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Rice cultivation requires high amounts of phosphorus (P). However, significant amounts of P fertilizer additions may be retained by iron (Fe) oxides and are thus unavailable for plants. At the same time, rice cultivation has a high demand for silicic acid (Si), reducing Si availability after short duration of rice cultivation. By studying a paddy chronosequence with rice cultivation up to 2000 years, we show that Si limitation, observed as early as a few decades of rice cultivation, is limiting P availability along the paddy soils chronosequence. Using near edge X-ray absorption fine structure spectroscopy (NEXAFS) in a scanning transmission (soft) X-ray microscope (STXM) we show release of available P was linked to a Si-induced change in speciation of Fe-phases in soil particles and competition of Si with P for binding sites. Hence, low Si availability is limiting P availability in paddy soils. We propose that proper management of Si availability is a promising tool to improve the P supply of paddy plants., (© 2022. The Author(s).)

Understanding P uptake in soil-plant systems requires suitable P tracers. The stable oxygen isotope ratio in phosphate (expressed as δ 18 O P ) is an alternative to radioactive labelling, but the degree to which plants preserve the δ 18 O P value of the P source is unclear. We hypothesised that the source signal will be preserved in roots rather than shoots. In soil and hydroponic experiments with spring wheat (Triticum aestivum), we replaced irrigation water by 18 O-labelled water for up to 10 d. We extracted plant inorganic phosphates with trichloroacetic acid (TCA), assessed temporal dynamics of δ 18 O TCA-P values after changing to 18 O-labelled water and combined the results with a mathematical model. Within 1 wk, full equilibration of δ 18 O TCA-P values with the isotope value of the water in the growth medium occurred in shoots but not in roots. Model results further indicated that root δ 18 O TCA-P values were affected by back transport of phosphate from shoots to roots, with a greater contribution of source P at higher temperatures when back transport was reduced. Root δ 18 O TCA-P partially preserved the source signal, providing an indicator of P uptake sources. This now needs to be tested extensively for different species, soil and climate conditions to enable application in future ecosystem studies., (© 2021 The Authors New Phytologist © 2021 New Phytologist Foundation.)

31 P nuclear magnetic resonance (NMR) spectra can be biased due to the hydrolysis of labile P species during sample treatment and NMR analysis. This paper offers an approach to circumvent this problem by performing sample preparation and analysis in 18 O-enriched medium. Heavy 18 O isotope atoms were introduced into the resulting artificial hydrolysis products. The NMR signal of 18 O-labeled P was shifted upfield relative to the unlabeled P nuclei in natural metabolites. This isotope shift enabled an immediate differentiation of artificial hydrolysis products from natural metabolites. Moreover, the hydrolysis products could be accurately quantified. Our data suggest that the extent to which artificial hydrolysis alters NMR spectra varies among different types of environmental samples. For instance, 72-84% of the detected monoesters in the organic soils of this study were actually artificially hydrolyzed diesters. By contrast, artificial hydrolysis products in the mineral soils used for this study accounted for less than 6% of the total monoesters. Polyphosphate was also hydrolyzed to yield 18 O-labeled products in algal biomass.

Neolithic and Bronze Age topsoil relicts revealed enhanced extractable phosphorus (P) and plant available inorganic P fractions, thus raising the question whether there was targeted soil amelioration in prehistoric times. This study aimed (i) at assessing the overall nutrient status and the soil organic matter content of these arable topsoil relicts, and (ii) at tracing ancient soil fertilizing practices by respective stable isotope and biomarker analyses. Prehistoric arable topsoils were preserved in archaeological pit fillings, whereas adjacent subsoils served as controls. One Early Weichselian humic zone represented the soil status before the introduction of agriculture. Recent topsoils served as an additional reference. The applied multi-proxy approach comprised total P and micronutrient contents, stable N isotope ratios, amino acid, steroid, and black carbon analyses as well as soil color measurements. Total contents of P and selected micronutrients (I, Cu, Mn, Mo, Se, Zn) of the arable soil relicts were above the limits for which nutrient deficiencies could be assumed. All pit fillings exhibited elevated δ15N values close to those of recent topsoils (δ15N>6 to 7‰), giving first hints for prehistoric organic N-input. Ancient legume cultivation as a potential source for N input could not be verified by means of amino acid analysis. In contrast, bile acids as markers for faecal input exhibited larger concentrations in the pit fillings compared with the reference and control soils indicating faeces (i.e. manure) input to Neolithic arable topsoils. Also black carbon contents were elevated, amounting up to 38% of soil organic carbon, therewith explaining the dark soil color in the pit fillings and pointing to inputs of burned biomass. The combination of different geochemical analyses revealed a sufficient nutrient status of prehistoric arable soils, as well as signs of amelioration (inputs of organic material like charcoal and faeces-containing manure).

