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The Application of Fourier Transform Infrared, Near Infrared and X-Ray Fluorescence Spectroscopy to Soil Analysis

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The Application of Fourier Transform Infrared, Near Infrared and X-Ray Fluorescence Spectroscopy to Soil Analysis VOL. 28 NO. 4 (2016) ARTICLE The application of Fourier transform infrared, near infrared and X-ray fluorescence spectroscopy to soil analysis A.H. Jean Robertson, Charles Shand and Estefania Perez-Fernandez The James Hutton Institute, Craigiebuckler, Aberdeen, Scotland, AB15 8QH. E-mail: [email protected] Introduction concentration has traditionally involved encompassing fundamental vibra- Soil is critical to life on earth and provides wet oxidation, although many labora- tions of both the organic and mineral not only the key functions of food and tories now use combustion with CHN components. The mineral components energy production but also many other analysers. There is now a drive towards present in soil are predominantly sili- important functions, such as water regu- using dry chemical methods such as cates, including clay minerals (alumi- lation and carbon sequestration.1 Soil is X-ray fluorescence (XRF) and infrared nosilicates), or carbonates, but can a highly complex material, consisting of (IR) spectroscopic analysis which mini- also include other types of minerals an extremely variable mixture of minerals, mise cost, improve speed and reduce such as sulfates. Clay minerals play an organic matter, liquids and gases. Soils environmental impact and waste. At the important part in the properties of a are heterogeneous on different scales: James Hutton Institute (and the legacy soil and have free OH groups present in the landscape they are heterogene- institutes of the Macaulay Institute and in their structures3 (i.e. without hydro- ous both horizontally and vertically and Scottish Crop Research Institute) we have gen bonding). The O–H stretching generally occur in distinguishable layers a long history of expertise in soil science bands for clay minerals (approximately termed horizons, as a result of modifica- and spectroscopic techniques, particularly 3700–3500 cm–1) are therefore sharp tion of inputs and outputs over time.2 On of IR spectroscopy in the mid-IR range. bands which are highly diagnostic. the microscopic scale, soil can be even In recent years we have been develop- Si–O stretching vibrations are strong more heterogeneous, moving, for exam- ing methods for Fourier transform (FT)-IR, bands found close to 1000 cm–1, and ple, over a very short distance from a near infrared (NIR) and XRF spectroscopic those for the carbonate anion are discrete mineral grain to a soil microbe. analysis of soil and creating databases close to 1400 cm–1. When consid - Soils can range from a mineral soil with of soil spectral data and calibrations to ered in combination with the bend - almost no organic matter content to an predict soil properties. Currently we are ing vibrations, below 900 cm–1, the entirely organic soil or peat. In the context working to move from laboratory-based individual minerals present can often of productive and sustainable agricul- analysis towards the development of be identified. For example, for carbon - ture there is a need to know soil prop- methodology for field-based soil analysis ates, it is relatively easy to differentiate erties such as pH, organic matter, and using FT-IR and XRF spectroscopy. between calcite (calcium carbonate), nutrient and pollutant concentrations. aragonite (a different form of calcium Traditionally, many soil analyses have Spectroscopic analysis of carbonate) and dolomite (a calcium involved wet chemical methods with soil magnesium carbonate). Silicate miner- liquid extraction and subsequent anal- Fourier transform infrared als can also be identified from their ysis of solutions with laboratory-based The highly complex and variable bending vibrations, e.g. quartz can be instruments. For example, the determina- nature of soil is reflected in the very readily identified by a sharp doublet at tion of the micronutrient concentration of different FT-IR spectra they produce in 797 c m–1 and 779 cm–1.4,5 soil involves extraction with acids (typi- the mid-IR region (4000–400 cm–1) The organic components present cally HF/HNO3 or HNO3/HCl) and subse- arising from the fundamental vibra- largely originate from vegetation and so quent analysis by inductively coupled tions of the components present. the IR spectral features of soil organic plasma (ICP)-based methods. Similarly, Usefully, the mid-IR spectra provide matter (SOM) have much in common the determination of soil organic matter an overall chemical profile of the soil, with IR spectral features of plants, www.spectroscopyeurope.com SPECTROSCOPYEUROPE 9 VOL. 28 NO. 4 (2016) ARTICLE although plants degrade to form other spectra8 and can be more difficult to ments with soil chemical or physical organic compounds such as humic interpret. attributes under study, for predictive and fulvic acids. A broad O–H