Relationship Between Particle Density and Soil Bulk Chemical Composition

Electronic Supplementary Material

soils, sec 2 • global change, environ risk assess, sustainable land use • short original communication

Relationship between particle density and soil bulk chemical composition

Dario Di Giuseppe1 • Massimiliano Melchiorre2 • Umberto Tessari1 • Barbara Faccini1

Received: 14 July 2015 / Accepted: 23 September 2015

Responsible editor: Fabio Scarciglia

Department of Physics and Earth Sciences, University of Ferrara, Via Saragat 1, 44122 Ferrara, Italy

Group of Dynamics of the Lithosphere, Institute of Earth Sciences Jaume Almera ICTJA – CSIC, LluísSolé i Sabarís s/n, 08028 Barcelona, Spain

Dario Di Giuseppe

Fig.S1 from Di Giuseppe et al. (2014) in which there is the location of all the samples used in this paper

Analytical methods

Sample preparation

For WD-XRF analyses each sample was quartered, dried at 60°C for 24 h to eliminate the hygroscopic water and then powdered using an agate mortar. Successively an amount of about 4 g of powder was pressed with addition of about 13.5g of boric acid by hydraulic press to obtain powder pellets applying a pressure of 101.81 kg·cm2. Simultaneously, 0.5–0.6 g of powder was heated for about 12 h in a furnace at 1000°C in order to determine the loss on ignition (LOI). This parameter measures the concentration of volatile species contained in the sample.

Sample analysis

The WD-XRF analysis of the powder pellets was carried out using an ARL Advant-XP spectrometer Thermo Scientific (Waltham, MA, USA). Calibrations were obtained analysing certified reference materials, and matrix correction was performed according to the method proposed by Lachance and Trail (1996).Accuracies and detection limits are reported in Table 1. More information about certified reference materials is available in Di Giuseppe et al. (2014).

Table S1 Comparison of major (wt%) and trace element (ppm) concentrations in reference samples analyzed using X-Ray Fluorescence spectrometry (XRF) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)
BE-N / BHVO-1
Relative / Relative / Detection
Recomm. / Measured / error (%) / Recomm. / Measured / error (%) / limit
XRF:
SiO2 / 38.48 / 38.59 / -0.3 / 49.94 / 49.57 / 0.7 / 0.05
TiO2 / 2.63 / 2.62 / 0.3 / 2.71 / 2.75 / -1.5 / 0.01
AL2O3 / 10.14 / 9.79 / 3.4 / 13.80 / 14.02 / -1.6 / 0.05
Fe2O3 / 12.93 / 12.77 / 1.3 / 12.23 / 12.52 / -2.4 / 0.10
MnO / 0.20 / 0.19 / 7.4 / 0.17 / 0.17 / 0.0 / 0.05
MgO / 13.25 / 13.61 / -2.8 / 7.23 / 6.90 / 4.6 / 0.01
CaO / 13.97 / 13.71 / 1.9 / 11.40 / 11.52 / -1.1 / 0.04
Na2O / 3.20 / 3.29 / -2.7 / 2.26 / 2.36 / -4.4 / 0.01
K2O / 1.40 / 1.35 / 3.6 / 0.52 / 0.50 / 3.8 / 0.01
P2O5 / 1.06 / 0.99 / 6.4 / 0.27 / 0.25 / 7.4 / 0.01
Zn / 120 / 116 / 3.3 / 105 / 98 / 6.7 / 2
Cu / 72 / 73 / -0.8 / 136 / 140 / -2.9 / 3
Sc / 22 / 21 / 4.6 / 31.8 / 32 / -0.6 / 3
Ga / 17 / 16 / 4.4 / 21 / 22 / -4.8 / 4
Ni / 267 / 261 / 2.2 / 121 / 124 / -2.5 / 2
Co / 60 / 63 / -5.0 / 45 / 46 / -2.2 / 2
Cr / 360 / 352 / 2.2 / 289 / 298 / -3.1 / 2
V / 235 / 231 / 1.7 / 317 / 312 / 1.6 / 2
Ba / 1025 / 991 / 3.3 / 139 / 145 / -4.3 / 3
Rb / 47 / 47 / 0.2 / 11 / 10 / 9.1 / 1
Sr / 1370 / 1362 / 0.6 / 403 / 408 / -1.2 / 2
Y / 30 / 28 / 5.3 / 27.6 / 28 / -1.4 / 2
Zr / 260 / 269 / -3.6 / 179 / 172 / 3.9 / 2
La / 82 / 81 / 1.6 / 15.8 / 17 / -7.6 / 5
Ce / 152 / 161 / -6.0 / 39 / 42 / -7.7 / 8
Nd / 67 / 65 / 3.7 / 25.2 / 24 / 4.8 / 3
Nb / 105 / 105 / -0.1 / 19 / 18 / 5.3 / 1
Th / 10.4 / 11 / -2.7 / 1.08 / 1 / 7.4 / 1
Recommended (Recomm.) values for international reference materials BE-N and BHVO-1 are from Govindaraju (1994). Detection limits were determined using 29 international reference standards run as unknowns.

WD-XRF spectrometer uses high energy X-rays to excite fluorescent radiation from a sample for elemental analysis. The different energies of the characteristic radiation emitted from the sample are diffracted by crystals under a wellcalibrated angle at which flow counter and scintillator detectors are positioned. ARL Advant-XP spectrometer Thermo Scientific works in a vacuum environment and is equipped with: 4GN end-window X-ray tube (Rh anode); thin Be window (0.075mm); microprocessor controlled goniometer (maximum slewing speed: 4800° 2θ/min, 0.015° of accuracy of peak positions, angular reproducibility: < ±0.0002°, total angle range: 0°–153° 2θ, step scan range: minimum step: 0.001°/maximum practical: 1.00°, time of measurement for each step: 0.1 s–655 s); multi-channel analyser to discriminate peaks of higher energies; Digital Automatic Gain Control for pulse shrinking correction; sample changer; primary beam filter and water cooling system.

References

Di Giuseppe D, Bianchini G, Faccini B, Coltorti M (2014) Combination of wavelength dispersive X-ray fluorescence analysis and multivariate statistic for alluvial soils classification: a case study from the Padanian Plain (Northern Italy). X-Ray Spectrom 43:165-174

Govindaraju K. (1994) 1994 compilation of working values and sampledescription for 383 geostandards.GeostandardsNewsletter 18 (Special Issue): 158 pp

Lachance GR, Traill RJ (1966) A Practical Solution to the Matrix Problem in X-Ray Analysis. I. Method Can Spectrosc 11:43-48