To meet the divergent needs of industry, SPECTRO offers advanced optical emission spectroscopy metal analyzers with arc and spark excitation (arc spark OES)

Optical emission spectrometry has been a preferred method for elemental analysis and quality control in the metallurgical industries for decades and is rightly regarded as robust, easy to use and realistically priced. Available instrumentation ranges from portable and mobile spectrometers for on-site use, through high performance laboratory systems to automated analyzers with robotic sample handling. Like many “mature“ techniques, in recent years it has attracted relatively little attention from the academic community, but leading manufacturers have been responsible for many technical innovations and improvements that have transformed the performance, reliability and ease of use of modern instrumentation.

The SPECTROLAB from SPECTRO Analytical Instruments brings together developments in sample excitation, optics and detector technology to meet the most demanding analytical requirements of the metals processing industries. Its exceptional stability, reliability and low maintenance requirements also make the SPECTROLAB especially suitable for automated applications. 

Because of its toxicity and wide occurrence in man-made artifacts, lead was one of the first elements to be covered by environmental legislation, and much effort has been devoted to its removal from the human environment. Its use is now effectively banned or severely restricted in products from paints and automotive fuel to toys and electronics. However the lead-acid battery is still a very popular power source, especially in the automotive industry, and the rapid growth of the emerging economies in the East has also dramatically increased the demand for the metal and increased its price. Simultaneously with this process however, the demand for low-carbon energy for transport and other applications requires the storage of electrical energy from renewable and perhaps intermittent sources, and the lead-acid battery is still one of the most commonly used devices for this purpose, creating a new demand for the metal. It is ironic that this most legislated-against metal is now part of the solution to another environmental problem. Most countries have strict guidelines for disposal of used products that contain lead, including batteries, and clearly it is more sustainable to recycle the lead into new batteries than to dispose of it by other means. The composition of the lead used in batteries has a marked effect on performance and needs to be strictly controlled. Depending on the type of battery, the presence of certain elements in the lead can either improve or impair battery performance. Many elements can only be tolerated as impurities at very low levels and the increasing use of recycled lead can introduce traces of contaminants not found in lead from natural sources. High performance Optical Emission Spectrometry (OES) is one of the techniques best suited to measuring these elements at the very low levels required. This paper discusses the use of the SPECTROLAB spectrometer from SPECTRO Analytical Instruments in this application.

The development of ferrous metallurgy is inextricably linked to the advance of civilization. It can also be truthfully said that without carbon there would be no cast iron or steel, as it has been the reducing agent used to liberate metallic iron from its ores since the earliest times. A few tenths of a percent difference in carbon content can have a dramatic effect on the mechanical properties of iron and steel, so its accurate measurement is critical to ferrous metallurgy.

Chemical and spectroscopic methods have been developed for the measurement of carbon in iron and steel. One of the most popular is Optical Emission Spectrometry (OES) using an electric spark source. When measuring carbon in cast iron, however, this method can be prone to errors traceable to the granular nature of the material and to the presence of particles of “free” carbon in the form of graphite. These errors can only be overcome by perfect sample preparation techniques, but a high degree of skill and experience is required to achieve reproducible and reliable results. New developments in OES technology incorporated in the SPECTROLAB and SPECTROMAXx from SPECTRO Analytical Instruments make it possible to detect and even analyze samples containing free graphite. Using this approach, results are comparable to those achieved by techniques such as combustion analysis.

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Inclusions have a large impact on the mechanical properties of steels and other metals. In applications where inclusions play a role, it is important to control size, shape and homogeneity of the inclusions. Very often the most important criterion is the absence of any inclusions. Here, of most importance, is the cleanliness of steel. In the last fifteen years OES technology has made significant progress with respect to fast readout of single sparks. This development enabled the fast detection of inclusions using the Single Spark Evaluation (SSE) technology with SPECTROLAB, which has to be regarded as complementary to the traditional optical and scanning electron microscope methods. The advantage of the SSE technology lies in the speed and multi-element analysis possibility. Although the traditional technologies are more quantitative methods, they are time consuming and expensive. The qualitative or semi-quantitative OES-SSE technology balances out against the traditional technologies with respect to the speed, simultaneous multielement correlation counting and simplicity of the detection method.

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. 

