Rigaku

http://www.spectroscopyonline.com/spec_w/virtual

 magazine and the Society for Applied Spectroscopy (SAS) are pleased to present a joint virtual conference on February 23 and 24, 2021, called “Atomic Spectroscopy in Practice.” This two-day event will provide highly practical information for atomic spectroscopists and analytical laboratory staff working with molecular atomic techniques.

The first day, February 23, will cover sample preparation, atomic absorption (AA), and inductively coupled plasma-optical emission spectroscopy (ICP-OES) and ICP–mass spectrometry (ICP-MS).

THE second day, February 24, will cover X-ray fluorescence, laser-induced breakdown spectroscopy (LIBS), and laser-ablation ICP-MS (LA-ICP-MS).

Each day, there will be a morning session and an afternoon session. The morning sessions will provide a series of tutorials on fundamentals and troubleshooting, followed by a question-and-answer (Q&A) period with all of the speakers. In the afternoon sessions, leading instrument suppliers will give 20-minute talks providing educational troubleshooting and tips-and-tricks.

The event will also include a special award plenary for the 2021 Emerging Leader in Atomic Spectroscopy, with a talk by this year’s winner, L. Robert Baker of the The Ohio State University.

All attendees will receive a certificate of completion from the Society for Applied Spectroscopy.

Tuesday, February 23: Sample Preparation, AA, and ICP Techniques

Laura Bush, Editorial Director, Spectroscopy

Introduction to Sample Preparation for Spectrochemical Analysis

This introductory session will offer both theory and practice of sample preparation methods for spectrochemical analysis (AAS, ICP-OES and ICP-MS). The conventional thermal methods (hot plate, dry ashing, fusion) as well as microwave-assisted digestions, and high-pressure high temperature acid digestions will be covered. The chemical and physical underpinnings of sample decomposition will be discussed. The participants will learn about how to minimize the background element concentrations and contaminant control, practical hints as well as safety issues. The session is an ideal starting point for beginners. Key learning objectives include:

Learn about various sample decomposition methods available for spectrochemical analysis.

How does sample digestion work? Learn about the chemical and physical basis.

How to determine the effectiveness of decomposition.

How to achieve low backgrounds and contaminant control and safety concerns.

Learn about sample preparation hints, pitfalls, and safety issues.

Introduction to Atomic Absorption Spectroscopy

This session will cover recent advances in analytical atomic spectroscopy including flame atomic absorption spectroscopy (FAAS), hydride generation (HG)-AAS, cold vapor(CV)-AAS, graphite furnace AAS (GF-AAS), and atomic emission spectroscopy (AES). Course content includes fundamentals, theory, instrumentation, practice, troubleshooting hints, as well as common applications. Analytical merits and limitations of each method will be presented. Key learning objectives include:

What’s in that box? We will learn about the theory, basic instrumentation, and practice of flame AAS, AES, (HG)-AAS, (CV)-AAS and GF-AAS.

How to choose suitable instruments conditions and how to remove potential spectral and chemical interferences.

Will learn about calibration approaches for quantitative analysis.

Introduction to ICP-OES and ICP-MS: Key Concepts, Processes and How They Affect Signals, Capabilities, and Potential Sources of Error

The (simple) fundamental processes that control ICP-OES (optical emission) and ICP-MS (mass spectrometry) signals will be described including conversion of samples to atoms and ions, excitation and light emission, and ion transport from the ICP through the mass spectrometer. How each process affects ICP-OES and ICP-MS signals (related to a corresponding component of the instrument) and how the sample itself can affect the fundamental processes, and therefore, signal intensities will be considered. Spectral overlaps and matrix effects that can affect analysis accuracy will be discussed.

Leading instrument suppliers give educational 20-minute talks providing troubleshooting and tips-and-tricks

Wednesday, February 24: XRF, LIBS, and LA-ICP-MS

X-ray Fluorescence Spectrometry with Emphasis on Field Applications

This session will start with brief description of X-ray fluorescence (XRF), including how it originated and then evolved from large laboratory setups into portable, handheld devices. Then it will highlight features and limitations of handheld XRF, followed by overview of its main applications. It will also discuss common misconceptions and typical mistakes associated with use of handheld XRF devices.

