes any comparison difficult. Additionally, a host of terms have been used within the analytical community to describe detection and quantitation capabilities. Without trying to create an order for the variety of terms, this paper is aimed at providing a practical proposal for answering the main questions for the analysts concerning quality measures above. These main questions and related parameters were explained and graphically demonstrated. Estimation and verification of these parameters are the two steps to get real measures. A rule for a practical verification is given in a table, where the analyst can read out what to measure, what to estimate and which criteria have to be fulfilled. In this manner verified parameters detection limit, reporting limit and limit of quantitation now are comparable and the analyst himself is responsible to the unambiguity and reliability of these measures.

Improved detection limits for electrospray ionization on a magnetic sector mass spectrometer by using an array detector.

PubMed

Cody, R B; Tamura, J; Finch, J W; Musselman, B D

1994-03-01

Array detection was compared with point detection for solutions of hen egg-white lysozyme, equine myoglobin, and ubiquitin analyzed by electrospray ionization with a magnetic sector mass spectrometer. The detection limits for samples analyzed by using the array detector system were at least 10 times lower than could be achieved by using a point detector on the same mass spectrometer. The minimum detectable quantity of protein corresponded to a signal-to-background ratio of approximately 2∶1 for a 500 amol/μL solution of hen egg-white lysozyme. However, the ultimate practical sample concentrations appeared to be in the 10-100 fmol/μL range for the analysis of dilute solutions of relatively pure proteins or simple mixtures.

Lower Limits on Aperture Size for an ExoEarth Detecting Coronagraphic Mission

NASA Technical Reports Server (NTRS)

Stark, Christopher C.; Roberge, Aki; Mandell, Avi; Clampin, Mark; Domagal-Goldman, Shawn D.; McElwain, Michael W.; Stapelfeldt, Karl R.

2015-01-01

The yield of Earth-like planets will likely be a primary science metric for future space-based missions that will drive telescope aperture size. Maximizing the exoEarth candidate yield is therefore critical to minimizing the required aperture. Here we describe a method for exoEarth candidate yield maximization that simultaneously optimizes, for the first time, the targets chosen for observation, the number of visits to each target, the delay time between visits, and the exposure time of every observation. This code calculates both the detection time and multiwavelength spectral characterization time required for planets. We also refine the astrophysical assumptions used as inputs to these calculations, relying on published estimates of planetary occurrence rates as well as theoretical and observational constraints on terrestrial planet sizes and classical habitable zones. Given these astrophysical assumptions, optimistic telescope and instrument assumptions, and our new completeness code that produces the highest yields to date, we suggest lower limits on the aperture size required to detect and characterize a statistically motivated sample of exoEarths.

Applying ISO 11929:2010 Standard to detection limit calculation in least-squares based multi-nuclide gamma-ray spectrum evaluation

NASA Astrophysics Data System (ADS)

Kanisch, G.

2017-05-01

The concepts of ISO 11929 (2010) are applied to evaluation of radionuclide activities from more complex multi-nuclide gamma-ray spectra. From net peak areas estimated by peak fitting, activities and their standard uncertainties are calculated by weighted linear least-squares method with an additional step, where uncertainties of the design matrix elements are taken into account. A numerical treatment of the standard's uncertainty function, based on ISO 11929 Annex C.5, leads to a procedure for deriving decision threshold and detection limit values. The methods shown allow resolving interferences between radionuclide activities also in case of calculating detection limits where they can improve the latter by including more than one gamma line per radionuclide. The co"mmon single nuclide weighted mean is extended to an interference-corrected (generalized) weighted mean, which, combined with the least-squares method, allows faster detection limit calculations. In addition, a new grouped uncertainty budget was inferred, which for each radionuclide gives uncertainty budgets from seven main variables, such as net count rates, peak efficiencies, gamma emission intensities and others; grouping refers to summation over lists of peaks per radionuclide.

A Supercompressible, Elastic, and Bendable Carbon Aerogel with Ultrasensitive Detection Limits for Compression Strain, Pressure, and Bending Angle.

PubMed

Zhuo, Hao; Hu, Yijie; Tong, Xing; Chen, Zehong; Zhong, Linxin; Lai, Haihong; Liu, Linxiang; Jing, Shuangshuang; Liu, Qingzhong; Liu, Chuanfu; Peng, Xinwen; Sun, Runcang

2018-05-01

Ultralight and compressible carbon materials have promising applications in strain and pressure detection. However, it is still difficult to prepare carbon materials with supercompressibility, elasticity, stable strain-electrical signal response, and ultrasensitive detection limits, due to the challenge in structural regulation. Herein, a new strategy to prepare a reduced graphene oxide (rGO)-based lamellar carbon aerogels with unexpected and integrated performances by designing wave-shape rGO layers and enhancing the interaction among the rGO layers is demonstrated. Addition of cellulose nanocrystalline and low-molecular-weight carbon precursors enhances the interaction among rGO layers and thus produces an ultralight, flexible, and superstable structure. The as-prepared carbon aerogel displays a supercompressibility (undergoing an extreme strain of 99%) and elasticity (100% height retention after 10 000 cycles at a strain of 30%), as well as stable strain-current response (at least 10 000 cycles). Particularly, the carbon aerogel is ultrasensitive for detecting tiny change in strain (0.012%) and pressure (0.25 Pa), which are the lowest detection limits for compressible carbon materials reported in the literature. Moreover, the carbon aerogel exhibits excellent bendable performance and can detect an ultralow bending angle of 0.052°. Additionally, the carbon aerogel also demonstrates its promising application as wearable devices. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Early breast cancer screening using iron/iron oxide-based nanoplatforms with sub-femtomolar limits of detection

PubMed Central

Samarakoon, Thilani N; Yapa, Asanka S; Abayaweera, Gayani; Basel, Matthew T; Maynez, Pamela; Ortega, Raquel; Toledo, Yubisela; Bossmann, Leonie; Robinson, Colette; Janik, Katharine E; Koper, Olga B; Li, Ping; Motamedi, Massoud; Higgins, Daniel A; Gadbury, Gary

2016-01-01

Summary Proteases, including matrix metalloproteinases (MMPs), tissue serine proteases, and cathepsins (CTS) exhibit numerous functions in tumor biology. Solid tumors are characterized by changes in protease expression levels by tumor and surrounding tissue. Therefore, monitoring protease levels in tissue samples and liquid biopsies is a vital strategy for early cancer detection. Water-dispersable Fe/Fe3O4-core/shell based nanoplatforms for protease detection are capable of detecting protease activity down to sub-femtomolar limits of detection. They feature one dye (tetrakis(carboxyphenyl)porphyrin (TCPP)) that is tethered to the central nanoparticle by means of a protease-cleavable consensus sequence and a second dye (Cy 5.5) that is directly linked. Based on the protease activities of urokinase plasminogen activator (uPA), MMPs 1, 2, 3, 7, 9, and 13, as well as CTS B and L, human breast cancer can be detected at stage I by means of a simple serum test. By monitoring CTS B and L stage 0 detection may be achieved. This initial study, comprised of 46 breast cancer patients and 20 apparently healthy human subjects, demonstrates the feasibility of protease-activity-based liquid biopsies for early cancer diagnosis. PMID:27335730

Early breast cancer screening using iron/iron oxide-based nanoplatforms with sub-femtomolar limits of detection.

PubMed

Udukala, Dinusha N; Wang, Hongwang; Wendel, Sebastian O; Malalasekera, Aruni P; Samarakoon, Thilani N; Yapa, Asanka S; Abayaweera, Gayani; Basel, Matthew T; Maynez, Pamela; Ortega, Raquel; Toledo, Yubisela; Bossmann, Leonie; Robinson, Colette; Janik, Katharine E; Koper, Olga B; Li, Ping; Motamedi, Massoud; Higgins, Daniel A; Gadbury, Gary; Zhu, Gaohong; Troyer, Deryl L; Bossmann, Stefan H

2016-01-01

Proteases, including matrix metalloproteinases (MMPs), tissue serine proteases, and cathepsins (CTS) exhibit numerous functions in tumor biology. Solid tumors are characterized by changes in protease expression levels by tumor and surrounding tissue. Therefore, monitoring protease levels in tissue samples and liquid biopsies is a vital strategy for early cancer detection. Water-dispersable Fe/Fe3O4-core/shell based nanoplatforms for protease detection are capable of detecting protease activity down to sub-femtomolar limits of detection. They feature one dye (tetrakis(carboxyphenyl)porphyrin (TCPP)) that is tethered to the central nanoparticle by means of a protease-cleavable consensus sequence and a second dye (Cy 5.5) that is directly linked. Based on the protease activities of urokinase plasminogen activator (uPA), MMPs 1, 2, 3, 7, 9, and 13, as well as CTS B and L, human breast cancer can be detected at stage I by means of a simple serum test. By monitoring CTS B and L stage 0 detection may be achieved. This initial study, comprised of 46 breast cancer patients and 20 apparently healthy human subjects, demonstrates the feasibility of protease-activity-based liquid biopsies for early cancer diagnosis.

Determining the 95% limit of detection for waterborne pathogen analyses from primary concentration to qPCR

USDA-ARS?s Scientific Manuscript database

The limit of detection (LOD) for qPCR-based analyses is not consistently defined or determined in studies on waterborne pathogens. Moreover, the LODs reported often reflect the qPCR assay rather than the entire sample process. Our objective was to develop a method to determine the 95% LOD (lowest co...

WE-H-207A-09: Theoretical Limits to Molecular Biomarker Detection Using Magnetic Nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Weaver, J; Geisel School of Medicine, Dartmouth College, Hanover, NH

Purpose: Estimate the limits of molecular biomarker detection using magnetic nanoparticle methods like in vivo ELISA. Methods: Magnetic nanoparticles in an alternating magnetic field produce a magnetization that can be detected at exceedingly low levels because the signal at the harmonic frequencies is uniquely produced by the nanoparticles. Because the magnetization can also be used to characterize the nanoparticle rotational freedom, the bound state can be found. If the nanoparticles are coated with molecules that bind the desired biomarker, the rotational freedom reflects the biomarker concentration. The irreducible noise limit is the thermal noise or Johnson noise of the tissuemore » and the contrast that can be measured must be larger than that limit. The contrast produced is a function of the applied field and depends strongly on nanoparticle volume. We have estimated the contrast using a Langevin function of a single composite variable to approximate the full stochastic Langevin equation for nanoparticle dynamics. Results: The thermal noise for a bandwidth reasonable for spectroscopy suggests mid zeptomolar (10–21) to low attomolar (10–18) concentrations can be measured in a volume that is 10cm in scale. The suggested sensitivity is far below the physiologically concentrations of almost all critical biomarkers including cytokines (picomolar), hormones (nanomolar) and heat shock proteins. Conclusion: The sensitivity of in vivo ELISA concentration measurements should be sufficient to measure physiological concentrations of critical biomarkers like cytokines in vivo. Further the sensitivity should be sufficient to measure concentrations of other biomarkers that are six to eight orders of magnitude lower in concentration than immune signaling molecules like cytokines. NIH - 1U54CA151662-01 Department of Radiology.« less

Evaluation of MidIR fibre optic reflectance: Detection limit, reproducibility and binary mixture discrimination

NASA Astrophysics Data System (ADS)

Sessa, Clarimma; Bagán, Héctor; García, José Francisco

2013-11-01

MidIR fibre optic reflectance (MidIR-FORS) is a promising analytical technique in the field of science conservation, especially because it is non-destructive. Another advantage of MidIR-FORS is that the obtained information is representative, as a large amount of spectral data can be collected. Although the technique has a high potential and is almost routinely applied, its quality parameters have not been thoroughly studied in the specific application of analysis of artistic materials. The objective of this study is to evaluate the instrumental capabilities of MidIR-FORS for the analysis of artwork materials in terms of detection limit, reproducibility, and mixture characterisation. The study has been focused on oil easel painting and several paints of known composition have been analysed. Paint layers include blue pigments not only because of their important role along art history, but also because their physical and spectroscopic characteristics allow a better evaluation of the MidIR-FORS capabilities. The results of the analysis indicate that MidIR-FORS supplies a signal affected by different factors, such as the optical, morphological and physical properties of the surface, in addition to the composition of materials analysed. Consequently, the detection limits established are relatively high for artistic objects (Prussian blue - PB 2.1-6.5%; Phthalocyanine blue - Pht 6.3-10.2%; synthetic Ultramarine blue - UM 12.1%) and may therefore lead to an incomplete description of the artwork. Reproducibility of the technique over time and across surface has been determined. The results show that the major sources of dispersion are the heterogeneity of the pigments distribution, physical features, and band shape distortions. The total dispersion is around 4% for the most intense bands (oil) and increases up to 26% when weak or overlapped bands are considered (PB, Pht, UM). The application of different pre-treatments (cutoff of fibres absorption, Savizky-Golay smoothing

Analytical performance of a versatile laboratory microscopic X-ray fluorescence system for metal uptake studies on argillaceous rocks

NASA Astrophysics Data System (ADS)

Gergely, Felicián; Osán, János; Szabó, B. Katalin; Török, Szabina

2016-02-01

Laboratory-scale microscopic X-ray fluorescence (micro-XRF) plays an increasingly important role in various fields where multielemental investigations of samples are indispensable. In case of geological samples, the reasonable detection limits (LOD) and spatial resolutions are necessary to identify the trace element content in microcrystalline level. The present study focuses on the analytical performance of a versatile laboratory-scale micro-XRF system with various options of X-ray sources and detectors to find the optimal experimental configuration in terms of sensitivities and LOD for selected elements in loaded petrographic thin sections. The method was tested for sorption studies involving thin sections prepared from cores of Boda Claystone Formation, which is a potential site for a high-level radioactive waste repository. Loaded ions in the sorption measurements were Cs(I) and Ni(II) chemically representing fission and corrosion products. Based on the collected elemental maps, the correlation between the elements representative of main rock components and the selected loaded ion was studied. For the elements of interest, Cs(I) and Ni(II) low-power iMOXS source with polycapillary and silicon drift detector was found to be the best configuration to reach the optimal LOD values. Laboratory micro-XRF was excellent to identify the responsible key minerals for the uptake of Cs(I). In case of nickel, careful corrections were needed because of the relatively high Ca content of the rock samples. The results were compared to synchrotron radiation micro-XRF.

Cs2AgBiBr6 single-crystal X-ray detectors with a low detection limit

NASA Astrophysics Data System (ADS)

Pan, Weicheng; Wu, Haodi; Luo, Jiajun; Deng, Zhenzhou; Ge, Cong; Chen, Chao; Jiang, Xiaowei; Yin, Wan-Jian; Niu, Guangda; Zhu, Lujun; Yin, Lixiao; Zhou, Ying; Xie, Qingguo; Ke, Xiaoxing; Sui, Manling; Tang, Jiang

2017-11-01

Sensitive X-ray detection is crucial for medical diagnosis, industrial inspection and scientific research. The recently described hybrid lead halide perovskites have demonstrated low-cost fabrication and outstanding performance for direct X-ray detection, but they all contain toxic Pb in a soluble form. Here, we report sensitive X-ray detectors using solution-processed double perovskite Cs2AgBiBr6 single crystals. Through thermal annealing and surface treatment, we largely eliminate Ag+/Bi3+ disordering and improve the crystal resistivity, resulting in a detector with a minimum detectable dose rate as low as 59.7 nGyair s-1, comparable to the latest record of 0.036 μGyair s-1 using CH3NH3PbBr3 single crystals. Suppressed ion migration in Cs2AgBiBr6 permits relatively large external bias, guaranteeing efficient charge collection without a substantial increase in noise current and thus enabling the low detection limit.

Investigation of detection limits for diffuse optical tomography systems: II. Analysis of slab and cup geometry for breast imaging.

PubMed

Ziegler, Ronny; Brendel, Bernhard; Rinneberg, Herbert; Nielsen, Tim

2009-01-21

Using a statistical (chi-square) test on simulated data and a realistic noise model derived from the system's hardware we study the performance of diffuse optical tomography systems for fluorescence imaging. We compare the predicted smallest size of detectable lesions at various positions in slab and cup geometry and model how detection sensitivity depends on breast compression and lesion fluorescence contrast. Our investigation shows that lesion detection is limited by relative noise in slab geometry and by absolute noise in cup geometry.

Equatorial Pacific Productivity Events and Intervals in the Middle and late Miocene through XRF-Scanned Bulk Sediment Composition Data

NASA Astrophysics Data System (ADS)

Lyle, M. W.; Stepanova, A.; Wilson, J. K.; Marcantonio, F.

2014-12-01

The equatorial Pacific is the largest open ocean productivity center, responsible for nearly half of global marine new production and about 40% of CaCO3 burial. Understanding how the equatorial Pacific upwelling system has evolved over the Neogene is critical to understand the evolution of the global carbon cycle. We know from reconnaissance studies that productivity in equatorial Pacific surface waters as well as dissolution driven by deep waters have strongly affected the sediment record. We have used calibrated XRF scanning to capture anomalies in equatorial Pacific upwelling and productivity at Milankovitch-resolving resolution since the early Miocene. The 8 elements calibrated in the XRF scans can be used to distinguish intervals of high carbonate dissolution from those of high productivity. Carbonate dissolution intervals are recorded by a drop of CaCO3 relative to Aeolian clays, with little change in the ratio between estimated opal and clay (estimated by TiO2). In contrast, high production intervals have high opal/TiO2 and low CaCO3. Low CaCO3 contents are caused partly by dilution, since high production skews tropical particulate rain to be more opal-rich relative to carbonate, and additional C-org rain can help to increase CaCO3 dissolution within near-surface sediments. We observe long-lived high production anomalies modulated by orbitally-driven climate variability. Prominent intervals are found at the end of the Miocene climate optimum (~ 14 Ma), interspersed with dissolution intervals in the Carbonate Crash interval (~9-11 Ma), and in the Biogenic Bloom interval (8-4.5 Ma). Using relationships among biogenic fluxes in modern equatorial sediment trap studies, especially the positive correlations between biogenic Ba , C-org, and CaCO3 fluxes, we find that the highest production intervals have much higher opal/C-org in the particulate rain, implying an inefficient carbon pump to the deep ocean. If confirmed, productivity was not as strong a feedback to

Limitation in the detection of Listeria monocytogenes in food in the presence of competing Listeria innocua.

PubMed

Oravcová, K; Trncíková, T; Kuchta, T; Kaclíková, E

2008-02-01

Detectability of Listeria monocytogenes at 10(0) CFU per food sample in the presence of Listeria innocua using standard microbiological detection was evaluated and compared with the real-time PCR-based method. Enrichment in half-Fraser broth followed by subculture in Fraser broth according to EN ISO 11290-1 was used. False-negative detection of 10(0) CFU L. monocytogenes was obtained in the presence of 10(1) CFU L. innocua per sample using the standard detection method in contrast to more than 10(5) CFU L. innocua per sample using real-time PCR. Identification of L. monocytogenes on the chromogenic medium by the standard procedure was impossible if L. innocua was able to overgrow L. monocytogenes by more than three orders of magnitude after the enrichment in model samples. These results were confirmed using naturally contaminated food samples. Standard microbiological method was insufficient for the reliable detection of 10(0) CFU L. monocytogenes in the presence of more than 10(0) CFU of L. innocua per sample. On the other hand, if the growth of L. monocytogenes was sufficient to reach the concentration equal to the detection limit of PCR, the amount of the other microflora present in the food sample including L. innocua was not relevant for success of the PCR detection of L. monocytogenes. After the enrichment, the PCR detection is more convenient than the standard one as PCR detection is not compromised by other present microflora.

pXRF quantitative analysis of the Otowi Member of the Bandelier Tuff: Generating large, robust data sets to decipher trace element zonation in large silicic magma chambers

NASA Astrophysics Data System (ADS)

Van Hoose, A. E.; Wolff, J.; Conrey, R.

