Bulk and Mapping Speciation Analyses Unveil the Pattern and Heterogeneity of Cu Species during Organic Waste Treatment

Organic wastes (OWs) can be a common source of copper (Cu) contamination of agricultural soils. Here we conducted a comprehensive study of 22 raw and treated OWs sampled at 6 different full-scale OW treatment plants. Bulk XANES analysis findings indicated that the Cu oxidation state was subject to c...

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Published inEnvironmental science & technology Vol. 58; no. 32; pp. 14439 - 14449
Main Authors Doelsch, Emmanuel, Le Bars, Maureen, Etschmann, Barbara, Formentini, Thiago, Legros, Samuel, Levard, Clément, Chaurand, Perrine, Basile-Doelsch, Isabelle, Rose, Jérôme, Brunetti, Gianluca, Doolette, Casey, Howard, Daryl L., Lombi, Enzo
Format Journal Article
LanguageEnglish
Published United States American Chemical Society 13.08.2024
American Chemical Society (ACS)
Subjects
Aerobic conditions
Agricultural land
Agricultural pollution
Agricultural wastes
Anaerobic conditions
Anaerobic digestion
Anaerobic processes
Anaerobic treatment
Composting
Composts
Copper
Crystallization
Engineering
Environmental Sciences
Environmental Sciences & Ecology
Heterogeneity
nanomaterials
Occurrence, Fate, and Transport of Aquatic and Terrestrial Contaminants
Organic waste treatment
Organic wastes
Oxidation
Pattern analysis
Scale (corrosion)
Soil pollution
Speciation
Species
Sulfides
Urban agriculture
Valence
Waste treatment
X-ray absorption spectroscopy
trace element
digestate
quantitative mapping
X-ray absorption spectroscopy
compost
copper sulfide
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Abstract Organic wastes (OWs) can be a common source of copper (Cu) contamination of agricultural soils. Here we conducted a comprehensive study of 22 raw and treated OWs sampled at 6 different full-scale OW treatment plants. Bulk XANES analysis findings indicated that the Cu oxidation state was subject to changes throughout the OW treatment process, mostly depending on the anaerobic/aerobic conditions prevailing in each treatment stage. These changes were independent of the OW origin (agricultural, urban or industrial). Cu­(I) prevailed in raw OWs and digestates (88–100%), whereas Cu­(II) dominated in composts (46–100%). Bulk EXAFS analysis confirmed these observations and revealed that Cu­(I) species in raw OWs and digestates consisted mainly of Cu­(I)-sulfide (76–100%), while Cu­(II) species (60–100%) in composts were Cu­(II)-citrate, Cu­(II)-carbonate and amorphous Cu­(II)-phosphate. Interestingly, we observed that anaerobic digestion was conducive to the formation of crystallized Cu­(I)-sulfides at the expense of nanosized and poorly crystalline Cu­(I)-sulfide species, and that the recalcitrant Cu­(I) species in composts was always crystallized Cu­(I)-sulfide. XANES imaging analysis revealed Cu­(II) species present in low proportions (2–4%) that were not detected using bulk XAS analysis in raw OWs and digestates. This demonstrated the potential of XANES imaging for probing minor species in complex matrices.
AbstractList Organic wastes (OWs) can be a common source of copper (Cu) contamination of agricultural soils. Here we conducted a comprehensive study of 22 raw and treated OWs sampled at 6 different full-scale OW treatment plants. Bulk XANES analysis findings indicated that the Cu oxidation state was subject to changes throughout the OW treatment process, mostly depending on the anaerobic/aerobic conditions prevailing in each treatment stage. These changes were independent of the OW origin (agricultural, urban or industrial). Cu(I) prevailed in raw OWs and digestates (88-100%), whereas Cu(II) dominated in composts (46-100%). Bulk EXAFS analysis confirmed these observations and revealed that Cu(I) species in raw OWs and digestates consisted mainly of Cu(I)-sulfide (76-100%), while Cu(II) species (60-100%) in composts were Cu(II)-citrate, Cu(II)-carbonate and amorphous Cu(II)-phosphate. Interestingly, we observed that anaerobic digestion was conducive to the formation of crystallized Cu(I)-sulfides at the expense of nanosized and poorly crystalline Cu(I)-sulfide species, and that the recalcitrant Cu(I) species in composts was always crystallized Cu(I)-sulfide. XANES imaging analysis revealed Cu(II) species present in low proportions (2-4%) that were not detected using bulk XAS analysis in raw OWs and digestates. This demonstrated the potential of XANES imaging for probing minor species in complex matrices.