Overview of Qualitative XRF with Application Examples from Cultural Heritage and Archaeology

X-ray fluorescence (XRF) spectrometry is a simple, nondestructive technique that provides valuable elemental information for a wide range of industries and areas of research. This presentation will provide an overview of XRF spectrometry with an emphasis on qualitative analysis. It will start with a tutorial on qualitative analysis via XRF, including spectral interpretation and interferences. This will be followed by a discussion of different data analysis approaches. The final part of the talk, drawing on the speaker’s years of research experience in cultural heritage analysis and archaeology, will emphasize applications of XRF spectrometry. Examples will include sample types such as glass tesserae and fabrics, pairing of XRF spectrometry with other instrumental methods, and different instrument designs such as portable XRF and micro-XRF.

Laser-induced Breakdown Spectroscopy: From Plasma Formation to Actionable Results

This session will guide the participants through an analysis concept to completed measurement and will focus on identifying measurements for which LIBS is not simply acceptable, but ideal. Topics to be covered include:

           -What is local thermodynamic equilibrium and why does it matter?

           -Beyond the raw spectra to concentrations, trends, depth profiling and imaging

Two use-cases that highlight the use of LIBS above other analytical techniques.

Laser Ablation ICP-MS: A Review of Fundamentals and Applications

This session will provide an introduction to the science behind laser ablation–inductively coupled plasma–mass spectrometry (LA-ICP-MS), including an overview of various instrumental components. The fundamentals will be illustrated with examples of practical applications of the technique.

Special Award Plenary: The Emerging Leader in Atomic Spectroscopy Award

Visualizing Charge and Spin Dynamics Using Ultrafast XUV Spectroscopy

L. Robert Baker, The Ohio State University

The need to characterize materials and devices that enable new technologies is pushing the boundaries of atomic, molecular, and material spectroscopies. For example, at the heart of energy conversion and information processing is the need to control charge and spin transport at interfaces. Many artificial systems rely on heterogenous catalysts to accomplish at surfaces what nature does using molecular assemblies, making it important to understand the material properties and surface states that mediate electron dynamics at interfaces. Despite its importance, the ability to directly measure charge and spin dynamics on the ultrafast time scale with chemical-state resolution remains a significant challenge, requiring the development of new spectroscopic tools. Toward this goal, we have developed extreme ultraviolet reflection-absorption (XUV-RA) spectroscopy as a surface-specific analog of X-ray absorption spectroscopy. This talk focuses on the development of this method and its recent applications, which range from directly observing charge separation at catalytic interfaces to studies of ultrafast spin state switching in magnetic semiconductors.

On demand available after final airing until Feb. 24, 2022

: CEM, Glass Expansion, Leco, Milestone, Millipore Sigma, Tofwerk, Rigaku

Webcasts

***Live: Tuesday February 23, 2021 & Wednesday February 24, 2021*** Spectroscopy magazine and the Society for Applied Spectroscopy (SAS) are pleased to present a joint virtual conference on February 23 and 24, 2021, called “Atomic Spectroscopy in Practice.” This two-day event will provide highly practical information for atomic spectroscopists and analytical laboratory staff working with molecular atomic techniques. *** On demand available after final airing until Feb. 24, 2022***

Atomic Spectroscopy in Practice: A Joint Virtual Conference Presented by Spectroscopy Magazine and The Society for Applied Spectroscopy

Articles

This application note describes a fast and simple means of obtaining elemental composition of unknown sample materials using the Rigaku NEX DE VS elemental spectrometer.

Industrial Forensics by Rigaku EDXRF

This application note demonstrates how to perform point and mapping analysis on the Rigaku ZSX Primus IV / Primus IVi general purpose WDXRF spectrometers.

Mapping and Small Spot Analysis with General Purpose XRF

This application note demonstrates the analysis of distinct polymorphs with the Rigaku Progeny 1064 nm handheld Raman analyzer.

Polymorph Monitoring with 1064 nm Handheld Raman Analyzer 

This application note demonstrates the use of the SQX Scatter Fundamental Parameter (FP) method for the screening of materials difficult to analyze by conventional SQX. 

Advanced SQX Analysis by Scatter FP Method on Benchtop Sequential WDXRF Spectrometer


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Quantitative Analysis of a Four-Component Sample Using a Benchtop X-ray Diffractometer

Measurement of metals, especially toxic heavy metals, in aerosols on air filters is demonstrated. Simple linear empirical calibration is discussed, and performance is shown for measurement precision and typical detection limits.

	Element analysis of aerosols and particulate matter released in smokestacks and other industrial gas discharge is vital to ensure that environmentally acceptable levels of toxic and hazardous elements are released properly into the air. Monitoring smoke or other gaseous waste is important in order to minimize air pollution and the release of toxic metals in compliance with United States Environmental Protection Agency and other world and regional or local governing regulations.

