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Plant Soil (2016) 401:93–107

DOI 10.1007/s11104-015-2519-0

REGULAR ARTICLE

Pig slurry acidification, separation technology and thermal
conversion affect phosphorus availability in soil amended
with the derived solid fractions, chars or ashes
Wibke Christel & Sander Bruun & Jakob Magid &
Witold Kwapinski & Lars Stoumann Jensen

Received: 17 December 2014 / Accepted: 13 May 2015 / Published online: 24 May 2015
# Springer International Publishing Switzerland 2015

Abstract declining with time, indicating soil P fixing reactions.
Aims The aim was to study effects of slurry acidifica- Chars and ashes on the other hand showed lower initial
tion, separation technology and thermal processing on P availability, but remained constant or increased slight-
the availability of P in soil amended with the solid ly with chars yielding P availability similar to solids
fraction of pig slurry. after 12 weeks.
Methods Acidified and non-acidified slurry were sepa-
rated using different technologies: screw press (SCR),
decanting centrifuge (DEC) and drainage after chemical Keywords Decanter centrifuge . Screw press . Slurry
pretreatment (CHE). Solids and pyrolysed (400 °C or flocculation . Pyrolysis . Combustion . Diffusive
600 °C, char) or combusted (625 °C, ash) solids were gradients in thin films (DGT)
applied to two soils, with triple superphosphate (TSP) as
a reference. Soil P availability was determined over
12 weeks using diffusive gradients in thin films (DGT).
Results The initial availability of P from DEC and CHE Introduction
solids was similar to TSP in both soils. After 6 weeks no
significant difference was observed between DEC solids Slurry separation is one management option for distribut-
and DEC chars. Acidification did not significantly affect ing and utilising the liquid and solid fraction of pig manure
P availability in the solids-amended soils over time, but in a more environmentally friendly way that is better suited
it did affect P availability with the thermally processed to plant demand for individual nutrients than the applica-
materials. tion of unprocessed slurry. The separated solid fraction is
Conclusions Application of separated pig slurry solids rich in particulate organic matter and nutrients, which may
generally increased soil P availability initially, but precipitate during storage and be captured during floccu-
lation or be bound in particulate organic matter and mi-
Responsible Editor: Tim S. George.
crobial residues (Hjorth et al. 2010; Peters et al. 2011).
Slurry separation is used on many large-scale animal farms
W. Christel : S. Bruun : J. Magid : L. S. Jensen (*) in livestock-intensive regions across Europe, i.e., in
Department for Plant and Environmental Sciences, University
Catalonia, Brittany, Flanders and the Netherlands; in
of Copenhagen, Thorvaldsensvej 40, DK-1871 Frederiksberg
C, Denmark Denmark around 3 % of all slurry is separated
e-mail: lsj@plen.ku.dk (Birkmose, pers. comm.). The essential nutrient phospho-
rus (P) is of great interest, since recycling of the solid
W. Kwapinski
fraction would reduce environmental issues associated
Carbolea Research Group, Department of Chemical and
Environmental Science, University of Limerick, Limerick, with surplus P on livestock-intensive farms and make
Ireland recipient farmers less dependent on mineral P fertiliser,