2013-12-01

Advances in portable X-Ray fluorescence (pXRF) analytical technology have made it possible for high-quality, quantitative data to be collected in a fraction of the time required by standard, non-portable analytical techniques. Not only do these advances reduce analysis time, but data may also be collected in the field in conjunction with sampling. Rhyolitic pumice, being primarily glass, is an excellent material to be analyzed with this technology. High-quality, quantitative data for elements that are tracers of magmatic differentiation (e.g. Rb, Sr, Y, Nb) can be collected for whole, individual pumices and subsamples of larger pumices in 4 minutes. We have developed a calibration for powdered rhyolite pumice from the Otowi Member of the Bandelier Tuff analyzed with the Bruker Tracer IV pXRF using Bruker software and influence coefficients for pumice, which measures the following 19 oxides and elements: SiO2, TiO2, Al2O3, FeO*, MnO, CaO, K2O, P2O5, Zn, Ga, Rb, Sr, Y, Zr, Nb, Ba, Ce, Pb, and Th. With this calibration for the pXRF and thousands of individual powdered pumice samples, we have generated an unparalleled data set for any single eruptive unit with known trace element zonation. The Bandelier Tuff of the Valles-Toledo Caldera Complex, Jemez Mountains, New Mexico, is divided into three main eruptive events. For this study, we have chosen the 1.61 Ma, 450 km3 Otowi Member as it is primarily unwelded and pumice samples are easily accessible. The eruption began with a plinian phase from a single source located near center of the current caldera and deposited the Guaje Pumice Bed. The initial Unit A of the Guaje is geochemically monotonous, but Units B through E, co-deposited with ignimbrite show very strong chemical zonation in trace elements, progressing upwards through the deposits from highly differentiated compositions (Rb ~350 ppm, Nb ~200 ppm) to less differentiated (Rb ~100 ppm, Nb ~50 ppm). Co-erupted ignimbrites emplaced during column collapse show

Assessment and forensic application of laser-induced breakdown spectroscopy (LIBS) for the discrimination of Australian window glass.

PubMed

El-Deftar, Moteaa M; Speers, Naomi; Eggins, Stephen; Foster, Simon; Robertson, James; Lennard, Chris

2014-08-01

A commercially available laser-induced breakdown spectroscopy (LIBS) instrument was evaluated for the determination of elemental composition of twenty Australian window glass samples, consisting of 14 laminated samples and 6 non-laminated samples (or not otherwise specified) collected from broken windows at crime scenes. In this study, the LIBS figures of merit were assessed in terms of accuracy, limits of detection and precision using three standard reference materials (NIST 610, 612, and 1831). The discrimination potential of LIBS was compared to that obtained using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), X-ray microfluorescence spectroscopy (μXRF) and scanning electron microscopy energy dispersive X-ray spectrometry (SEM-EDX) for the analysis of architectural window glass samples collected from crime scenes in the Canberra region, Australia. Pairwise comparisons were performed using a three-sigma rule, two-way ANOVA and Tukey's HSD test at 95% confidence limit in order to investigate the discrimination power for window glass analysis. The results show that the elemental analysis of glass by LIBS provides a discrimination power greater than 97% (>98% when combined with refractive index data), which was comparable to the discrimination powers obtained by LA-ICP-MS and μXRF. These results indicate that LIBS is a feasible alternative to the more expensive LA-ICP-MS and μXRF options for the routine forensic analysis of window glass samples. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Preliminary study on multi-element profile mapping of crustal and mantle zircons by using Synchrotron Radiation X-ray Fluorescence (SR-XRF)

NASA Astrophysics Data System (ADS)

Hasözbek, Altug; Shyam, Badri; Siebel, Wolfgang; Schmitt, Axel; Akay, Erhan; Skinner, Lawrie

2013-04-01

Zircon (ZrSiO4) is a mineral of singular importance in the geosciences. Zircon microanalysis has greatly contributed to our understanding of key events in earth's history as certain radioactive heavy elements and their daughter products are well-preserved within the exceptionally stable inorganic matrix of the mineral. A prevailing notion in this field is that zircon, as a mineral, is predominantly a crustal mineral; this has been contested in the last few years with more reports of mantle-derived zircons (Siebel et al., 2009). Zircons enriched from different parts of the upper mantle to lower crust from Turkey (Hasozbek et al. 2010) and Germany (Siebel et al., 2009) will be presented in this study using SR-XRF mapping carried out at beamline 2-IDE at the Advanced Photon Source synchrotron facility (Argonne National Laboratory, USA). The high-resolution (5-10 µm) elemental maps were obtained with collimated and linearly polarized synchrotron radiation (10 to 17 keV) and possess the advantage of being a completely non-destructive technique. Elemental maps of various trace and rare-earth elements along the cross-section of the zircons reveal a zonation-related distribution, which may be used to reveal factors affecting the growth history and dynamics of the crystal formation. Further, abrupt changes in elemental distribution or concentration were found to correspond to faults or inclusions within the zircon crystal. If such observations are found to be applicable for a wide range of samples, elemental mapping with this technique may serve as an important qualitative diagnostic to locating µ-meter inclusions that may be challenging to identify using other techniques (ICP-MS LA, SHRIMP,…) Through these preliminary elemental profile mapping studies of crustal and mantle zircons using SR-XRF methods, we aim to highlight a relatively quick and promising analytical method that may be used to study various geological problems.

Elemental concentration variations in Plio-Pleistocene sediments from ODP Site 1143 (southern South China Sea) obtained by XRF analyses

NASA Astrophysics Data System (ADS)

Tian, J.; Xie, X.; Jin, H.; Wang, P.; Jian, Z.

2009-12-01

Energy dispersive X-ray fluorescence (XRF) scanning technology provides the most accurate and most economic analytical methods for the determination of major and minor elements of the deep-sea sediment ranging from sodium (11) to uranium (92). Scanning on the smooth core surface by XRF Core scanner is reliable and non-destructive to the sediment, requiring little or no time to prepare the core. This method overcomes the drawback of the traditional analytical method by ICP-AES or ICP-MS which requires long time for sample preparation. Thus, it makes it viable to reconstruct long and high-resolution elemental time series from sediment cores. We have performed relatively elemental concentration analyses on the deep sea sediment cores from ODP site 1143 (southern SCS) down to 190.77 mcd (meters composite depth) by XRF core scanner. The depth resolution of the scanning is 1 cm, equivalent to a time resolution of ~250 years. The age model is based on tuning the benthic foraminiferal d18O at Site 1143 to obliquity and precession (Tian et al., 2002) which indicates that the 190.77 meters long sediment spans the past 5 Myr. We compared the records between 99.5 and 136.46 mcd with the elemental records from the same site obtained by Philips PW 2400 X-ray spectrometer (Wehausen et al., online publication). Comparison reveals, regardless of the absolute changes of the elements, that the elemental records (Si, Ti, Al, Fe, Mn, Ca, K, P, Ba, Rb, Sr) obtained by two methods are nearly the same. Results show that the relative concentration variations of the productivity related elements such as Ba and Ca display distinctive glacial-interglacial cycles for the past 5 Myr. These productivity cycles recorded show one-on-one relationship with the glacial-interglacial cycles of the global ice volume change recorded in the benthic foraminiferal d18O. The glacial-interglacial cycles in productivity and global ice volume changes are consistent with each other not only in amplitude but also

Comparison of two confocal micro-XRF spectrometers with different design aspects

PubMed Central

Smolek, S; Nakazawa, T; Tabe, A; Nakano, K; Tsuji, K; Streli, C; Wobrauschek, P

2014-01-01

Two different confocal micro X-ray fluorescence spectrometers have been developed and installed at Osaka City University and the Vienna University of Technology Atominstitut. The Osaka City University system is a high resolution spectrometer operating in air. The Vienna University of Technology Atominstitut spectrometer has a lower spatial resolution but is optimized for light element detection and operates under vacuum condition. The performance of both spectrometers was compared. In order to characterize the spatial resolution, a set of nine specially prepared single element thin film reference samples (500 nm in thickness, Al, Ti, Cr, Fe Ni, Cu, Zr, Mo, and Au) was used. Lower limits of detection were determined using the National Institute of Standards and Technology standard reference material glass standard 1412. A paint layer sample (cultural heritage application) and paint on automotive steel samples were analyzed with both instruments. The depth profile information was acquired by scanning the sample perpendicular to the surface. © 2013 The Authors. X-Ray Spectrometry published by John Wiley & Sons, Ltd. PMID:26430286

Comparison of two confocal micro-XRF spectrometers with different design aspects.

PubMed

Smolek, S; Nakazawa, T; Tabe, A; Nakano, K; Tsuji, K; Streli, C; Wobrauschek, P

2014-03-01

Two different confocal micro X-ray fluorescence spectrometers have been developed and installed at Osaka City University and the Vienna University of Technology Atominstitut. The Osaka City University system is a high resolution spectrometer operating in air. The Vienna University of Technology Atominstitut spectrometer has a lower spatial resolution but is optimized for light element detection and operates under vacuum condition. The performance of both spectrometers was compared. In order to characterize the spatial resolution, a set of nine specially prepared single element thin film reference samples (500 nm in thickness, Al, Ti, Cr, Fe Ni, Cu, Zr, Mo, and Au) was used. Lower limits of detection were determined using the National Institute of Standards and Technology standard reference material glass standard 1412. A paint layer sample (cultural heritage application) and paint on automotive steel samples were analyzed with both instruments. The depth profile information was acquired by scanning the sample perpendicular to the surface. © 2013 The Authors. X-Ray Spectrometry published by John Wiley & Sons, Ltd.

Limited copy number-high resolution melting (LCN-HRM) enables the detection and identification by sequencing of low level mutations in cancer biopsies.

PubMed

Do, Hongdo; Dobrovic, Alexander

2009-10-08

Mutation detection in clinical tumour samples is challenging when the proportion of tumour cells, and thus mutant alleles, is low. The limited sensitivity of conventional sequencing necessitates the adoption of more sensitive approaches. High resolution melting (HRM) is more sensitive than sequencing but identification of the mutation is desirable, particularly when it is important to discriminate false positives due to PCR errors or template degradation from true mutations.We thus developed limited copy number - high resolution melting (LCN-HRM) which applies limiting dilution to HRM. Multiple replicate reactions with a limited number of target sequences per reaction allow low level mutations to be detected. The dilutions used (based on Ct values) are chosen such that mutations, if present, can be detected by the direct sequencing of amplicons with aberrant melting patterns. Using cell lines heterozygous for mutations, we found that the mutations were not readily detected when they comprised 10% of total alleles (20% tumour cells) by sequencing, whereas they were readily detectable at 5% total alleles by standard HRM. LCN-HRM allowed these mutations to be identified by direct sequencing of those positive reactions.LCN-HRM was then used to review formalin-fixed paraffin-embedded (FFPE) clinical samples showing discordant findings between sequencing and HRM for KRAS exon 2 and EGFR exons 19 and 21. Both true mutations present at low levels and sequence changes due to artefacts were detected by LCN-HRM. The use of high fidelity polymerases showed that the majority of the artefacts were derived from the damaged template rather than replication errors during amplification. LCN-HRM bridges the sensitivity gap between HRM and sequencing and is effective in distinguishing between artefacts and true mutations.

Iron meteorite fragment studied by atomic and nuclear analytical methods

NASA Astrophysics Data System (ADS)

Cesnek, Martin; Štefánik, Milan; Kmječ, Tomáš; Miglierini, Marcel

2016-10-01

Chemical and structural compositions of a fragment of Sikhote-Alin iron meteorite were investigated by X-ray fluorescence analysis (XRF), neutron activation analysis (NAA) and Mössbauer spectroscopy (MS). XRF and NAA revealed the presence of chemical elements which are characteristic for iron meteorites. XRF also showed a significant amount of Si and Al on the surface of the fragment. MS spectra revealed possible presence of α-Fe(Ni, Co) phase with different local Ni concentration. Furthermore, paramagnetic singlet was detected in Mössbauer spectra recorded at room temperature and at 4.2 K.

Drug development and manufacturing

DOEpatents

Warner, Benjamin P.; McCleskey, T. Mark; Burrell, Anthony K.

2015-10-13

X-ray fluorescence (XRF) spectrometry has been used for detecting binding events and measuring binding selectivities between chemicals and receptors. XRF may also be used for estimating the therapeutic index of a chemical, for estimating the binding selectivity of a chemical versus chemical analogs, for measuring post-translational modifications of proteins, and for drug manufacturing.

Determining the 95% limit of detection for waterborne pathogen analyses from primary concentration to qPCR.

PubMed

Stokdyk, Joel P; Firnstahl, Aaron D; Spencer, Susan K; Burch, Tucker R; Borchardt, Mark A

2016-06-01

The limit of detection (LOD) for qPCR-based analyses is not consistently defined or determined in studies on waterborne pathogens. Moreover, the LODs reported often reflect the qPCR assay alone rather than the entire sample process. Our objective was to develop an approach to determine the 95% LOD (lowest concentration at which 95% of positive samples are detected) for the entire process of waterborne pathogen detection. We began by spiking the lowest concentration that was consistently positive at the qPCR step (based on its standard curve) into each procedural step working backwards (i.e., extraction, secondary concentration, primary concentration), which established a concentration that was detectable following losses of the pathogen from processing. Using the fraction of positive replicates (n = 10) at this concentration, we selected and analyzed a second, and then third, concentration. If the fraction of positive replicates equaled 1 or 0 for two concentrations, we selected another. We calculated the LOD using probit analysis. To demonstrate our approach we determined the 95% LOD for Salmonella enterica serovar Typhimurium, adenovirus 41, and vaccine-derived poliovirus Sabin 3, which were 11, 12, and 6 genomic copies (gc) per reaction (rxn), respectively (equivalent to 1.3, 1.5, and 4.0 gc L(-1) assuming the 1500 L tap-water sample volume prescribed in EPA Method 1615). This approach limited the number of analyses required and was amenable to testing multiple genetic targets simultaneously (i.e., spiking a single sample with multiple microorganisms). An LOD determined this way can facilitate study design, guide the number of required technical replicates, aid method evaluation, and inform data interpretation. Published by Elsevier Ltd.

Determining the 95% limit of detection for waterborne pathogen analyses from primary concentration to qPCR

USGS Publications Warehouse

Stokdyk, Joel P.; Firnstahl, Aaron; Spencer, Susan K.; Burch, Tucker R; Borchardt, Mark A.

2016-01-01

The limit of detection (LOD) for qPCR-based analyses is not consistently defined or determined in studies on waterborne pathogens. Moreover, the LODs reported often reflect the qPCR assay alone rather than the entire sample process. Our objective was to develop an approach to determine the 95% LOD (lowest concentration at which 95% of positive samples are detected) for the entire process of waterborne pathogen detection. We began by spiking the lowest concentration that was consistently positive at the qPCR step (based on its standard curve) into each procedural step working backwards (i.e., extraction, secondary concentration, primary concentration), which established a concentration that was detectable following losses of the pathogen from processing. Using the fraction of positive replicates (n = 10) at this concentration, we selected and analyzed a second, and then third, concentration. If the fraction of positive replicates equaled 1 or 0 for two concentrations, we selected another. We calculated the LOD using probit analysis. To demonstrate our approach we determined the 95% LOD for Salmonella enterica serovar Typhimurium, adenovirus 41, and vaccine-derived poliovirus Sabin 3, which were 11, 12, and 6 genomic copies (gc) per reaction (rxn), respectively (equivalent to 1.3, 1.5, and 4.0 gc L−1 assuming the 1500 L tap-water sample volume prescribed in EPA Method 1615). This approach limited the number of analyses required and was amenable to testing multiple genetic targets simultaneously (i.e., spiking a single sample with multiple microorganisms). An LOD determined this way can facilitate study design, guide the number of required technical replicates, aid method evaluation, and inform data interpretation.

A Control Allocation System for Automatic Detection and Compensation of Phase Shift Due to Actuator Rate Limiting

NASA Technical Reports Server (NTRS)

Yildiz, Yidiray; Kolmanovsky, Ilya V.; Acosta, Diana

2011-01-01

This paper proposes a control allocation system that can detect and compensate the phase shift between the desired and the actual total control effort due to rate limiting of the actuators. Phase shifting is an important problem in control system applications since it effectively introduces a time delay which may destabilize the closed loop dynamics. A relevant example comes from flight control where aggressive pilot commands, high gain of the flight control system or some anomaly in the system may cause actuator rate limiting and effective time delay introduction. This time delay can instigate Pilot Induced Oscillations (PIO), which is an abnormal coupling between the pilot and the aircraft resulting in unintentional and undesired oscillations. The proposed control allocation system reduces the effective time delay by first detecting the phase shift and then minimizing it using constrained optimization techniques. Flight control simulation results for an unstable aircraft with inertial cross coupling are reported, which demonstrate phase shift minimization and recovery from a PIO event.

Use of an Ultrasonic/Sonic Driller/Corer to Obtain Sample Powder for CHEMIN, a Combined XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Chipera, S. J.; Bish, D. L.; Vaniman, D. T.; Sherrit, S.; Bar-Cohen, Y.; Sarrazin, P.; Blake, D. F.

2003-01-01

A miniature CHEMIN XRD/XRF (X-Ray Diffraction/X-Ray Fluourescence) instrument is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed in order to enable XRD analysis on an extraterrestrial body is how best to obtain a representative sample powder for analysis. For XRD powder diffraction analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a 2-dimensional detector as used in the CHEMIN instrument will produce good results with poorly prepared powders, the quality of the data will improve if the sample is fine-grained and randomly oriented. An Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL is an effective mechanism of sampling rock to produce cores and powdered cuttings. It requires low axial load (< 5N) and thus offers significant advantages for operation from lightweight platforms and in low gravity environments. The USDC is lightweight (<0.5kg), and can be driven at low power (<5W) using duty cycling. It consists of an actuator with a piezoelectric stack, ultrasonic horn, free-mass, and drill bit. The stack is driven with a 20 kHz AC voltage at resonance. The strain generated by the piezoelectric is amplified by the horn by a factor of up to 10 times the displacement amplitude. The tip impacts the free-mass and drives it into the drill bit in a hammering action. The free-mass rebounds to interact with the horn tip leading to a cyclic rebound at frequencies in the range of 60-1000 Hz. It does not require lubricants, drilling fluid or bit sharpening and it has the potential to operate at high and low temperatures using a suitable choice of piezoelectric material. To assess whether the powder from an ultrasonic drill would be adequate for analyses by an XRD/XRF spectrometer such as CHEMIN, powders obtained from the JPL

A method for evaluating the performance of computer-aided detection of pulmonary nodules in lung cancer CT screening: detection limit for nodule size and density

PubMed Central

Kobayashi, Hajime; Ohkubo, Masaki; Narita, Akihiro; Marasinghe, Janaka C; Murao, Kohei; Matsumoto, Toru; Sone, Shusuke

2017-01-01

Objective: We propose the application of virtual nodules to evaluate the performance of computer-aided detection (CAD) of lung nodules in cancer screening using low-dose CT. Methods: The virtual nodules were generated based on the spatial resolution measured for a CT system used in an institution providing cancer screening and were fused into clinical lung images obtained at that institution, allowing site specificity. First, we validated virtual nodules as an alternative to artificial nodules inserted into a phantom. In addition, we compared the results of CAD analysis between the real nodules (n = 6) and the corresponding virtual nodules. Subsequently, virtual nodules of various sizes and contrasts between nodule density and background density (ΔCT) were inserted into clinical images (n = 10) and submitted for CAD analysis. Results: In the validation study, 46 of 48 virtual nodules had the same CAD results as artificial nodules (kappa coefficient = 0.913). Real nodules and the corresponding virtual nodules showed the same CAD results. The detection limits of the tested CAD system were determined in terms of size and density of peripheral lung nodules; we demonstrated that a nodule with a 5-mm diameter was detected when the nodule had a ΔCT > 220 HU. Conclusion: Virtual nodules are effective in evaluating CAD performance using site-specific scan/reconstruction conditions. Advances in knowledge: Virtual nodules can be an effective means of evaluating site-specific CAD performance. The methodology for guiding the detection limit for nodule size/density might be a useful evaluation strategy. PMID:27897029

Limited copy number - high resolution melting (LCN-HRM) enables the detection and identification by sequencing of low level mutations in cancer biopsies

PubMed Central

Do, Hongdo; Dobrovic, Alexander

2009-01-01

Background Mutation detection in clinical tumour samples is challenging when the proportion of tumour cells, and thus mutant alleles, is low. The limited sensitivity of conventional sequencing necessitates the adoption of more sensitive approaches. High resolution melting (HRM) is more sensitive than sequencing but identification of the mutation is desirable, particularly when it is important to discriminate false positives due to PCR errors or template degradation from true mutations. We thus developed limited copy number - high resolution melting (LCN-HRM) which applies limiting dilution to HRM. Multiple replicate reactions with a limited number of target sequences per reaction allow low level mutations to be detected. The dilutions used (based on Ct values) are chosen such that mutations, if present, can be detected by the direct sequencing of amplicons with aberrant melting patterns. Results Using cell lines heterozygous for mutations, we found that the mutations were not readily detected when they comprised 10% of total alleles (20% tumour cells) by sequencing, whereas they were readily detectable at 5% total alleles by standard HRM. LCN-HRM allowed these mutations to be identified by direct sequencing of those positive reactions. LCN-HRM was then used to review formalin-fixed paraffin-embedded (FFPE) clinical samples showing discordant findings between sequencing and HRM for KRAS exon 2 and EGFR exons 19 and 21. Both true mutations present at low levels and sequence changes due to artefacts were detected by LCN-HRM. The use of high fidelity polymerases showed that the majority of the artefacts were derived from the damaged template rather than replication errors during amplification. Conclusion LCN-HRM bridges the sensitivity gap between HRM and sequencing and is effective in distinguishing between artefacts and true mutations. PMID:19811662

Using XRF Geochemical Data to Differentiate Storm Event Deposits in a Backbarrier Lake in Coastal Louisiana

NASA Astrophysics Data System (ADS)

Dietz, M.; Liu, K. B.; Bianchette, T. A.; Yao, Q.; McCloskey, T.

