Synchrotron Radiation Total Reflection X-ray Research Articles

Comparison of synchrotron radiation total reflection X-ray fluorescence excitation–detection geometries for samples with differing matrices

The linear polarization of synchrotron radiation (SR) in the orbital plane leads to a background reduction in total reflection X-ray fluorescence (TXRF) analysis if a side-looking detector is used. The optimum orientation of the sample carrier in a SR-TXRF experiment, however, is determined by a trade-off between the exploitation of the linear polarization, the efficiency of excitation and the solid angle of detection and depends on the nature and size of the sample. SR-TXRF measurements on different sample types and using different reflector orientations have been carried out at the Hamburger Synchrotronstrahlungslabor bending magnet beamline L. A NIST standard water sample, a steel sample and an oil standard were analyzed with both a horizontal and a vertical sample carrier orientation. Strongly scattering samples led to lower detection limits with a horizontal reflector whereas weakly scattering samples showed lower detection limits with a vertical reflector configuration. On an intentionally contaminated wafer absolute detection limits of 6.6 fg for Ni could be extrapolated.

Analysis of Medicinal Plants and Crude Extracts by Synchrotron Radiation Total Reflection X-Ray Fluorescence

Abstract Plants and aqueous extracts of Alternanthera maritima (aerial parts and roots), Alternanthera brasiliana and Alternanthera tenella colla (total plant) were selected for analysis of metals bioaccumulation. The synchrotron radiation total reflection X-ray fluorescence (SRTXRF) was used for excitation of the samples and a Si(Li) detector for the detection of the characteristic X-rays emitted by the sample elements. The elements P, S, K, Ca, Ti, Mn, Fe, Cu, Zn, Rb, and Sr were detected in all samples. Further-more Al, Si, Cl, Ni, Br, Rb, Cd, Sn, Sb, Hg, and Pb in Alternanthera maritima samples; Si, Co, Cd, Sn, Sb, and Ce in Alternanthera brasiliana and Al, Si, Co, Ni, Br, Cd, Sn, Sb, and Ce in Alternanthera tenella colla were found. The concentration obtained in the samples for K-shell lines varied from 1.63 µg g−1 for Ni to 3.34 × 105 µg g−1for K, and for L-shell the values ranged from 1.64 x 101 µg g−1 for Cd to 6.71 × 102 µg g−1 for Sn.

Trace Elemental Analysis of Drugs of Abuse Using Synchrotron Radiation Total Reflection X-Ray Fluorescence Analysis (SR-TXRF)

Synchrotron radiation total reflection X-ray fluorescence spectroscopy (SR-TXRF) was utilized to analyze various trace elements in small amounts of drugs of abuse. Sample amounts of 1 microL solutions containing 10 microg of drugs (methamphetamine, amphetamine, 3,4-methylenedioxymethamphetamine, cocaine, and heroin) were spotted on silicon wafers for direct analysis. In addition, a leaflet of marijuana was set directly on a silicon wafer, and opium in the form of a soft lump was smeared on another silicon wafer for analysis. In these experiments, about 10 pg of contaminant elements could be detected. For example, in a seized methamphetamine sample, iodine was found, which could be indicative of synthetic route. In seized 3,4-methylenedioxymethamphetamine samples, variable amounts of phosphorus, calcium, sulfur, and potassium were found, which could not be detected in a control 3,4-methylenedioxymethamphetamine sample. For marijuana and opium, two spectral patterns were obtained that were far different from each other and could be easily discriminated. Using SR-TXRF, pg amounts of each trace element in 10 microg of various drugs can be easily detected, which is not the case either for a standard TXRF experimental system or for other elemental analysis techniques.

