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1- DTSA-II

DTSA-II is a multi-platform software package for quantitative x-ray microanalysis. DTSA-II was inspired by the popular Desktop Spectrum Analyzer (DTSA) package developed by Chuck Fiori, Carol Swyt-Thomas, and Bob Myklebust at NIST and NIH in the ’80’s and early ’90’s.

DTSA-II has being designed with the goal of making standards-based microanalysis more accessible for the novice microanalyst. We want to encourage standards-based analysis by making it as easy as possible to get reliable results. Many operations which had previously required user intervention under DTSA now are performed entirely by the software. Furthermore, the software attempts to guide the user step-by-step through common processes while performing quality control sanity checks. While this might not provide the flexibility that some sophisticated users may desire, we feel that this philosophy is more consistent with the way laboratories are moving towards technicians responsible for multiple techniques and away from experts in single techiques. We encourage users who desire the additional power and flexibility available in the EPQ library to learn to script using Jython or to create their own alternative user interface. EPQ is much more capable than the fraction exposed via DTSA-II.

DTSA-II is based on an entirely new code base written by Nicholas W. M. Ritchie. The codebase has been carefully divided into a shared algorithm library which forms the basis for a handful of software products and a user interface shell. DTSA-II is the user interface shell and the EPQ library is the algorithm library.

DTSA-II remains under active development. Many features – some fairly basic – remain unimplemented. Other features have not been tested as much as the developer might like. The program made available to the public via this web site represents the current best available version in the judgement of the developer. DTSA-II remains experimental software and no representations are made regarding the suitability of the product for any particular application.

Major features:

• Basic IO and Display
  • Read energy dispersive x-ray spectra in a variety of different commercial and non-commercial formats including the industry standard EMSA format
  • Display and overlay spectra with various scaling options on linear/log/sqrt axes
  • Copy/save/print the spectrum display as a bitmap/PNG file
  • Output the spectra as a GNUPlot file for publication quality output
  • Overlay labeled x-ray emission lines and x-ray absorption edges
  • Define and integrate regions-of-interest
  • View spectrum contextual information
  • Archive spectra to a searchable database
  • Sub-sampling of spectral data to simulate shorter acquisition times
  • Basic spectrum math functions
  • Background modeling or background stripping
  • Energy axis linearization
  • Spectrum smoothing
  • Peak removal (trimming)
  • Peak search / identification
• Spectrum Simulation
  • Analytical (φ(ρz)) simulations of energy dispersive x-ray spectra
    • Normal or oblique incidence angle
    • Variable beam energies, beam fluxes, materials
  • Monte carlo simulations of energy dispersive x-ray spectra
    • Spectra from bulk samples
    • Mounted or unmounted thin films
    • Cubical or spherical particles with or without a substrate
  • Simulated spectra may be manipulated as experimental spectra
  • Variety of detector options including Si(Li), SDD and microcalorimeter
• Standards-based Quantification
  • Standards-based quantification of EDS spectra
  • Filter-fit linear-least squares fitting of reference spectra
  • Quantification based on references or like-standards
  • φ(ρz) correction of the k-ratios
  • ζ-factor correction of thin-film samples
  • Results reported as HTML with estimates of uncertainty
• Reporting
  • Actions are recorded in a daily HTML activity report
  • Report may be opened in an alternative HTML viewer
• Platforms and Source Code
  • DTSA-II is based on the EPQ library – a full-featured library of electron probe quantification algorithms
  • DTSA-II only exposes a fraction of the power within the EPQ library. The remainder may be accessed via custom Java applications or via Jython scripting.
  • The EPQ library includes the full NISTMonte for Monte Carlo simulation of electron/x-ray transport
  • DTSA-II / EPQ library are available as source code
  • DTSA-II / EPQ library are written in Java SE 6 compatible source
  • DTSA-II / EPQ library can execute on any platform supporting Java SE 6 or later
  • DTSA-II / EPQ library is regularly tested on Windows XP, Ubuntu Linux & Apple OS X

Disclaimer

This software was developed at the National Institute of Standards and Technology by employees of the Federal Government in the course of their official duties. Pursuant to title 17 Section 105 of the United States Code this software is not subject to copyright protection and is in the public domain. DTSA and the EPQ library are experimental systems. NIST assumes no responsibility whatsoever for its use by other parties, and makes no guarantees, expressed or implied, about its quality, reliability, or any other characteristic. We would appreciate acknowledgement if the software is used. This software can be redistributed and/or modified freely. The author requests that any derivative works bear some notice that they are derived from it, and any modified versions bear some notice that they have been modified.

