An elemental analyzer designed for demanding applications – the SPECTRO XEPOS energy dispersive X-ray fluorescence (ED-XRF) spectrometer redefines XRF analysis with exceptional new levels of performance

Scientific evidence plays a vital role in today’s justice system: many high profile criminal investigations reach their conclusions almost entirely on this evidence. Many branches of science are employed in accumulating forensic evidence, from highly publicized techniques like DNA profiling to pathology, botany and of course chemical analysis. Elemental analysis of an object found in the course of an investigation can yield valuable clues to its origin and history. The object itself may, however, need to be presented as evidence, so any technique used for this analysis should ideally be non-destructive. Variation in sample type and size may be almost infinite: from a soil sample to a bullet to a microscopic speck of gunshot residue or fragment of glass. Archaeometry, the application of scientific methods to archaeology, has very similar requirements. Energy Dispersive X-ray Fluorescence (EDXRF) spectrometry is a versatile analytical technique that can satisfy both of these needs: it is non-destructive, requires very little sample preparation and can be configured to handle any sample size from a large surface to a few microns. The wide range of EDXRF spectrometers from SPECTRO Analytical Instruments and EDAX, member companies of AMETEK Inc.‘s Materials Analysis Division, provide solutions to many elemental analysis tasks in forensic investigation and archaeometry. 

Regulations restricting the use of hazardous substances in manufacturing are proliferating worldwide. Their aim: reducing the health and environmental impacts of certain harmful materials in consumer goods and other products. Different standards apply in different countries, affecting products from electrical and electronic components to toys and cosmetics, as well as raw materials and additives.

Fortunately, analytical technology has kept pace with regulatory demands. Analyzers employing X-ray fluorescence (XRF) spectrometry have evolved excellent capabilities for rapid screening. For example, the new SPECTROCUBE XRF spectrometer can deliver elemental testing for compliance with exceptional speed, plus demonstrated ease of use and reliability. Its design also enables adding new elements via simple software updates. This paper will focus on benchtop XRF instrumentation, while noting where other analyzer types are recommended.

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One unfortunate legacy of man’s activity is contamination of the environment. Soil, water and air can all be polluted by harmful substances, and this contamination can be directly toxic or can pass into food or other products for human consumption. Controlling harmful emissions from industry and the safe and environmentally responsible disposal of waste are major issues for governments and industries worldwide.

The analysis of environmental samples is an essential part of detecting and controlling pollution. Certain elements, particularly the “heavy metals” like lead, cadmium and mercury are notorious for their toxicity, and usually need to be measured in the parts-per-million concentration range. The most popular and convenient analytical technique for environmental screening for these elements is Energy Dispersive X-ray Fluorescence (EDXRF). Screening waste material or contaminated land is made much easier if analytical measurements can be made rapidly on site, and the new SPECTRO xSORT is a portable hand-held EDXRF instrument ideal for this type of work. The SPECTRO XEPOS is a high performance laboratory EDXRF system especially suitable for the determination of trace elements.

Huge quantities of waste oil and related wastes are generated each year. Properly collected and processed, these wastes can be a valuable energy source or be refined to produce usable products such as new lubricating oil. However waste oil is usually contaminated, because of its previous use, with water and other liquids, halogens and other elements including heavy metals. In most countries it is regarded as potentially hazardous waste and must be handled, processed and stored accordingly. Its transport, storage and ultimate uses are governed by a variety of direct and indirect national and international legislation and industry standards. A worldwide specialist industry has developed to collect, transport and process waste oil and to market the products derived from it. Elemental analysis is an essential part of the environmental protection and quality control procedures associated with the recycling of waste oil. The two analytical techniques most frequently used for elemental analysis in this industry are Energy Dispersive X-ray Fluorescence (EDXRF) spectrometry and Inductively Coupled Plasma – Optical Emission Spectrometry (ICP-OES). This paper describes these techniques and how the range of instruments from SPECTRO Analytical Instruments meet the current and future requirements for elemental analysis in the waste oil recycling industry. 

The analysis processes that are recommended in many pharmacopoeias for the determination of impurities can require complex sample preparation. They sometimes do not show very good reproducibility and have to be matched to the sample matrix. Energy-dispersive XRF conforms to the analysis processes described without the requirement of extensive sample preparation. Using optimized excitation and evaluation parameters, the technology provides detection limits that are sufficient for the analysis of most of the relevant elements.

The production of pharmaceutical products requires the analysis of a series of essential trace elements such as Fe, Cu, Zn, Se, Ca, Mg, Co, Si, and Mn as well as elements that are toxic in larger concentrations such as Cd, Pb, As, Hg, Cr, Mo, Ni, V, and Cu. In addition elements from the use of catalysts like Ir, Os, Pd, Pt, Rh, and Ru have to be monitored.

Aspects such as the bio-availability, toxicity, and quantity of the elements must be considered. The sources of such impurities can be production-related contamination from sieving and grinding processes, treatment with catalysts, and transportation in piping. Additional impurities may result from packing material and preservatives. It is also possible that the raw material, e.g. from plants, is already contaminated.

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Air pollution is a continuous concern of industries, governments, and populations worldwide. Particularly the harmful health effects of the exposure to heavy metals such as lead, arsenic, or cadmium absorbed into particulate matter, carried through the air, and introduced into the lungs and body are within focus.

These particles are principally generated by processes such as combustion. Monitoring and analysis of the elements present in these airborne particles is performed by a variety of organizations, - by industry, environmental protection agencies, as well as research institutes and testing laboratories for environmental and occupational health and safety.

Fortunately, modern laboratory-grade spectrometric analyzers are available that can handle the necessary analyses. They provide accurate, efficient airborne elemental particle identification and measurement. This paper explains several of the methodologies commonly employed for these applications focusing on ED-XHE ICP-OES, and ICP-MS technologies and describes the desirable attributes of suitable analyzer models for each.

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Precious metals require — and reward — careful analysis. But analysts face various difficulties. The scope of precious metals analysis extends from trace levels to 100%. Most of these metals are resistant to dissolution by all but the strongest acids. Some traditional analytical methods like fire assay are time-consuming and demand a high level of skill.

Three modern techniques offer widely used solutions. Energy-dispersive X-ray fluorescence (ED-XRF) and optical emission spectrometry (OES) can be used without specialist analytical training to rapidly and accurately analyze bullion, jewelry, and alloys. A variation of OES, inductively coupled plasma optical emission spectrometry (ICP-OES), is an ideal tool for the analysis of bulk materials such as ores, and for the determination of trace impurities.

Several instruments available from SPECTRO Analytical Instruments represent the state of the art in these techniques. This paper describes their application to precious metals analysis.