Abstract
X-ray fluorescence spectroscopy (XRF) has been used extensively to analyze many types of environmental samples, including lake sediments. In most cases, however, analyses have required either a relatively large sample mass or sample pretreatment, e.g. lithium borate fusion, and have not taken advantage of the potential of XRF analysis as a non-destructive technique. This paper describes the development of two completely non-destructive calibration methods that use small, i.e. 200- and 500-mg loose-powder sediment samples. Analytical performance of these methods was assessed using ten different certified reference materials and a previously analyzed sediment profile, and for both methods, accuracy and precision were less than ±10 % (or a few ppm) for 26 elements (Na, Mg, Al, Si, K, Ca, Sc, Ti, V, Mn, Fe, Ni, Cu, Zn, Ga, As, Br, Rb, Sr, Y, Zr, Sn, Sb, Ba, W and Pb). This shows that quantitative wavelength dispersive X-ray fluorescence analysis, using small loose-powder samples, can be a useful geochemical tool for many paleolimnological applications, especially because lack of pretreatment ensures that samples can be used for further analysis.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
References
Battarbee R, Jones V, Flower R, Cameron N, Bennion H, Carvalho L, Juggins S (2001) Diatoms. In: Smol J, Birks HJ, Last W, Bradley R, Alverson K (eds) Tracking environmental change using lake sediments. Springer, Netherlands, pp 155–202
Bennett KD, Willis KJ (2001) Pollen. In: Smol J, Birks HJ, Last W, Bradley R, Alverson K (eds) Tracking environmental change using lake sediments. Springer, Netherlands, pp 5–32
Bindler R, Segerstrom U, Pettersson-Jensen IM, Berg A, Hansson S, Holmstrom H, Olsson K, Renberg I (2011) Early medieval origins of iron mining and settlement in central Sweden: multiproxy analysis of sediment and peat records from the Norberg mining district. J Archaeol Sci 38:291–300
Boyle JF (2000) Rapid elemental analysis of sediment samples by isotope source XRF. J Paleolimnol 23:213–221
Brodie CR, Casford JSL, Lloyd JM, Leng MJ, Heaton THE, Kendrick CP, Zong YQ (2011) Evidence for bias in C/N, delta C-13 and delta N-15 values of bulk organic matter, and on environmental interpretation, from a lake sedimentary sequence by pre-analysis acid treatment methods. Quat Sci Rev 30:3076–3087
Brown GC, Hughes DJ, Esson J (1973) New XRF data retrieval techniques and their application to USGS standard rocks. Chem Geol 11:223–229
Butler OT, Cook JM, Harrington CF, Hill SJ, Rieuwerts J, Miles DL (2008) Atomic spectrometry update. Environmental analysis. J Anal At Spectrom 23:249–286
Cheburkin AK, Shotyk W (1996) An energy-dispersive miniprobe multielement analyzer (EMMA) for direct analysis of Pb and other trace elements in peat. Fresenius J Anal Chem 354:688–691
Coulson CA, Zauli C (1963) The K-alpha transition in compounds of sulphur. Mol Phys 6:525–533
Ek AS, Renberg I (2001) Heavy metal pollution and lake acidity changes caused by one thousand years of copper mining at Falun, central Sweden. J Paleolimnol 26:89–107
Farmer JG, Eades LJ, Mackenzie AB, Kirika A, BaileyWatts TE (1996) Stable lead isotope record of lead pollution in Loch Lomond sediments since 1630 AD. Environ Sci Technol 30:3080–3083
Gazulla MF, Vicente S, Orduña M, Ventura MJ (2012) Chemical analysis of very small-sized samples by wavelength-dispersive X-ray fluorescence. X-Ray Spectrom 41:176–185
Glew JR, Smol JP, Last WM (2001) Sediment core collection and extrusion. In: Last WM, Smol JP (eds) Tracking environmental change using lake sediments vol 1: basin analysis, coring and chronological techniques. Kluwer Academic, Dordrecht, pp 73–105
Heiri O, Lotter AF, Lemcke G (2001) Loss on ignition as a method for estimating organic and carbonate content in sediments: reproducibility and comparability of results. J Paleolimnol 25:101–110
Koinig KA, Shotyk W, Lotter AF, Ohlendorf C, Sturm M (2003) 9000 years of geochemical evolution of lithogenic major and trace elements in the sediment of an alpine lake: the role of climate, vegetation, and land-use history. J Paleolimnol 30:307–320
Lachance GR (1993) Correction procedures using influence coefficients in X-Ray-fluorescence spectrometry. Spectrochim Acta B 48:343–357
Margui E, Hidalgo M, Queralt I (2005) Multielemental fast analysis of vegetation samples by wavelength dispersive X-ray fluorescence spectrometry: possibilities and drawbacks. Spectrochim Acta B 60:1363–1372
Mucke A, Farshad F (2005) Whole-rock and mineralogical composition of Phanerozoic ooidal ironstones: comparison and differentiation of types and subtypes. Ore Geol Rev 26:227–262
Norrish K, Hutton JT (1969) An accurate X-ray spectrographic method for the analysis of a wide range of geological samples. Geochim Cosmochim Ac 33:431–453
Ohlendorf C, Sturm M (2008) A modified method for biogenic silica determination. J Paleolimnol 39:137–142
Renberg I, Hansson H (2008) The HTH sediment corer. J Paleolimnol 40:655–659
Revenko AG (2011) Development of X-ray fluorescence analysis in Russia in 1991–2010. J Anal Chem 66:1059–1072
Rousseau RM (2006) Corrections for matrix effects in X-ray fluorescence analysis: a tutorial. Spectrochim Acta B 61:759–777
Rydberg J, Gälman V, Renberg I, Lambertsson L, Martinez Cortizas A, Bindler R (2008) Assessing the stability of mercury and methylmercury in a varved lake sediment deposit. Environ Sci Technol 42:4391–4396
Rydberg J, Rosén P, Lambertsson L, De Vleeschouwer F, Tomasdotter S, Bindler R (2012) Assessment of the spatial distributions of total- and methyl-mercury and their relationship to sediment geochemistry from a whole-lake perspective. J Geophys Res 117:G04005
Yang HD, Rose NL, Battarbee RW, Boyle JF (2002) Mercury and lead budgets for Lochnagar, a Scottish mountain lake and its catchment. Environ Sci Technol 36:1383–1388
Zaborska A, Carroll J, Papucci C, Pempkowiak J (2007) Intercomparison of alpha and gamma spectrometry techniques used in Pb-210 geochronology. J Environ Radioact 93:38–50
Acknowledgments
The WD-XRF instrument was funded by the Kempe foundation through a grant awarded to Professor Richard Bindler, Department of Ecology and Environmental Science, Umeå University. Financial support was also granted from the faculty of Science and Technology at Umeå University. I also thank Lars Lidén and Anne Wenger at Bruker-AXS for support with technical and software questions.
Author information
Authors and Affiliations
Corresponding author
Electronic supplementary material
Below is the link to the electronic supplementary material.
Rights and permissions
About this article
Cite this article
Rydberg, J. Wavelength dispersive X-ray fluorescence spectroscopy as a fast, non-destructive and cost-effective analytical method for determining the geochemical composition of small loose-powder sediment samples. J Paleolimnol 52, 265–276 (2014). https://doi.org/10.1007/s10933-014-9792-4
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10933-014-9792-4