Supplementary Material
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Validation of soil phosphate removal by alkaline and acidic reagents in a Vertosol soil
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using XANES spectroscopy
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Supplementary Material
Supplementary Material
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Table SI - 1. Some chemical and physical properties of the low and medium P Vertosol.
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†
Measured using method 4A1 as described by Rayment and Lyons (2011), ‡measured using
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method 6B3 as described by Rayment and Lyons (2011), §measured as described by Walker
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and Adams (1958), ¶a microwave aqua regia digestion as set out by Tighe et al. (2004), ††FT
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refers to the field texture test as set out by McDowell et al. (2003), and §§the soil was below
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the detection limit of the soft X-ray beamline using P K-edge XANES spectroscopy at the
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Australian Synchrotron.
Soil property
pH†
Organic-C (%)‡
Organic-P (mg kg-1)§
Total-P (mg kg-1)¶
Clay (FT)††
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29
30
31
32
33
34
35
36
37
38
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Low P Vertosol§§
8.3
1.4
159
987
Medium clay
Medium P Vertosol§§
8.3
1.3
212
2424
Light medium clay
Supplementary Material
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Table SI - 2. Total element concentrations in the solution extracts of 0.1 M NaOH and 1 M HCl extractants for the low and medium P Vertosol.
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†
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for each treatment of an individual element and soil, and ‡“-” refers to elements not measured in the 0.1 M NaOH solution extract due to precipitation of the
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Al, Ca, Fe and Mn metal hydroxide species in the NaOH solution standards.
Standard errors are reported in parentheses following treatment mean for each element, and ANOVA significant (P = 0.05) differences are indicated (a,b,c)
Vertosol
Treatment
Low P
0.1 M NaOH
0.1 M NaOH + 1 M HCl
0.005 M H2SO4
0.1 M NaOH
0.1 M NaOH + 1 M HCl
0.005 M H2SO4
Medium P
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45
46
47
48
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Al
–
3115 (24)b
1103 (10)c
–
7245 (529)b
1338 (11)c
Ca
–
4740 (8)b
5353 (69)c
–
94774 (69)b
10339 (198)c
Element (mg kg-1)†,‡
Fe
–
4246 (25)b
79 (0)c
–
10981 (843)b
100 (5)c
Mn
–
589 (5)b
204 (2)c
–
855 (61)b
201 (3)c
P
37 (0)a
516 (2)b
441 (5)c
19 (1)a
1858 (165)b
1284 (21)c
Supplementary Material
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List of Figures
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Fig. SI- 1. Total fluorescence yield (TFY) obtained by bulk P K-edge XANES spectroscopy
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on individual replicates for the 0.1 M NaOH soil residues of the medium P Vertosol. Linear
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combination fitting did not accurately identify any reference materials that may represent the
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0.1 M NaOH soil residues. Spectra are background and baseline corrected, and the photon
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energy corrected using the Na4P2O7 concurrent standard.
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Fig. SI- 2. Total fluorescence yield (TFY) obtained by bulk P K-edge XANES spectroscopy
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on individual replicates for the 0.1 M NaOH + 1 M HCl soil residues of the medium P
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Vertosol. Linear combination fitting did not accurately identify any reference materials that
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may represent the 0.1 M NaOH + 1 M HCl soil residues. Spectra are background and baseline
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corrected, and the photon energy corrected using the Na4P2O7 concurrent standard.
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Fig. SI- 3. Total fluorescence yield (TFY) obtained by bulk P K-edge XANES spectroscopy
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on individual replicates for the 0.005 M H2SO4 soil residues of the medium P Vertosol. Linear
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combination fitting did not accurately identify any reference materials that may represent the
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0.005 M H2SO4 soil residues. Spectra are background and baseline corrected, and the photon
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energy corrected using the Na4P2O7 concurrent standard.
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Fig. SI- 4. Total fluorescence yield (TFY) obtained by bulk P K-edge XANES spectroscopy
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on the adsorbed P (ferruginous smectite, iron hydroxide, gibbsite and montmorillonite)
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reference materials. Spectra are background and baseline corrected, and the photon energy
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corrected using the Na4P2O7 concurrent standard.
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Supplementary Material
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Fig. SI- 5. Total fluorescence yield (TFY) obtained by bulk P K-edge XANES spectroscopy
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on individual replicates for the 0.1 M NaOH soil residues of the medium P Vertosol. Linear
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combination fitting did not accurately identify any reference materials that may represent the
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0.1 M NaOH soil residues. Spectra are background and baseline corrected, and the photon
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energy corrected using the Na4P2O7 concurrent standard.
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Supplementary Material
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Fig. SI- 6. Total fluorescence yield (TFY) obtained by bulk P K-edge XANES spectroscopy
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on individual replicates for the 0.1 M NaOH + 1 M HCl soil residues of the medium P
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Vertosol. Linear combination fitting did not accurately identify any reference materials that
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may represent the 0.1 M NaOH + 1 M HCl soil residues. Spectra are background and baseline
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corrected, and the photon energy corrected using the Na4P2O7 concurrent standard.
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Supplementary Material
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Fig. SI- 7. Total fluorescence yield (TFY) obtained by bulk P K-edge XANES spectroscopy
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on individual replicates for the 0.005 M H2SO4 soil residues of the medium P Vertosol. Linear
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combination fitting did not accurately identify any reference materials that may represent the
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0.005 M H2SO4 soil residues. Spectra are background and baseline corrected, and the photon
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energy corrected using the Na4P2O7 concurrent standard.
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Supplementary Material
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Fig. SI- 8. Total fluorescence yield (TFY) obtained by bulk P K-edge XANES spectroscopy
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on the adsorbed P (ferruginous smectite, iron hydroxide, gibbsite and montmorillonite)
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reference materials. Spectra are background and baseline corrected, and the photon energy
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corrected using the Na4P2O7 concurrent standard.
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Supplementary Material
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References
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McDowell RW, Condron LM, Mahieu N (2003) Analysis of phosphorus in sequentially
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extracted grassland soils using solid state NMR. Communications in Soil Science and
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Plant Analysis 34(11-12), 1623-1636.
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Rayment GE, Lyons DJ (2011) 'Soil chemical methods: Australasia.' (CSIRO publishing:
Victoria, Australia)
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Tighe M, Lockwood P, Wilson S, Lisle L (2004) Comparison of digestion methods for ICP-
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OES analysis of a wide range of analytes in heavy metal contaminated soil samples
134
with specific reference to arsenic and antimony. Communications in Soil Science and
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Plant Analysis 35(9-10), 1369-1385.
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Walker TW, Adams AFR (1958) Studies on soil organic matter: I. Influence of phosphorus
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content of parent materials on accumulations of carbon, nitrogen, sulfur, and organic
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phosphorus in grassland soils. Soil Science 85(6), 307-318.
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