X-Ray Spectroscopy: An Introduction


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In this latter case, the tube must be liquid-cooled since the majority of the power is dissipated as heat. The anode materials must be carefully chosen as well, since the wavelength of their characteristic lines is important for proper excitation of the sample.

Background information - What is energy dispersive X-ray spectroscopy?

Some example single-element anode materials are aluminum, chromium, tungsten, palladium, or gold. For detection of light elements, a high intensity of low energy, i. It is also important to keep in mind that the primary source of detector background will be the intense primary radiation from the tube, above which the secondary sample radiation must be detected.

The use of secondary targets, or filters, can greatly reduce the background and improve sensitivity for specific portions of the spectrum. For instruments that are designed to acquire the entire spectrum with good sensitivity on light as well as heavy elements, a different approach is taken. A tube anode material is chosen to give a high bremsstrahlung or continuum output, which is used to excite a secondary fluorescer, or target , which gives off its own characteristic lines without the continuum. The sample is then excited by the emission from the target, which is chosen to efficiently excite elements in a certain Z range.

A system may be set up to change targets automatically during the analysis so that the low, middle, and high end of the sample spectrum may be sequentially boosted. When an EDXRF instrument uses such a system, tube powers must be increased dramatically since most of the original X-ray intensity is lost. Certainly XRF excitation is not limited only to X-ray tubes. Less common excitation sources include gamma-emitting radioisotopes Am, Cd, Gd, and others , electron sources where the sample is the tube anode, and synchrotrons, which produce highly intense, coherent, monochromatic X-ray beams Jenkins 56, Jenkins Up to this point, little has been said regarding what kinds of samples may be analyzed by XRF.


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There is no longer a need to fit a sample into a small chamber. In the case of PXRF, it is possible to analyze the samples with the instrument in a stand or the instrument can be moved to the sample, as in the case of analyzing a exposed rock outcrop or a large painting. We have recently acquired an automated sample changer that allows us to load up to 20 samples at a time and operated much like the sample changers on large lab-based instruments. EDXRF systems depend on semiconductor-type detectors which receive the entire emitted spectrum from the sample and decode it into a histogram of number of counts versus photon energy.

WDXRF spectrometers, however, use an analyzing crystal to disperse the emitted photons based on their wavelength and place the detector in the correct physical location to receive X-rays of a given energy. Please refer to Figure 2, which displays a block diagram for a WD setup.

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X-ray and radio-frequency spectroscopy

More collimators, usually made from a series of closely spaced parallel metal plates, are needed to direct the beam in order to closely control the diffraction angle of all detected photons. In the instrument shown, the analyzing crystal may be rotated with the detector assembly simultaneously revolving around it to scan through the possible wavelengths.

To resolve wavelengths in all regions, different crystals must be used, since crystals with large spacings must be used for long wavelengths but they make the short wavelengths irresolvable at low q Jenkins The system in the diagram utilizes two detectors in series. Most high-energy X-rays pass through it, however, and are counted by the NaI Tl scintillation detector. The gas-flow proportional detector works by placing a high voltage across a volume of gas usually Ar with methane. An X-ray photon will ionize a number of Ar atoms proportional to its energy.

The freed electrons are accelerated in the high voltage, ionizing other Ar atoms and creating an electron cascade which is controlled by the quench gas methane. The freed charges are measured in the circuitry as a voltage pulse whose height is proportional to the energy of the photon that initiated the cascade Jenkins An NaI Tl detector contains a large single crystal of sodium iodide that has been doped with thallium. This crystal is sealed from light by a Be window. When an X-ray photon enters the crystal, it places primarily the I atoms in an excited state, in numbers again proportional to its energy.

These excited states decay exponentially with time, giving off a flash of light or scintillation when they go. The summed intensity of light strikes a photocathode, which releases photoelectrons that are amplified in a discrete dynode detector. The pulse height measured from this detector is proportional to the energy of the original X-ray photon Jenkins 96, Knoll One may wonder why these detectors need to have any energy resolution at all, since the X-ray energies are supposed to be dispersed by the Bragg crystal.

With WDXRF systems, it may be possible to have several detector assemblies placed at fixed angular locations in order to analyze for a few selected elements over and over. WDXRF spectrometers often offer more flexibility for the researcher as well as very good sensitivities. The detector outputs are also simpler to use directly and do not generally require heavy use of electronics and computer algorithms in order to deconvolute.

