The recent acquisition of PANalytical (formerly Philips Analytical) brings new technologies and markets to Spectris. Analytical X-ray methods have been used for many years, and their ease of use and high level of precision are welcomed by users in markets ranging from the oil industry to materials research, the pharmaceutical industry and many others. Increasing regulatory pressure, together with the requirement for greater levels of quality control and growing environmental considerations, mean that testing is now an essential and growing application. In this feature we take a look at the benefits of X-ray analysis and its application in a range of industries.

X-ray analysis is used to obtain detailed information about the chemical composition and physical nature of all kinds of natural and manufactured materials, from metals, minerals, oils and other liquids, to plastics, pharmaceuticals and semiconductors. X-ray analysis methods have a number of practical and economic advantages. First and foremost, they are non-destructive, meaning that analysed samples are not destroyed or changed by exposure to X-rays. Another major advantage is that X-ray analysis requires relatively little sample preparation effort. Many of the alternative techniques require the sample to be dissolved, which is time consuming, costly in terms of reagents required and potentially hazardous for the environment. These difficulties and potential dangers are thus avoided.

X-ray analysis is also fast and highly accurate. Modern instruments are computer-controlled with powerful software to handle calibration and data processing. The technology enables chemical compositions to be determined in real time, in just seconds. This is why X-ray analysis is the preferred method for many primary industries such as steel and cement production, where any delays in quality checks can lead to dramatic increases in energy consumption and costly plant usage. Materials research laboratories benefit most from the easy and very accurate measurements.

There are two types of X-ray analyses: X-ray fluorescence (XRF) and X-ray diffractometry (XRD). XRF is a highly accurate and reproducible technique for identifying and determining the concentrations of the chemical elements present in solids, liquids and powders. Its primary applications are in industries such as minerals and mining, cement, petrochemical for production and process control, quality control, and also in research and development.

XRD looks at the structure of materials and is used to identify and determine the various crystalline compounds known as "phases", present in solid materials and powders. Each crystalline compound has its unique characteristic X-ray powder pattern, which is used for its identification just like a "fingerprint" in forensics. This method is used extensively in scientific and industrial research, but has a growing market share in production control.

Both methods are totally different from the density contrast pictures used in medical diagnostics. Some examples of key applications for PANalytical's X-ray analysis instrumentation are described below.

Petrochemical
Speed and reliability are essential in the processing and refining of crude oil and XRF equipment is used by many of the major oil companies. It is also used to control the nature and quantity of additives in the manufacture of by-products such as polymers and plastics.

In industry, lubricating oils are essential to the smooth running of machines and wear and tear on machines varies depending on the lubricant and its quality. The primary reason for failure and wear of lubricated machine parts is the lubricant itself and so analysis and monitoring of the lubricating oil is essential for the identification of possible machine failures. In the analysis process, the condition, contamination and water debris of the lubricating oil are measured using XRF spectrometry in order to detect metals such as iron and copper as well as common additives such as zinc and others. Importantly for wear analysis, XRF analysis is not limited in particle size and thus also detects the presence of larger particles, which are a strong indicator of abnormal wear modes. Less downtime of the unit and reduced energy costs are just some of the benefits of ensuring proper lubrication of machinery.

Mining
In Australia, a big mining corporation is using PANalytical's XRF spectrometers to analyse ore for copper and uranium. More than 9 million tonnes of ore per year are extracted and pre-treated or processed on site before shipment to the customer. Fast and accurate analysis is essential and the customer has found PANalytical's instrumentation to be precise, reliable and easy to operate.

Environmental
Increasing environmental legislation worldwide is putting pressure on companies to better understand the composition of their products in order to identify toxic elements in their production as well as to permit effective recycling. In particular, legislation has been tightened to improve the environmental impact of fuels, with the focus on reducing lead and sulphur content. In order to meet these stricter requirements, various oil companies have started to use XRF equipment to determine the amount of these substances in petrol. X-ray equipment is also used to analyse and quantify hazardous compounds in many more materials such as the chromium concentration in cement, where the rules on heavy metal contamination levels have become increasingly stricter. This in turn pushes the required detection limits to lower and lower values.

Building materials
XRD has many applications in the cement and plaster industries,starting with the analysis of raw materials from the quarries. The silica content of limestones directly influences the wear of the giant crushers and mills, while certain clay minerals cause blockage in the preheaters. The amount of free lime in clinker is a key measure to effective control of the kiln temperature, which saves energy and thus reduces costs. Analysing the amount and nature of all clinker phases ensures a constant quality and guarantees the physical properties of the final products.

Metals
Major aluminium smelters such as Alcoa and Alcan use PANalytical's XRD instrumentation for Potflux analysis to maximise the efficiency of aluminium production, a very energy-intensive process. The types and amounts of crystalline phases in solidified samples of the bath electrolyte are determined with XRD, while the total amount of calcium is measured with XRF. Both methods are combined into one instrument and customers are impressed with the ease of use of the system. Additionally XRD is used to verify particle size and uniformity of the fine carbon powder used to manufacture baked anodes for the electrolytic smelting process.

Pharmaceutical
The market for analytical X-ray equipment in the pharmaceutical industry is growing, as companies need to provide a detailed understanding of drug purity to meet strict FDA and other regulations. Customers such as GlaxoSmithKline, AstraZeneca and Merck use PANalytical's XRD instrumentation for research into the crystalline phases of the drug ingredients, and to determine possible structure changes due to certain storage conditions. The structure of a drug influences the way it is absorbed into the human body. X-ray instrumentation can also be used for production control during the manufacture of drugs.

Materials research
X-ray diffraction analysis is often the only solution to specific applications. For example, grains of clay minerals are frequently less than 1 micrometer in size and cannot be positively identified by alternative technologies such as chemical analysis or microscopy, so XRD methods are used for their identification.

Similarly, many natural and synthetic compounds exist in two or more different crystalline forms and X-ray diffraction is the only solution to identify and quantify the relative amounts of these forms. White pigments of titanium dioxide are a typical example of this phenomenon, which is called polymorphism.

In industry, XRD equipment is used to analyse, for example, film thicknesses, composition and density for semiconductors and magnetic materials. Multi-layered coatings on glass are also studied with this technique.

Conclusion
X-ray analytical systems are setting new standards for monitoring production processes and enhancing quality control whilst bringing significant savings for customers in terms of lower energy costs, reduced downtime and less wastage. As the world leader in development and manufacturing of analytical X-ray systems, PANalytical is well placed to benefit from the opportunities that are arising.

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