National and international legislation has been introduced around the world aimed at reducing the health and environmental impacts of a variety of harmful substances in consumer goods and other manufactured products. Controls exist not only on the materials used in manufacture but on the procedures used for disposal of products at the end of their useful lives. Different standards apply in different countries to products as diverse as electrical and electronic products, toys and cosmetics. Certain notorious “heavy” elements, especially lead, figure widely in the legislation, so elemental analysis may be the only way of demonstrating compliance. X-Ray Fluorescence Spectrometry is not only very suitable for the detection of these heavy elements, but in many applications has the added advantage of being non-destructive. This makes it particularly attractive for rapid screening tests. The SPECTRO xSORT hand-held XRF spectrometer from SPECTRO Analytical Instruments has exceptional performance for this class of instrument, and can provide laboratory quality screening results in a matter of seconds. SPECTRO also produces a range of other analytical instruments with applications in compliance testing.

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.

Optical Emission Spectroscopy (OES) is generally regarded as the oldest instrumental technique for elemental analysis, tracing its origins to the mid 19th century. By the middle of the last century, developments in instrument design, optics, detector technology and electronics had created an analytical tool that had become one of the most widely used in materials testing. This is still the case today. OES instruments from SPECTRO Analytical Instruments have earned an enviable reputation for performance and reliability and thousands are to be found in laboratories and metallurgical industries throughout the world. The heart of any OES instrument is the optics and detection system. Traditionally, the photomultiplier has been the detector of choice, but developments in semiconductor technology have yielded solid-state detectors such as CCD’s that can approach the performance of the photomultiplier. Both types of detector have their advantages in terms of analytical performance, but compromises inevitably have to be made when choosing which to use in an instrument, and most commercially available instruments use either photomultiplier or CCD detection. The SPECTROLAB M10 has a revolutionary hybrid optical design that incorporates both types of detector in the same instrument in optimized configurations, allowing the analyst to choose the detector best suited for the individual application – truly the best of both worlds! 

Optical Emission Spectroscopy (OES) is the most popular and best established technique for the quantitative analysis of metals and alloys. Like most instrumental methods it is a relative technique, where sample measurements are compared to calibration measurements made on standards of known concentration. Any short-term or long-term instability of the measuring system will adversely affect the quality of the results, and instrument suppliers often rely on precision data and results on Certified Reference Materials to indicate the performance of their products. In industries such as aerospace or automotive, accuracy may be of paramount importance.

ASTM E 1009 describes a method for evaluating an OES instrument for the analysis of carbon and low-alloy steels, using specified CRM’s as standards, and includes a way of defining the accuracy of the analysis. Work at SPECTRO Analytical Instruments has used the approach in ASTM E 1009 as the basis for a software-controlled quality control and qualification procedure, the SPECTRO Performance Qualification System (SPQS), which has the potential to be applied to any OES measurement. Calibration and validation specifications can be developed for the user’s specific analyses, using standards chosen to suit the application and imposing accuracy, precision and stability limits agreed between SPECTRO and the customer at the time of ordering. The SPQS can then be applied throughout the life of the OES spectrometer to ensure that this level of performance is maintained, while at the same time generating a secure trail of measurement data for quality audit purposes.

Explosions, fires, and other incidents in industrial environments receive wide publicity. Financial losses to operators and insurers can easily run to many millions of dollars. Not infrequently, these incidents are traced to the use of piping, valves, and similar components made of inappropriate materials.

In many cases, the presence or absence of a particular alloying element in a steel component is critical to its performance but impossible to detect by physical inspection. It’s why today, spectrometric analyzers have become vital components for the performance of PMI in these environments.

This new paper reviews several situations that occur regularly and then explains the leading technologies and the instruments that are most effective in detecting the inappropriate alloying elements. Sample test results are included to demonstrate each instrument’s analytical capability.

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REACH (Registration, Evaluation, Authorization and Restriction of Chemical substances, EC/1907/2006) is the new and harmonized directive for chemicals and their usage in the european union. An important part is the responsibility for manufacturers to inform their customers when the products contain specific substances >0.1%. This legislation is in process of enactment and will replace earlier legislation like the Restriction on the Marketing and Use of Dangerous Chemicals (76/796/EC) by 2015. REACH places requirements on the classification, packaging and labeling of chemicals. A Candidate List of Substances of Very High Concern (SVHC) published by the European Chemicals Agency (ECHA), lists chemicals to which the legislation already applies (in 2009). Included in the list are several heavy metal compounds like TBTO (tributyltin oxide). 

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. 

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.

Over 400 million tons of metal is recycled each year. Recycling conserves precious natural resources, and the benefits to the environment in saved energy and reduced greenhouse gas emissions are also well recognized. Scrap metal in a raw, unsorted form has low monetary value, is bulky and expensive to handle and transport, and attracts low margins as a trade commodity. Manual sorting based on appearance, magnetic behavior and similar physical properties to identify higher value metals is labor intensive, inaccurate and unreliable. The SPECTRO xSORT handheld metals analyzer can take the uncertainty out of scrap sorting and positively identify alloy grades in seconds.

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