2016-12-01

Hurricanes Gustav and Ike consecutively impacted coastal Louisiana in 2008 and generated significant storm surges. Three sediment cores taken from Bay Champagne, a coastal backbarrier lake near Port Fourchon, Louisiana, clearly show a deposition layer of clastic sediment up to 17 cm thick attributable to these two storms. X-ray fluorescence (XRF) analysis indicates that the two storm events can be distinguished from one another based on contrasting geochemical profiles. The bottom layer, presumably deposited by Hurricane Gustav, has high concentrations of S, Cl, Ca, and Sr, suggesting a strong marine influence. The top layer, presumably attributed to Hurricane Ike, has high concentrations of Ti, Mn, Fe and Zn, indicative of material of terrestrial origin. The elemental concentration profiles suggest that the storm deposits in each core were deposited through two distinct hydrological processes: a storm surge -driven marine intrusion during Hurricane Gustav, followed by intensive freshwater flooding during Hurricane Ike. Using these deposits as modern analogs, this technique could be applied to characterize older storm layers in the sedimentary record and potentially provide information about their respective depositional mechanisms.

Microanalysis (micro-XRF, micro-XANES, and micro-XRD) of a tertiary sediment using microfocused synchrotron radiation.

PubMed

Denecke, Melissa A; Somogyi, Andrea; Janssens, Koen; Simon, Rolf; Dardenne, Kathy; Noseck, Ulrich

2007-06-01

Micro-focused synchrotron radiation techniques to investigate actinide elements in geological samples are becoming an increasingly used tool in nuclear waste disposal research. In this article, results using mu-focus techniques are presented from a bore core section of a U-rich tertiary sediment collected from Ruprechtov, Czech Republic, a natural analog to nuclear waste repository scenarios in deep geological formations. Different methods are applied to obtain various, complementary information. Elemental and element chemical state distributions are obtained from micro-XRF measurements, oxidation states of As determined from micro-XANES, and the crystalline structure of selected regions are studied by means of micro-XRD. We find that preparation of the thin section created an As oxidation state artifact; it apparently changed the As valence in some regions of the sample. Results support our previously proposed hypothesis of the mechanism for U-enrichment in the sediment. AsFeS coating on framboid Fe nodules in the sediment reduced mobile groundwater-dissolved U(VI) to less-soluble U(IV), thereby immobilizing the uranium in the sediment.

Detection limits of 405 nm and 633 nm excited PpIX fluorescence for brain tumor detection during stereotactic biopsy

NASA Astrophysics Data System (ADS)

Markwardt, Niklas; Götz, Marcus; Haj-Hosseini, Neda; Hollnburger, Bastian; Sroka, Ronald; Stepp, Herbert; Zelenkov, Petr; Rühm, Adrian

2016-04-01

5-aminolevulinic-acid-(5-ALA)-induced protoporphyrin IX (PpIX) fluorescence may be used to improve stereotactic brain tumor biopsies. In this study, the sensitivity of PpIX-based tumor detection has been investigated for two potential excitation wavelengths (405 nm, 633 nm). Using a 200 μm fiber in contact with semi-infinite optical phantoms containing ink and Lipovenös, PpIX detection limits of 4.0 nM and 200 nM (relating to 1 mW excitation power) were determined for 405 nm and 633 nm excitation, respectively. Hence, typical PpIX concentrations in glioblastomas of a few μM should be well detectable with both wavelengths. Additionally, blood layers of selected thicknesses were placed between fiber and phantom. Red excitation was shown to be considerably less affected by blood interference: A 50 μm blood layer, for instance, blocked the 405- nm-excited fluorescence completely, but reduced the 633-nm-excited signal by less than 50%. Ray tracing simulations demonstrated that - without blood layer - the sensitivity advantage of 405 nm rises for decreasing fluorescent volume from 50-fold to a maximum of 100-fold. However, at a tumor volume of 1 mm3, which is a typical biopsy sample size, the 633-nm-excited fluorescence signal is only reduced by about 10%. Further simulations revealed that with increasing fiber-tumor distance, the signal drops faster for 405 nm. This reduces the risk of detecting tumor tissue outside the needle's coverage, but diminishes the overlap between optically and mechanically sampled volumes. While 405 nm generally offers a higher sensitivity, 633 nm is more sensitive to distant tumors and considerably superior in case of blood-covered tumor tissue.

Detection limits of quantitative and digital PCR assays and their influence in presence-absence surveys of environmental DNA

USGS Publications Warehouse

Hunter, Margaret; Dorazio, Robert M.; Butterfield, John S.; Meigs-Friend, Gaia; Nico, Leo; Ferrante, Jason A.

2017-01-01

A set of universal guidelines is needed to determine the limit of detection (LOD) in PCR-based analyses of low concentration DNA. In particular, environmental DNA (eDNA) studies require sensitive and reliable methods to detect rare and cryptic species through shed genetic material in environmental samples. Current strategies for assessing detection limits of eDNA are either too stringent or subjective, possibly resulting in biased estimates of species’ presence. Here, a conservative LOD analysis grounded in analytical chemistry is proposed to correct for overestimated DNA concentrations predominantly caused by the concentration plateau, a nonlinear relationship between expected and measured DNA concentrations. We have used statistical criteria to establish formal mathematical models for both quantitative and droplet digital PCR. To assess the method, a new Grass Carp (Ctenopharyngodon idella) TaqMan assay was developed and tested on both PCR platforms using eDNA in water samples. The LOD adjustment reduced Grass Carp occupancy and detection estimates while increasing uncertainty – indicating that caution needs to be applied to eDNA data without LOD correction. Compared to quantitative PCR, digital PCR had higher occurrence estimates due to increased sensitivity and dilution of inhibitors at low concentrations. Without accurate LOD correction, species occurrence and detection probabilities based on eDNA estimates are prone to a source of bias that cannot be reduced by an increase in sample size or PCR replicates. Other applications also could benefit from a standardized LOD such as GMO food analysis, and forensic and clinical diagnostics.

Lowering thresholds for speed limit enforcement impairs peripheral object detection and increases driver subjective workload.

PubMed

Bowden, Vanessa K; Loft, Shayne; Tatasciore, Monica; Visser, Troy A W

2017-01-01

Speed enforcement reduces incidences of speeding, thus reducing traffic accidents. Accordingly, it has been argued that stricter speed enforcement thresholds could further improve road safety. Effective speed monitoring however requires driver attention and effort, and human information-processing capacity is limited. Emphasizing speed monitoring may therefore reduce resource availability for other aspects of safe vehicle operation. We investigated whether lowering enforcement thresholds in a simulator setting would introduce further competition for limited cognitive and visual resources. Eighty-four young adult participants drove under conditions where they could be fined for travelling 1, 6, or 11km/h over a 50km/h speed-limit. Stricter speed enforcement led to greater subjective workload and significant decrements in peripheral object detection. These data indicate that the benefits of reduced speeding with stricter enforcement may be at least partially offset by greater mental demands on drivers, reducing their responses to safety-critical stimuli on the road. It is likely these results under-estimate the impact of stricter speed enforcement on real-world drivers who experience significantly greater pressures to drive at or above the speed limit. Copyright © 2016 Elsevier Ltd. All rights reserved.

Thermal background noise limitations

NASA Technical Reports Server (NTRS)

Gulkis, S.

1982-01-01

Modern detection systems are increasingly limited in sensitivity by the background thermal photons which enter the receiving system. Expressions for the fluctuations of detected thermal radiation are derived. Incoherent and heterodyne detection processes are considered. References to the subject of photon detection statistics are given.

Determination of minor and trace elements concentration in kidney stones using elemental analysis techniques

NASA Astrophysics Data System (ADS)

Srivastava, Anjali

The determination of accurate material composition of a kidney stone is crucial for understanding the formation of the kidney stone as well as for preventive therapeutic strategies. Radiations probing instrumental activation analysis techniques are excellent tools for identification of involved materials present in the kidney stone. The X-ray fluorescence (XRF) and neutron activation analysis (NAA) experiments were performed and different kidney stones were analyzed. The interactions of X-ray photons and neutrons with matter are complementary in nature, resulting in distinctly different materials detection. This is the first approach to utilize combined X-ray fluorescence and neutron activation analysis for a comprehensive analysis of the kideny stones. Presently, experimental studies in conjunction with analytical techniques were used to determine the exact composition of the kidney stone. The use of open source program Python Multi-Channel Analyzer was utilized to unfold the XRF spectrum. A new type of experimental set-up was developed and utilized for XRF and NAA analysis of the kidney stone. To verify the experimental results with analytical calculation, several sets of kidney stones were analyzed using XRF and NAA technique. The elements which were identified from XRF technique are Br, Cu, Ga, Ge, Mo, Nb, Ni, Rb, Se, Sr, Y, Zr. And, by using Neutron Activation Analysis (NAA) are Au, Br, Ca, Er, Hg, I, K, Na, Pm, Sb, Sc, Sm, Tb, Yb, Zn. This thesis presents a new approach for exact detection of accurate material composition of kidney stone materials using XRF and NAA instrumental activation analysis techniques.

City Core - detecting the anthropocene in urban lake cores

NASA Astrophysics Data System (ADS)

Kjaer, K. H.; Ilsøe, P.; Andresen, C. S.; Rasmussen, P.; Andersen, T. J.; Frei, R.; Schreiber, N.; Odgaard, B.; Funder, S.; Holm, J. M.; Andersen, K.

2011-12-01

Here, we presents the preliminary results from lake cores taken in ditches associated with the historical fortifications enclosing the oldest - central Copenhagen to achieve new knowledge from sediment deposits related to anthropogenic activities. We have examined sediment cores with X-ray fluorescence (XRF) analyzers to correlate element patterns from urban and industrial emissions. Thus, we aim to track these patterns back in time - long before regular routines of recording of atmospheric environment began around 1978. Furthermore, we compare our data to alternative sources of information in order to constrain and expand the temporal dating limits (approximately 1890) achieved from 210Pb activity. From custom reports and statistic sources, information on imported volumes from coal, metal and oil was obtained and related contaminants from these substances to the sediment archives. Intriguingly, we find a steep increase in import of coal and metals matching the exponential increase of lead and zinc counts from XRF-recordings of the sediment cores. In this finding, we claim to have constrain the initiation of urban industrialization. In order to confirm the age resolution of the lake cores, DNA was extracted from sediments, sedaDNA. Thus we attempt to trace plantation of well documented exotic plants to, for instance, the Botanical Garden. Through extraction and sampling of sedaDNA from these floral and arboreal specimens we intend to locate their strataigraphic horizons in the sediment core. These findings may correlate data back to 1872, when the garden was established on the area of the former fortification. In this line of research, we hope to achieve important supplementary knowledge of sedaDNA-leaching frequencies within freshwater sediments.

Estimation of the limit of detection in semiconductor gas sensors through linearized calibration models.

PubMed

Burgués, Javier; Jiménez-Soto, Juan Manuel; Marco, Santiago

2018-07-12

The limit of detection (LOD) is a key figure of merit in chemical sensing. However, the estimation of this figure of merit is hindered by the non-linear calibration curve characteristic of semiconductor gas sensor technologies such as, metal oxide (MOX), gasFETs or thermoelectric sensors. Additionally, chemical sensors suffer from cross-sensitivities and temporal stability problems. The application of the International Union of Pure and Applied Chemistry (IUPAC) recommendations for univariate LOD estimation in non-linear semiconductor gas sensors is not straightforward due to the strong statistical requirements of the IUPAC methodology (linearity, homoscedasticity, normality). Here, we propose a methodological approach to LOD estimation through linearized calibration models. As an example, the methodology is applied to the detection of low concentrations of carbon monoxide using MOX gas sensors in a scenario where the main source of error is the presence of uncontrolled levels of humidity. Copyright © 2018 Elsevier B.V. All rights reserved.

AN ALTERNATIVE CALIBRATION OF CR-39 DETECTORS FOR RADON DETECTION BEYOND THE SATURATION LIMIT.

PubMed

Franci, Daniele; Aureli, Tommaso; Cardellini, Francesco

2016-12-01

Time-integrated measurements of indoor radon levels are commonly carried out using solid-state nuclear track detectors (SSNTDs), due to the numerous advantages offered by this radiation detection technique. However, the use of SSNTD also presents some problems that may affect the accuracy of the results. The effect of overlapping tracks often results in the underestimation of the detected track density, which leads to the reduction of the counting efficiency for increasing radon exposure. This article aims to address the effect of overlapping tracks by proposing an alternative calibration technique based on the measurement of the fraction of the detector surface covered by alpha tracks. The method has been tested against a set of Monte Carlo data and then applied to a set of experimental data collected at the radon chamber of the Istituto Nazionale di Metrologia delle Radiazioni Ionizzanti, at the ENEA centre in Casaccia, using CR-39 detectors. It has been proved that the method allows to extend the detectable range of radon exposure far beyond the intrinsic limit imposed by the standard calibration based on the track density. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Heavy-metal contamination of soils in Saxony/Germany by foundry fumes and low-cost rapid analyses of contaminated soils by XRF

NASA Astrophysics Data System (ADS)

Mucke, D.

2012-04-01

Heavy-metal contamination of soils in Saxony/Germany by foundry fumes and low-cost rapid analysis of contaminated soils by XRF Dieter Mucke, Rolf Kumann, Sebastian Baldauf GEOMONTAN Gesellschaft für Geologie und Bergbau mbH&Co.KG, Muldentalstrasse 56, 09603 Rothenfurth, Saxony/Germany For hundreds of years in the Ore Mountains between Bohemia and Saxony silver and other ores are produced and smelted. Sulphide- and sulpharsenide-ores needed to be roasted first. In doing so the sulphide sulphur was oxidised under formation of sulphur dioxide SO2 and arsenide conversed into elemental arsenic and arsenide trioxide As2O3 respectively. Also the metals lead, cadmium and zinc are components of hut smokes, in the field of nickel foundries also nickel. The contents of soils basically reflect the geogenic conditions, which are caused by decomposition- and relocation-effects of the mineralisations, in the area of foundries also with influences by with the hut smokes anthropogenic mobilised elements. The Saxonian Agency for Environment and Geology drafted in 1992 a Soil Investigation Program with the aim of investigation of the contamination of Saxonian soils with arsenic and toxic heavy metals. In order of this Agency GEOMONTAN investigated 1164 measuring points in the grid 4 * 4 km.soil profiles and extracted soil samples for analysis. In the result of the laboratory examinations the Agency edited the "Soil atlas of the Free State of Saxony". 27 elements, pH and PAK are shown in detailed maps and allow in whole Saxony the first assessment of the contamination of soils with arsenic and toxic heavy metals. Each of the investigated soil profiles represent an area of 16 km2. Already by the different use of the districts (agricultural, industrial, urban) restricts representative values. GEOMONTAN in the meantime used at the exploration of a copper deposit in Brandenburg/Germany with approx. 50,000 single tests at drill cores a very fast low-cost method: the X Ray fluorescence

Elemental Scanning Devices Authenticate Works of Art

NASA Technical Reports Server (NTRS)

2013-01-01

To better detect aluminum compounds, Marshall Space Flight Center partnered with KeyMaster Inc. (later acquired by Madison, Wisconsin-based Bruker AXS Inc.) to develop a vacuum pump system that could be attached to X-ray fluorescence (XRF) scanners. The resulting technology greatly expanded XRF scanner capabilities, and hundreds of museums now use them to authenticate artifacts and works of art.

Detection limits of quantitative and digital PCR assays and their influence in presence-absence surveys of environmental DNA.

PubMed

Hunter, Margaret E; Dorazio, Robert M; Butterfield, John S S; Meigs-Friend, Gaia; Nico, Leo G; Ferrante, Jason A

2017-03-01

A set of universal guidelines is needed to determine the limit of detection (LOD) in PCR-based analyses of low-concentration DNA. In particular, environmental DNA (eDNA) studies require sensitive and reliable methods to detect rare and cryptic species through shed genetic material in environmental samples. Current strategies for assessing detection limits of eDNA are either too stringent or subjective, possibly resulting in biased estimates of species' presence. Here, a conservative LOD analysis grounded in analytical chemistry is proposed to correct for overestimated DNA concentrations predominantly caused by the concentration plateau, a nonlinear relationship between expected and measured DNA concentrations. We have used statistical criteria to establish formal mathematical models for both quantitative and droplet digital PCR. To assess the method, a new Grass Carp (Ctenopharyngodon idella) TaqMan assay was developed and tested on both PCR platforms using eDNA in water samples. The LOD adjustment reduced Grass Carp occupancy and detection estimates while increasing uncertainty-indicating that caution needs to be applied to eDNA data without LOD correction. Compared to quantitative PCR, digital PCR had higher occurrence estimates due to increased sensitivity and dilution of inhibitors at low concentrations. Without accurate LOD correction, species occurrence and detection probabilities based on eDNA estimates are prone to a source of bias that cannot be reduced by an increase in sample size or PCR replicates. Other applications also could benefit from a standardized LOD such as GMO food analysis and forensic and clinical diagnostics. Published 2016. This article is a U.S. Government work and is in the public domain in the USA.

Methodological challenges of optical tweezers-based X-ray fluorescence imaging of biological model organisms at synchrotron facilities.

PubMed

Vergucht, Eva; Brans, Toon; Beunis, Filip; Garrevoet, Jan; Bauters, Stephen; De Rijcke, Maarten; Deruytter, David; Janssen, Colin; Riekel, Christian; Burghammer, Manfred; Vincze, Laszlo

2015-07-01

Recently, a radically new synchrotron radiation-based elemental imaging approach for the analysis of biological model organisms and single cells in their natural in vivo state was introduced. The methodology combines optical tweezers (OT) technology for non-contact laser-based sample manipulation with synchrotron radiation confocal X-ray fluorescence (XRF) microimaging for the first time at ESRF-ID13. The optical manipulation possibilities and limitations of biological model organisms, the OT setup developments for XRF imaging and the confocal XRF-related challenges are reported. In general, the applicability of the OT-based setup is extended with the aim of introducing the OT XRF methodology in all research fields where highly sensitive in vivo multi-elemental analysis is of relevance at the (sub)micrometre spatial resolution level.

