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GeoloGy, ecoloGy, and landscapes, 2018 Vol . 2, no . 2, 148– 154 https://doi.org/10.1080/24749508.2018.1452459 INWASCON OPEN ACCESS X-ray fluorescence (XRF) in the investigation of the composition of earth materials: a review and an overview a,b Temitope D. Timothy Oyedotun a b Research and c oncept Unit, a friGeos erv (a Gs), Ibadan, n igeria; c oastal and estuarine Research Unit, d epartment of Geography, University c ollege l ondon, l ondon, UK ABSTRACT ARTICLE HISTORY Received 24 July 2017 X-ray fluorescence (XRF) spectrometry is a well-known, well-established and widely applied a ccepted 30 november 2017 technique in the determination of many major elemental compositions of earth materials. XRF confers the ability to analyse solid samples non-destructively through X-radiation. The orderliness KEYWORDS and clarity of its emission spectrum, its great accuracy and precision make this technique a spectrometry; earth geochemical method of choice in mineralogy and investigation of the chemical composition materials; samples; X-ray of earth materials. There are limitations regarding the age and calibration of instruments, costs fluorescence; major element of setting up, matrix effects to be considered and the stringent sets of standards; however, XRF laboratory analyses remain the standard technique for providing high-quality geochemical data analyses in the investigation of earth elemental composition. With further improvements in XRF technology, it is expected that this technique will be of continued importance/utility in geological and geomorphological investigations. 1. Introduction applications of XRF in geochemical investigations; and highlight the examples of its diverse applications. This X-ray fluorescence (XRF) spectroscopy is one of the most is intended as a simple overview of a useful technique widely used and well-established methods of routine esti- for geo-scientific investigations of geological formation mation of geochemical composition of rocks, sediments and landscapes. Its usefulness is illustrated by analysis and earth material samples (Kramar, 1997; Ling et al., of coastal-estuarine sediments, a case study example. 2017; Tolosana-Delgado & McKinley, 2016; Weltje & Tjallingii, 2008; Young, Evans, Hodges, Bleacher, & Gra, ff 2. XRF 2016). For many years, XRF spectrometry is used in the determination of geochemical concentrations for a range e m Th ajor elemental composition of Earth material sam - of major and trace elements at parts per million (ppm) ples can be analysed by various instruments (Baedecker, level. It has, also, been utilised in the successful investiga- 1987; Sabaou, Ait-Salem, & Zazoun, 2009). However, tion of geological, archaeological and industrial samples XRF spectrometry is particularly valuable because of its (Jenkins, Gould, & Gedcke, 1995; Young et al., 2016). ability to rapidly provide a high-resolution assessment of One reason why this technique is widely used is because relative variations of most Earth elemental compositions of its ability to analyse solid samples through X-ray radi- (Löwemark et al., 2011). XRF spectrometry is based on ation (Weltje & Tjallingii, 2008). The geochemistry of the wavelength-dispersive principle, which states that many of the Earth’s solid materials is regarded as the individual atoms emit a relative abundance of X-ray pho- product of parent rock, climatic-environmental condi- tons of energy or wavelength feature that can be esti- tions, and possible anthropogenic interactions with the mated (Weltje & Tjallingii, 2008). This technique has material (Jalali & Jalali, 2016). Hence, the ability of XRF been applied in the examination of Earth materials from to determine the major oxide/element composition of a range of settings and environments (e.g., Chalmers & many earth materials (either in glass discs, powder pel- Bustin, 2017; Löwemark, Jakobsson, Mörth, & Backman, lets or bulk powder samples) has made it useful in many 2008; Oyedotun, 2016; Özkul, Çiftçi, Tokel, & Savaş, laboratory settings (Jenkins et al., 1995; Kramar, 1997; 2017; Rivera, Giráldez, & Fernádez-Caliani, 2016; Young et al., 2016). It remains a standard method of geo- Sabaou et al., 2009). The wide range of XRF’s uses is due chemical investigation of Earth’s mineral and chemical to its capacity to provide probable higher precision and accuracy than alternative methods (Taggart, Lindsay, compositions. This paper summarises the theories and CONTACT Temitope d. Timothy o yedotun firstname.lastname@example.org, email@example.com © 2018 The a uthor(s). published by Informa UK limited, trading as Taylor & Francis Group. This is an open a ccess article distributed under the terms of the creative c ommons a ttribution license (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. GEOLOGY, ECOLOGY, AND LANDSCAPES 149 Scott, Bartel, & Stewart, 1987; Weltje & Tjallingii, 2008) provision of the highest possible quality of geochemical and to identify the detection limits for many elements data analyses of Earth materials (Janssens, 2013; Young in the ppm range (Löwemark et al., 2011). et al., 2016). 