stretch purposes.9 As opposed to FT-IR spec- between approximately 3600 cm–1 and Near infrared troscopy in the mid-IR region, which 3200 cm–1 is characteristic of SOM and While the fundamental vibrations of has mainly been used qualitatively, NIR the C–O stretch for polysaccharide is molecular bonds and functional groups spectroscopy is mostly used as a quan- found at 1030 cm–1, which can coincide occur in the mid-IR region, the NIR titative technique that provides a very with the silicate stretch if minerals are region extends between 750 nm and rapid means of simultaneously meas- also present. The C–H stretching region 2500 nm (i.e. 12,500–4000 cm–1) uring multiple physical and chemical can reveal whether long chain mole - and consists of broad absorption properties of soil. cules are present or whether the organic bands, overtones and combina- material is more polysaccharide based. tions of the fundamental absorptions X-ray fluorescence In addition, functional groups present found in the mid-IR range. NIR spec- Unlike the IR spectroscopic methods in the SOM such as those arising from tra contain absorbance bands mainly which are molecular, XRF using labo - esters, carboxylic acid, amide (protein) due to chemical bonds of C–H (fats, ratory-based instruments has been a and lignin can be identified and hence oil, alkanes), O–H (water, alcohol) and prime and widely used method for the the SOM characterised.6 Interpretation N–H (protein). Other chemical bonds determination of the elemental compo- of FT-IR spectra therefore allows a rapid may exhibit overtone bands in the sition of soils. The main elements in assessment of the relative proportions NIR region, but are generally weaker. soil expressed on a weight/weight and nature of both SOM and clay miner- NIR spectra of soil therefore reflect basis are generally in the order O, Si, als present and also the determination the SOM and clay minerals well, but Al, Fe, C, Ca, K, Mg, Na, Ti, N and P. Soil of the underlying mineralogy. provide much less information on the also contains other minor elements, Generally, FT-IR spectroscopic analy- full mineralogy of the samples than including those which are essential for sis of soil samples in the laboratory is their counterpart mid-IR FT-IR spectra. plant growth such as Cu and Zn. The carried out on dried, milled samples, Although NIR spectra do not have XRF method is based on excitation with an optimal particle size <2 µm, in the resolution of the mid-IR spectra, of the sample with a beam of X-rays order to avoid problems of reflection of NIR has the advantage of being a more resulting in the emission of secondary the radiation, poor resolution of peaks energetic radiation that penetrates X-rays with energies characteristic of and sloping baselines. An effective deeper into samples thus allowing the the elements in the sample (see, for protocol for preparation of soil samples scanning of samples with little, or no, example, Figure 3). To obtain reproduc- for FT-IR spectroscopic analysis, to allow previous preparation. Nonetheless, ible and accurate data, soil samples are the production of reliable and reproduc- samples are usually dried and sieved to generally converted into a pressed disc ible spectra, has been developed at the 1–2 mm for homogenisation purposes. or fused using a flux before pouring the James Hutton Institute.7 Historically FT-IR The most common spectral collec- melt into a mould to produce a glassy spectroscopy of soils was carried out in tion mode used is diffuse reflection, disc when cooled. These discs have a transmission, using KBr discs prepared in which the light interacts with the flat surface that is relatively homoge - from the milled soil, but more recently, sample and re-radiates diffuse reflected neous and so the sample is in a repro - diamond attenuated total reflection energy, which is detected (and plotted ducible position in relation to the X-ray (DATR) sampling accessories have as log 1/Reflectance) at a 45° angle in source and detector. With technologi- become routinely used for soil analysis, order to minimise specular reflection. cal developments in devices for the having the advantage of allowing spec- Its ease of use has given NIR spec- production and detection of X-rays, tra to be recorded of unprocessed soil, troscopy some advantage over other portable XRF point and shoot instru- automatically producing spectra of opti- techniques for soil analysis; however, ments (PXRF) have become widely mum intensity and being non-destruc- the combinations and overtones that available and used on soil samples that tive. The spectra produced are similar form the spectra conceal the sum have received little or no preparation in appearance to transmission spectra. of the numerous bands that corre - apart from drying and milling. Because Alternatively diffuse reflection or DRIFTS spond to functional groups present of the ease of use of PXRF, it is easy (diffuse reflection infrared Fourier trans- in the sample, making its interpreta- to obtain numerical data.
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