Detection of Hepatitis B Virus DNA among Chronic and potential Occult HBV patients in resource-limited settings by Loop-Mediated Isothermal Amplification assay.

PubMed

Akram, Arifa; Islam, S M Rashedul; Munshi, Saif Ullah; Tabassum, Shahina

2018-05-16

Transmission of Hepatitis B Virus (HBV) usually occurs due to the transfusion of blood or blood products from chronic HBV (CHB) or occult HBV infected (OBI) patients. Besides serological tests e.g. HBsAg and anti-HBc (total), detection of HBV-DNA is necessary for the diagnosis of OBI patients. Different nucleic acid tests (NATs) including real-time-Polymerase Chain Reaction (qPCR) are used for the detect HBV-DNA. The NATs are expensive and require technical expertise which are barriers to introducing them in resource-limited settings. This study was undertaken to evaluate the use of Loop-Mediated Isothermal Amplification (LAMP) assay as an alternative to qPCR for the detection of HBV-DNA in CHB and potential OBI patients in resource-limited settings. Following the published protocols with some modifications, a LAMP assay was developed for detection of HBV-DNA by either using a heat block followed by detection in an agarose gel or using a qPCR thermocycler. The LAMP assay was applied to supernatant prepared from heat treated serum collected from CHB and potential OBI patients. HBV viral load in serum was measured by qPCR using a single step HBV-DNA quantification kit. Among 200 samples tested, qPCR was capable to detect HBV-DNA in 25.5% of cases, whereas LAMP assay detected HBV-DNA in 43.5% cases. The qPCR was able to detect 11 (9.16%) potential OBI cases, whereas LAMP assay identified HBV-DNA in 43 (35.83%) cases. In addition to tests for HBsAg and/or anti-HBc (total), detection of HBV-DNA by LAMP assay may aid in preventing post-transfusion HBV infection in resource-limited settings. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Determination of selenium in biological samples with an energy-dispersive X-ray fluorescence spectrometer.

PubMed

Li, Xiaoli; Yu, Zhaoshui

2016-05-01

Selenium is both a nutrient and a toxin. Selenium-especially organic selenium-is a core component of human nutrition. Thus, it is very important to measure selenium in biological samples. The limited sensitivity of conventional XRF hampers its widespread use in biological samples. Here, we describe the use of high-energy (100kV, 600W) linearly polarized beam energy-dispersive X-Ray fluorescence spectroscopy (EDXRF) in tandem with a three-dimensional optics design to determine 0.1-5.1μgg(-1) levels of selenium in biological samples. The effects of various experimental parameters such as applied voltage, acquisition time, secondary target and various filters were thoroughly investigated. The detection limit of selenium in biological samples via high-energy (100kV, 600W) linearly polarized beam energy-dispersive X-ray fluorescence spectroscopy was decreased by one order of magnitude versus conventional XRF (Paltridge et al., 2012) and found to be 0.1μg/g. To the best of our knowledge, this is the first report to describe EDXRF measurements of Se in biological samples with important implications for the nutrition and analytical chemistry communities. Copyright © 2016 Elsevier Ltd. All rights reserved.

MicroXRF tomographic visualization of zinc and iron in the zebrafish embryo at the onset of the hatching period

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bourassa, Daisy; Gleber, Sophie-Charlotte; Vogt, Stefan

2016-01-01

Transition metals such as zinc, copper, and iron play key roles in cellular proliferation, cell differentiation, growth, and development. Over the past decade, advances in synchrotron X-ray fluorescence instrumentation presented new opportunities for the three-dimensional mapping of trace metal distributions within intact specimens. Taking advantage of microXRF tomography, we visualized the 3D distribution of zinc and iron in a zebrafish embryo at the onset of the hatching period. The reconstructed volumetric data revealed distinct differences in the elemental distributions, with zinc predominantly localized to the yolk and yolk extension, and iron to various regions of the brain as well asmore » the myotome extending along the dorsal side of the embryo. The data set complements an earlier tomographic study of an embryo at the pharyngula stage (24 hpf), thus offering new insights into the trace metal distribution at key stages of embryonic development.« less

SUPPLEMENT TO EPA COMPENDIUM METHOD TO-15 - REDUCTION OF METHOD DETECTION LIMITS TO MEET VAPOR INTRUSION MONITORING NEEDS

EPA Science Inventory

The Supplement to EPA Compendium Method TO-15 provides guidance for reducing the method detection limit (MDL) for the compound 1,1- dichloroethene (1,1-DCE) and for other volatile organic compounds (VOCs) from 0.5 ppbv, as cited in Method TO-15, to much lower concentrations. R...

SUPPLEMENT TO EPA COMPENDIUM METHOD TO-15 - REDUCTION OF METHOD DETECTION LIMITS TO MEET VAPOR INTRUSION MONITORING NEEDS

EPA Science Inventory

The Supplement to EPA Compendium Method TO-15 provides guidance for reducing the method detection limit (MDL) for the compound 1,1-dichloroethene (1,1-DCE) and for other volatile organic compounds (VOCs) from 0.5 parts per billion by volume (ppbv), as cited in Method TO-15, to ...

Natural history of optical coherence tomography-detected non-flow-limiting edge dissections following drug-eluting stent implantation.

PubMed

Radu, Maria D; Räber, Lorenz; Heo, Jungho; Gogas, Bill D; Jørgensen, Erik; Kelbæk, Henning; Muramatsu, Takashi; Farooq, Vasim; Helqvist, Steffen; Garcia-Garcia, Hector M; Windecker, Stephan; Saunamäki, Kari; Serruys, Patrick W

2014-01-22

Angiographic evidence of edge dissections has been associated with a risk of early stent thrombosis. Optical coherence tomography (OCT) is a high-resolution technology detecting a greater number of edge dissections--particularly non-flow-limiting--compared to angiography. Their natural history and clinical implications remain unclear. The objectives of the present study were to assess the morphology, healing response, and clinical outcomes of OCT-detected edge dissections using serial OCT imaging at baseline and at one year following drug-eluting stent (DES) implantation. Edge dissections were defined as disruptions of the luminal surface in the 5 mm segments proximal and distal to the stent, and categorised as flaps, cavities, double-lumen dissections or fissures. Qualitative and quantitative OCT analyses were performed every 0.5 mm at baseline and one year, and clinical outcomes were assessed. Sixty-three lesions (57 patients) were studied with OCT at baseline and one-year follow-up. Twenty-two non-flow-limiting edge dissections in 21 lesions (20 patients) were identified by OCT; only two (9%) were angiographically visible. Flaps were found in 96% of cases. The median longitudinal dissection length was 2.9 mm (interquartile range [IQR] 1.6-4.2 mm), whereas the circumferential and axial extensions amounted to 1.2 mm (IQR: 0.9-1.7 mm) and 0.6 mm (IQR: 0.4-0.7 mm), respectively. Dissections extended into the media and adventitia in seven (33%) and four (20%) cases, respectively. Eighteen (82%) OCT-detected edge dissections were also evaluated with intravascular ultrasound which identified nine (50%) of these OCT-detected dissections. No stent thrombosis or target lesion revascularisation occurred up to one year. At follow-up, 20 (90%) edge dissections were completely healed on OCT. The two cases exhibiting persistent dissection had the longest flaps (2.81 mm and 2.42 mm) at baseline. OCT-detected edge dissections which are angiographically silent in the majority of

Dual-balanced detection scheme with optical hard-limiters in an optical code division multiple access system

NASA Astrophysics Data System (ADS)

Liu, Maw-Yang; Hsu, Yi-Kai

2017-03-01

Three-arm dual-balanced detection scheme is studied in an optical code division multiple access system. As the MAI and beat noise are the main deleterious source of system performance, we utilize optical hard-limiters to alleviate such channel impairment. In addition, once the channel condition is improved effectively, the proposed two-dimensional error correction code can remarkably enhance the system performance. In our proposed scheme, the optimal thresholds of optical hard-limiters and decision circuitry are fixed, and they will not change with other system parameters. Our proposed scheme can accommodate a large number of users simultaneously and is suitable for burst traffic with asynchronous transmission. Therefore, it is highly recommended as the platform for broadband optical access network.

Breath Analysis Using Laser Spectroscopic Techniques: Breath Biomarkers, Spectral Fingerprints, and Detection Limits

PubMed Central

Wang, Chuji; Sahay, Peeyush

2009-01-01

Breath analysis, a promising new field of medicine and medical instrumentation, potentially offers noninvasive, real-time, and point-of-care (POC) disease diagnostics and metabolic status monitoring. Numerous breath biomarkers have been detected and quantified so far by using the GC-MS technique. Recent advances in laser spectroscopic techniques and laser sources have driven breath analysis to new heights, moving from laboratory research to commercial reality. Laser spectroscopic detection techniques not only have high-sensitivity and high-selectivity, as equivalently offered by the MS-based techniques, but also have the advantageous features of near real-time response, low instrument costs, and POC function. Of the approximately 35 established breath biomarkers, such as acetone, ammonia, carbon dioxide, ethane, methane, and nitric oxide, 14 species in exhaled human breath have been analyzed by high-sensitivity laser spectroscopic techniques, namely, tunable diode laser absorption spectroscopy (TDLAS), cavity ringdown spectroscopy (CRDS), integrated cavity output spectroscopy (ICOS), cavity enhanced absorption spectroscopy (CEAS), cavity leak-out spectroscopy (CALOS), photoacoustic spectroscopy (PAS), quartz-enhanced photoacoustic spectroscopy (QEPAS), and optical frequency comb cavity-enhanced absorption spectroscopy (OFC-CEAS). Spectral fingerprints of the measured biomarkers span from the UV to the mid-IR spectral regions and the detection limits achieved by the laser techniques range from parts per million to parts per billion levels. Sensors using the laser spectroscopic techniques for a few breath biomarkers, e.g., carbon dioxide, nitric oxide, etc. are commercially available. This review presents an update on the latest developments in laser-based breath analysis. PMID:22408503

[Estimation of time detection limit for human cytochrome b in females of Lutzomyia evansi].

PubMed

Vergara, José Gabriel; Verbel-Vergara, Daniel; Montesino, Ana Milena; Pérez-Doria, Alveiro; Bejarano, Eduar Elías

2017-03-29

Molecular biology techniques have allowed a better knowledge of sources of blood meals in vector insects. However, the usefulness of these techniques depends on both the quantity of ingested blood and the digestion process in the insect. To identify the time limit for detection of the human cytochrome b (Cyt b) gene in experimentally fed females of Lutzomyia evansi. Eight groups of L. evansi females were fed on human blood and sacrificed at intervals of 24 hours post-ingestion. Total DNA was extracted from each female and a segment of 358 bp of Cyt b was amplified. In order to eliminate false positives, amplification products were subjected to a restriction fragment length polymorphism (RFLP) analysis. The human Cyt b gene segment was detected in 86% (49/57) of the females of L. evansi, from 0 to 168 hours after blood ingestion. In 7% (4/57) of the individuals we amplified insect DNA, while in the remaining 7%, the band of interest was not amplified. We did not find any statistical differences between groups of females sacrificed at different times post-blood meal regarding the amplification of the human Cyt b gene segment or the number of samples amplified. The human Cyt b gene segment was detectable in L. evansi females up to 168 hours after blood ingestion.

Scheme for efficient extraction of low-frequency signal beyond the quantum limit by frequency-shift detection.

PubMed

Yang, R G; Zhang, J; Zhai, Z H; Zhai, S Q; Liu, K; Gao, J R

2015-08-10

Low-frequency (Hz~kHz) squeezing is very important in many schemes of quantum precision measurement. But it is more difficult than that at megahertz-frequency because of the introduction of laser low-frequency technical noise. In this paper, we propose a scheme to obtain a low-frequency signal beyond the quantum limit from the frequency comb in a non-degenerate frequency and degenerate polarization optical parametric amplifier (NOPA) operating below threshold with type I phase matching by frequency-shift detection. Low-frequency squeezing immune to laser technical noise is obtained by a detection system with a local beam of two-frequency intense laser. Furthermore, the low-frequency squeezing can be used for phase measurement in Mach-Zehnder interferometer, and the signal-to-noise ratio (SNR) can be enhanced greatly.

Quantitative analysis of trace levels of surface contamination by X-ray photoelectron spectroscopy Part I: statistical uncertainty near the detection limit.

PubMed

Hill, Shannon B; Faradzhev, Nadir S; Powell, Cedric J

2017-12-01

We discuss the problem of quantifying common sources of statistical uncertainties for analyses of trace levels of surface contamination using X-ray photoelectron spectroscopy. We examine the propagation of error for peak-area measurements using common forms of linear and polynomial background subtraction including the correlation of points used to determine both background and peak areas. This correlation has been neglected in previous analyses, but we show that it contributes significantly to the peak-area uncertainty near the detection limit. We introduce the concept of relative background subtraction variance (RBSV) which quantifies the uncertainty introduced by the method of background determination relative to the uncertainty of the background area itself. The uncertainties of the peak area and atomic concentration and of the detection limit are expressed using the RBSV, which separates the contributions from the acquisition parameters, the background-determination method, and the properties of the measured spectrum. These results are then combined to find acquisition strategies that minimize the total measurement time needed to achieve a desired detection limit or atomic-percentage uncertainty for a particular trace element. Minimization of data-acquisition time is important for samples that are sensitive to x-ray dose and also for laboratories that need to optimize throughput.

X-ray fluorescence analysis of wear metals in used lubricating oils

NASA Technical Reports Server (NTRS)

Maddox, W. E.; Kelliher, W. C.

1986-01-01

Used oils from several aircraft at NASA's Langley Research Center were analyzed over a three year period using X-ray fluorescence (XRF) and atomic emission spectrometry. The results of both analyses are presented and comparisons are made. Fe and Cu data for oil from four internal combustion engines are provided and XRF and atomic emission spectrometry measurements were found to be in perfect agreement. However, distributions were found in the case of oil from a jet aircraft engine whereby the latter method gave values for total iron concentration in the oil and did not distinguish between suspended particles and oil additives. XRF does not have these particle-size limitations; moreover, it is a faster process. It is concluded that XRF is the preferred method in the construction of a man-portable oil wear analysis instrument.

Detection of flow limitation in obstructive sleep apnea with an artificial neural network.

PubMed

Norman, Robert G; Rapoport, David M; Ayappa, Indu

2007-09-01

During sleep, the development of a plateau on the inspiratory airflow/time contour provides a non-invasive indicator of airway collapsibility. Humans recognize this abnormal contour easily, and this study replicates this with an artificial neural network (ANN) using a normalized shape. Five 10 min segments were selected from each of 18 sleep records (respiratory airflow measured with a nasal cannula) with varying degrees of sleep disordered breathing. Each breath was visually scored for shape, and breaths split randomly into a training and test set. Equally spaced, peak amplitude normalized flow values (representing breath shape) formed the only input to a back propagation ANN. Following training, breath-by-breath agreement of the ANN with the manual classification was tabulated for the training and test sets separately. Agreement of the ANN was 89% in the training set and 70.6% in the test set. When the categories of 'probably normal' and 'normal', and 'probably flow limited' and 'flow limited' were combined, the agreement increased to 92.7% and 89.4% respectively, similar to the intra- and inter-rater agreements obtained by a visual classification of these breaths. On a naive dataset, the agreement of the ANN to visual classification was 57.7% overall and 82.4% when the categories were collapsed. A neural network based only on the shape of inspiratory airflow succeeded in classifying breaths as to the presence/absence of flow limitation. This approach could be used to provide a standardized, reproducible and automated means of detecting elevated upper airway resistance.

An initial examination of carbonate production in the western equatorial Pacific: XRF results from the Pliocene-Pleistocene of IODP Site U1490

NASA Astrophysics Data System (ADS)

Chapman, J.; Kulhanek, D. K.; Rosenthal, Y.; Holbourn, A. E.

2017-12-01

International Ocean Discovery Program (IODP) Expedition 363 sought to determine the nature of and driving forces behind climate variability in the Western Pacific Warm Pool (WPWP) region throughout the Neogene on millennial, orbital, and geologic timescales. Our research focuses on the Pliocene to recent (4-0 Ma) sediment record from IODP Site U1490 to examine changes in carbonate production and burial in the WPWP as a record of variations in the regional/global carbon cycle. This interval is of particular interest because it spans the Middle Pliocene Warm Period, the initiation of Northern Hemisphere Glaciation, and the Mid-Pleistocene Transition. Site U1490 is located on the northern edge of Eauripik Rise at 05°58.95'N, 142°39.27'E in the northern part of the WPWP. At 2341 m water depth, today the site is bathed in Upper Circumpolar Deepwater. Pliocene to recent sediment primarily consists of foraminifer-rich nannofossil ooze, with the sedimentation rate varying between 1.5 and 3 cm/kyr. Initial shipboard measurement of calcium carbonate content shows little variation at low resolution (1 sample every few meters), varying between 90 and 95 wt%. We collected X-ray fluorescence (XRF) data at 2 cm resolution along the composite stratigraphic section to obtain a qualitative measure of the bulk chemistry of the sediment. We will use the weight percent calcium carbonate of discrete samples to calibrate the XRF data to generate a high-resolution carbonate record. We observe cyclical variations in the Ca/Ba, which may reflect variations in productivity and/or dissolution through this interval, although additional work is needed to fully interpret these data. Ultimately our research will allow for comparison between records obtained from these cores located in the western equatorial Pacific to those obtained in the eastern and central Pacific, which will better elucidate the nature of the carbon system during the Plio-Pleistocene.

Confocal laser-induced fluorescence detector for narrow capillary system with yoctomole limit of detection.

PubMed

Weaver, Mitchell T; Lynch, Kyle B; Zhu, Zaifang; Chen, Huang; Lu, Joann J; Pu, Qiaosheng; Liu, Shaorong

2017-04-01

Laser-induced fluorescence (LIF) detectors for low-micrometer and sub-micrometer capillary on-column detection are not commercially available. In this paper, we describe in details how to construct a confocal LIF detector to address this issue. We characterize the detector by determining its limit of detection (LOD), linear dynamic range (LDR) and background signal drift; a very low LOD (~70 fluorescein molecules or 12 yoctomole fluorescein), a wide LDR (greater than 3 orders of magnitude) and a small background signal drift (~1.2-fold of the root mean square noise) are obtained. For detecting analytes inside a low-micrometer and sub-micrometer capillary, proper alignment is essential. We present a simple protocol to align the capillary with the optical system and use the position-lock capability of a translation stage to fix the capillary in position during the experiment. To demonstrate the feasibility of using this detector for narrow capillary systems, we build a 2-μm-i.d. capillary flow injection analysis (FIA) system using the newly developed LIF prototype as a detector and obtain an FIA LOD of 14 zeptomole fluorescein. We also separate a DNA ladder sample by bare narrow capillary - hydrodynamic chromatography and use the LIF prototype to monitor the resolved DNA fragments. We obtain not only well-resolved peaks but also the quantitative information of all DNA fragments. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of a Limited Scope Network's Lightning Detection Efficiency

NASA Technical Reports Server (NTRS)

Rompala, John T.; Blakeslee, R.

2008-01-01

This paper outlines a modeling technique to map lightning detection efficiency variations over a region surveyed by a sparse array of ground based detectors. A reliable flash peak current distribution (PCD) for the region serves as the technique's base. This distribution is recast as an event probability distribution function. The technique then uses the PCD together with information regarding: site signal detection thresholds, type of solution algorithm used, and range attenuation; to formulate the probability that a flash at a specified location will yield a solution. Applying this technique to the full region produces detection efficiency contour maps specific to the parameters employed. These contours facilitate a comparative analysis of each parameter's effect on the network's detection efficiency. In an alternate application, this modeling technique gives an estimate of the number, strength, and distribution of events going undetected. This approach leads to a variety of event density contour maps. This application is also illustrated. The technique's base PCD can be empirical or analytical. A process for formulating an empirical PCD specific to the region and network being studied is presented. A new method for producing an analytical representation of the empirical PCD is also introduced.

Addressing the Limit of Detectability of Residual Oxide Discontinuities in Friction Stir Butt Welds of Aluminum using Phased Array Ultrasound

NASA Technical Reports Server (NTRS)

Johnston, P. H.