Soil water status, which refers to the wetness or dryness of soils, is crucial for the productivity of agroecosystems, as it determines nutrient cycling and uptake physically via transport, biologically via the moisture‐dependent activity of soil flora, fauna, and plants, and chemically via specific hydrolyses and redox reactions. Here, we focus on the dynamics of nitrogen (N), phosphorus (P), and sulfur (S) and review how soil water is coupled to the cycling of these elements and related stoichiometric controls across different scales within agroecosystems. These scales span processes at the molecular level, where nutrients and water are consumed, to processes in the soil pore system, within a soil profile and across the landscape. We highlight that with increasing mobility of the nutrients in water, water‐based nutrient flux may alleviate or even exacerbate imbalances in nutrient supply within soils, for example, by transport of mobile nutrients towards previously depleted microsites (alleviating imbalances), or by selective loss of mobile nutrients from microsites (increasing imbalances). These imbalances can be modulated by biological activity, especially by fungal hyphae and roots, which contribute to nutrient redistribution within soils, and which are themselves dependent on specific, optimal water availability. At larger scales, such small‐scale effects converge with nutrient inputs from atmospheric (wet deposition) or nonlocal sources and with nutrient losses from the soil system towards aquifers. Hence, water acts as a major control in nutrient cycling across scales in agroecosystems and may either exacerbate or remove spatial disparities in the availability of the individual nutrients (N, P, S) required for biological activity. [ABSTRACT FROM AUTHOR]

Phosphorus (P) research still lacks techniques for rapid imaging of P use and allocation in different soil, sediment, and biological systems in a quantitative manner. In this study, we describe a time-saving and cost-efficient digital autoradiographic method for in situ quantitative imaging of 33P radioisotopes in plant materials. Our method combines autoradiography of the radiotracer applications with additions of commercially available 14C polymer references to obtain 33P activities in a quantitative manner up to 2000 Bq cm−2. Our data show that linear standard regressions for both radioisotopes are obtained, allowing the establishment of photostimulated luminescence equivalence between both radioisotopes with a factor of 9.73. Validating experiments revealed a good agreement between the calculated and applied 33P activity (R2 = 0.96). This finding was also valid for the co-exposure of 14C polymer references and 33P radioisotope specific activities in excised plant leaves for both maize (R2 = 0.99) and wheat (R2 = 0.99). The outlined autoradiographic quantification procedure retrieved 100% ± 12% of the 33P activity in the plant leaves, irrespective of plant tissue density. The simplicity of this methodology opens up new perspectives for fast quantitative imaging of 33P in biological systems and likely, thus, also for other environmental compartments. [ABSTRACT FROM AUTHOR]

Elemental contents in catchment headwaters are indicative of the load of nutrients and minerals cycled or released from ecosystems, yet little is known about natural colloids (1-1000 nm) and especially natural nanoparticles (NNP, 1-100 nm) as nutrient carriers in forested headwater streams. We hypothesize that the majority of P is bound to NNP in forest streams but that their size and composition varies for different forested headwater systems. Four forested sites in Germany and one in Norway, which differ in total P content, were sampled for stream water and analyzed for colloids. The samples were fractionated using field flow fractionation coupled to inductively coupled plasma-mass spectrometry and an organic C detector. The results showed that NNP and colloids from all sites could be separated into three distinct fractions (approximately 1-20 nm, >20-60 nm, and >60 nm). The elemental concentrations of P, organic C, Al, Si, Fe, and Mn in the fractions differed among the five sites. However, cluster analysis showed that each fraction had unique elemental signatures with different preferential P binding partners. Phosphorus was preferentially associated with Fe in the smallest size fraction, with an increasing contribution of organic-C-associated P as the fraction size increased. The largest fraction was dominated by clay minerals. Also, the data indicated that the relative contribution of the NNP and colloidal fractions for ecosystem nutrient supply rises as total P concentrations decline. The study highlighted the still underestimated importance of NNP for matter transport in forest streams and thus P cycling. [ABSTRACT FROM AUTHOR]