Disadvantages include the inability to quickly acquire the entire X-ray spectrum for full-element analyses, higher hardware costs, and a larger instrumental footprint when compared to EDXRF systems. While simpler in terms of the positioning of the detector versus the sample, EDXRF spectrometers require sophisticated electronics and computer software in order to interpret the detector output.

Nowadays this is less complicated, though, due to important technological advances in multichannel analyzers and faster computers, and EDXRF is often the technique of choice for fast multielement analyses. Although germanium detectors are utilized, the most common type in service is the Si Li , or lithium-drifted silicon, detector. A semiconductor detector operates based on the principle that an X-ray photon incident upon the diode material will give up its energy to form electron-hole pairs, the number of which is proportional to the energy of the photon.

The high voltage applied across the diode quickly collects the released charge on a feedback capacitor, and the resulting proportional voltage pulse amplified by a charge-sensitive preamplifier. The output of the preamp is fed to a main amplifier system. The pileup rejector, part of this system, deals with the probable event that two pulses will arrive very close together in time. From this point, the pulse is converted to a digital signal and processed in the multichannel analyzer MCA Jenkins In the MCA, dead time , caused by high counting rates, must be corrected.

Peaks in the energy spectrum, once acquired, are subject to a large degree of massaging by the software in the connected computer. Sophisticated algorithms sense and quantitatively correct for high backgrounds due to Compton scattering from low atomic number matrices Metz Spectrometers that use secondary targets may acquire several energy spectra for each sample, one from each target. Since each target yields better sensitivity in one part of the spectrum, the information from the energy spectra is combined to quantitate each element being analyzed.

Accurate quantitative data on the entire mass spectrum may be obtained in a matter of minutes using EDXRF. For both of the Bruker Tracer instruments we use we have incorporated a secondary target made of thin sheets of copper, aluminum and titanium to optimize the spectra for the analysis of obsidian and any other analyses focusing on elements with with fluorescent energies between about 10 and 20 kV.

Fundamental Principles of X-Ray Fluorescence (XRF)

We have developed a world-renowned set of obsidian calibration standards that we have used to calibrate our own instruments and Bruker now runs this calibration on all portable XRF instruments heading out to museums and archaeologists. With this calibrations it is possible to acquire quantitative concentrations for many elements that are comparable to data acquired by mosre costly and destructive neutron activation analysis NAA.

The tube voltage can be varied up to 45 kV, although we generally analyze the obsidian with a setting of 40kV. The secondary target, or filter, primarily used includes a 6 mil thick sheet of copper used to block X-rays below about 20kV a 2 mil sheet of titanium added to remove the secondary copper X-rays and a 12 mil sheet of aluminum to absorb the titanium X-rays. Sample preparation is highly variable depending on the matrix and goals of the analysis. Most of the materials we analyze obsidian, metals, and ceramic paints do not require any sample preparation.

The choice of sample preparation depends on the nature of the X-ray beam relative to the sample. For example, a piece of obsidian that is 1 cm thick and has a clean, flat surface will provide ideal results. As sample sget smaller, thinner, or less homogenous it is necessary to understand the nature of the X-ray beam and how it interacts with the sample. This small beam is fine for homogenous materials, but heterogenous material such as crystalline rocks and tempered pottery may need to be analyzed multiple times in numerous areas to generate a representative average composition.

The small beam size is ideal for isolating specific painted elements on the surface of ceramics and also aids in the analysis of very small obsidian artifacts. Perhaps even more important than the area of the beam is the depth of analysis.

X-Ray Fluorescence (XRF)

As a general rule, the higher up the energy spectrum, the greater the depth of X-ray penetration in the sample. For example, the analysis of iron 6. In thick homogenous samples this depth of analysis makes little difference, but if samples are thinner, it effects to resulting spectrum in different ways depending on the specific sample thickness and particular element of interest. Ferguson in press addresses a number of approaches to quantitative analysis of thin samples. The ability to analyze samples without destructive sample preparation procedures has been a great advancement for archaeologists.

What is X-Ray Fluorescence (XRF)

We can now analyze large and valuable artifact assemblages that would have been off-limits to destructive proceedures. However, for non-archaeological applications of XRFthe most common method of sample prep is pelletizing, which can be made to work for most matrices that can be ground into an homogeneous powder, including soil, minerals, and dried organic matrices such as tissues or leaves. Difficult grinding is accomplished with a hard agate mortar and pestle but many samples can be adequately homogenized by placing into a hard plastic vial, adding a plastic mixing ball, and violently shaking in a mixer mill.