2008-01-01

This activity seeks to estimate a theoretical upper bound of detectability for a layer of oxide embedded in a friction stir weld in aluminum. The oxide is theoretically modeled as an ideal planar layer of aluminum oxide, oriented normal to an interrogating ultrasound beam. Experimentally-measured grain scattering level is used to represent the practical noise floor. Echoes from naturally-occurring oxides will necessarily fall below this theoretical limit, and must be above the measurement noise to be potentially detectable.

Detection of Matrix Elements and Trace Impurities in Cu(In, Ga)Se2 Photovoltaic Absorbers Using Surface Analytical Techniques.

PubMed

Kim, Min Jung; Lee, Jihye; Kim, Seon Hee; Kim, Haidong; Lee, Kang-Bong; Lee, Yeonhee

2015-10-01

Chalcopyrite Cu(In, Ga)Se2 (CIGS) thin films are well known as the next-generation solar cell materials notable for their high absorption coefficient for solar radiation, suitable band gap, and ability for deposition on flexible substrate materials, allowing the production of highly flexible and lightweight solar panels. To improve solar cell performances, a quantitative and depth-resolved elemental analysis of photovoltaic thin films is much needed. In this study, Cu(In, Ga)Se2 thin films were prepared on molybdenum back contacts deposited on soda-lime glass substrates via three-stage evaporation. Surface analyses via AES and SIMS were used to characterize the CIGS thin films and compare their depth profiles. We determined the average concentration of the matrix elements, Cu, In, Ga, and Se, using ICP-AES, XRF, and EPMA. We also obtained depth profiling results using TOF-SIMS, magnetic sector SIMS and AES, and APT, a sub-nanometer resolution characterization technique that enables three-dimensional elemental mapping. The SIMS technique, with its high detection limit and ability to obtain the profiles of elements in parallel, is a powerful tool for monitoring trace elements in CIGS thin films. To identify impurities in a CIGS layer, the distribution of trace elements was also observed according to depth by SIMS and APT.

Potential and limits of Raman spectroscopy for carotenoid detection in microorganisms: implications for astrobiology

PubMed Central

Jehlička, Jan; Edwards, Howell G. M.; Osterrothová, Kateřina; Novotná, Julie; Nedbalová, Linda; Kopecký, Jiří; Němec, Ivan; Oren, Aharon

2014-01-01

In this paper, it is demonstrated how Raman spectroscopy can be used to detect different carotenoids as possible biomarkers in various groups of microorganisms. The question which arose from previous studies concerns the level of unambiguity of discriminating carotenoids using common Raman microspectrometers. A series of laboratory-grown microorganisms of different taxonomic affiliation was investigated, such as halophilic heterotrophic bacteria, cyanobacteria, the anoxygenic phototrophs, the non-halophilic heterotrophs as well as eukaryotes (Ochrophyta, Rhodophyta and Chlorophyta). The data presented show that Raman spectroscopy is a suitable tool to assess the presence of carotenoids of these organisms in cultures. Comparison is made with the high-performance liquid chromatography approach of analysing pigments in extracts. Direct measurements on cultures provide fast and reliable identification of the pigments. Some of the carotenoids studied are proposed as tracers for halophiles, in contrast with others which can be considered as biomarkers of other genera. The limits of application of Raman spectroscopy are discussed for a few cases where the current Raman spectroscopic approach does not allow discriminating structurally very similar carotenoids. The database reported can be used for applications in geobiology and exobiology for the detection of pigment signals in natural settings. PMID:25368348

Iodine X-ray fluorescence computed tomography system utilizing a cadmium telluride detector in conjunction with a cerium-target tube

NASA Astrophysics Data System (ADS)

Hagiwara, Osahiko; Watanabe, Manabu; Sato, Eiichi; Matsukiyo, Hiroshi; Osawa, Akihiro; Enomoto, Toshiyuki; Nagao, Jiro; Sato, Shigehiro; Ogawa, Akira; Onagawa, Jun

2011-06-01

An X-ray fluorescence computed tomography system (XRF-CT) is useful for determining the main atoms in objects. To detect iodine atoms without using a synchrotron, we developed an XRF-CT system utilizing a cadmium telluride (CdTe) detector and a cerium X-ray generator. CT is performed by repeated linear scans and rotations of an object. When cerium K-series characteristic X-rays are absorbed by iodine atoms in objects, iodine K fluorescence is produced from atoms and is detected by the CdTe detector. Next, event signals of X-ray photons are produced with the use of charge-sensitive and shaping amplifiers. Iodine Kα fluorescence is isolated using a multichannel analyzer, and the number of photons is counted using a counter card. In energy-dispersive XRF-CT, the tube voltage and tube current were 70 kV and 0.40 mA, respectively, and the X-ray intensity was 115.3 μGy/s at a distance of 1.0 m from the source. The demonstration of XRF-CT was carried out by the selection of photons in an energy range from 27.5 to 29.5 keV with a photon-energy resolution of 1.2 keV.

Development of a micro-XRF system for biological samples based on proton-induced quasimonochromatic X-rays

NASA Astrophysics Data System (ADS)

Ploykrachang, K.; Hasegawa, J.; Kondo, K.; Fukuda, H.; Oguri, Y.

2014-07-01

We have developed a micro-XRF system based on a proton-induced quasimonochromatic X-ray (QMXR) microbeam for in vivo measurement of biological samples. A 2.5-MeV proton beam impinged normally on a Cu foil target that was slightly thicker than the proton range. The emitted QMXR behind the Cu target was focused with a polycapillary X-ray half lens. For application to analysis of wet or aquatic samples, we prepared a QMXR beam with an incident angle of 45° with respect to the horizontal plane by using a dipole magnet in order to bend the primary proton beam downward by 45°. The focal spot size of the QMXR microbeam on a horizontal sample surface was evaluated to be 250 × 350 μm by a wire scanning method. A microscope camera with a long working distance was installed perpendicular to the sample surface to identify the analyzed position on the sample. The fluorescent radiation from the sample was collected by a Si-PIN photodiode X-ray detector. Using the setup above, we were able to successfully measure the accumulation and distribution of Co in the leaves of a free-floating aquatic plant on a dilute Co solution surface.

Reducing bone lead content by chelation treatment in chronic lead poisoning: an in vivo X-ray fluorescence and bone biopsy study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Batuman, V.; Wedeen, R.P.; Bogden, J.D.

1989-02-01

A stained-glass artist with longstanding exposure to lead presented with neuropsychiatric symptoms. He was evaluated before and after chelation treatment by the CaNa2 EDTA lead mobilization test, iliac crest bone lead measurement, and in vivo tibial X-ray fluorescence (XRF). The three methods showed a progressive fall in body lead stores during chelation therapy in association with improvement in symptoms and a fall in blood lead and zinc protoporphyrin levels. In vivo tibial XRF is a safe, rapid, and noninvasive technique for detecting excessive body lead burdens. XRF measurement of bone lead content is a practical method for monitoring the efficacymore » of therapy as well as for establishing the diagnosis.« less

40 CFR Appendix C to Part 425 - Definition and Procedure for the Determination of the Method Detection Limit 1

Code of Federal Regulations, 2010 CFR

2010-07-01

... Determination of the Method Detection Limit 1 C Appendix C to Part 425 Protection of Environment ENVIRONMENTAL... CATEGORY Pt. 425, App. C Appendix C to Part 425—Definition and Procedure for the Determination of the... reagent water. (c) The concentration value that corresponds to the region of the standard curve where...

ON COMPUTING UPPER LIMITS TO SOURCE INTENSITIES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kashyap, Vinay L.; Siemiginowska, Aneta; Van Dyk, David A.

2010-08-10

A common problem in astrophysics is determining how bright a source could be and still not be detected in an observation. Despite the simplicity with which the problem can be stated, the solution involves complicated statistical issues that require careful analysis. In contrast to the more familiar confidence bound, this concept has never been formally analyzed, leading to a great variety of often ad hoc solutions. Here we formulate and describe the problem in a self-consistent manner. Detection significance is usually defined by the acceptable proportion of false positives (background fluctuations that are claimed as detections, or Type I error),more » and we invoke the complementary concept of false negatives (real sources that go undetected, or Type II error), based on the statistical power of a test, to compute an upper limit to the detectable source intensity. To determine the minimum intensity that a source must have for it to be detected, we first define a detection threshold and then compute the probabilities of detecting sources of various intensities at the given threshold. The intensity that corresponds to the specified Type II error probability defines that minimum intensity and is identified as the upper limit. Thus, an upper limit is a characteristic of the detection procedure rather than the strength of any particular source. It should not be confused with confidence intervals or other estimates of source intensity. This is particularly important given the large number of catalogs that are being generated from increasingly sensitive surveys. We discuss, with examples, the differences between these upper limits and confidence bounds. Both measures are useful quantities that should be reported in order to extract the most science from catalogs, though they answer different statistical questions: an upper bound describes an inference range on the source intensity, while an upper limit calibrates the detection process. We provide a recipe for computing

Occurrence of brominated diphenyl ethers, dibenzo-p-dioxins and dibenzofurans in foam materials in scrapped car seats from 1985 to 2012.

PubMed

Redin, L; Niinipuu, M; Jansson, S

2017-03-01

The purpose of this study was to evaluate the occurrence of polybrominated diphenyl ethers (PBDEs), dibenzo-p-dioxins (PBDDs) and dibenzofurans (PBDFs) in polyurethane foam (PUF) from car seats of end-of-life vehicles (ELVs) and compare the concentrations of PBDEs with the stipulated regulations in the POP Directive. The method comprised screening by X-ray fluorescence (XRF) and GG-MS analysis. Of 59 tested samples from ELVs, 17 samples showed lines above limit of detection (LOD) levels when screening by XRF. Those samples were selected as replicates and for further analysis by GC-MS. The majority of the studied samples showed low or non-detectable concentrations of PBDEs and PBDD/Fs, but two samples showed concentrations of Σ Te-HpBDEs close to the regulated level for Te-HpBDEs in waste (1000mgkg -1 ); one was slightly higher (1390mgkg -1 ) and the other slightly lower (570mgkg -1 ). It was concluded that brominated pollutants such as Te-HpBDEs occur in low levels in automotive applications in scrapped cars produced in years when brominated flame retardants were used. However, two of the 59 samples tested showed levels close to those stipulated by regulations concerning POPs in waste. Copyright © 2016 Elsevier Ltd. All rights reserved.

Markov Dynamics as a Zooming Lens for Multiscale Community Detection: Non Clique-Like Communities and the Field-of-View Limit

PubMed Central

Schaub, Michael T.; Delvenne, Jean-Charles; Yaliraki, Sophia N.; Barahona, Mauricio

2012-01-01

In recent years, there has been a surge of interest in community detection algorithms for complex networks. A variety of computational heuristics, some with a long history, have been proposed for the identification of communities or, alternatively, of good graph partitions. In most cases, the algorithms maximize a particular objective function, thereby finding the ‘right’ split into communities. Although a thorough comparison of algorithms is still lacking, there has been an effort to design benchmarks, i.e., random graph models with known community structure against which algorithms can be evaluated. However, popular community detection methods and benchmarks normally assume an implicit notion of community based on clique-like subgraphs, a form of community structure that is not always characteristic of real networks. Specifically, networks that emerge from geometric constraints can have natural non clique-like substructures with large effective diameters, which can be interpreted as long-range communities. In this work, we show that long-range communities escape detection by popular methods, which are blinded by a restricted ‘field-of-view’ limit, an intrinsic upper scale on the communities they can detect. The field-of-view limit means that long-range communities tend to be overpartitioned. We show how by adopting a dynamical perspective towards community detection [1], [2], in which the evolution of a Markov process on the graph is used as a zooming lens over the structure of the network at all scales, one can detect both clique- or non clique-like communities without imposing an upper scale to the detection. Consequently, the performance of algorithms on inherently low-diameter, clique-like benchmarks may not always be indicative of equally good results in real networks with local, sparser connectivity. We illustrate our ideas with constructive examples and through the analysis of real-world networks from imaging, protein structures and the power grid

Contrast limited adaptive histogram equalization image processing to improve the detection of simulated spiculations in dense mammograms.

PubMed

Pisano, E D; Zong, S; Hemminger, B M; DeLuca, M; Johnston, R E; Muller, K; Braeuning, M P; Pizer, S M

1998-11-01

The purpose of this project was to determine whether Contrast Limited Adaptive Histogram Equalization (CLAHE) improves detection of simulated spiculations in dense mammograms. Lines simulating the appearance of spiculations, a common marker of malignancy when visualized with masses, were embedded in dense mammograms digitized at 50 micron pixels, 12 bits deep. Film images with no CLAHE applied were compared to film images with nine different combinations of clip levels and region sizes applied. A simulated spiculation was embedded in a background of dense breast tissue, with the orientation of the spiculation varied. The key variables involved in each trial included the orientation of the spiculation, contrast level of the spiculation and the CLAHE settings applied to the image. Combining the 10 CLAHE conditions, 4 contrast levels and 4 orientations gave 160 combinations. The trials were constructed by pairing 160 combinations of key variables with 40 backgrounds. Twenty student observers were asked to detect the orientation of the spiculation in the image. There was a statistically significant improvement in detection performance for spiculations with CLAHE over unenhanced images when the region size was set at 32 with a clip level of 2, and when the region size was set at 32 with a clip level of 4. The selected CLAHE settings should be tested in the clinic with digital mammograms to determine whether detection of spiculations associated with masses detected at mammography can be improved.

Late Holocene glacial history of Petermann Fjord, Northwest Greenland: Non-destructive CT, XRF, and magnetic results from OD1507 sediment cores

NASA Astrophysics Data System (ADS)

Reilly, B. T.; Stoner, J. S.; Mix, A. C.; Jakobsson, M.; Jennings, A. E.; Walczak, M.; Dyke, L. M.; Cheseby, M.; Albert, S. W.; Wiest, J.

2016-12-01

An international and interdisciplinary expedition to Nares Strait and Petermann Fjord, Northwest Greenland, onboard the Swedish Icebreaker Oden July-September 2015 (OD1507) sought to understand the Holocene history of the Petermann glacial system among other research objectives. Petermann Glacier, which terminates as a floating ice-tongue in Petermann Fjord, is thought to be especially sensitive to ice-ocean interactions. While limited historical observations dating back to 1876 suggest the Petermann Ice Tongue extends about 70-90 km from the grounding-line, large calving events in 2010 and 2012 reduced the ice-tongue extent to about 45 km from the grounding-line. A suite of 14 marine sediment cores recovered a range of glacio-marine facies that form an along fjord (15-80 km from the grounding-line) and an across fjord depth (473-1041 meters water depth) transect. CT scans clearly identify four primary fjord facies, including bioturbated, IRD-rich, laminated and mud with stratified graded sand layers. The latter of these occurs near the modern grounding-line. Additionally, a new MATLAB routine is used to quantify clasts >2 mm in size from the CT scans. XRF sediment geochemical changes mirror magnetic mineral concentrations and are driven by varying contribution of Ca-rich and Ca-poor sources, which we interpret as a reflection of the mixing of the local carbonate rocks and crystalline basement excavated by the ice sheet. Initial paleomagnetic results isolate a strong and stable characteristic remanent magnetization which show remarkable similarity to paleosecular variation (PSV) recorded in nearby mid-late Holocene varved lakes on Ellesmere Island. This non-destructive dataset provides robust correlations, indicating a coherent and dynamic record of changes in the Petermann glacial system during the late Holocene, including evidence for a significant grounding-line retreat followed by the growth and relative paleo-extent of the modern Petermann Ice Tongue.

Trace elements in natural azurite pigments found in illuminated manuscript leaves investigated by synchrotron x-ray fluorescence and diffraction mapping

NASA Astrophysics Data System (ADS)

Smieska, Louisa M.; Mullett, Ruth; Ferri, Laurent; Woll, Arthur R.

2017-07-01

We present trace-element and composition analysis of azurite pigments in six illuminated manuscript leaves, dating from the thirteenth to sixteenth century, using synchrotron-based, large-area x-ray fluorescence (SR-XRF) and diffraction (SR-XRD) mapping. SR-XRF mapping reveals several trace elements correlated with azurite, including arsenic, zirconium, antimony, barium, and bismuth, that appear in multiple manuscripts but were not always detected by point XRF. Within some manuscript leaves, variations in the concentration of trace elements associated with azurite coincide with distinct regions of the illuminations, suggesting systematic differences in azurite preparation or purification. Variations of the trace element concentrations in azurite are greater among different manuscript leaves than the variations within each individual leaf, suggesting the possibility that such impurities reflect distinct mineralogical/geologic sources. SR-XRD maps collected simultaneously with the SR-XRF maps confirm the identification of azurite regions and are consistent with impurities found in natural mineral sources of azurite. In general, our results suggest the feasibility of using azurite trace element analysis for provenance studies of illuminated manuscript fragments, and demonstrate the value of XRF mapping in non-destructive determination of trace element concentrations within a single pigment.

Evaluation of the veracity of one work by the artist Di Cavalcanti through non-destructive techniques: XRF, imaging and brush stroke analysis

NASA Astrophysics Data System (ADS)

Kajiya, E. A. M.; Campos, P. H. O. V.; Rizzutto, M. A.; Appoloni, C. R.; Lopes, F.

2014-02-01

This paper presents systematic studies and analysis that contributed to the identification of the forgery of a work by the artist Emiliano Augusto Cavalcanti de Albuquerque e Melo, known as Di Cavalcanti. The use of several areas of expertise such as brush stroke analysis ("pinacologia"), applied physics, and art history resulted in an accurate diagnosis for ascertaining the authenticity of the work entitled "Violeiro" (1950). For this work we used non-destructive methods such as techniques of infrared, ultraviolet, visible and tangential light imaging combined with chemical analysis of the pigments by portable X-Ray Fluorescence (XRF) and graphic gesture analysis. Each applied method of analysis produced specific information that made possible the identification of materials and techniques employed and we concluded that this work is not consistent with patterns characteristic of the artist Di Cavalcanti.

Employing a portable X-Ray fluorescence (P-XRF) analyser and GIS to identify and map heavy metal pollution in soils of a traditional bonfire site

NASA Astrophysics Data System (ADS)

Dao, Ligang; Zhang, Chaosheng; Morrison, Liam

2010-05-01

Soils in the vicinity of bonfires are recipients of metal contaminants from burning of metal-containing materials. In order to better understand the impacts of bonfires on soils, a total of 218 surface soil samples were collected from a traditional bonfire site in Galway City, Ireland. Concentrations of Cu, Pb and Zn were determined using a portable X-ray Fluorescence (P-XRF) analyser. Strong variations were observed for these metals, and several samples contained elevated Zn concentrations which exceeded the intervention threshold of the Dutch criteria (720 mg kg-1). Spatial clusters and spatial outliers were detected using the local Moran's I index and were mapped using GIS. Two clear high value spatial clusters could be observed on the upper left side and centre part of the study area for Cu, Pb and Zn. Results of variogram analyses showed high nugget-sill-ratios for Cu, Pb and Zn, indicating strong spatial variation over short distances which could be resulted from anthropogenic activities. The spatial interpolation method of ordinary kriging was applied to produce the spatial interpolation maps for Cu, Pb and Zn, and the areas with elevated concentrations were in line with historical locations of the bonfires. The hazard maps showed small parts of the study area with Zn concentrations exceeding the Dutch intervention values. In order to prevent further contamination from bonfires, it is advised that tyres and other metal-containing wastes should not be burnt. The results in this study provide useful information for management of bonfires.

Highly selective optical fluoride ion sensor with submicromolar detection limit based on aluminum(III) octaethylporphyrin in thin polymeric film.

PubMed

Badr, Ibrahim H A; Meyerhoff, Mark E

2005-04-20

A highly selective, sensitive, and reversible fluoride optical sensing film based on aluminum(III)octaethylporphyrin as a fluoride ionophore and a lipophilic pH indicator as the optical transducer is described. The fluoride optical sensing films exhibit a submicromolar detection limit and high discrimination for fluoride over several lipophilic anions such as nitrate, perchlorate, and thiocyanate.