	As a tool to help ensure compliance and proper release, Rigaku offers the NEX DE EDXRF analyzer with 60 kV excitation source and high resolution and throughput Si Drift Detector, providing a fast, simple, yet powerful means for elemental analysis of air filters.

Nuclepore(r) polycarbonate Aerosol membranes

Helium (for optimum light element performance)

10-position 40 mm Automatic Sample Changer 

	Air filter material used was Nuclepore polycarbonate aerosol membrane. The filter membrane is supported by a 40 mm diameter plastic outer ring. Samples lie flat and smooth in the 10-position autosampler, covering the analysis aperture.

	A single-point linear empirical calibration was made for each element using the Standard Value loading levels.

	To determine the Lower Limit of Detection (LLD) using the empirical method, ten repeat analyses of a blank filter membrane sample were measured and the standard deviation calculated. The LLD is then defined as three times the standard deviation. This approach ensures that analyses above the determined LLD are measuring signal above background.

	To demonstrate typical measurement recovery and instrument precision, each calibration standard was measured in 10 repeat analyses using a total analysis time of 1200 s (300 s per measurement condition).

	The Rigaku NEX DE combines filtered direct excitation with a high performance SDD detector capable of 500,000+ cps throughput to deliver excellent sensitivity for the measurement of metals in aerosols on air filters. The NEX DE analyzer is capable of elemental analysis from Na–U, making the XRF technique ideal for other elements on air filters, as well. For the measurement of light elements Na-Cl, helium purge is used to remove air from the optical path and optimize analysis sensitivity. Elements from Cr and above can be easily measured in air without the need for helium purge.

	The NEX DE analyzer also gives the user a very versatile tool not only for monitory air filters, but also elemental analysis of solids, powders and liquids.

	9009 New Trails Drive, The Woodlands, TX 77381

Analysis of Metals in Aerosols on Air Filters

This report introduces an X-ray fluorescence (XRF) analysis for the detection of ppb levels of hazardous heavy elements in wastewater and river water using "Ultracarry®" high sensitivity micro-droplet filter paper and the "Ultradry™" vacuum dryer.

	There has been growing demand globally for the analysis of environmentally hazardous substances. Detection of a trace amount of wastewater and heavy elements in wastewater and river water is achieved by XRF analysis with the UltraCarry® sample preparation technique.

	A liquid sample of wastewater or river water is dropped onto an Ultracarry filter paper. An Ultradry, which dries the solution by decompression and heating, was employed to shorten the drying time. The dried Ultracarry pads were mounted on aluminum or titanium cups to avoid scattered X-rays. The cups were set in the sample holders of the XRF instrument.

	The Rigaku ZSX Primus II wavelength-dispersive X-ray fluorescence spectrometer was used for the analysis. It has a high spectral resolution that enables a high precision analysis of wastewater with a complex sample matrix. The combination of ZSX Primus II and Ultracarry enables wastewater analysis of a trace of zinc down to about 1 ppb. The time for drying the Ultracarry was about 30 min, and the time for the XRF qualitative analysis was 2 to 3 min per sample. It is typically necessary to use condensed sample solutions to meet environmental regulations for hazardous heavy elements in river water. The Ultradry can be used for this type of analysis because it is equipped with a decompression evaporating apparatus. A NIST1643c standard (reference solution of river water) was used. The material was first condensed by 50 times with an Ultradry then dropped onto an Ultracarry and dried.


	Figure 1: XRF spectrum of river water (21°–36°2q , LiF (200) analyzing crystal, Cu primary-beam filter, 50 kV and 50 mA.

	XRF peaks for As (82.1 ppb), Pb (35.3 ppb), Se (12.7 ppb), and Rb (11.4 ppb) contained in the reference solution were clearly detectable.

	The technique of using Ultracarry filter paper and an Ultradry vacuum dryer shows that the XRF method can be used effectively for a low ppb level analysis of environmental heavy hazardous elements in wastewater and river water due to its simple and rapid sample preparation. Since industrial wastewater likely contains a number of heavy elements, a prescreening analysis is useful before a conventional analysis with an atomic absorption spectrometer or inductively coupled plasma spectrometer.


	9009 New Trails Drive, The Woodlands, TX 77381
	tel. (281) 362-2300, fax (281) 364-3628
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