2.1. Strengths and weaknesses of XRF 2.2. Theory of XRF e Th advantages of the XRF technique (aer T ft aggart e XRF p Th rocedure involves inter-linked processes et al., 1987; Kramar, 1997; Weltje & Tjallingii, 2008) are (summarised from Sakurai et al., 2004; Weltje & many. First is its ability to analyse the bulk chemical con- Tjallingii, 2008). The incoming X-rays from an XRF tents of major elements (e.g., Al, Mn, Ca, Na, K, Ti, P, Si, instrument knock the electron of an atom out of the Mg, etc.) found in Earth materials. The X-ray emission inner orbital. This results in the excitation of the atom associated with the XRF technique is simple, system- and the production of high-energy radiation (photons, atic, relatively independent of the chemical state, and protons, electrons, etc.). The third process involves the with uniform excitation and absorption dependent on detection and integration of characterised emitted lines an atomic number. Also, interference in the line of X-ray to give varying levels of intensity. The last stage in this radiation can be easily corrected thereby enabling high process is the conversion of the detected line intensi- accuracy and precision to be easily attained. Another ties to elemental concentrations. Earth materials (e.g., advantage of XRF, in a geochemical investigation, is natural rocks) consist of diverse elemental minerals sample preparation, which is fast, simple and can be at highly variable compositions and structures which non-destructive. ae ff ct the behaviour of light in many complex ways, the Although XRF has many advantages, there are some identification of these elements is vitally possible using drawbacks that should be considered before embark- X-ray methods, (e.g., XRF) through the characteristic ing on a study using this technique. Firstly, most com- emitted-radiation of these compositions under certain mercially available XRF instruments are very limited conditions. in their ability to accurately and precisely measure the abundance of geochemical elements of the natural earth 2.3. XRF instrumentation materials that have minimal levels of elements (generally, Diverse advances have been made on instrumentation fewer than eleven elements) (Taggart et al., 1987), with- for XRF laboratory analyses and in situ field measure- out any form of modification/calibration. Secondly, most ments because of its abilities for geochemical analyses elemental variations are measured as counts instead of and investigations (Marguí, Queralt, & Van Grieken, as concentrations. Calibration of the XRF instruments 2016; Weltje & Tjallingii, 2008; Young et al., 2016; to measure concentration requires quantitative analysis etc.). Two types of these instruments are in use today of bulk sediment chemistry (Löwemark et al., 2011). and these are reported in literatures. Since the early Thirdly, sensitivity to low isotopes of an element is very 1960s, the Wavelength Dispersive (WD) XRF instru- poor, and this shortcoming necessitates the use in rou- ments have been widely adapted to geochemical inves- tine analyses of some other instrumentation – for exam- tigations/applications, and these remain common in ple, the surface roughness, water content, and grain size laboratory analyses of major elemental compositions variations of a material can influence the sensitivity of (Kramar, 1997). The second form of XRF instrumen- XRF measurements (Weltje & Tjallingii, 2008). Fourthly, tation that is still in use is based on the energy-dis- on many occasions, XRF methods cannot distinguish the persive (ED) discrimination principle with its ability inter-element effect within some earth material samples. to simultaneously discriminate the X-ray spectra of In the past, this shortcoming has necessitated the imple- ten to thirty elements (Kramar, 1984). Because of mentation of various other geochemical techniques such the sensitivity of XRF to background ratio, various as Mossbauer spectroscopy (e.g., Günzler & Williams, modifications have been made to the early ED instru- 2001; Gütlich, 2012). This limitation may be com- ments and these have given rise to many new variants pounded by the age of the X-ray instrument used. An (Vincze, Janssens, Vekemans, Adams, & Lemberge, ageing instrument may influence the counts measured, 2004), such as the Total reflection XRF (TXRF) (Prost, thereby impeding the comparison of results. Fifthly, the Wobrauschek, & Streli, 2017), Polarised XRF (PXRF) initial costs of setting up