Any mention of commercial products is for information only; it does not imply recommendation or endorsement by NIST nor does it imply that the products mentioned are necessarily the best available for the purpose.

See: https://cstl.nist.gov/div837/837.02/epq/dtsa2/

2. HyperSpy

HyperSpy is an open source Python library which provides tools to facilitate the interactive data analysis of multi-dimensional datasets that can be described as multi-dimensional arrays of a given signal (e.g. a 2D array of spectra a.k.a spectrum image). HyperSpy aims at making it easy and natural to apply analytical procedures that operate on an individual signal to multi-dimensional arrays, as well as providing easy access to analytical tools that exploit the multi-dimensionality of the dataset. Its modular structure makes it easy to add features to analyze different kinds of signals.

Highlights

• Two families of named and scaled axes: signal and navigation.
• Visualization tools for multi-dimensional spectra and images.
• Easy access multi-dimensional curve fitting and blind source separation.
• Built on top of NumPy, SciPy, matplotlib and scikit-learn.
• Modular design for easy extensibility.

The development has been motivated by the data analysis needs of the electron microscopy community but it is proving useful in many other fields.

See: https://hyperspy.org/

3. AZtec

• AZtecFeature is an innovative particle analysis system specifically optimised for usability and high-speed throughput. It combines the raw speed and sensitivity of the Ultim Max Silicon Drift Detector with the superior analytical performance and ease of use of the AZtec® EDS analysis suite to create the most advanced automated particle analysis platform on the market. Gunshot Residue Analysis in the SEM with AZtecGSR is fast and accurate: it gives reproducible Gunshot Residue Analysis results to ASTM E1588 – 10e1.
• AZtecGSR combines ease of use through its guided workflow, with the ultimate accuracy using the latest Ultim Max detectors and Tru-Q® algorithms. LayerProbe is an exciting software tool for thin film analysis in the SEM. An option for the AZtec EDS microanalysis system, LayerProbe is faster, more cost-effective and higher resolution than dedicated thin film measurement tools.The most powerful EBSD software available, AZtecHKL combines speed and accuracy of results for routine analysis, with the flexibility and power required for applications that push the frontiers of EBSD.
• AZtec3D combines simultaneous EDS and EBSD data acquisition & analysis with the automated milling capabilities of a FIB-SEM.AZtecLiveOne software platform is the ideal solution for carrying out a complex task like EDS as quickly and as easily as possible. No need for substantial training or advanced knowledge of the EDS technique. Users can be trained in a matter of minutes and will have complete confidence in their results. AZtecTEM is an innovative EDS software specifically optimised for advanced TEM applications. AZtecSynergy provides a powerful solution for the simultaneous collection of EDS and EBSD data. All of the tools to collect excellent integrated data are included in one place with no complicated switching from one navigator to another.
• AZtecSteel is an automated steel inclusion analysis package developed specifically for the analysis and classification of steel inclusions using Energy Dispersive X-ray microanalysis (EDS) in a scanning electron microscope (SEM). It detects, measures and analyses the inclusions, processes the resulting data set to published standard methods, and includes functionality to plot complex ternary diagrams. AZtecLive is a revolutionary new approach to EDS analysis that enables a radical change in the way users perform sample investigation in the SEM. It combines a live electron image with live X-ray chemical imaging to give an intuitive new way of interacting with your samples. Collecting good quality data is only the beginning of any complete EBSD analysis. AZtecCrystal provides all the necessary tools to process and interrogate your EBSD data and to solve your materials problems. Seamlessly integrated with AZtecHKL or operated as a standalone program, AZtecCrystal sets the standard in EBSD data processing for experts and novices alike.
• AZtecAM is a powerful, automated, solution for the analysis of metal powders used in additive manufacturing. Based on AZtecFeature, AZtecAM optimises the particle analysis workflow to enable the rapid and accurate characterisation of metal powders. AZtecMineral is a powerful, automated, Mineral Liberation Analysis solution. It enables ore characterisation, provides vital data on metal recovery and enables process yield characterisation using multipurpose SEMs. It is also a valuable tool for the characterisation of rocks in research environments, enabling the automation of otherwise laborious optical analyses.