Stagnant water conditions may release phosphorus (P) in soil solution that was formerly bound to Fe oxides. To understand which P species are potentially involved, we obtained water extracts from the surface soils of a gradient from Cambisol, Stagnic Cambisol to Stagnosol from temperate grassland, Germany. These were filtered to < 450 nm, and divided into three procedurally-defined fractions: small-sized colloids (20-450 nm), nano-sized colloids (1-20 nm), and "dissolved P" (< 1 nm), using asymmetric flow field flow fractionation (AF4), as well as filtration for solution 31P-NMR spectroscopy. The total P of soil water extracts increased in the order Cambisol< Stagnic Cambisol< Stagnosol due to increasing contributions from the dissolved P fraction. Associations of C-Fe/Al-PO43-/pyrophosphate were absent in nano-sized (1-20 nm) colloids from the Cambisol but not in the Stagnosol. The 31P-NMR results indicated that this was accompanied by elevated portions of organic P in the order Cambisol > Stagnic Cambisol > Stagnosol. Across all soil types, elevated proportions of inositol hexakisphosphate species (e.g. myo-, scyllo-, and D-chiro-IHP) were associated with soil mineral particles (i.e. bulk soil and small-sized soil colloids) whereas other orthophosphate monoesters and phosphonates were found in the 'dissolved' P fraction. We conclude that stagnic properties affect P speciation and availability by potentially releasing dissolved inorganic and ester-bound P forms as well as nano-sized organic matter-Fe/Al-P colloids. [ABSTRACT FROM AUTHOR]

Understanding and quantification of phosphorus (P) fluxes are key requirements for predictions of future forest ecosystems changes as well as for transferring lessons learned from natural ecosystems to croplands and plantations. This review summarizes and evaluates the recent knowledge on mechanisms, magnitude, and relevance by which dissolved and colloidal inorganic and organic P forms can be translocated within or exported from forest ecosystems. Attention is paid to hydrological pathways of P losses at the soil profile and landscape scales, and the subsequent influence of P on aquatic ecosystems. New (unpublished) data from the German Priority Program 1685 ' Ecosystem Nutrition: Forest Strategies for limited Phosphorus Resources' were added to provide up-to-date flux-based information. Nitrogen (N) additions increase the release of water-transportable P forms. Most P found in percolates and pore waters belongs to the so-called dissolved organic P (DOP) fractions, rich in orthophosphate-monoesters and also containing some orthophosphate-diesters. Total solution P concentrations range from ca. 1 to 400 µg P L−1, with large variations among forest stands. Recent sophisticated analyses revealed that large portions of the DOP in forest stream water can comprise natural nanoparticles and fine colloids which under extreme conditions may account for 40-100% of the P losses. Their translocation within preferential flow passes may be rapid, mediated by storm events. The potential total P loss through leaching into subsoils and with streams was found to be less than 50 mg P m−2 a−1, suggesting effects on ecosystems at centennial to millennium scale. All current data are based on selected snapshots only. Quantitative measurements of P fluxes in temperate forest systems are nearly absent in the literature, probably due to main research focus on the C and N cycles. Therefore, we lack complete ecosystem-based assessments of dissolved and colloidal P fluxes within and from temperate forest systems. [ABSTRACT FROM AUTHOR]

Phosphorus (P) is an indispensable element for all life on Earth and, during the past decade, concerns about the future of its global supply have stimulated much research on soil P and method development. This review provides an overview of advanced state-of-the-art methods currently used in soil P research. These involve bulk and spatially resolved spectroscopic and spectrometric P speciation methods (1 and 2D NMR, IR, Raman, Q-TOF MS/MS, high resolution-MS, NanoSIMS, XRF, XPS, (µ)XAS) as well as methods for assessing soil P reactions (sorption isotherms, quantum-chemical modeling, microbial biomass P, enzymes activity, DGT, 33P isotopic exchange, 18O isotope ratios). Required experimental set-ups and the potentials and limitations of individual methods present a guide for the selection of most suitable methods or combinations. [ABSTRACT FROM AUTHOR]