Detection limits of intraoperative near infrared imaging for tumor resection.

PubMed

Thurber, Greg M; Figueiredo, Jose-Luiz; Weissleder, Ralph

2010-12-01

The application of fluorescent molecular imaging to surgical oncology is a developing field with the potential to reduce morbidity and mortality. However, the detection thresholds and other requirements for successful intervention remain poorly understood. Here we modeled and experimentally validated depth and size of detection of tumor deposits, trade-offs in coverage and resolution of areas of interest, and required pharmacokinetics of probes based on differing levels of tumor target presentation. Three orthotopic tumor models were imaged by widefield epifluorescence and confocal microscopes, and the experimental results were compared with pharmacokinetic models and light scattering simulations to determine detection thresholds. Widefield epifluorescence imaging can provide sufficient contrast to visualize tumor margins and detect tumor deposits 3-5  mm deep based on labeled monoclonal antibodies at low objective magnification. At higher magnification, surface tumor deposits at cellular resolution are detectable at TBR ratios achieved with highly expressed antigens. A widefield illumination system with the capability for macroscopic surveying and microscopic imaging provides the greatest utility for varying surgical goals. These results have implications for system and agent designs, which ultimately should aid complete resection in most surgical beds and provide real-time feedback to obtain clean margins. © 2010 Wiley-Liss, Inc.

A practical approach to determination of laboratory GC-MS limits of detection.

PubMed

Underwood, P J; Kananen, G E; Armitage, E K

1997-01-01

Determination of limit of detection (LOD) values in a forensic laboratory serves a fundamental forensic requirement for assay performance. In addition to demonstrating assay capability, LOD values can also be used to fulfill certification requirements of a high-volume forensic drug laboratory. The LOD was defined as the lowest concentration of drug that the laboratory can detect in a specimen with forensic certainty at a minimum of 85% of the time. Overall batch acceptance criteria included acceptable quantitation of control materials (within 20% of target), acceptable chromatography (symmetry, peak integration, peak shape, peak, and baseline resolution), retention time within +/-1% of the extracted standard, and mass ion ratios within +/-20% of the extracted standard mass ion ratios. Individual specimen acceptance criteria were the same as the batch acceptance criteria excluding the quantitation requirement. Data were collected from all instruments on different runs. A minimum of ten data points was required for each certified instrument, and a minimum of 85% of data points was acceptable. Quantitation within +/-20% of the LOD concentration was not required, but acceptable mass ratios were required. Data points with poor chromatography (internal standard failed mass ratios; interference of the baseline, for example, shoulders; asymmetry; and baseline resolution) was omitted from the acceptable rate calculation. Data points with good chromatography with failed mass ion ratios were included in the acceptable rate calculation. With these criteria, we established the following LODs: 11-nor-delta 9-tetrahydrocannabinol-9-carboxylic acid, 2 ng/mL; benzoylecgonine, 5 ng/mL; phencyclidine, 2.5 ng/mL; amphetamine, 150 ng/mL; methamphetamine, 100 ng/mL; codeine, 500 ng/mL; and morphine, 1000 ng/mL.

Suppression of plasma virus load below the detection limit of a human immunodeficiency virus kit is associated with longer virologic response than suppression below the limit of quantitation.

PubMed

Raboud, J M; Rae, S; Hogg, R S; Yip, B; Sherlock, C H; Harrigan, P R; O'Shaughnessy, M V; Montaner, J S

1999-10-01

Suppression of human immunodeficiency virus type 1 plasma virus load (PVL) to <20 copies/mL is associated with a longer virologic response after initiation of antiretroviral therapy. The relationship between duration of virologic response and PVL nadir according to a less sensitive assay was explored. When compared with subjects with a PVL nadir >500 copies/mL, the relative risks of PVL rising above 1000 copies/mL for participants in the INCAS trial and the British Columbia Drug Treatment Program with a PVL nadir below the limit of detection (LOD) were 0.04 (95% confidence interval [CI], 0.02-0.09) and 0.06 (95% CI, 0.03-0.12), respectively. The corresponding relative risks for persons with a detectable but not quantifiable PVL nadir were 0.25 (95% CI, 0.13-0.50) and 0.54 (95% CI, 0.25-1.19). The relative risks of virologic failure associated with a PVL nadir detectable but not quantifiable and a PVL nadir below the LOD were statistically different (P<.0001) in both data sets.

Hallmarks in prostate cancer imaging with Ga68-PSMA-11-PET/CT with reference to detection limits and quantitative properties.

PubMed

Sanchez-Crespo, Alejandro; Jussing, Emma; Björklund, Ann-Charlotte; Pokrovskaja Tamm, Katja

2018-04-04

Gallium-68-labeled prostate-specific antigen positron emission tomography/computed tomography imaging (Ga68-PSMA-11-PET/CT) has emerged as a potential gold standard for prostate cancer (PCa) diagnosis. However, the imaging limitations of this technique at the early state of PCa recurrence/metastatic spread are still not well characterized. The aim of this study was to determine the quantitative properties and the fundamental imaging limits of Ga68-PSMA-11-PET/CT in localizing small PCa cell deposits. The human PCa LNCaP cells (PSMA expressing) were grown and collected as single cell suspension or as 3D-spheroids at different cell numbers and incubated with Ga68-PSMA-11. Thereafter, human HCT116 cells (PSMA negative) were added to a total cell number of 2 × 10 5 cells per tube. The tubes were then pelleted and the supernatant aspirated. A whole-body PET/CT scanner with a clinical routine protocol was used for imaging the pellets inside of a cylindrical water phantom with increasing amounts of background activity. The actual activity bound to the cells was also measured in an automatic gamma counter. Imaging detection limits and activity recovery coefficients as a function of LNCaP cell number were obtained. The effect of Ga68-PSMA-11 mass concentration on cell binding was also investigated in samples of LnCaP cells incubated with increasing concentrations of radioligand. A total of 1 × 10 4 LNCaP cells mixed in a pellet of 2 × 10 5 cells were required to reach a 50% detection probability with Ga68-PSMA-11-PET/CT without background. With a background level of 1 kBq/ml, between 4 × 10 5 and 1 × 10 6 cells are required. The radioligand equilibrium dissociation constant was 27.05 nM, indicating high binding affinity. Hence, the specific activity of the radioligand has a profound effect on image quantification. Ga68-PSMA-11-PET detects a small number of LNCaP cells even when they are mixed in a population of non-PSMA expressing cells and in the

The Use and Abuse of Limits of Detection in Environmental Analytical Chemistry

PubMed Central

Brown, Richard J. C.

2008-01-01

The limit of detection (LoD) serves as an important method performance measure that is useful for the comparison of measurement techniques and the assessment of likely signal to noise performance, especially in environmental analytical chemistry. However, the LoD is only truly related to the precision characteristics of the analytical instrument employed for the analysis and the content of analyte in the blank sample. This article discusses how other criteria, such as sampling volume, can serve to distort the quoted LoD artificially and make comparison between various analytical methods inequitable. In order to compare LoDs between methods properly, it is necessary to state clearly all of the input parameters relating to the measurements that have been used in the calculation of the LoD. Additionally, the article discusses that the use of LoDs in contexts other than the comparison of the attributes of analytical methods, in particular when reporting analytical results, may be confusing, less informative than quoting the actual result with an accompanying statement of uncertainty, and may act to bias descriptive statistics. PMID:18690384

Finding Kuiper Belt Objects Below the Detection Limit

NASA Astrophysics Data System (ADS)

Whidden, Peter; Kalmbach, Bryce; Bektesevic, Dino; Connolly, Andrew; Jones, Lynne; Smotherman, Hayden; Becker, Andrew

2018-01-01

We demonstrate a novel approach for uncovering the signatures of moving objects (e.g. Kuiper Belt Objects) below the detection thresholds of single astronomical images. To do so, we will employ a matched filter moving at specific rates of proposed orbits through a time-domain dataset. This is analogous to the better-known "shift-and-stack" method; however it uses neither direct shifting nor stacking of the image pixels. Instead of resampling the raw pixels to create an image stack, we will instead integrate the object detection probabilities across multiple single-epoch images to accrue support for a proposed orbit. The filtering kernel provides a measure of the probability that an object is present along a given orbit, and enables the user to make principled decisions about when the search has been successful, and when it may be terminated. The results we present here utilize GPUs to speed up the search by two orders of magnitudes over CPU implementations.

Variation in the limit-of-detection of the ProSpecT Campylobacter microplate enzyme immunoassay in stools spiked with emerging Campylobacter species.

PubMed

Bojanić, Krunoslav; Midwinter, Anne Camilla; Marshall, Jonathan Craig; Rogers, Lynn Elizabeth; Biggs, Patrick Jon; Acke, Els

2016-08-01

Campylobacter enteritis in humans is primarily associated with C. jejuni/coli infection. The impact of other Campylobacter spp. is likely to be underestimated due to the bias of culture methods towards Campylobacter jejuni/coli diagnosis. Stool antigen tests are becoming increasingly popular and appear generally less species-specific. A review of independent studies of the ProSpecT® Campylobacter Microplate enzyme immunoassay (EIA) developed for C. jejuni/coli showed comparable diagnostic results to culture methods but the examination of non-jejuni/coli Campylobacter spp. was limited and the limit-of-detection (LOD), where reported, varied between studies. This study investigated LOD of EIA for Campylobacter upsaliensis, Campylobacter hyointestinalis and Campylobacter helveticus spiked in human stools. Multiple stools and Campylobacter isolates were used in three different concentrations (10(4)-10(9)CFU/ml) to reflect sample heterogeneity. All Campylobacter species evaluated were detectable by EIA. Multivariate analysis showed LOD varied between Campylobacter spp. and faecal consistency as fixed effects and individual faecal samples as random effects. EIA showed excellent performance in replicate testing for both within and between batches of reagents, in agreement between visual and spectrophotometric reading of results, and returned no discordance between the bacterial concentrations within independent dilution test runs (positive results with lower but not higher concentrations). This study shows how limitations in experimental procedures lead to an overestimation of consistency and uniformity of LOD for EIA that may not hold under routine use in diagnostic laboratories. Benefits and limitations for clinical practice and the influence on estimates of performance characteristics from detection of multiple Campylobacter spp. by EIA are discussed. Copyright © 2016 Elsevier B.V. All rights reserved.

Estimation of the limit of detection using information theory measures.

PubMed

Fonollosa, Jordi; Vergara, Alexander; Huerta, Ramón; Marco, Santiago

2014-01-31

Definitions of the limit of detection (LOD) based on the probability of false positive and/or false negative errors have been proposed over the past years. Although such definitions are straightforward and valid for any kind of analytical system, proposed methodologies to estimate the LOD are usually simplified to signals with Gaussian noise. Additionally, there is a general misconception that two systems with the same LOD provide the same amount of information on the source regardless of the prior probability of presenting a blank/analyte sample. Based upon an analogy between an analytical system and a binary communication channel, in this paper we show that the amount of information that can be extracted from an analytical system depends on the probability of presenting the two different possible states. We propose a new definition of LOD utilizing information theory tools that deals with noise of any kind and allows the introduction of prior knowledge easily. Unlike most traditional LOD estimation approaches, the proposed definition is based on the amount of information that the chemical instrumentation system provides on the chemical information source. Our findings indicate that the benchmark of analytical systems based on the ability to provide information about the presence/absence of the analyte (our proposed approach) is a more general and proper framework, while converging to the usual values when dealing with Gaussian noise. Copyright © 2013 Elsevier B.V. All rights reserved.

Chlorine-trapped CVD bilayer graphene for resistive pressure sensor with high detection limit and high sensitivity

NASA Astrophysics Data System (ADS)

Phuong Pham, Viet; Triet Nguyen, Minh; Park, Jin Woo; Kwak, Sung Soo; Nguyen, Dieu Hien Thi; Kyeom Mun, Mu; Danh Phan, Hoang; San Kim, Doo; Kim, Ki Hyun; Lee, Nae-Eung; Yeom, Geun Young

2017-06-01

Pressure sensing is one of the key functions for smart electronics. Considerably more effort is required to achieve the fabrication of pressure sensors that can imitate and overcome the sophisticated pressure sensing characteristics in nature and industry, especially in the innovation of materials and structures. Almost all of the pressure sensors reported until now have a high sensitivity at a low-pressure detection limit (<10 kPa). While the exploration of a pressure sensor with a high sensitivity and a high responsivity at a high-pressure is challenging, it is required for next generation smart electronics. Here, we report an exotic heterostructure pressure sensor based on ZnO/chlorine radical-trap doped bilayer graphene (ZGClG) as an ideal channel for pressure sensors. Using this ZGClG as the channel, this study shows the possibility of forming a pressure sensor with a high sensitivity (0.19 kPa-1) and a high responsivity (0.575 s) at V  =  1 V on glass substrate. Further, the pressure detection limit of this device was as high as 98 kPa. The investigation of the sensing mechanism under pressure has revealed that the significant improved sensing effect is related to the heavy p-type chlorine trap doping in the channel graphene with chlorine radicals without damaging the graphene. This work indicates that the ZGClG channel used for the pressure sensing device could also provide a simple and essential sensing platform for chemical-, medical-, and biological-sensing for future smart electronics.

Lower limits of spin detection efficiency for two-parameter two-qubit (TPTQ) states with non-ideal ferromagnetic detectors

NASA Astrophysics Data System (ADS)

Majd, Nayereh; Ghasemi, Zahra

2016-10-01

We have investigated a TPTQ state as an input state of a non-ideal ferromagnetic detectors. Minimal spin polarization required to demonstrate spin entanglement according to entanglement witness and CHSH inequality with respect to (w.r.t.) their two free parameters have been found, and we have numerically shown that the entanglement witness is less stringent than the direct tests of Bell's inequality in the form of CHSH in the entangled limits of its free parameters. In addition, the lower limits of spin detection efficiency fulfilling secure cryptographic key against eavesdropping have been derived. Finally, we have considered TPTQ state as an output of spin decoherence channel and the region of ballistic transmission time w.r.t. spin relaxation time and spin dephasing time has been found.

Evaluating detection limits of next-generation sequencing for the surveillance and monitoring of international marine pests.

PubMed

Pochon, Xavier; Bott, Nathan J; Smith, Kirsty F; Wood, Susanna A

2013-01-01

Most surveillance programmes for marine invasive species (MIS) require considerable taxonomic expertise, are laborious, and are unable to identify species at larval or juvenile stages. Therefore, marine pests may go undetected at the initial stages of incursions when population densities are low. In this study, we evaluated the ability of the benchtop GS Junior™ 454 pyrosequencing system to detect the presence of MIS in complex sample matrices. An initial in-silico evaluation of the mitochondrial cytochrome c oxidase subunit I (COI) and the nuclear small subunit ribosomal DNA (SSU) genes, found that multiple primer sets (targeting a ca. 400 base pair region) would be required to obtain species level identification within the COI gene. In contrast a single universal primer set was designed to target the V1-V3 region of SSU, allowing simultaneous PCR amplification of a wide taxonomic range of MIS. To evaluate the limits of detection of this method, artificial contrived communities (10 species from 5 taxonomic groups) were created using varying concentrations of known DNA samples and PCR products. Environmental samples (water and sediment) spiked with one or five 160 hr old Asterias amurensis larvae were also examined. Pyrosequencing was able to recover DNA/PCR products of individual species present at greater than 0.64% abundance from all tested contrived communities. Additionally, single A. amurensis larvae were detected from both water and sediment samples despite the co-occurrence of a large array of environmental eukaryotes, indicating an equivalent sensitivity to quantitative PCR. NGS technology has tremendous potential for the early detection of marine invasive species worldwide.

Detection of nanoplastics in food by asymmetric flow field-flow fractionation coupled to multi-angle light scattering: possibilities, challenges and analytical limitations.

PubMed

Correia, Manuel; Loeschner, Katrin

2018-02-06

We tested the suitability of asymmetric flow field-flow fractionation (AF4) coupled to multi-angle light scattering (MALS) for detection of nanoplastics in fish. A homogenized fish sample was spiked with 100 nm polystyrene nanoparticles (PSNPs) (1.3 mg/g fish). Two sample preparation strategies were tested: acid digestion and enzymatic digestion with proteinase K. Both procedures were found suitable for degradation of the organic matrix. However, acid digestion resulted in large PSNPs aggregates/agglomerates (> 1 μm). The presence of large particulates was not observed after enzymatic digestion, and consequently it was chosen as a sample preparation method. The results demonstrated that it was possible to use AF4 for separating the PSNPs from the digested fish and to determine their size by MALS. The PSNPs could be easily detected by following their light scattering (LS) signal with a limit of detection of 52 μg/g fish. The AF4-MALS method could also be exploited for another type of nanoplastics in solution, namely polyethylene (PE). However, it was not possible to detect the PE particles in fish, due to the presence of an elevated LS background. Our results demonstrate that an analytical method developed for a certain type of nanoplastics may not be directly applicable to other types of nanoplastics and may require further adjustment. This work describes for the first time the detection of nanoplastics in a food matrix by AF4-MALS. Despite the current limitations, this is a promising methodology for detecting nanoplastics in food and in experimental studies (e.g., toxicity tests, uptake studies). Graphical abstract Basic concept for the detection of nanoplastics in fish by asymmetric flow field-flow fractionation coupled to multi-angle light scattering.

Monitoring the environmental effects of CeO2 and ZnO nanoparticles through the life cycle of corn (Zea mays) plants and in situ μ-XRF mapping of nutrients in kernels.

PubMed

Zhao, Lijuan; Sun, Youping; Hernandez-Viezcas, Jose A; Hong, Jie; Majumdar, Sanghamitra; Niu, Genhua; Duarte-Gardea, Maria; Peralta-Videa, Jose R; Gardea-Torresdey, Jorge L

2015-03-03

Information about changes in physiological and agronomic parameters through the life cycle of plants exposed to engineered nanoparticles (NPs) is scarce. In this study, corn (Zea mays) plants were cultivated to full maturity in soil amended with either nCeO2 or nZnO at 0, 400, and 800 mg/kg. Gas exchange was monitored every 10 days, and at harvest, bioaccumulation of Ce and Zn in tissues was determined by ICP-OES/MS. The effects of NPs exposure on nutrient concentration and distribution in ears were also evaluated by ICP-OES and μ-XRF. Results showed that nCeO2 at both concentrations did not impact gas exchange in leaves at any growth stage, while nZnO at 800 mg/kg reduced net photosynthesis by 12%, stomatal conductance by 15%, and relative chlorophyll content by 10% at day 20. Yield was reduced by 38% with nCeO2 and by 49% with nZnO. Importantly, μ-XRF mapping showed that nCeO2 changed the allocation of calcium in kernels, compared to controls. In nCeO2 treated plants, Cu, K, Mn, and Zn were mainly localized at the insertion of kernels into cobs, but Ca and Fe were distributed in other parts of the kernels. Results showed that nCeO2 and nZnO reduced corn yield and altered quality of corn.

Obsidian provenance determination by using the beam stability controlled BSC-XRF and the PIXE-alpha portable spectrometers of the LANDIS laboratory of the LNS-INFN and IBAM-CNR in Catania (Italy)

NASA Astrophysics Data System (ADS)

Pappalardo, L.; Bracchitta, D.; Palio, O.; Pappalardo, G.; Rizzo, F.