See: https://engineering.virginia.edu/oxford-instruments-offering-free-aztec-suite-software-electron-microscopy-analysis

4. ESPRIT Family

ESPRIT 2 unites four analytical methods under a single user interface. These include EDS for SEM and (S)TEM, WDS, Micro-XRF for SEM and EBSD. This makes it easy for the user to switch between methods with a single mouse click. Additionally, it facilitates combining different method results from the same sample area and to so gain much more information. To name only the most important, coupling of following methods is supported:

• EDS and EBSD
• EDS and WDS
• EDS and Micro-XRF for SEM

The software is designed to suit the needs of all levels of users – from beginner to expert. Novices will benefit from the assistants that help performing routine tasks without having to learn details of the measurement method. More experienced users will value the option to drill down deeper, when they need it, meaning both detailed setup of measurements as well as in-depth analysis of results and automation of tasks.

See: https://www.bruker.com/en/products-and-solutions/elemental-analyzers/eds-wds-ebsd-SEM-Micro-XRF/software-esprit-family.html

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Interaction of an electron beam with a sample target produces a variety of emissions, including x-rays. An energy-dispersive (EDS) detector is used to separate the characteristic x-rays of different elements into an energy spectrum, and EDS system software is used to analyze the energy spectrum in order to determine the abundance of specific elements. EDS can be used to find the chemical composition of materials down to a spot size of a few microns, and to create element composition maps over a much broader raster area. Together, these capabilities provide fundamental compositional information for a wide variety of materials.

How it Works – EDS

EDS systems are typically integrated into either an SEM or EPMA instrument. EDS systems include a sensitive x-ray detector, a liquid nitrogen dewar for cooling, and software to collect and analyze energy spectra. The detector is mounted in the sample chamber of the main instrument at the end of a long arm, which is itself cooled by liquid nitrogen. The most common detectors are made of Si(Li) crystals that operate at low voltages to improve sensitivity, but recent advances in detector technology make availabale so-called “silicon drift detectors” that operate at higher count rates without liquid nitrogen cooling.

An EDS detector contains a crystal that absorbs the energy of incoming x-rays by ionization, yielding free electrons in the crystal that become conductive and produce an electrical charge bias. The x-ray absorption thus converts the energy of individual x-rays into electrical voltages of proportional size; the electrical pulses correspond to the characteristic x-rays of the element.

Strengths

• When used in “spot” mode, a user can acquire a full elemental spectrum in only a few seconds. Supporting software makes it possible to readily identify peaks, which makes EDS a great survey tool to quickly identify unknown phases prior to quantitative analysis.
• EDS can be used in semi-quantitative mode to determine chemical composition by peak-height ratio relative to a standard.

Limitations

• There are energy peak overlaps among different elements, particularly those corresponding to x-rays generated by emission from different energy-level shells (K, L and M) in different elements. For example, there are close overlaps of Mn-K_α and Cr-K_β, or Ti-K_α and various L lines in Ba. Particularly at higher energies, individual peaks may correspond to several different elements; in this case, the user can apply deconvolution methods to try peak separation, or simply consider which elements make “most sense” given the known context of the sample.
• Because the wavelength-dispersive (WDS) method is more precise and capable of detecting lower elemental abundances, EDS is less commonly used for actual chemical analysis although improvements in detector resolution make EDS a reliable and precise alternative.
• EDS cannot detect the lightest elements, typically below the atomic number of Na for detectors equipped with a Be window. Polymer-based thin windows allow for detection of light elements, depending on the instrument and operating conditions.

