Atomic Spectroscopy

Our annual review of new spectroscopy products introduced at Pittcon, or during the previous year.

Cement is one of the most important materials for construction. ASTM C114-11 covers chemical analysis of hydraulic cement. XRF spectrometry is used for chemical composition analysis of cement due to its simple sample preparation and high precision. This application note demonstrates quantitative analysis for Portland cement by the pressed powder method according to ASTM C114-11 on the Rigaku Supermini200, a benchtop sequential wavelength dispersive XRF spectrometer.

The measurement of zirconium (Zr) conversion coating on aluminum is demonstrated.

Black pepper is often subject to counterfeiting and adulteration. Creating elemental profiles for an individual spice can be used as a tool to identify possible adulteration.

The measurement of gold is demonstrated in used ore material such as that from ore dumps and tailing piles. The recovery of uranium from the used ore material is also presented. The results how the Rigaku NEX DE EDXRF can achieve excellent results for monitoring and measuring the concentration of gold and other valuable elements in the recovery of used ore materials.

Teledyne Leeman Labs QuickTrace® M7600 was used to analyze and determine total elemental mercury (Hg0) concentration in Tuna (CRM 463) following the guidance in USDA Method CLG-MERC1.01 and the operating conditions.

A PFA cyclonic spray chamber was used with an HR-ICP-MS for the measurement of trace element/calcium ratios in foraminiferal calcite. The signal stability and washout were studied.

The measurement of chromium (Cr) conversion coating on aluminum is demonstrated.

The measurement of Cr, Hg, Pb, Br and Cd in polyethylene (PE) is demonstrated for RoHS rapid screening by XRF. Energy Dispersive X-ray Fluorescence (EDXRF) is employed for rapid screening and quantification according to RoHS norms.

Guide to Speciation: What is Speciation? Who Should be Concerned with Speciation Testing? What are the Obstacles to Adapting to Speciation Testing?

Quality control and quality assurance during the lube oil blending and manufacturing process is essential. Basic lube oil formulations containing only P, S, Ca and Zn are often augmented with additional elements and additives to create lubricating oils for specific needs.. This report demonstrates the measurement of Mg, Si, P, S, Cl, Ca, Zn, Ba and Mo in new lube oils is using the empirical approach.

Preparing soil samples for pesticide analysis is a crucial step in ensuring the safety of all consumers. Typical soil samples for analysis are often a heterogeneous mix that are unable to be directly analyzed; thus, the handling and homogenizing of the sample must conducted with the proper tools and techniques in order to obtain a reproducible and meaningful result.

Semi-quantitative analysis in modern XRF instruments is a unique method which is performed without reference materials for the unknown samples. This report demonstrates determination of chemical composition in geological samples using semi-quantitative analysis by the pressed powder method on a WDXRF spectrometer.

EPA methods 200.7 and 6010 specify ICP; however, analysis of the major components may involve dilution of off-scale peaks, making the analysis more difficult. This work demonstrates a method that uses low-sensitivity analytical lines for the high-concentration major components and high-sensitivity analytical lines for the low-concentration trace components. This eliminates the need for multiple dilutions to get major elements on-scale.

Selecting the correct wavelengths or isotopes and optimizing flame, furnace, or plasma conditions can seem a daunting task for a novice user, with a multitude of opportunities to introduce errors and generate poor quality data. While most elemental analysis instruments have intuitive operating software, they lack the intelligence to guide the operator through the early stages of method development and overcome associated problems along the way. This study describes an automated, intelligent approach to method development for trace element analysis using optical emission spectroscopy, and exemplifies this capability with a suite of real-world sample matrices.

This application highlights performance of the Agilent Multimode Sample Introduction System for simultaneous determination of mercury, hydride forming and routine elements in a water CRM using the PerkinElmer Optima ICP-OES.

Biodiesel fuel is easily analyzed using the Prodigy7 ICP. The detection limit of Teledyne Leeman Lab’s Prodigy7 ICP-OES readily exceeds the requirements of the ASTM D-6751 Standard against which biodiesel must be measured. Samples are easily prepared by dilution with a suitable solvent. Sample spike recoveries and reference standards results indicate that the method is suitable for the analysis of biodiesel fuels and that matrix interferences are not an issue.

Preparing samples for analysis carries a set of difficulties that are often expounded on when cryogenic treatment of the material is necessary to meet the analytical requirements. In order to achieve the application requirements, selection of the correct milling device and technique is a critical decision.

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.

Terephthalic acid (TPA) and purified terephthalic acid (PTA) are precursors in the making of polyester PET for polyester films, bottle resin, textile fabrics, and specialty chemicals. During production and use of TPA and PTA, the catalysts Co, Br and Mn must be closely monitored to ensure optimum product quality. Rigaku EDXRF Application Note #1539 describes the analysis of concentrations of Co, Br and Mn in TPA and PTA solutions and highlights the performance of the Rigaku NEX OL on-line EDXRF process analyzer.

The elegant design of the Elegra results in a very compact accessory (Figure 1), making it easy to fit every ICP model without overcrowding the sample compartment. The Elegra utilizes highly efficient membrane technology to add moisture to the argon as it flows through the inert metal-free construction. The device runs at atmospheric pressure and does not require heating or electric power. The Elegra is also configured with a bypass switch so that the operator can turn humidification on and off without connecting or disconnecting any tubing. For easy installation on any ICP instrument and nebulizer, each Elegra Kit is packaged with customized gas connectors.

To optimize the mapping collection parameters, it is important to factor the size of the mapping area, the beam diameter, and the desired beam spacing. For this sample, the area being mapped is shown in red outline in Figure 2, approximately 50.4 x 3.5 mm.

Moxtek's MAGPRO miniature X-ray source is capable of up to 60 kV 200 µA and down to 4 kV and 1000 µA, and limited to an output power of 12 watts. The 12 W source is meant for use in small bench top systems where small size is valued.

The Rigaku NEX CG combines secondary and polarization target excitation, with a high performance SDD detector, to deliver optimal EDXRF sensitivity. In conjunction with UltraCarry, the NEX CG is an ideal tool for the trace elemental analysis of aqueous solutions down to parts-per-billion levels. This technique is suitable for many applications, including: 1) monitor effluents, waste streams, and discharge waters; 2) screen for common metals; 3) measure hazardous elements; 4) QC of production rinse waters; 5) pavement run-off; 6) storm water run-off; 7) agricultural run-off; 8) site remediation; and 9) soil leachates.

The United States Pharmacopeia (USP) is in the process of developing new USP chapters and for the measurement of inorganic contaminants in pharmaceutical samples. While samples can be dissolved in aqueous or organic solvents, the large majority will require digestion, and closed vessel microwave digestion is stipulated by USP. Single reaction chamber (SRC) microwave digestion is a new type of closed vessel digestion that was developed by Milestone and offers many advantages over closed vessel digestion-particularly for pharmaceutical sample types.