Synchrotron radiation total reflection X-ray fluorescence and energy dispersive X-ray fluorescence analysis on AP1™ films applied to the analysis of trace elements in metal alloys for the construction of nuclear reactor core components: a comparison

Synchrotron radiation induced total reflection X-ray fluorescence and conventional 45° energy dispersive X-ray fluorescence analysis using a 150-nm-thick AP1™ film as sample carrier have been exploited for the elemental analysis of traces in alloys used for the construction of reactor core components of nuclear power plants. Both techniques are well suited for the analysis since they require a low amount of sample (μl), important on one hand because of the limited disposal and on the other hand because of its high specific activity. The methods provide a very low background due to the total reflection phenomenon in TXRF and the thin AP1™ film sample support, respectively. The employment of synchrotron radiation was necessary since there are no laboratory sources which can deliver a collimated beam of the energy and intensity needed to excite the K-shell of the rare earth elements, allowing the achievement of minimum detection limits relevant for the proposed purpose (ng/g range). Moreover, the linear polarization of synchrotron radiation combined with a side-looking detection geometry manages to reduce the scattering due to the remaining matrix of the analyzed samples. Detection limits for Nb and for some of the rare earth elements (pg range for absolute detection limits and ng–μg/g range for concentration detection limits) obtained with the two techniques are presented and the two approaches are compared.

Laboratory and synchrotron radiation total-reflection X-ray fluorescence: new perspectives in detection limits and data analysis

Having established detection limits for transition elements exceeding current requirements of the semiconductor industry, our recent efforts at the Stanford Synchrotron Radiation Laboratory (SSRL) have focused on the improvement of the detection sensitivity for light elements such as Al. Data analysis is particularly challenging for Al, due to the presence of the neighboring Si signal from the substrate. Detection limits can be significantly improved by tuning the excitation energy below the Si–K absorption edge. For conventional TXRF systems this can be done by using a W–Mα fluorescence line (1.78 keV) for excitation. At a synchrotron radiation facility energy tunability is available. However, in both cases this results in a substantial increase in background due to resonant X-ray Raman scattering. This scattering dominates the background under the Al Kα fluorescence line, and consequently limits the achievable sensitivity for the detection of Al surface contaminants. In particular, we find that for a precise determination of the achievable sensitivity, the specific shape of the continuous Raman background must be taken into account in the data analysis. The data deconvolution presented here opens a new perspective for conventional TXRF systems to mitigate this background limitation. This results in a minimum detection limit of 2.4×10 9 atoms/cm 2 for Al. Based on these results it will also be demonstrated that by improving the detector resolution, the minimum detection limit can be improved significantly. For a detector resolution of 15 eV as predicted for novel superconducting tunnel junction detectors, an improvement in minimum detection limit of approximately a factor of 3 can be estimated.

Beijing synchrotron radiation total-reflection X-ray fluorescence analysis facility and its applications on trace element study of cells

The feasibility of total-reflection X-ray fluorescence (TXRF) analysis excited by synchrotron radiation applied to trace element analysis of biological cells is investigated. The Beijing synchrotron radiation TXRF facility and the related experimental method are also described. The elemental minimum detection limits of some standard reference materials are determined. The elemental compositions of a cluster of small intestine cells of a small white mouse are given, and hence the average trace element contents of the single small intestine cell are also obtained. With this technique, the changes of some trace elements in the cells of lung and cervix cancer before and after apoptosis are also preliminarily studied.

Trace element analysis on Si wafer surfaces by TXRF at the ID32 ESRF undulator beamline.

Synchrotron radiation total-reflection X-ray fluorescence (SR-TXRF) has been applied to the impurity analysis of Si wafers using a third-generation synchrotron radiation undulator source. A lower limit of detectability (LLD) for Ni atoms of 17 fg (1.7 x 10(8) atoms cm(-2)) has been achieved with an optical set-up based on an Si(111) double-crystal monochromator and a horizontal sample geometry. These first results are very promising for synchrotron radiation trace element analysis since we estimate that it is possible to lower the LLD by a factor of about 25 by employing appropriate optics and detectors. The use of a crystal monochromator opens new possibilities to perform absorption and scattering experiments (NEXAFS and X-ray standing-wave methods) for chemical and structural analysis of ultratrace elements.