the XRF instrumentation and (Sakurai et al., 2004; Zhan, Luo, & Fan, 2007) etc. In equipment are relatively high. Lastly, strict adherence to laboratories, these have been used for decades with sets of standards and principles is required with intensive great success (Janssens, 2013; Young et al., 2016). sample preparation and analyses to meet the set stand- Because of the advantages inherent in mobility of XRF ard – although this may appear as a limitation to some, instrumentation, many manufacturers have developed it can also be regarded as essential good practice in an handheld XRF (hXRF) instruments which are now XRF laboratory ethic. being deployed on the field for in situ measurements However, despite the weaknesses of this method, XRF (Coccato et al., 2017; Marguí et al., 2016; Young et al., laboratory analyses remain the geochemical standard for 150 T. D. T. OYEDOTUN 2016). However, in geological sciences, these hXRFs each element occurs at a fixed position. XRF can be are still seldom used (Young et al., 2016) but currently readily utilised as a quantitative method of elemen- growing with much success. tal composition analysis since the peak height of an element is often related to the concentration in the sample. Quantitative XRF analysis generally uses two 2.4. XRF applications main techniques, the Fundamental Parameters Method e v Th ersatility and rapidity of the XRF technique have (FPM) and the calibration with standards method. given it a wide application in many industrial and sci- These two techniques are always incorporated in the entific fields (Table 1). XRF instrument software (Horiba, URL). The FPM is used to calculate the element concentration based on the peak intensities, while the Calibration Standard is 2.5. XRF method used to relate peak intensities to element concentra- 2.5.1. Sample collection and preparation tion by deriving calibration curves from materials of The Earth material samples (liquid or solid) must be known/certified composition. collected carefully to prevent contamination of the natural concentrations of the elements in the mate- 2.5.3. Precision and accuracy in XRF rial. Also, the sample collection and preparation must Two basic quality principles with XRF analysis are follow the established standards for the type of investi- precision and accuracy. These are necessary for unbi- gation being undertaken. Indeed, sample preparation is ased analysis. The ability of a method to give the same highly variable and is mostly dependent on the materi- result on a repeated analysis of the same sample is als being analysed and the goals of the analysis. For the stated to be precise. Precision is the deviation of a set XRF analysis of solid components of the Earth materi- of determinations from their random error (mean), als, samples must be larger than the largest particle or while accuracy is the level of conformity with the grain size in the materials (typically larger than 10× the elimination of systematic and random error (Taggart largest particle). This is imperative since, depending et al., 1987). Although a highly precise technique can on the XRF technique involved, the sampled material yield unbiased results, these results may be inaccurate may be subjected to a series of preparatory processes, especially if impurities have been introduced during including crushing and grinding to grains of a few sample preparation or because of calibration errors. millimetres in size or to a fine powder. Full details of To achieve high-quality and acceptable XRF results, sample collection and preparation can be found in attention must be given to achieving both precision and Marguí et al. (2016). accuracy. In addressing the drift (imprecision, whether short-term or long-term), multiple variables must be 2.5.2. Analysis taken into consideration. These include stability of the XRF results can be reported both qualitatively and XRF instrument, precision in sample preparation, cali- quantitatively. Although the energy-dispersive (ED) bration of the instrument to the most appropriate and XRF can be used to generate quantitative data if appro- acceptable reference standard, monitoring and man- priate standard-controlled calibration exists, often it is agement of room temperature, monitoring of voltage ideally suited for qualitative elemental analysis since changes because of fluctuating power supply, and giv- band assignment for the XRF spectrum is easy and ing attention to barometric pressure and other external factors. Table 1. Recent applications of XRF spectrometry. 