Results

A typical EDS spectrum is portrayed as a plot of x-ray counts vs. energy (in keV). Energy peaks correspond to the various elements in the sample. Generally they are narrow and readily resolved, but many elements yield multiple peaks. For example, iron commonly shows strong K_α and K_βpeaks. Elements in low abundance will generate x-ray peaks that may not be resolvable from the background radiation.

EDS spectrum of multi-element glass (NIST K309) containing O, Al, Si, Ca, Ba and Fe (Goldstein et al., 2003). 

EDS spectrum of biotite, containing detectable Mg, Al, Si, K, Ti and Fe (from Goodge, 2003). 

References

• Severin, Kenneth P., 2004, Energy Dispersive Spectrometry of Common Rock Forming Minerals. Kluwer Academic Publishers, 225 p.–Highly recommended reference book of representative EDS spectra of the rock-forming minerals, as well as practical tips for spectral acquisition and interpretation.
• Goldstein, J. (2003) Scanning electron microscopy and x-ray microanalysis. Kluwer Adacemic/Plenum Pulbishers, 689 p.
• Reimer, L. (1998) Scanning electron microscopy : physics of image formation and microanalysis. Springer, 527 p.
• Egerton, R. F. (2005) Physical principles of electron microscopy : an introduction to TEM, SEM, and AEM. Springer, 202.
• Clarke, A. R. (2002) Microscopy techniques for materials science. CRC Press (electronic resource)

Related Links

• Petroglyph–An atlas of images using electron microscope, backscattered electron images, element maps, energy dispersive x-ray spectra, and petrographic microscope– Eric Chrisensen, Brigham Young University
• SEM/EDX webpage from Indiana University – Purdue University Fort Wayne

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X-ray is a kind of electromagnetic wave, the same as light. The wavelength of visible light is 400 to 800nm, while the wavelength of x-ray is much shorter (higher energy), at 0.001nm to 10nm, and is known to have strong penetrating power.

Fig. 1 shows the interactions between a material and X-ray, and various analysis methods that make use of these interactions. These interactions provide important clues for learning the state of a material. As a familiar example, an X-ray image for medical application is a well-known use of transmission X-ray. Here we will introduce an elemental analysis method called fluorescent X-ray spectrometry.

Fig.1 Analytical methods and its application interaction of X-ray and matter

Fluorescent X-ray Spectrometry

When irradiating X-rays onto a material, fluorescent X-ray (characteristic X-ray), which has energy (wavelength) unique to the element that composes the material will be generated. When we measure the fluorescent X-ray energy, the contained element is identified (qualitative analysis), and we can calculate the concentration (quantitative analysis) from the intensity of the fluorescent X-ray of each element. Thus, the qualitative or quantitative analyses of a material by irradiating X-rays onto an unknown material and analyzing the fluorescent X-ray that is generated, is called fluorescent X-ray spectrometry.

There are two types of fluorescent X-ray spectrometry; the wavelength dispersive type (WDXRF) using analyzing crystals, and the energy dispersive type (EDXRF) using semiconductor detectors (EDS).

Comparison between Energy Dispersive Type and Wavelength Dispersive Type Spectrometers

The characteristics of a wavelength dispersive type spectrometer (WDXRF) are high sensitivity, high accuracy, high resolution, and high reproducibility. We can expect sensitivity and accuracy at levels one order of magnitude higher than those of the energy dispersive type spectrometer (EDXRF). These characteristics are provided by a high-power X-ray tube (3 to 4 kW) and its cooling device, a goniometer which makes complicated movements and an exchange mechanism for the analyzing crystal and detector and so on. Naturally, the instruments are larger, with a complicated structure and high price. The specimen surface is required to be flat and the available analysis area is from several mm to 30mm or so. This type of device is suitable for process management where specimens with the same form are analyzed one after another.

