Sample Preparation for Evaluation of Detection Limits in X-ray Fluorescence Spectrometry

Tiwari, M. K.; Singh, Ashish; Sawhney, Kawal

doi:10.2116/analsci.21.143

Cited by 26 publications

(8 citation statements)

References 24 publications

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“…25 mg of each standard was separately mixed into suspension with 1 l of Milli‐Q water in a sealed flask and vacuum filtered through individual QFFs to yield 42 filter paper standards. Dispersing the sediment this way ensured that each QFF had a homogeneous covering of sediment after filtering, an essential step because surface roughness, uneven sediment distribution, differing densities, and mixtures of different particle sizes can all produce spectra that deviate from the expected theory making them difficult to interpret quantitatively (Tiwari et al ., ; Maruyama et al ., ). The sediment loaded filters were dried at 105 °C for 2 h before being re‐weighed to determine the mass of trapped sediment.…”

Section: Methodsmentioning

confidence: 98%

Combining two filter paper‐based analytical methods to monitor temporal variations in the geochemical properties of fluvial suspended particulate matter

Cooper

Rawlins

Lézé

et al. 2013

Hydrological Processes

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9Many of the commonly used analytical techniques for assessing the properties of fluvial suspended 10 particulate matter (SPM) are neither cost-effective nor time-efficient, making them prohibitive to 11 long-term high-resolution monitoring. We present an in-depth methodology utilising two types of 12 spectroscopy which, when combined with automatic water samplers, can generate accurate, high-13 temporal resolution SPM geochemistry data, inexpensively and semi-destructively, directly from 14 sediment covered filter papers. A combined X-ray fluorescence spectroscopy (XRFS) and diffuse 15 reflectance infrared Fourier transform spectroscopy (DRIFTS) approach is developed to estimate 16 concentrations for a range of elements (Al, Ca, Ce, Fe, K, Mg, Mn, Na, P, Si, Ti) and compounds 17 (organic carbon, Al dithionate , Al oxalate , Fe dithionate , and Fe oxalate ) within SPM trapped on quartz fibre filters 18 at masses as low as 3 mg. Calibration models with small prediction errors are derived, along with 19 mass correction factor models to account for variations in retained SPM mass. Spectral pre-processing 20 methods are shown to enhance the reproducibility of results for some compounds, and the importance 21 of filter paper selection and homogeneous sample preparation in minimising spectral interference is 22 emphasized. The geochemical signal from sediment covered filter papers is demonstrated to be time 23 stable enabling samples to be stored for several weeks prior to analysis. Example results obtained 24 during a heavy precipitation event in October 2012, demonstrate the methodology presented here has 25 considerable potential to be utilized for high-resolution monitoring of SPM geochemistry under a 26 range of in-stream hydrological conditions. 27

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Section: Methodsmentioning

confidence: 98%

Combining two filter paper‐based analytical methods to monitor temporal variations in the geochemical properties of fluvial suspended particulate matter

Cooper

Rawlins

Lézé

et al. 2013

Hydrological Processes

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“…Furthermore, the location or distribution of heteroatoms can be revealed by analyzing an EDX map (Pendashteh et al, 2017). Compared to EDX, the XRF measuring setup is less complicated, and the detection limit of XRF is lower (XRF ppm; EDX 0.1%) (Jembrih-Simbürger et al, 2002;Tiwari et al, 2005). Additionally, no vacuum is needed because no scattering takes place between the X-rays and the air.…”

Section: Chemical Functionalitiesmentioning

confidence: 99%

Current Trends in the Optical Characterization of Two-Dimensional Carbon Nanomaterials

Kröner

Hirsch

2020

Front. Chem.

