The ICH Harmonised Guideline for Elemental Impurities of drug products specifies limits on the residual amounts of 24 elements whose toxicities are of concern. The recommended analytical techniques to achieve this are ICP-MS and ICP-AES, but the regulations allow other methods if they exist. One such method is XRF spectrometry. The method is shown to meet the regulations and is a useful, cost-effective alternative to ICP-MS and ICP-AES.
Sampling particulate matter is in many fields performed without a scientific basis, mostly because its critical role is ignored, or at best, misunderstood, and because of an unawareness of, sometimes a disregard for, the Theory of Sampling. This two-part column illustrates this important point using experience in the field of geo-environmental engineering.
FT-IR spectroscopy and ED-XRF are used to determine the origin of contaminants in food that may, or may not, have originated from dental materials.
With a significant proportion of our regular readership probably under home lock-down, we were wondering if we could help you at this difficult time by pointing out some useful online resources. So, when we finally come out of this pandemic, you could do so better skilled and more up-to-date than when we went in to it.
Tony and Lutgarde Buydens give us an update on the planning for the major EuroAnalysis 2021 conference, which is being held in Nijmegen, the Netherlands, at the end of August 2021. At this stage, they are keen to gather suggestions from readers on topics they would like to see covered. Groups are also invited to consider hosting their own event under the EuroAnalysis 2021 banner.
Total reflection X-ray fluorescence (TXRF) is a “Cinderella” technique: not widely known but with great potential. The author and other members of the TXRF Workgroup are making strenuous efforts both to spread the word about TXRF and to improve communication within the TXRF community. As Ramón points out, atomic absorption or plasma spectroscopies may be the “go to” techniques for many, but TXRF is worthy of consideration.
Pentti Minkkinen and Kim Esbensen present case histories and examples all focusing on the potential for economic loss or gain—by following, or more importantly, by not following TOS.
Significant research is underway globally into both improving corrosion protection as well as removing chemicals of concern from existing corrosion protection coatings. This is because the cost of corrosion in developed economies has been consistently shown to lie in the range 2–4% of Gross National Product.
Nanomaterials find widespread applications in many fields of science and nanotechnology, especially as catalysts in the chemical, bio-nanotechnology, nano-electronics and pharmaceutical industries. Understanding the physical and chemical properties of nanoscale materials is important, not only because of the fascinating nature of the subject, but also due to their potential applicability in almost every branch of science and technology. Nanostructured materials offer interesting properties, because at the atomic or molecular scale, the physical properties of a material become size dependent due to the quantum confinement and surface states effects.
In this article the question of the certification of calibration samples for the characterisation of advanced thin film materials is addressed within the framework of reliable process control or quality management purposes. Reference measurement techniques can be used in order to address the gap in appropriate certified reference materials (CRMs) for thin film analyses. They allow for qualifying out-of-production samples originating from an operating production line as calibration samples. As a template for this procedure, CIGS [Cu(In,Ga)Se2] layers, that are absorber layers for high efficiency thin-film solar cells, have been used for establishing and validating reference-free X-ray fluorescence (XRF) analysis and Auger-electron spectroscopy (AES) as reference measurement techniques.
Different spectroscopic techniques have been combined to provide additional and complementary information for decades. Increasingly, this is being expanded beyond just two techniques and may include spatial/imaging information as well. All of which bring their own challenges. In “Multimodal imaging of cells and tissues: all photons are welcome”, David Perez-Guaita, Kamila Kochana Anja Rüther, Phillip Heraud, Guillermo Quintas and Bayden Wood report an example of these new approaches. They look at the use of infrared, Raman and X-ray fluorescence spectroscopies to obtain combined imaging data of whole algal cells and discuss how to overcome the challenges.
X-ray spectroscopy techniques have some advantages over other atomic spectroscopy techniques in the analysis of foods, for instance in not requiring significant sample preparation. Amongst these, TXRF has higher sensitivity and limits of detection in the ng range. The authors look at the analysis of a number of very different foods, including seafood, honey and vegetables.
It is not every issue that one of our articles starts with a quotation in medieval English, and it is appropriate as two of our articles cover the use of spectroscopy in cultural heritage. This is yet another field where the rich information provided by spectroscopy, along with its non-destructive nature (for many techniques), portability and ability to generate chemical images make it the answer to many questions. Kate Nicholson, Andrew Beeby and Richard Gameson are responsible for the medieval English at the start of their article “Shedding light on medieval manuscripts”. They describe the general use of Raman spectroscopy for the analysis of historical artefacts, and, in particular, their work on medieval European manuscripts and 18th century watercolour pigments. They stess the importance of checking the actual laser power density to avoid damage to priceless artefacts.
Once again developments in portable instruments lead to greater ease of use and the ability to measure far more samples. They describe the application of FT-IR, NIR and XRF spectroscopies to the development of the National Soils Inventory of Scotland, and their work in developing the use of handheld instruments, particularly FT-IR spectrometers.
This article looks at the use of Raman and XRF spectroscopies to investigate the different deterioration processes caused by marine aerosols. These techniques can detect the decay compounds and the original composition of the different materials from historical buildings close to the sea, which can then be used to explain the reactions that take place on them. This helps in the development of remedial actions and preventive conservation strategies for historical buildings.
Several earthworm species secrete very small granules of calcium carbonate, and the authors think these are involved in pH regulation. These granules contain different polymorphs of calcium carbonate, including the amorphous form which is very unstable in the laboratory. To investigate this they have FT-IR spectroscopy and mapping, and are continuing this work with Ca XANES.
Yvonne Fors, Håkan Grudd, Anders Rindby and Lennart Bornmalm tell us about “X-ray fluorescence for cultural heritage: scanning biochemical fingerprints in archaeological shipwrecks”. Two outstanding examples of the preservation of wood are the warships Vasa, in Stockholm and the Mary Rose in Portsmouth and this article looks at the role XRF has played in the preservation of the wood of both ships.
Another area of application of XRF, “Determination of elemental distribution or heterogeneity by X-ray fluorescence”, is considered by Christopher Shaffer and Didier Bonvin. The ability of modern X-ray spectrometers to perform small spot analysis as well as mapping has opened up new applications in non-homogeneous samples. The authors show applications in metals, precious alloys as well as rocks.
Knowledge about the particles in the air is important because of their effect on our health and their impact on our climate through cloud formation and transport of nutrients into the oceans. Ursula Fittschen describes “Strategies for ambient aerosols characterisation using synchrotron X-ray fluorescence: a review”. This technique can provide elemental determination and speciation of aerosol particulates with limits of detection in the pg m–3 range for many elements.
Both the size and chemical composition of airborne particles have an effect on human health. Whilst the effects of size have been much studied, many of the toxic chemicals in particles are at very low concentration and have been less studied. Monitoring their composition and concentration over time helps to determine their source. Synchrotron radiation-induced XRF spectrometry proves to be a good tool for this purpose.