The characteristics of the energy dispersive type spectrometer (EDXRF) are simple structure and low price, its adaptability to a variety of specimens, and its user-friendliness. The X-ray bulb is compact (several tens W) and air-cooled, and since the EDS (semiconductor detector) itself performs the analysis, a complicated spectroscopy section is not necessary.

The roughness or shape of specimen does not matter, so analysis of large specimens or micro areas is possible. Each characteristic is shown in Fig. 2. The images are the large instrument for WDXRF, and the compact simple instrument for EDXRF.

Wavelength Dispersive Type (WDXRF) Advantages: High Sensitivity, High Resolution High Accuracy, High Reproducibility Disadvantages: Complicated and large-sized, high price Specimen is limited to flat platesEnergy Dispersive Type (EDXRF) Advantages: Simple Operation, compact, low price Flexibility in specimen shape Disadvantages: Low resolution (overlapped peaks) Cooling mechanism requiring liquid nitrogen or the like

Fig.2 Comparison between Wavelength Dispersive Type (WDXRF) and Energy Dispersive Type (EDXRF)

Sampling of Solid/Powder/Liquid Samples

One of the characteristics of EDXRF is the ease of use. Sampling of solid, powder, and liquid samples is explained below.

Sampling of Solid Sample

Analysis of a solid sample is possible by simply placing the sample at the X-ray illumination position.

In case of small sample, use of a dedicated cell will make it easier to set the sample. Fig. 3 shows a simplified illustration of the solid sample sampling method.

Fig.3 Sampling of Solid Sample

Sampling of Powder Sample (rock, soil, incinerated ash, etc)

Powder samples are typically analyzed by producing a pellet using a compression device. As a simplified method, analysis is possible on the powder placed into a specially-designed cell. Fig. 4 shows a simplified illustration of the powder sample sampling method.

Fig.4 Sampling of Powder Sample

Sampling of Liquid Sample

For liquid samples, a dedicated cell is used. Fill a dedicated cell with the liquid and analyze. In addition, there is another method where you can drop liquid onto a filter, dry it, and then analyze it. Fig. 5 shows a simplified illustration of liquid sample sampling methods.

Fig.5 Sampling of Liquid Sample

FP Quantitative Method / Film Thickness Analysis of Thin Film Sample

FP (fundamental parameter) quantitative method

The EDXRF instrument employs a theoretical calculation method called the FP quantitative method, allowing quantitative analysis of an unknown sample without the need for a standard sample.
The FP quantitative method assumes that the sample is uniform, sufficiently large and thick, and that all elements (100% in total) are quantified. Naturally, a sample must satisfy these assumptions, so attention is needed.The flow chart of FP quantitative method is shown in Fig. 6.

Fig.6 The flow chart of FP quantitative method

Flow Chart Explanation

1. First, measure the unknown sample and obtain the measurement intensity.
2. Assume the initial concentration of the sample and obtain a calculated intensity using the FP method.
3. Compare the measurement intensity and the calculated intensity.
4. Change the assumed concentration so that the measurement intensity and the calculated intensity match.
5. Obtain a new calculated intensity with the new assumed concentration using the FP method.
6. Repeat steps 3 to 5.
7. The assumed concentration that gives a calculated concentration that matches the measurement concentration is the analysis result.

Film Thickness Analysis of Thin Film Sample

In the case of a thin film sample, there is a correlation between the x-ray intensity of the elements composing the film and the film thickness. Therefore, by irradiating X-rays onto the surface of a thin film and measuring the X-ray intensity of the elements composing the film, the film thickness can be analyzed without destroying it.

A Single layer film can be analyzed using a calibration curve, but with the calibration curve method, a standard sample must be prepared for each kind of film. When the thin film FP quantitative method is used, it is not only possible to analyze single layer films, but also to analyze the thickness and composition of each layer in a multi-layer thin film, up to 5 layers , without a standard sample, which is very convenient. Fig. 7 shows a diagram of the thin film FP method, Fig. 8 shows a measurement example of Au/Ni/Cu film.