Organic wastes (OWs) can be a common source of copper (Cu) contamination of agricultural soils. Here we conducted a comprehensive study of 22 raw and treated OWs sampled at 6 different full-scale OW treatment plants. Bulk XANES analysis findings indicated that the Cu oxidation state was subject to changes throughout the OW treatment process, mostly depending on the anaerobic/aerobic conditions prevailing in each treatment stage. These changes were independent of the OW origin (agricultural, urban or industrial). Cu(I) prevailed in raw OWs and digestates (88-100%), whereas Cu(II) dominated in composts (46-100%). Bulk EXAFS analysis confirmed these observations and revealed that Cu(I) species in raw OWs and digestates consisted mainly of Cu(I)-sulfide (76-100%), while Cu(II) species (60-100%) in composts were Cu(II)-citrate, Cu(II)-carbonate and amorphous Cu(II)-phosphate. Interestingly, we observed that anaerobic digestion was conducive to the formation of crystallized Cu(I)-sulfides at the expense of nanosized and poorly crystalline Cu(I)-sulfide species, and that the recalcitrant Cu(I) species in composts was always crystallized Cu(I)-sulfide. XANES imaging analysis revealed Cu(II) species present in low proportions (2-4%) that were not detected using bulk XAS analysis in raw OWs and digestates. This demonstrated the potential of XANES imaging for probing minor species in complex matrices.Organic wastes (OWs) can be a common source of copper (Cu) contamination of agricultural soils. Here we conducted a comprehensive study of 22 raw and treated OWs sampled at 6 different full-scale OW treatment plants. Bulk XANES analysis findings indicated that the Cu oxidation state was subject to changes throughout the OW treatment process, mostly depending on the anaerobic/aerobic conditions prevailing in each treatment stage. These changes were independent of the OW origin (agricultural, urban or industrial). Cu(I) prevailed in raw OWs and digestates (88-100%), whereas Cu(II) dominated in composts (46-100%). Bulk EXAFS analysis confirmed these observations and revealed that Cu(I) species in raw OWs and digestates consisted mainly of Cu(I)-sulfide (76-100%), while Cu(II) species (60-100%) in composts were Cu(II)-citrate, Cu(II)-carbonate and amorphous Cu(II)-phosphate. Interestingly, we observed that anaerobic digestion was conducive to the formation of crystallized Cu(I)-sulfides at the expense of nanosized and poorly crystalline Cu(I)-sulfide species, and that the recalcitrant Cu(I) species in composts was always crystallized Cu(I)-sulfide. XANES imaging analysis revealed Cu(II) species present in low proportions (2-4%) that were not detected using bulk XAS analysis in raw OWs and digestates. This demonstrated the potential of XANES imaging for probing minor species in complex matrices.
An initial large area survey scan of 7x4 mm for raw and compost from Urban-3 or of 8x2 mm for raw and treated OWs from Agri-1 and Central-1 was collected at 15.8 keV to reveal the overall elemental distribution. Subsequently, a smaller area of interest (5x0.22 mm for raw and compost from Urban-3 or of 3x0.2 mm for raw and treated OWs from Agri-1 and Central-1) was chosen to conduct XANES imaging (XANES stack) consisting of 95 individual maps collected at increasing incident energies from 8900 eV to 9300 eV across the Cu K-edge. Energies were selected as follows: 8900-8960 eV in 10 eV increments, 8970-8975 eV in 1 eV increments, 8976-8999.5 eV in 0.5 eV in increments, 9000-9009 eV in 1 eV increments, 9010-9046 eV in 4 eV increments, 9050-9090 eV in 10 eV increments, and 9100-9300 in 25 eV increments. XANES maps were collected with a 1 ms dwell time and 2 µm steps using a motorised sample stage, and a micro-focussed X-ray beam to a spot size of 2 µm. XANES stack contained 275 000 pixels for raw and compost from Urban-3 or 150 000 pixels for raw and treated OWs from Agri-1 and Central-1 and 95 energies per pixel. Individual XANES maps were extracted as TIFF files from GeoPIXE™ and were imported into ImageJ v1.53 to be converted into a stack of TIFF images. This stack was then imported into Mantis 3.1.12 32 where PCA followed by cluster analysis were applied. 33, 34 PCA was used to find a reduced set of eigenspectra and cluster analysis was used to group spectroscopically similar pixels together. The average XANES spectra from each cluster were further analysed by LCF using the Athena software (SI-4).