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Graphene and graphene-related materials have received great attention because of their outstanding properties like Young's modulus, chemical inertness, high electrical and thermal conductivity, or large mobility. To utilize two-dimensional (2D) materials in any practical application, an excellent characterization of the nanomaterials is needed as such dimensions, even small variations in size, or composition, are accompanied by drastic changes in the material properties. Simultaneously, it is sophisticated to perform characterizations at such small dimensions. This review highlights the wide range of different characterization methods for the 2D materials, mainly attributing carbon-based materials as they are by far the ones most often used today. The strengths as well as the limitations of the individual methods, ranging from light microscopy, scanning electron microscopy, transmission electron microscopy, scanning transmission electron microscopy, scanning tunneling microscopy (conductive), atomic force microscopy, scanning electrochemical microscopy, Raman spectroscopy, UV-vis, X-ray photoelectron spectroscopy, X-ray fluorescence spectroscopy, energy-dispersive X-ray spectroscopy, Auger electron spectroscopy, electron energy loss spectroscopy, X-ray diffraction, inductively coupled plasma atomic emission spectroscopy to dynamic light scattering, are discussed. By using these methods, the flake size and shape, the number of layers, the conductivity, the morphology, the number and type of defects, the chemical composition, and the colloidal properties of the 2D materials can be investigated.

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“…Portable X‐ray fluorescence analysis (pXRF) is a nondestructive method, that has been used for the element's hotspot analysis since the beginning of the 2000s (Kalnicky & Singhvi, 2001; Ravansari et al, 2020; Ravansari & Lemke, 2018). The technique is based on measuring the atomic emission of X‐ray fluorescence to determine both qualitative and quantitative elemental composition (Tiwari et al, 2005). Feasibility of this method for heavy metals analysis in soil has been proven in literature (Chakraborty et al, 2017; Paulette et al, 2015; Rouillon & Taylor, 2016) and standardized (USEPA, 2007).…”

Section: Introductionmentioning

confidence: 99%

Feasibility of pXRF to evaluate chosen heavy metals in soil highly influenced by municipal waste disposal—A monitoring study of a former sewage farm

et al. 2022

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Sewage disposal onto agricultural land may result in the high accumulation of organic wastes, which questions the applicability of typical elemental analysis used for the soil components. To monitor the contamination status of agricultural soils at a former sedimentation basin, after the long‐term cessation of wastewater irrigation, 110 locations (15–20 cm depth) and 4 boreholes (up to 100 cm depth) were sampled to determine pH, loss on ignition, and concentration of Ni, Cu, Pb, Zn, and Cr. Additionally, the applicability of portable X‐ray fluorescence (pXRF) for the soil samples highly influenced by the organic wastes was evaluated. The study revealed the presence of a relatively homogenous sewage waste layer (depth of 20 cm), characterized by slightly acidic to neutral pH (6.3–7.5), high organic matter (OM) accumulation (up to 49%), and elevated concentration (mg kg −1) ranges between: Pb (5–321), Cu (31–2828), Ni (10–193), Cr (14–966), and Zn (76–6639). The pXRF analysis revealed metal concentration increase in mineral samples (up to 50%). The regression models and correction factors demonstrated high correlation and significance of pXRF measurement with response to increasing OM content, with the lowest r 2 = 0.86 obtained for Ni. Correlation of pXRF and AES measurement illustrated element‐dependent response for soils high in organics. Zn, Cu, and Cr pXRF analysis led to a slight underestimation in lower values, but overall good correlations (0.87; 0.89; and 0.88 respectively). Pb and Ni pXRF measurement revealed higher deviation from the reference in both lower and higher concentrations (0.74 and 0.70, respectively).

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Sample Preparation for Evaluation of Detection Limits in X-ray Fluorescence Spectrometry

Cited by 26 publications

References 24 publications

Combining two filter paper‐based analytical methods to monitor temporal variations in the geochemical properties of fluvial suspended particulate matter

Combining two filter paper‐based analytical methods to monitor temporal variations in the geochemical properties of fluvial suspended particulate matter

Current Trends in the Optical Characterization of Two-Dimensional Carbon Nanomaterials

Feasibility of pXRF to evaluate chosen heavy metals in soil highly influenced by municipal waste disposal—A monitoring study of a former sewage farm

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