2012-04-01

About 1300 obsidian artefacts coming from various archaeological sites of Sicily were analyzed by using the BSC-XRF (Beam Stability Controlled - X-ray Fluorescence) and PIXE-alpha (Particle Induced X-ray Emission, using low energy alpha particles) portable spectrometers developed at the Landis laboratory at the LNS-INF and IBAM-CNR in Catania (Italy). The portable BSC-XRF system allows the non-destructive analysis of the Rb, Sr, Y, Zr and Nb trace concentrations, which are considered to be characteristic of the obsidian samples and consequently are indicative of the provenance quarries. Quantitative data on Rb, Sr, Y, Zr, Nb trace element concentrations where deduced through the use of a method that makes use of a multi parameter linear regression, previously The portable PIXE-alpha spectrometer allows the quantitative determination of the matrix major elements, from Na to Zn. In the present work the two instrumental devices are presented. The data are from: Milena (Cl), Ustica (Pa), Rocchicella (Ct), Poggio dell'Acquila (Ct), San Marco (Ct), Villaggio del Petraro* (Sr) and Licodia Eubea* (Ct). Results on compositional data for trace elements and major elements allowed to identify Lipari and Pantelleria islands as the only two sources of the analysed samples. Analyses carried out on vitreous artefact found in Rocchicella, showed for the first time that the Palagonite was used as row material. *Preliminary data. Topic of conference: Application of XRS in archaeometry Kind of presentation: oral

Correlations of trace elements in breast human tissues: Evaluation of spatial distribution using μ-XRF

NASA Astrophysics Data System (ADS)

Silva, Marina Piacenti da; Silva, Deisy Mara da; Ribeiro-Silva, Alfredo; Poletti, Martin Eduardo

2012-05-01

The aim of this work is to investigate microscopic correlations between trace elements in breast human tissues. A synchrotron X-ray fluorescence microprobe system (μ-XRF) was used to obtain two-dimensional distribution of trace element Ca, Fe, Cu and Zn in normal (6 samples) and malignant (14 samples) breast tissues. The experiment was performed in X-ray Fluorescence beam line at Laboratório Nacional de Luz Síncrotron (LNLS), Campinas, Brazil. The white microbeam was generated with a fine conical capillary with a 20 μm output diameter. The samples were supported on a XYZ table. An optical microscope with motorized zoom was used for sample positioning and choice the area to be scanned. Automatic two-dimensional scans were programmed and performed with steps of 30 μm in each direction (x, y) on the selected area. The fluorescence signals were recorded using a Si(Li) detector, positioned at 90 degrees with respect to the incident beam, with a collection time of 10 s per point. The elemental maps obtained from each sample were overlap to observe correlation between trace elements. Qualitative results showed that the pairs of elements Ca-Zn and Fe-Cu could to be correlated in malignant breast tissues. Quantitative results, achieved by Spearman correlation tests, indicate that there is a spatial correlation between these pairs of elements (p < 0.001) suggesting the importance of these elements in metabolic processes associated with the development of the tumor.

The reasons for the color green fluorite Mehmandooye cover using UV spectroscopy and XRF results

NASA Astrophysics Data System (ADS)

Pirzadeh, Sara; Zahiri, Reza

2016-04-01

Fluorite mineral or fluorine with chemical formula CaF2 is most important mineralfluor in nature. This mineral crystallization to colors yellow, green, pink, blue, purple, colorless and sometimes black andin cubic system crystallized.assemi transparent and glass with polished.fluoritethe purity include 48/9% fluoreand 51/9% calcium. How the creation colors in minerals different greatly indebted to Kurt Nassau research from Bell Labs, Murray Hill, New Jersey.almostall the mechanisms that cause color in minerals, are the result of the interaction of light waves with the electrons The main factors affecting the color generation include the following: 1)the presence of a constructive element inherent (essential ingredient mineral composition) 2)The presence of a minor impurities (such a element as involved in latticesolid solution) 3) appearancedefects in the crystal structure 4) There are some physical boundaries with distances very small and delicate, like blades out of the solution (which may be the play of colors or Chatvyansy) 5) Mixing mechanical impurities dispersed in a host mineral Based on the results of the analysis, XRF and UV spectrum and also based on the results of ICP, because the color green fluorite examined, the focus color (F_center) and also the presence of some elementsintermediate (such as Y (yttrium). [1] Bill, H., Calas, G. Color centres associated rare earth ions and the origin of coloration in natural fluorites// PhysChem Min, (1978), v 3, pp. 117-131.

Uranium speciation as a function of depth in contaminated hanford sediments--a micro-XRF, micro-XRD, and micro- and bulk-XAFS study.

PubMed

Singer, David M; Zachara, John M; Brown, Gordon E

2009-02-01

The distribution and speciation of U and Cu in contaminated vadose zone and aquifer sediments from the U.S. DOE Hanford site (300 Area) were determined using a combination of synchrotron-based micro-X-ray fluorescence (microXRF) imaging, micro-X-ray absorption near edge structure (microXANES) spectroscopy, and micro-X-ray diffraction (microXRD) techniques combined with bulk U LIII-edge X-ray absorption fine structure (XAFS) spectroscopy. Samples were collected from within the inactive North Process Pond (NPP2) at 8 ft (2.4 m, NPP2-8) depth and 12 ft (3.7 m, NPP2-12) depth in the vadose zone, and fines were isolated from turbid groundwater just below the water Table (12-14 ft, approximately 4 m, NPP2-GW). microXRF imaging, microXRD, and microXANES spectroscopy revealed two major U occurrences within the vadose and groundwater zones: (1) low to moderate concentrations of U(VI) associated with fine-textured grain coatings that were consistently found to contain clinochlore (referred to here as chlorite) observed in all three samples, and (2) U(VI)-Cu(II) hotspots consisting of micrometer-sized particles associated with surface coatings on grains of muscovite and chlorite observed in samples NPP2-8' and NPP2-GW. In the aquifer fines (NPP2-GW), these particles were identified as cuprosklodowskite (cps: Cu[(UO2)(SiO2OH)]2 x 6H2O) and metatorbernite (mtb: Cu(UO2)2(PO4)2 x 8H2O). In contrast, the U-Cu-containing particles in the vadose zone were X-ray amorphous. Analyses of U LIII-edge XAFS spectra by linear-combination fitting indicated that U speciation consisted of (1) approximately 75% uranyl sorbed to chlorite and approximately 25% mtb-like X-ray amorphous U-Cu-phosphates (8 ft depth), (2) nearly 100% sorbed uranyl (12 ft depth), and (3) approximately 70% uranyl sorbed to chlorite and approximately 30% cps/mtb (groundwater zone). These findings suggest that dissolution of U(VI)-Cu(II)-bearing solids as well as desorption of U(VI), mainly from phyllosilicates, are

Quantum Limits of Space-to-Ground Optical Communications

NASA Technical Reports Server (NTRS)

Hemmati, H.; Dolinar, S.

2012-01-01

For a pure loss channel, the ultimate capacity can be achieved with classical coherent states (i.e., ideal laser light): (1) Capacity-achieving receiver (measurement) is yet to be determined. (2) Heterodyne detection approaches the ultimate capacity at high mean photon numbers. (3) Photon-counting approaches the ultimate capacity at low mean photon numbers. A number of current technology limits drive the achievable performance of free-space communication links. Approaching fundamental limits in the bandwidth-limited regime: (1) Heterodyne detection with high-order coherent-state modulation approaches ultimate limits. SOA improvements to laser phase noise, adaptive optics systems for atmospheric transmission would help. (2) High-order intensity modulation and photon-counting can approach heterodyne detection within approximately a factor of 2. This may have advantages over coherent detection in the presence of turbulence. Approaching fundamental limits in the photon-limited regime (1) Low-duty cycle binary coherent-state modulation (OOK, PPM) approaches ultimate limits. SOA improvements to laser extinction ratio, receiver dark noise, jitter, and blocking would help. (2) In some link geometries (near field links) number-state transmission could improve over coherent-state transmission

Quantum-limited evanescent single molecule sensing.

NASA Astrophysics Data System (ADS)

Bowen, Warwick; Mauranyapin, Nicolas; Madsen, Lars; Taylor, Michael; Waleed, Muhammad

Sensors that are able to detect and track single unlabeled biomolecules are an important tool both to understand biomolecular dynamics and interactions, and for medical diagnostics operating at their ultimate detection limits. Recently, exceptional sensitivity has been achieved using the strongly enhanced evanescent fields provided by optical microcavities and plasmonic resonators. However, at high field intensities photodamage to the biological specimen becomes increasingly problematic. Here, we introduce a new approach that combines dark field illumination and heterodyne detection in an optical nanofibre. This allows operation at the fundamental precision limit introduced by quantisation of light. We achieve state-of-the-art sensitivity with a four order-of-magnitude reduction in optical intensity. This enables quantum noise limited tracking of single biomolecules as small as 3.5 nm and surface-molecule interactions to be montored over extended periods. By achieving quantum noise limited precision, our approach provides a pathway towards quantum-enhanced single-molecule biosensors. We acknkowledge financial support from AFOSR and AOARD.

Compositional classification and sedimentological interpretation of the laminated lacustrine sediments at Baumkrichen (Western Austria) using XRF core scanning data

NASA Astrophysics Data System (ADS)

Barrett, Samuel; Tjallingii, Rik; Bloemsma, Menno; Brauer, Achim; Starnberger, Reinhard; Spötl, Christoph; Dulski, Peter

2015-04-01

The outcrop at Baumkirchen (Austria) encloses part of a unique sequence of laminated lacustrine sediments deposited during the last glacial cycle. A ~250m long composite sediment record recovered at this location now continuously covers the periods ~33 to ~45 ka BP (MIS 3) and ~59 to ~73 ka BP (MIS 4), which are separated by a hiatus. The well-laminated (mm-cm scale) and almost entirely clastic sediments reveal alternations of clayey silt and medium silt to very-fine sand layers. Although radiocarbon and optically stimulated luminescence (OSL) dating provide a robust chronology, accurate dating of the sediment laminations appears to be problematic due to very high sedimentation rates (3-8 cm/yr). X-ray fluorescence (XRF) core scanning provided a detailed ~150m long record of compositional changes of the sediments at Baumkirchen. Changes in the sediments are subtle and classification into different facies based on individual elements is therefore subjective. We applied a statistically robust clustering analysis to provide an objective compositional classification without prior knowledge, based on XRF measurements for 15 analysed elements (all those with an acceptable signal-noise ratio: Zr, Sr, Ca, Mn, Cu, Zn, Rb, Ni, Fe, K, Cr, V, Si, Ba, T). The clustering analysis indicates a distinct compositional change between sediments deposited below and above the stratigraphic hiatus, but also differentiates between individual different laminae. Preliminary results suggest variations in the sequence are largely controlled by the relative occurrence of different kinds of sediment represented by different clusters. Three clusters identify well-laminated sediments, visually similar in appearance, each dominated by an anti-correlation between Ca and one or more of the detrital elements K, Zr, Ti, Si and Fe. Two of these clusters occur throughout the entire sequence, one frequently and the other restricted to short sections, while the third occurs almost exclusively below the

Soft tissue measurement of arsenic and selenium in an animal model using portable X-ray fluorescence

NASA Astrophysics Data System (ADS)

Fleming, David E. B.; Groves, John W.; Gherase, Mihai R.; George, Graham N.; Pickering, Ingrid J.; Ponomarenko, Olena; Langan, George; Spallholz, Julian E.; Alauddin, Mohammad; Ahsan, Habibul; Ahmed, Selim; La Porte, Paul F.

2015-11-01

The ingestion of trace amounts of arsenic (As) through drinking water is a relatively common pathway of exposure with potentially serious long-term health effects. Studies involving animal models have indicated that selenium (Se) may bind with As inside the body and facilitate excretion. A portable X-ray fluorescence (XRF) technique was previously developed to allow in vivo measurement of As and Se in human tissue. In the current paper, this portable XRF approach was tested for the first time using animal tissue. Seven female Lakeview Golden/LVG Syrian hamsters were dosed under either control, As-only, Se-only, or As and Se conditions. Minimum XRF detection limits in soft tissue of 1.00±0.05 ppm for As and 0.83±0.02 ppm for Se were determined from phantom calibration trials. For dosed hamsters, consistently higher concentrations of As and Se were found in the liver and gall bladder, with elevated levels also observed in the intestines. Concentrations ranged up to 26.4±1.4 ppm for As and 11.8±0.8 ppm for Se. The stomach and heart exhibited more moderate concentrations, while the brain, lung, and muscle demonstrated lower levels. For a given organ, As concentrations generally exceeded Se concentrations. A ratio of approximately 2.5:1 was observed for concentrations of As:Se when considering the same or similar tissue sites in dosed hamsters. Implications for potential in vivo human applications of the technique are briefly considered.

Graphic products used in the evaluation of traditional and emerging remote sensing technologies for the detection of fugitive contamination at selected superfund hazardous waste sites

USGS Publications Warehouse

Slonecker, E. Terrence; Fisher, Gary B.

2011-01-01

This report presents the overhead imagery and field sampling results used to prepare U.S. Geological Survey Open-File Report 2011-1050, 'Evaluation of Traditional and Emerging Remote Sensing Technologies for the Detection of Fugitive Contamination at Selected Superfund Hazardous Waste Sites'. These graphic products were used in the evaluation of remote sensing technology in postclosure monitoring of hazardous waste sites and represent an ongoing research effort. Soil sampling results presented here were accomplished with field portable x-ray fluoresence (XRF) technology and are used as screening tools only representing the current conditions of metals and other contaminants at selected Superfund hazardous waste sites.

Characteristics of right-sided colonic neoplasia and colonoscopy barriers limiting their early detection and prognosis: a review of the literature.

PubMed

Fischbach, Wolfgang; Elsome, Rory; Amlani, Bharat

2018-06-05

Colonoscopy provides less protection from colorectal cancer in the right colon than the left. Areas covered: This review examines patient outcomes and colonoscopy success rates to identify factors that limit the protective effect of colonoscopy in the right colon. The MEDLINE and Embase databases were searched for literature from 2000 onwards, on the long-term outcomes and differences in screening practice between the right and left colon. In total, 12 systematic reviews (including nine meta-analyses) and 44 primary data records were included. Differences in patient outcomes and colonoscopy practice were identified between the right and left colon, suggesting that several factors, many of which disproportionally affect the right colon, impact lesion detection rates. Shorter withdrawal times reduce detection rates, while longer times significantly increase detection; mostly of adenomas in the right colon. Colonoscope attachments often only show a significant improvement in detection rates in the right colon, suggesting detection is more challenging due to visibility of the right colonic mucosa. Higher bowel cleansing grades significantly improve detection rates in the right colon compared to the left. Expert commentary: These findings confirm the need for continued improvement of colonoscopy effectiveness, and obligatory quality assessment, overall and especially in the right colon.

Development of Detectability Limits for On-Orbit Inspection of Space Shuttle Wing Leading Edge

NASA Technical Reports Server (NTRS)

Stephan, Ryan A.; Johnson, David G.; Mastropietro, A. J.; Ancarrow, Walt C.

2005-01-01

At the conclusion of the Columbia Accident Investigation, one of the recommendations of the Columbia Accident Investigation Board (CAIB) was that NASA develop and implement an inspection plan for the Reinforced Carbon-Carbon (RCC) system components of the Space Shuttle. To address these issues, a group of scientists and engineers at NASA Langley Research Center proposed the use of an IR camera to inspect the RCC. Any crack in an RCC panel changes the thermal resistance of the material in the direction perpendicular to the crack. The change in thermal resistance can be made visible by introducing a heat flow across the crack and using an IR camera to image the resulting surface temperature distribution. The temperature difference across the crack depends on the change in the thermal resistance, the length of the crack, the local thermal gradient, and the rate of radiation exchange with the environment. This paper describes how the authors derived the minimum thermal gradient detectability limits for a through crack in an RCC panel. This paper will also show, through the use of a transient, 3-dimensional, finite element model, that these minimum gradients naturally exist on-orbit. The results from the finite element model confirm that there are sufficient thermal gradient to detect a crack on 96% of the RCC leading edge.

Detecting position using ARKit II: generating position-time graphs in real-time and further information on limitations of ARKit

NASA Astrophysics Data System (ADS)

Dilek, Ufuk; Erol, Mustafa

2018-05-01

ARKit is a framework which allows developers to create augmented reality apps for the iPhone and iPad. In a previous study, we had shown that it could be used to detect position in educational physics experiments and emphasized that the ability to provide position data in real-time was one of the prominent features of this newly emerging technology. In this study, we demonstrate an example of how real-time data acquisition can be employed in educational settings, report some of the limitations of ARKit and how we have overcome these limitations. By means of ARKit or a similar framework, ordinary mobile devices can be adapted for use in microcomputer-based lab activities.

Theoretical limitations of quantification for noncompetitive sandwich immunoassays.

PubMed

Woolley, Christine F; Hayes, Mark A; Mahanti, Prasun; Douglass Gilman, S; Taylor, Tom

2015-11-01

Immunoassays exploit the highly selective interaction between antibodies and antigens to provide a vital method for biomolecule detection at low concentrations. Developers and practitioners of immunoassays have long known that non-specific binding often restricts immunoassay limits of quantification (LOQs). Aside from non-specific binding, most efforts by analytical chemists to reduce the LOQ for these techniques have focused on improving the signal amplification methods and minimizing the limitations of the detection system. However, with detection technology now capable of sensing single-fluorescence molecules, this approach is unlikely to lead to dramatic improvements in the future. Here, fundamental interactions based on the law of mass action are analytically connected to signal generation, replacing the four- and five-parameter fittings commercially used to approximate sigmoidal immunoassay curves and allowing quantitative consideration of non-specific binding and statistical limitations in order to understand the ultimate detection capabilities of immunoassays. The restrictions imposed on limits of quantification by instrumental noise, non-specific binding, and counting statistics are discussed based on equilibrium relations for a sandwich immunoassay. Understanding the maximal capabilities of immunoassays for each of these regimes can greatly assist in the development and evaluation of immunoassay platforms. While many studies suggest that single molecule detection is possible through immunoassay techniques, here, it is demonstrated that the fundamental limit of quantification (precision of 10 % or better) for an immunoassay is approximately 131 molecules and this limit is based on fundamental and unavoidable statistical limitations.

Satellite based Global Flood Detection System - strengths and limitations

NASA Astrophysics Data System (ADS)

Revilla-Romero, Beatriz; Salamon, Peter; Thielen, Jutta; De Groeve, Tom; Zajac, Zuzanna

2014-05-01

One of the main problems for global hydrological models is that for many regions only very limited or no observational data for a model assessment is available. This problem could be overcome with filling the gaps using information derived from satellite observations. Thus, an evaluation of the remote sensing signal of the Global Flood Detection System (GFDS) against observed discharge data was performed in order to test the use of this data in sparsely gauged river basins. The study was carried out at 398 locations near the main rivers and in Africa, Asia, Europe, North America and South America. After evaluating different methodologies for extracting the satellite signal, a temporal (4 days) and spatial (4 GFDS pixels) average was chosen to proceed with the analysis. For the 340 stations with a concurrent time series longer than seven years for both, the signal and the in situ observed discharge (obtained mainly from the Global Runoff Data Centre), a calibration based on monthly linear models was carried out. The validation was executed and several skill scores were calculated such as the R2, Nash-Sutcliffe (NSE), and Root Mean Square Error (RMSE). It is important to highlight that, for this study, 230 stations globally had Nash-Sutcliffe efficient score higher than zero, indicating that for specific conditions the satellite signal as used in GFDS can fill the gaps where observations are not available. For example, several locations in African catchments have good performance as in the Niger, Volta and Zambezi for which Nash-Sutcliffe is greater than 0.75. It is known that a number of factors affect total upwelling microwave brightness from a mixed water and land surface measured by a single image pixel. Aiming to better understand how some features of the sites could affect the satellite signal and the correlation with in situ observations, apart from the dependency on the river geometry, a multivariate analysis was carried out between the skill scores (NSE and

Lowering detection limits for 1,2,3-trichloropropane in water using solid phase extraction coupled to purge and trap sample introduction in an isotope dilution GC-MS method.