Not provided.
Organic wastes (OWs) can be a common source of copper (Cu) contamination of agricultural soils. Here we conducted a comprehensive study of 22 raw and treated OWs sampled at 6 different full-scale OW treatment plants. Bulk XANES analysis findings indicated that the Cu oxidation state was subject to changes throughout the OW treatment process, mostly depending on the anaerobic/aerobic conditions prevailing in each treatment stage. These changes were independent of the OW origin (agricultural, urban or industrial). Cu­(I) prevailed in raw OWs and digestates (88–100%), whereas Cu­(II) dominated in composts (46–100%). Bulk EXAFS analysis confirmed these observations and revealed that Cu­(I) species in raw OWs and digestates consisted mainly of Cu­(I)-sulfide (76–100%), while Cu­(II) species (60–100%) in composts were Cu­(II)-citrate, Cu­(II)-carbonate and amorphous Cu­(II)-phosphate. Interestingly, we observed that anaerobic digestion was conducive to the formation of crystallized Cu­(I)-sulfides at the expense of nanosized and poorly crystalline Cu­(I)-sulfide species, and that the recalcitrant Cu­(I) species in composts was always crystallized Cu­(I)-sulfide. XANES imaging analysis revealed Cu­(II) species present in low proportions (2–4%) that were not detected using bulk XAS analysis in raw OWs and digestates. This demonstrated the potential of XANES imaging for probing minor species in complex matrices.
Author Etschmann, Barbara
Legros, Samuel
Basile-Doelsch, Isabelle
Brunetti, Gianluca
Levard, Clément
Rose, Jérôme
Howard, Daryl L.
Formentini, Thiago
Doelsch, Emmanuel
Doolette, Casey
Lombi, Enzo
Le Bars, Maureen
Chaurand, Perrine
AuthorAffiliation Recyclage et Risque
Australian Synchrotron
Université de Montpellier, CIRAD
ETH Zurich, CHN
Environmental Engineering Program
Regional University of Blumenau (FURB)
School of Earth, Atmosphere and Environment
Soil Chemistry Group, Institute of Biogeochemistry and Pollutant Dynamics, Department of Environmental Systems Science
CIRAD, UPR Recyclage et Risque
Future Industries Institute
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Keywords trace element
digestate
quantitative mapping
X-ray absorption spectroscopy
compost
copper sulfide
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Snippet Organic wastes (OWs) can be a common source of copper (Cu) contamination of agricultural soils. Here we conducted a comprehensive study of 22 raw and treated...
An initial large area survey scan of 7x4 mm for raw and compost from Urban-3 or of 8x2 mm for raw and treated OWs from Agri-1 and Central-1 was collected at...
Not provided.
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StartPage 14439
SubjectTerms Aerobic conditions
Agricultural land
Agricultural pollution
Agricultural wastes
Anaerobic conditions
Anaerobic digestion
Anaerobic processes
Anaerobic treatment
Composting
Composts
Copper
Crystallization
Engineering
Environmental Sciences
Environmental Sciences & Ecology
Heterogeneity
nanomaterials
Occurrence, Fate, and Transport of Aquatic and Terrestrial Contaminants
Organic waste treatment
Organic wastes
Oxidation
Pattern analysis
Scale (corrosion)
Soil pollution
Speciation
Species
Sulfides
Urban agriculture
Valence
Waste treatment
X-ray absorption spectroscopy
Title Bulk and Mapping Speciation Analyses Unveil the Pattern and Heterogeneity of Cu Species during Organic Waste Treatment
URI http://dx.doi.org/10.1021/acs.est.4c02887
https://www.ncbi.nlm.nih.gov/pubmed/39073989
https://www.proquest.com/docview/3098300771
https://www.proquest.com/docview/3086061548
https://www.proquest.com/docview/3153820659
https://hal.science/hal-04752939
https://www.osti.gov/biblio/2581451
Volume 58
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