3. Case study: identifying patterns of major Field of application Examples elemental composition using XRF ecology/ecosystem Rodríguez-Zorro, enters, Hermanowski, lima da c oasta, and Behling (2015) e H Th ayle, the Gannel and the Camel estuaries, within Metallurgy Mighall, Timberlake, Martínez-c ortizas, silva-s ánchez, and Foster (2017); Turner St Ives, Crantock, and Padstow bays, respectively (Figure and Filella (2017) 1), have received considerable attention in terms of the Forensics c astillo-peinado and l uque de c astro (2017); Rim et al. (2017) impacts of mining on estuarine sedimentation (e.g., polymers Bull, Brown, and Turner (2017); Guo, ye, li, Oyedotun, 2016; Pirrie, Power, Payne, & Wheeler, 2000; Han, and l oh (2017); Turner and Filella (2017) Pirrie, Power, Wheeler, & Ball, 2000). The effects of min - archaeology Hunt and speakman (2015); Turco, davit, ing on sediment supply, sedimentology and mineralogy c ossio, a gostino, and operti (2017) environmental analysis Tolosana-d elgado and McKinley (2016); were explored extensively in those studies. Here, XRF is Rivera et al. (2016) used to compare the composition of major elements in Geology Jalali and Jalali (2016); ling et al. (2017); the sediments of these three coastal-estuarine systems Özkul et al. (2017) Mining chalmers and Bustin (2017); p avilonis, Grass- with the aim of identifying the anthropogenic influences man, Johnson, diaz, and c aravanos (2017) on the geological landscapes; and explore the sedimen- s oils/landscapes Hartemink and Minasny (2014); Kitchel (2016) tary connectivity of the individual systems. GEOLOGY, ECOLOGY, AND LANDSCAPES 151 Figure 1. southwest england showing three estuarine systems (Hayle, Gannel, and camel) where sediments were sampled. s ource: c ontains os data © crown copyright and database right (2015). Figure 2. Major element composition (%) of intertidal sediments of three estuaries determined by X-ray fluorescence of 21 samples. 3.1. Method major elements in their oxidised state were determined X-ray Fluorescence Spectrometry (XRF) was used to as a percentage of composition (Oyedotun, 2015, 2016). determine the major elemental composition of 21 sedi- e s Th amples used in the XRF analyses were obtained ment samples from the estuarine and coastal systems. The from 0 to 5 cm sediment depth randomly collected from 152 T. D. T. OYEDOTUN the intertidal locations around the Hayle, Gannel, and non-destructive manner – the qualities which are vital in Camel systems of southwest England between 24 and 27 the understanding the composition of the earth’s mate- October 2011 (Figure 1). rial and landscapes. With the continuous developments Samples were prepared at the Coastal and Estuarine and improvements in XRF equipment, this technique will continue to flourish in the future. Research Unit of the Department of Geography, University College London (Oyedotun, 2015). The sediments were freeze-dried at ~60 °C in a Modulo 4 k Acknowledgement Freeze Drier for 5 days. The dried samples were pulver - I sincerely appreciate the supervisory assistance and sup- ised into a fine powder with an agate mortar and pestle. port of Dr. Helene Burningham and Professor Jon French To avoid contamination and the mixture of samples dur- when XRF analysis was undertaken as part of my Ph.D. ing preparation, both faces of the compression die for Geography programme at University College London, UK. I also appreciate the guidance and assistance of Janet Hope each of the samples were well covered. Each pulverised with the laboratory analyses; Dan Shuman and Ann Grant ground sample (powder pellet) was then weighed prior with reading through and commenting on the drafts of this to analysis; weights of samples ranged from 4 to 6 grams. article. es Th e samples were analysed with a Spectro XLab Pro 2000 which produces high X-ray intensity and permits Disclosure statement quantitative analysis of elements in the ng range (aer ft Jenkins et al., 1995). No potential conflict of interest was reported by the author. 3.2. Comparison of major element (XRF) ORCID composition (%) of intertidal sediments T emitope D. Timothy Oyedotun http://orcid.org/0000-0002- 3926-0358 e e Th lements analysed were Ca, Si, Al, Fe, Cl, Mg, Na, K, Ti, S, P, Mn, V, and Cr. The total base cation per - centages (Si, Mn, P, CI and Fe) of the Hayle estuary was References high compared to total content for the other estuaries; Baedecker, P.A. (Ed.). (1987). Methods for geochemical whereas Mg, Al, S, and K were higher in the Camel analysis. US Geological Survey Bulletin 1770. Estuary (Figure 2). e Th total base cation content (Na, Bull, A., Brown, M.T., & Turner, A. (2017). Novel use of field- portable-XRF for the direct analysis of trace elements in Mg and K) was low (<5% in total) in all the sites but marine macroalgae. 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Geology Ecology and Landscapes – Taylor & Francis
Published: Apr 3, 2018
Keywords: Spectrometry; earth materials; samples; X-ray fluorescence; major element
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