(Kumaragamage et al. using poultry manure as the fractions are also highly dependent on the separation tech. 2012) or in the types of minerals present in the ashes Manure solids (Huang et al. Italy) and iii) chemical their applicability. 2013). pyrolysis conditions (Tsai tion (Kai et al. been identified as key factors controlling P dynamics in The physicochemical properties of the solid and liquid soils in a related study. Besides energy production. large-scale facilities in operation in the UK and the Denmark in the spring of 2012: (I) untreated pig slurry and Netherlands. 2013). However. 2009). Germany). 2014). at farm scale using three different separation technologies: It is not yet clear.). With such a nology used (Jørgensen and Jensen 2009). while also stabilising it for long-term storage thermal processing of one of the solid fractions. Firstly. However soil properties.94 Plant Soil (2016) 401:93–107 thereby contributing to a more sustainable use of this non. flocculation using polymers). whereas more advanced slurry sepa.. separation and field applica. approximately 12 % of all animal slurry in (Christel et al. but mineral phase and presence of sorption sites. the high temperatures dur- ing processing have been shown to decrease the easily available fraction of the contained P through changes in Materials and methods the char’s biochemical structure (Cantrell et al. 2011. 2011). sulphuric acid (H2SO4). Thermal processing has so far mainly been employed with high Two pig slurries from fattening pigs were collected from a dry-matter manures such as poultry litter. methods and scales. 2013. Tsai et al. gasification and com. soil amendment have investigated the effect of just one Slurry acidification is a treatment option that can be slurry treatment option at a time: either acidification used to minimise ammonia volatilisation in the animal (Roboredo et al. pers. and transportation. derived products and their potential use as a P-fertilising renewable resource. with the current proliferation (II) pig slurry that had been continuously acidified to across Europe of anaerobic digestion for biogas and pH 5. Based on extractions. amendment (Waldrip-Dail et al. Few studies on pig manure-derived mate- European countries its application is highly scattered. have also this proportion is expected to increase. 2010.5 in the animal house through the addition of subsequent liquid–solid separation of the digestate. alone or. such as pyrolysis. In rials have addressed the influence of soil properties 2014. However. Popovic et al. the discussion concerning interac- mainly used on livestock farms in Denmark due to very tions with the soil after amendment has been limited to one strict ammonia emission regulations. pretreatment (CHE. 2015. 2012. 2012) or combustion temperature (Thygesen et al. ther. 2009. various solid materials derived from pig slurry. i. Cantrell et al. Acidification et al. however. technology and thermal treatment (pyrolysis or combus- ration techniques ensure a high P separation coefficient tion) on P availability in soils after amendment with (Kumaragamage et al. . 2005. if the change in P availability in soil over time has 2015). ii) a treatments of manure products could potentially improve decanter centrifuge (DEC. as organic P fertiliser in two different soils and then test 2007. Peters et al. Slurry acidification technologies are currently been investigated at all. Petersen et al. Börger BS50. 2012). affects the chemical and physical properties of the pig 2011). 2011). Thygesen et al. with several research farm at the Grønhøj Pig Trial Station in Karup. Pieralisi. Both pig slurries were separated mal processing of solids is expected to increase. Wnetrzak whether the effect of acidification was preserved after et al. has also been suggested as a pact on the potential use of the respective solid fractions suitable way of enriching P in the product (Møller et al. Most studies of different manure. it is difficult to draw a general (<250 μm or even <10 μm) in particular is crucial for P conclusion on the combined effect of the above-mentioned content in the dry-matter rich fraction (Masse et al. 2012). slurry separation by different technologies had an im- bustion of the dried solids. Hjorth et al. the Denmark was acidified (Birkmose. whereas in other soil type only. whether further combined i) a screw press (SCR. 2008. comm. separation in the solid fraction. Simple mechanical techniques are The objective of the current study was to investigate usually rather inefficient at retaining the smallest particles the combined effect of slurry acidification. Ro et al. The perfor. 2008.e. fragmented collection of results from greatly varying ma- mance with respect to separation of the smallest particles terials. thermal processing of the the aim was to examine whether acidification prior to solid fraction. these studies either charac- slurry and the resulting fractions obtained by subsequent terise P fractions in the resulting manure-derived products slurry separation (Sommer et al. the separation technology used house and during storage. slurry treatment processes. 2012).