Whereas many researchers still approach Terra Preta (TP) as a soil category, new evidence suggests that TP refers to a directional grading of soil property changes (i.e., color, pH, nutrients, etc.) within human-made soils, originating from human activities in pre-Columbian times. Currently, most TP research focuses on the Brazilian part of the Amazon basin, but only little information is available on TP soils in the Colombian Amazon. Here, we sampled four TP and surrounding soils in the Colombian Amazon region at different soil depths and analyzed them for (i) general soil properties such as color, pH and texture, (ii) soil organic carbon and black carbon (BC) contents, the latter using benzene polycarboxylic acids as molecular marker, (iii) phosphorus availability based on sequential fractionation, and (iv) microbial residue contents using amino sugars. Our data from Colombia's middle Caquetá River and Leticia confirmed that SOC, BC, and total P were present in significantly higher concentrations in the TP areas than the surrounding soils, while pH values and microbial residue contents were unchanged. The enrichment of P forms comprised both easily extractable and stable P pools, which both dominated to a different degree, both in TP and adjacent soils. The different degree of SOC, BC and P enrichment suggests different amounts of waste disposal by the ancient populations at different TP sites, now warranting further research for reconstructing ancient population sizes from TP chemical analyses. [ABSTRACT FROM AUTHOR]

• Nanocolloids dominated soil colloids in Acrisols. • Fine and medium-sized colloids dominated soil colloids in Terra Preta soils (TP). • Elevated pH and Ca2+ conc. correlated with SOM involvement in colloid formation in TP. • Enriched water-extractable and colloidal P in TP. Amazonian Dark Earths (or terra preta de índico) are known as highly fertile soils that can maintain elevated crop yields for centuries. While this fertility was frequently ascribed to the presence of black carbon, the availability and colloidal binding of major nutrients received limited attention. We examined the size distribution and the elemental compositions of water-dispersible colloids (WDC) in both forested and cultivated Terra Preta topsoils (0–10 cm, Anthrosols), as well as in their adjacent non-Terra Preta controls (Acrisols) via asymmetric flow field-flow fractionation (FFF). Liquid-state 31P-nuclear magnetic resonance (NMR) spectra, black carbon content, and scanning electron microscope (SEM) images were also obtained. We found that WDC in Terra Preta soils contained a significant proportion of organo-mineral associations in the size range 30–300 nm, whereas, in contrast, water-dispersible nanoparticles with a diameter < 30 nm were dominant in the adjacent Acrisols. The shifts to larger WDC sizes in the Terra Preta soils went along with elevated pH values, as well as with elevated contents of Si, Al, Fe, Ca and organic matter-containing particles. Also P concentrations were enriched in both the water-extractable phase (WEP) and WDC extracts of Terra Preta soils relative to the adjacent Acrisols. We assume that the higher pH values and Ca ion concentrations promoted the involvement of soil organic matter (SOM) into the formation of larger-sized colloids consisting of kaolinite-like clay minerals, iron oxides and Ca ions in the Terra Preta soils. The elevated content of Ca in Terra Preta soil colloids may also contribute to the retention of P, likely via bridging of anionic P like orthophosphate to SOM. Preventing soil acidification is thus not only to be recommended for Acrisols, but also for maintaining colloidal structures and related fertility in Terra Preta soils. [ABSTRACT FROM AUTHOR]

• Elevated pH promoted colloid formation in calcareous soils. • Ca acted as the bridging agent for colloidal formation. • Colloids in mineral soil layers originated from surface organic layers. • Retention of dissolved P accounted for P accumulation in deeper soil layers. • Colloids were more responsible than soil electrolytes for P loss to deeper soil horizons. Dissolved and colloidal phosphorus (P) represent the mobile P fractions in soils, but their role in P cycling in forests is still largely unclear. In this study of four calcareous forest soil profiles, the elemental compositions of different size fractions of water dispersible colloids (WDC) were investigated by asymmetric field flow fractionation. Nuclear magnetic resonance spectroscopy (NMR) was applied to identify the organic P compounds in soils, WDC, and soil solutions. Carbon was the dominant element in WDC of all soil horizons, including mineral soils that were rich in Ca or Si. Although chemical composition of P varied dramatically with increasing depth, the colloidal P composition remained unchanged. This contrasting difference between mineral soil and its WDC fraction indicated that the colloids were not locally generated but originated from the overlying organic soil horizons. Carbonate minerals were unlikely involved in colloid formation under acidic condition. Instead, Ca2+ probably drove colloid formation by bridging organic matter, including P-containing compounds released from litter degradation. Colloid formation was influenced by climate, vegetation, and soil characteristics. No dissolved P was detected in deeper mineral soil horizons due to efficient retention by Ca minerals. Colloidal P was still present in deeper soil layers and thus of significance for potential P vertical transfer. [ABSTRACT FROM AUTHOR]