A powdery binder containing cellulose, starch, polyvinyl alcohol or other organics is usually weighed in and blended thoroughly with the sample, and the resulting mixture added to a deformable aluminum cup. Buhrke p. Here particle size and homogeneity play a big factor. This is due to the variance in X-ray penetration depths with energy Jenkins Particles may be inhomogeneous also, having a different surface composition than their bulk.


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For example, copper sulfides may become partially oxidized at the surface, causing the relative absorption for Cu K lines to differ from that of the L lines. The L line photons will not penetrate as deeply and will tend to be emitted more from the oxide layer. One way to get around sample grinding is to fuse the sample at high temperatures with sodium or lithium tetraborate and then to pour this glass-like mixture into a mold Buhrke: Chemical reactions occur within the melt which dissolve particles and create a homogeneous liquid that hardens upon cooling. The disadvantages to this technique include the additional time to prepare the melt and the possibility of the sample reacting with even inert crucible materials such as platinum.

Homogeneous solid samples such as metals may be machined and smoothed to form disks. Whatever type of preparation is done, the surface roughness of the sample should be taken into account. A rough surface causes the penetration layer to look heterogeneous to the spectrometer. Currently XRF spectrometry is very widely applied in many industries and scientific fields. The steel and cement industries routinely utilize XRF devices for material development tasks and quality control.

What is X-ray Spectroscopy?

Anzelmo Part 1 NIST utilizes XRF as one technique to quantitatively analyze and acceptance-test many of its standard reference materials SRMs , from spectrometric solutions to diesel fuel to coal to metal alloys Sieber The plastics industry is looking at a modified XRF spectrometer as an on-line wear monitor, taking advantage of its ability to detect particles of worn-off metal in extruded plastic pieces Metz Polish scientists are accomplishing XRF analyses on very thin films by placing the source and detector at very low angles with respect to the sample.

This technique is being applied to trace element determinations in water samples that have been evaporated to a thin film of residue Holynska XRF has been one of the tools of choice for geologists for many years, so much so that graduating geologists usually receive practical training with these devices, whereas graduating chemists probably haven't even heard of the technique.

Seminaire - X-ray spectroscopy of transition metal oxides

For geologists, the ability to determine major and trace components in one quick analysis with relatively little sample preparation has been a boon Anzelmo Part 1, Part 2. Current basic research aimed at improving XRF analyses for geological and ecological samples focuses on methods for correcting for matrix effects, in which major components absorb some of the X-rays emitted from trace components Revenko Archaeometrists have applied XRF in order to solve their ancient mysteries.

An example of this was the study of the composition of blue soda glass from York Minster, England, which distinguished three compositional groups, indicating this number of possible sources for the glass. Trace metal signatures also can effectively differentiate genuine artifacts from modern copies Jenkins Forensic scientists utilize XRF spectrometry to match samples associated with suspects i. As for other applications, here XRF can help elucidate an elemental fingerprint, without need to analyze the evidence destructively Jenkins XRF is a versatile, rapid technique which lends itself to a wide variety of samples from powders to liquids.

The instruments have few moving parts, tend to be low-maintenance, and on a regular basis consume only liquid nitrogen and electricity. Disadvantages include fairly high limits of detection LODs when compared to other methods, as well as the possibility of matrix effects, although these can usually be accounted for using software-based correction procedures. GFAAS is also relatively slow, with one element determined at a time, and is destructive Jenkins PXRF instruments are capable of producing results comparable in many ways to the lab-based XRF at a fraction of the cost.

Taking full advantage of such techniques requires a wide range of specialized expertise not found in any university course. Therefore, there is a need for reference books and training courses to introduce young scientists to the underlying principles and methods. Neutron and X-Ray Spectroscopy delivers an up-to-date account of the principles and practice of inelastic and spectroscopic methods available at neutron and synchrotron sources , including recent developments. Each chapter, written by a leading specialist in the field, introduces the basic concepts of the technique and provides an overview of recent work.

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X-Ray Spectroscopy: An Introduction X-Ray Spectroscopy: An Introduction
X-Ray Spectroscopy: An Introduction X-Ray Spectroscopy: An Introduction
X-Ray Spectroscopy: An Introduction X-Ray Spectroscopy: An Introduction
X-Ray Spectroscopy: An Introduction X-Ray Spectroscopy: An Introduction
X-Ray Spectroscopy: An Introduction X-Ray Spectroscopy: An Introduction
X-Ray Spectroscopy: An Introduction X-Ray Spectroscopy: An Introduction

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