PubMed

Liao, Wenta; Ghabour, Miriam; Draper, William M; Chandrasena, Esala

2016-09-01

Purge and trap sample introduction (PTI) has been the premier sampling and preconcentration technique for gas chromatographic determination of volatile organic compounds (VOCs) in drinking water for almost 50 years. PTI affords sub parts-per-billion (ppb) detection limits for purgeable VOCs including fixed gases and higher boiling hydrocarbons and halocarbons. In this study the coupling of solid phase extraction (SPE) to PTI was investigated as a means to substantially increase enrichment and lower detection limits for the emerging contaminant, 1,2,3-trichloropropane (TCP). Water samples (500 mL) were dechlorinated, preserved with a biocide, and spiked with the isotope labeled internal standard, d5-TCP. The entire 500 mL sample was extracted with activated carbon or carbon molecular sieve SPE cartridges, and then eluted with dichloromethane -- excess solvent was removed in a nitrogen evaporator and diethylene glycol "keeper" remaining was dispersed in 5 mL of water for PTI GC-MS analysis. The experimental Method Detection Limit (MDL) for TCP was 0.11 ng/L (ppt) and accuracy was 95-103% in sub-ppt determinations. Groundwater samples including impaired California sources and treated water (n = 21) were analyzed with results ranging from below the method reporting limit (0.30 ng/L) to > 250 ng/L. Coupling of SPE with PTI may provide similar reductions in detection limits for other VOCs with appropriate physical-chemical properties. Copyright © 2016 Elsevier Ltd. All rights reserved.

Evaluating Detection Limits of Next-Generation Sequencing for the Surveillance and Monitoring of International Marine Pests

PubMed Central

Pochon, Xavier; Bott, Nathan J.; Smith, Kirsty F.; Wood, Susanna A.

2013-01-01

Most surveillance programmes for marine invasive species (MIS) require considerable taxonomic expertise, are laborious, and are unable to identify species at larval or juvenile stages. Therefore, marine pests may go undetected at the initial stages of incursions when population densities are low. In this study, we evaluated the ability of the benchtop GS Junior™ 454 pyrosequencing system to detect the presence of MIS in complex sample matrices. An initial in-silico evaluation of the mitochondrial cytochrome c oxidase subunit I (COI) and the nuclear small subunit ribosomal DNA (SSU) genes, found that multiple primer sets (targeting a ca. 400 base pair region) would be required to obtain species level identification within the COI gene. In contrast a single universal primer set was designed to target the V1–V3 region of SSU, allowing simultaneous PCR amplification of a wide taxonomic range of MIS. To evaluate the limits of detection of this method, artificial contrived communities (10 species from 5 taxonomic groups) were created using varying concentrations of known DNA samples and PCR products. Environmental samples (water and sediment) spiked with one or five 160 hr old Asterias amurensis larvae were also examined. Pyrosequencing was able to recover DNA/PCR products of individual species present at greater than 0.64% abundance from all tested contrived communities. Additionally, single A. amurensis larvae were detected from both water and sediment samples despite the co-occurrence of a large array of environmental eukaryotes, indicating an equivalent sensitivity to quantitative PCR. NGS technology has tremendous potential for the early detection of marine invasive species worldwide. PMID:24023913

Current limiter circuit system

DOEpatents

Witcher, Joseph Brandon; Bredemann, Michael V.

2017-09-05

An apparatus comprising a steady state sensing circuit, a switching circuit, and a detection circuit. The steady state sensing circuit is connected to a first, a second and a third node. The first node is connected to a first device, the second node is connected to a second device, and the steady state sensing circuit causes a scaled current to flow at the third node. The scaled current is proportional to a voltage difference between the first and second node. The switching circuit limits an amount of current that flows between the first and second device. The detection circuit is connected to the third node and the switching circuit. The detection circuit monitors the scaled current at the third node and controls the switching circuit to limit the amount of the current that flows between the first and second device when the scaled current is greater than a desired level.

The detection and stabilisation of limit cycle for deterministic finite automata

NASA Astrophysics Data System (ADS)

Han, Xiaoguang; Chen, Zengqiang; Liu, Zhongxin; Zhang, Qing

2018-04-01

In this paper, the topological structure properties of deterministic finite automata (DFA), under the framework of the semi-tensor product of matrices, are investigated. First, the dynamics of DFA are converted into a new algebraic form as a discrete-time linear system by means of Boolean algebra. Using this algebraic description, the approach of calculating the limit cycles of different lengths is given. Second, we present two fundamental concepts, namely, domain of attraction of limit cycle and prereachability set. Based on the prereachability set, an explicit solution of calculating domain of attraction of a limit cycle is completely characterised. Third, we define the globally attractive limit cycle, and then the necessary and sufficient condition for verifying whether all state trajectories of a DFA enter a given limit cycle in a finite number of transitions is given. Fourth, the problem of whether a DFA can be stabilised to a limit cycle by the state feedback controller is discussed. Criteria for limit cycle-stabilisation are established. All state feedback controllers which implement the minimal length trajectories from each state to the limit cycle are obtained by using the proposed algorithm. Finally, an illustrative example is presented to show the theoretical results.

Detecting the limits of bronchial closure methods in an animal model.

PubMed

Tezel, C; Urek, S; Keles, M; Kiral, H; Koşar, A; Dudu, C; Arman, B

2006-04-01

Bronchopleural fistula is a serious complication of major lung resections that may lead to mortality. An experimental animal model was designed to find out the safest bronchial closure method by comparing leakage rates under pressure. The tracheobronchial trees of 50 freshly dead sheep were prepared for either manual closure or closure with a stapler. After left pneumonectomy, the specimens were divided into five groups (n = 10); 3/0 Premilene suture was used with two "u" sutures + interrupted sutures in Group I; in Group II, 3/0 Premilene sutures with continuous horizontal mattress + over-over continuous sutures were used. In Group III and IV the same techniques were used with 3/0 Vicryl. A stapler was used in Group V. Specimens were intubated with an endotracheal tube, connected to a sphygmomanometer, and subsequently positioned under water. The pressure level at which we detected air bubbles indicated the limits of the technique. The median leakage pressure resistance was significantly lower in Group III (135 mm Hg) ( P = 0.001). The best results were achieved by using the continuous horizontal mattress + over-over continuous suture technique. No statistical significance difference was found between the stapler group, Groups I, II, and IV in terms of median leakage pressures. This trial suggests that manual suture closure using an appropriate technique and monofilament materials is as safe as the stapler.

Estimation of potential and limits of bivalve closure response to detect contaminants: application to cadmium.

PubMed

Tran, Damien; Ciret, Pierre; Ciutat, Aurélie; Durrieu, Gilles; Massabuau, Jean-Charles

2003-04-01

Bivalve closure responses to detect contaminants have often been studied in ecotoxicology as an aquatic pollution biosensor. We present a new laboratory procedure to estimate its potential and limits for various contaminants and animal susceptible to stress. The study was performed in the Asiatic clam Corbicula fluminea and applied to cadmium. To take into account the rate of spontaneous closures, we integrated stress problems associated with fixation by a valve in common apparatus and the spontaneous rhythm associated with circadian activity to focus on conditions with the lowest probability of spontaneous closing. Moreover, we developed an original system by impedance valvometry, using light-weight impedance electrodes, to study free-ranging animals in low-stress conditions and a new analytical approach to describe valve closure behavior as a function of response time and concentration of contaminant. In C. fluminea, we show that cadmium concentrations above 50 microg/L can be detected within less than 1 h, concentrations down to 16 microg/L require 5 h of integration time, and values lower than 16 microg/L cannot be distinguished from background noise. Our procedure improved by a factor of six the cadmium sensitivity threshold reported in the literature. Problems of field applications are discussed.

Limited irrigation research and infrared thermometry for detecting water stress

USDA-ARS?s Scientific Manuscript database

The USDA-ARS Limited Irrigation Research Farm, located outside of Greeley Colorado, is an experiment evaluating management perspectives of limited irrigation water. An overview of the farm systems is shown, including drip irrigation systems, water budgeting, and experimental design, as well as preli...

Heisenberg limit for displacements with semiclassical states

NASA Astrophysics Data System (ADS)

Luis, Alfredo

2004-04-01

We analyze the quantum limit to the sensitivity of the detection of small displacements. We focus on the case of free particles and harmonic oscillators as the systems experiencing the displacement. We show that the minimum displacement detectable is proportional to the inverse of the square root of the mean value of the energy in the state experiencing the displacement (Heisenberg limit). We present a measuring scheme that reaches this limit using semiclassical states. We examine the performance of this strategy under realistic practical conditions by computing the effect of imperfections such as losses and nonunit detection efficiencies. This analysis confirms the robustness of this measuring strategy by showing that the experimental imperfections can be suitably compensated by increasing the mean energy of the input state.

Detection limits of tidal-wetland sequences to identify variable rupture modes of megathrust earthquakes

NASA Astrophysics Data System (ADS)

Shennan, Ian; Garrett, Ed; Barlow, Natasha

2016-10-01

Recent paleoseismological studies question whether segment boundaries identified for 20th and 21st century great, >M8, earthquakes persist through multiple earthquake cycles or whether smaller segments with different boundaries rupture and cause significant hazards. The smaller segments may include some currently slipping rather than locked. In this review, we outline general principles regarding indicators of relative sea-level change in tidal wetlands and the conditions in which paleoseismic indicators must be distinct from those resulting from non-seismic processes. We present new evidence from sites across southcentral Alaska to illustrate different detection limits of paleoseismic indicators and consider alternative interpretations for marsh submergence and emergence. We compare predictions of coseismic uplift and subsidence derived from geophysical models of earthquakes with different rupture modes. The spatial patterns of agreement and misfits between model predictions and quantitative reconstructions of coseismic submergence and emergence suggest that no earthquake within the last 4000 years had a pattern of rupture the same as the Mw 9.2 Alaska earthquake in 1964. From the Alaska examples and research from other subduction zones we suggest that If we want to understand whether a megathrust ruptures in segments of variable length in different earthquakes, we need to be site-specific as to what sort of geological-based criteria eliminate the possibility of a particular rupture mode in different earthquakes. We conclude that coastal paleoseismological studies benefit from a methodological framework that employs rigorous evaluation of five essential criteria and a sixth which may be very robust but only occur at some sites: 1 - lateral extent of peat-mud or mud-peat couplets with sharp contacts; 2 - suddenness of submergence or emergence, and replicated within each site; 3 - amount of vertical motion, quantified with 95% error terms and replicated within each

Localization and Speciation of Arsenic in Soil and Desert Plant Parkinsonia florida using μXRF and μXANES

PubMed Central

Castillo-Michel, Hiram; Hernandez-Viezcas, Jose; Dokken, Kenneth M.; Marcus, Matthew A.; Peralta-Videa, Jose R.; Gardea-Torresdey, Jorge L.

2011-01-01

Parkinsonia florida is a plant species native to the semi-desert regions of North America. The cultivation characteristics of this shrub/tree suggest that it could be used for phytoremediation purposes in semiarid regions. This work describes, through the use of synchrotron μXRF and μXANES techniques and ICP-OES, the arsenic (As) accumulation and distribution in P. florida plants grown in two soils spiked with As at 20 mg kg-1. Plants grown in a sandy soil accumulated at least twice more As in the roots compared to plants grown in a loamy soil. The lower As accumulation in plants grown in the loamy soil corresponded to a lower concentration of As in the water soluble fraction (WSF) of this soil. LC-ICP-MS speciation analysis showed only As(V) in the WSF from all treatments. In contrast, linear combination XANES speciation analysis from the root tissues showed As mainly present in the reduced As(III) form. Moreover, a fraction of the reduced As was found coordinating to S in a form consistent with As-Cys3. The percentage of As coordinated to sulfur was smaller for plants grown in the loamy soil when compared to the sandy soil. PMID:21842861

Localization and speciation of arsenic in soil and desert plant Parkinsonia florida using μXRF and μXANES.

PubMed

Castillo-Michel, Hiram; Hernandez-Viezcas, Jose; Dokken, Kenneth M; Marcus, Matthew A; Peralta-Videa, Jose R; Gardea-Torresdey, Jorge L

2011-09-15

Parkinsonia florida is a plant species native to the semidesert regions of North America. The cultivation characteristics of this shrub/tree suggest that it could be used for phytoremediation purposes in semiarid regions. This work describes, through the use of synchrotron μXRF and μXANES techniques and ICP-OES, the arsenic (As) accumulation and distribution in P. florida plants grown in two soils spiked with As at 20 mg kg(-1). Plants grown in a sandy soil accumulated at least twice more As in the roots compared to plants grown in a loamy soil. The lower As accumulation in plants grown in the loamy soil corresponded to a lower concentration of As in the water-soluble fraction (WSF) of this soil. LC-ICP-MS speciation analysis showed only As(V) in the WSF from all treatments. In contrast, linear combination XANES speciation analysis from the root tissues showed As mainly present in the reduced As(III) form. Moreover, a fraction of the reduced As was found coordinating to S in a form consistent with As-Cys(3). The percentage of As coordinated to sulfur was smaller for plants grown in the loamy soil when compared to the sandy soil.

Provenance and flux of detrital materials in Lake Suigetsu sediment (SG12 core) and their temporal changes during the last 20 kyrs based on color and XRF data

NASA Astrophysics Data System (ADS)

Suzuki, Y.; Tada, R.; Nakagawa, T.; Gotanda, K.; Haraguchi, T.; Nagashima, K.; Irino, T.; Sugisaki, S.; Kojima, H.; Horiuchi, D.

2013-12-01

Lake Suigetsu in Central Japan is known for its annual lamination (varve) starting from 70kys ago. Extremely precise Age-depth model is established for SG06 core based on over 800 14C dates obtained on terrestrial leaf fossils and wiggle-matched to stalagmite 14C records constrained by varve counts (Staff et al., 2013). By projecting this age model to newly drilled core from the same site, we can obtain precisely age-controlled high resolution paleoenvironmental record around the Lake Suigetsu drainage. It is likely that detrital materials in Lake Suigetsu sediments have several different sources such as soil on the slopes around the lake itself, aeolian dust from inland Asia, and suspended particles supplied from Hasu river through lake Mikata, which is located immediately upstream of Lake Suigetsu and trapping most of coarse detrital grains. However, the relative contribution from each detrital source and its temporal changes are poorly known. The lack of knowledge on relative contribution of different detrital sources limits utility of detrital materials as proxies of paleo-environments. In this study, we are aiming to reconstruct the history of precipitation changes in the drainage area of Lake Suigetsu during the Holocene to explore the relationship between precipitation in the Japan Sea side of SW Japan, behavior of Asian monsoon system as an important component of the global climate system. It is well known that flux of suspended particles in rivers increases with precipitation. In order for us to be able to use the Hasu river's flux of suspended particles as the precipitation proxy, however, we first need to establish a simple and swift way to estimate the contribution of detrital materials from Hasu River flowing through Lake Mikata into Lake Suigetsu. We carried out color measurement with 5mm resolution on split half core surface of the sediment drilled in the summer of 2012(SG12), and compared these values to chemical composition data by XRF microscanner

Mathematical simulations of photon interactions using Monte Carlo analysis to evaluate the uncertainty associated with in vivo K X-ray fluorescence measurements of stable lead in bone

NASA Astrophysics Data System (ADS)

Lodwick, Camille J.

This research utilized Monte Carlo N-Particle version 4C (MCNP4C) to simulate K X-ray fluorescent (K XRF) measurements of stable lead in bone. Simulations were performed to investigate the effects that overlying tissue thickness, bone-calcium content, and shape of the calibration standard have on detector response in XRF measurements at the human tibia. Additional simulations of a knee phantom considered uncertainty associated with rotation about the patella during XRF measurements. Simulations tallied the distribution of energy deposited in a high-purity germanium detector originating from collimated 88 keV 109Cd photons in backscatter geometry. Benchmark measurements were performed on simple and anthropometric XRF calibration phantoms of the human leg and knee developed at the University of Cincinnati with materials proven to exhibit radiological characteristics equivalent to human tissue and bone. Initial benchmark comparisons revealed that MCNP4C limits coherent scatter of photons to six inverse angstroms of momentum transfer and a Modified MCNP4C was developed to circumvent the limitation. Subsequent benchmark measurements demonstrated that Modified MCNP4C adequately models photon interactions associated with in vivo K XRF of lead in bone. Further simulations of a simple leg geometry possessing tissue thicknesses from 0 to 10 mm revealed increasing overlying tissue thickness from 5 to 10 mm reduced predicted lead concentrations an average 1.15% per 1 mm increase in tissue thickness (p < 0.0001). An anthropometric leg phantom was mathematically defined in MCNP to more accurately reflect the human form. A simulated one percent increase in calcium content (by mass) of the anthropometric leg phantom's cortical bone demonstrated to significantly reduce the K XRF normalized ratio by 4.5% (p < 0.0001). Comparison of the simple and anthropometric calibration phantoms also suggested that cylindrical calibration standards can underestimate lead content of a human leg up

Partial Least Squares Calibration Modeling Towards the Multivariate Limit of Detection for Enriched Isotopic Mixtures via Laser Ablation Molecular Isotopic Spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harris, Candace; Profeta, Luisa; Akpovo, Codjo

The psuedo univariate limit of detection was calculated to compare to the multivariate interval. ompared with results from the psuedounivariate LOD, the multivariate LOD includes other factors (i.e. signal uncertainties) and the reveals the significance in creating models that not only use the analyte’s emission line but also its entire molecular spectra.

Visual acuity of the honey bee retina and the limits for feature detection.

PubMed

Rigosi, Elisa; Wiederman, Steven D; O'Carroll, David C

2017-04-06

Visual abilities of the honey bee have been studied for more than 100 years, recently revealing unexpectedly sophisticated cognitive skills rivalling those of vertebrates. However, the physiological limits of the honey bee eye have been largely unaddressed and only studied in an unnatural, dark state. Using a bright display and intracellular recordings, we here systematically investigated the angular sensitivity across the light adapted eye of honey bee foragers. Angular sensitivity is a measure of photoreceptor receptive field size and thus small values indicate higher visual acuity. Our recordings reveal a fronto-ventral acute zone in which angular sensitivity falls below 1.9°, some 30% smaller than previously reported. By measuring receptor noise and responses to moving dark objects, we also obtained direct measures of the smallest features detectable by the retina. In the frontal eye, single photoreceptors respond to objects as small as 0.6° × 0.6°, with >99% reliability. This indicates that honey bee foragers possess significantly better resolution than previously reported or estimated behaviourally, and commonly assumed in modelling of bee acuity.

Statistical Limits to Super Resolution

NASA Astrophysics Data System (ADS)

Lucy, L. B.

1992-08-01

The limits imposed by photon statistics on the degree to which Rayleigh's resolution limit for diffraction-limited images can be surpassed by applying image restoration techniques are investigated. An approximate statistical theory is given for the number of detected photons required in the image of an unresolved pair of equal point sources in order that its information content allows in principle resolution by restoration. This theory is confirmed by numerical restoration experiments on synthetic images, and quantitative limits are presented for restoration of diffraction-limited images formed by slit and circular apertures.

Analysis of Thousands of Prehistoric Mediterranean Obsidian Artifacts Using a Nondestructive Portable X-Ray Fluorescence Spectrometer

NASA Astrophysics Data System (ADS)

Tykot, Robert

A portable, hand-held X-ray fluorescence spectrometer has been used for a decade to elementally analyze prehistoric obsidian artifacts in the Mediterranean. Nearly 400 geological obsidian samples and 7500 obsidian artifacts have been analyzed. The pXRF can distinguish all individual sources, as well as assign artifacts specifically to most subsources. For the island sources of Lipari, Pantelleria, Sardinia, and Melos, it is important to address the usage of obsidian from specific subsources due to human selection based on physical properties of the raw material and their production practices, which may have changed over time from the Early Neolithic to the Bronze Age. The analysis of 50 or more artifacts from 60 different archaeological sites allows for statistical comparison between sites, and their contexts, geographic areas (e.g. coastal/inland, highland/lowland) and distance from geological sources. The frequency of transport between island sources and mainland sites is suggestive of maritime capabilities also for the transport of domesticated animals, ceramics, and other materials. This presentation will specifically address potential limitations of the portable XRF, including non-destructive surface analysis of potentially heterogeneous materials, and limited trace element detection compared to other analytical methods, versus its highly beneficial ``package'' of analyzing great numbers of artifacts non-destructively and rapidly without needing to export them from museums and facilities in many countries.

On the distribution of uranium in hair: Non-destructive analysis using synchrotron radiation induced X-ray fluorescence microprobe techniques