Thin Film FP (fundamental parameter) method

• Simultaneous non-destructive analysis of thickness and composition of thin film
• Up to 5 layers, and up to 20 elements for each layer
• Film thickness of about 10nm to 10μm (differs depending on element)
• Standard sample is not necessary (theoretical calculation)
• Information of layering order, elements, and density of the film is needed.

Fig.7 Schematic diagram of a thin film FP method

Fig.8 Measurement of the film Au / Ni / Cu thin film FP method

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What is EDS?

Energy-dispersive X-ray spectroscopy (also known as EDS, EDX, or EDXA) is a powerful technique that enables the user to analyze the elemental composition of a desired sample. The major operating principle that allows EDS to function is the capacity of high energy electromagnetic radiation (X-rays) to eject ‘core’ electrons (electrons that are not in the outermost shell) from an atom. This principle is known as Moseley’s Law, which determined that there was a direct correlation between the frequency of light released and the atomic number of the atom.

Removing these electrons from the system will leave behind a hole that a higher energy electron can fill in, and it will release energy as it relaxes. The energy released during this relaxation process is unique to each element on the periodic table, and as such bombarding a sample with X-rays can be used to identify what elements are present, as well as what proportion they are present in.

Shown below is an example of how EDS works. The letters K, L, and M refer to the n value that electrons in that shell have (K electrons, closest to the nucleus, are n=1 electrons), while α and β indicate the size of the transition. The relaxation from M to L or L to K are therefore described as Lα or Kα, while going from M to K would be a Kβ transition. The means that are used for describing these processes as a whole are known as Siegbahn notation.

How is data collected?

EDS functions with a series of three major parts: an emitter, a collector, and an analyzer. These parts are additionally typically equipped on an electron microscope such as SEM or TEM. The combination of these three pieces enables analysis of both how many X-rays are released, as well as what their energy is (in comparison to the energy of the initial X-rays that were emitted).

The EDS data is presented as a graph with KeV on the x-axis and peak intensity on the y-axis. The peak location on the x-axis are converted into the atoms that the energy changes represent by a computer program.

Figure. EDS chart from a research group that was analyzing the composition of shrimp and the associated bacteria that associate with these minerals. The EDS helped support the researcher’s case that the endosymbiotic bacteria living on these shrimp actually do influence the iron oxide composition in these minerals. This is evident by the peaks at 0.5 and 6.5 KeV.² 

What are some drawbacks of EDS?

Although EDS is an extremely useful technique, there are a number of difficulties involved with the process which hinder its utility. First, EDS is generally not a particularly sensitive technique. If the concentration of an element in the sample is too low, the amount of energy given off by X-rays after hitting the sample will be insufficient to adequately measure its proportion. Second, EDS generally does not work for elements with a low atomic number. Hydrogen and helium both only have an n=1 shell, meaning there aren’t core electrons to be removed that can allow for X-ray emission. Lithium and beryllium, meanwhile, have sufficiently low atomic numbers that the energy of X-rays given off by Li or Be samples is insufficient for measurement, and often times they cannot be tested as a result.

One additional difficulty associated with the technique is the thickness of the sample. Sample thickness can bring energy levels closer together, thus making electrons easier to move to outer energy levels, which can in turn cause deviation in the results. Another error source is overlapping emitted x-rays, which can alter the KeV readings. Additionally, X-rays are not particularly effective at penetrating beyond several nanometers in samples, which means that only surface layers can be efficiently measured by the technique. As such, if there is a discrepancy between the outer and inner material layers, it will not necessarily appear in EDS.

Work Cited

1. https://en.wikipedia.org/wiki/Energy-dispersive_X-ray_spectroscopy
2. https://cfamm.ucr.edu/documents/eds-intro.pdf
3. L. Corbari, M.-A. Cambon-Bonavita, G. J. Long, F. Grandjean, M. Zbinden, F. Gaill, and P. Compere “Iron oxide deposits associated with the ectosymbiotic bacteria in the hydrothermal vent shrimp Rimicaris exoculata” Biogeosciences 2008, 5, 1295–1310.