the dried fractions were pelletised (JS Aarhus. The pellets were soil (B) was collected from the long-term Nutrient slowly pyrolised (heating rate 20 °C min−1) in a self. covered with a The water-extractable share of P in the DEC-Char600 tight-fitting lid and frozen to −18 °C for storage within was approximately 2 % of total P. Denmark (56° 08′ N. soil (A) was sampled from an arable field near the city of Subsequently. hydrogen peroxide (1 mL 15 % H2O2) and field soil with a bulk density of 1. tion study (Christel et al.25 m thick layer of fibre material until an approximate pH and (B) a sandy loam with a neutral soil pH. Ash was found to be extractable in water (1:60 solid:water Shortly before experimental use. granules were also crushed and coarsely ground. tions were collected in plastic buckets. providing two different ash materials.Plant Soil (2016) 401:93–107 95 followed by drainage on a filter band separator (AL-2 Subsequently total P (Table 1) was analysed by inductively model 812P. mainly Ca(H2PO4)2 • H2O) fertiliser. from a plot that had not received any reactor was evacuated for oxygen at low temperatures in P fertiliser since 1964. soils were selected for this incubation study that varied in ing slightly preheated ambient air (<30 °C) through a both texture and pH: (A) a sandy soil with a strongly acidic 0. pellets were disintegrated by coarse grinding. (2009). Finely ground aliquots (50–70 mg) of the chars. order to be able to weigh off a representative. The drying was necessary in processed DEC-materials is extractable in citric acid. polymers: Praestol K133L and coupled plasma optical emission spectrometry (ICP-OES. Ireland. 16 h shaking).5 mL ha−1 if the materials were incorporated into the top 5 cm of 69 % HNO3). United States of America) for un. two Danish agricultural separation (DEC. pH and P availability of the sampled soils are manure solid feedstock remained for one hour at a peak given in Table 2. Perkin Elmer. 12° 17′ E). Phosphorus fertiliser as the reference treatment The origin and a detailed description of the slurries and solid fractions (for abbreviations see Table 1). Denmark). Before soil amendment. thoroughly mixed and subsequently moistened . Details on to enter the reactor. Denmark (55° the laboratories of the University of Limerick. Based on the findings of Christel each solid fraction was defrosted and subsequently dried et al. 2014). the procedure described in detail by Hansen et al. whereas it ranged between 12 % and level (see below). but pyrolysis gases could escape. Ontario. with a in Sommer et al. The sandy gravimetrical water content of 13 % was attained. The 40′ N. was used as a total P was below 5 % of total P for the non-acidified reference treatment and applied at the same target P fresh solid fraction. the char materials combusting the pellets in a laboratory-scale fur. but small mass needed as amendment for soil incubation. Denmark.5 L capacity in University of Copenhagen in Taastrup. Fredericia. 38 kg P ashes and dried solids were digested in nitric acid (2. whereas no P in DEC- 3 days of sampling. United Kingdom) at 625 °C until constant mass. as A commercially available granulated triple superphos- well as their (bio)chemical characterisation can be found phate (TSP. over 50 % of total P in the thermally at 80 °C for water removal. a large aliquot of mass ratio. no air was able and had therefore reached a very low P status.& DECacid-Solids) were dried by blow. The Netherlands). dried soil. Denmark). Before soil application. (2015). nace (Lenton. During pyrolysis. K144L (Demols Inc. Pyrolysis and combustion of the manure solids Soil properties In the Bygholm Research Centre of Aarhus University Based on the experience acquired from an earlier incuba- (Horsens. Ash was produced from the same dried and sieved (2 mm). After sampling from the 0–25 cm horizon temperature of 400 or 600 °C. Optima 5300 DV. the TSP 29 % for the acidified solids (Sommer et al.0 g of air- system (CPI International. but had been continuously cropped the early heating phase. 2015). The respective hydrofluoric acid (200 μL 49 % HF) in a ModBlock mass of treatment dry matter was mixed into 10. 9° 59′ E).3 g cm−3). The the texture. Depletion Trial (NDT) on the research farm of the constructed bench-periodic reactor of 1. resulting in four different of the agricultural fields. Canada) using treated and acidified slurry respectively). the bulk soil samples were air- char samples in total. The solid frac. while the loamy Trading ApS. (2014). The water-extractable share of P content of 173 mg g−1 (Table 1).. (Table 3) in all treatments (corresponding to ca. the solid fractions from DEC. Dry matter Incubation set-up loss during pyrolysis and combustion was determined and the respective char yields and ash content are given in The aim was to use the same target P application rate Table 1.

7) (35. (CON) and soil with triple superphosphate (TSP) were ready described in Christel et al. 2013). char and ash materials applied P in comparison to traditional soil P tests listed in Table 1 were incubated in the pH-neutral sandy (Mason et al.0 7. 2013.8) a average Olsen-P (Olsen et al. in italics) of the six solid slurry fractions peratures (400 and 600 °C) and ash products after combustion (3 control+3 acidified). three blank centrifuge (DEC & DECacid) plus the derived chars DGT devices.3) B sandy loam 16. and the (625 °C).8 TSP Triple superphosphate (reference) 173 with purified water (MilliQ.6 (26. United Kingdom) were applied several times materials: all the treatments separated by the decanting during incubation. This method was chosen as it has compensated for by the addition of purified water. Three gradient in thin films (DGT) technique replicates were prepared for each type of sample.0 17. filtered by Millipore.0 67.6 (55.7) (10.5 w/w % for the Soil phosphorus availability testing with the diffusive sandy soil and 19.0 w/w % for the sandy loam. As al. technique (e.2 and ashes (DEC(acid)-Ash). Commercially loam (B).2 (7. separated by the given technology.0 53..2 9.4 89.6 DEC Decanter centrifuge Control 20. but still well- aggregated and aerated soil was different for the two soils due to the different textures of the soils: 16.6 21. water content needed to obtain a moist. Six et al. Davison and Zhang 2012.4) 39.1 17. the gravimetrical prepared for both soil types as reference treatments.g.2) (38.1 SCRacid Screw press Acidified 5.3 (4. For each sampling time.. 18.4 40.. which were placed in incubation con- (600 °C pyrolysis temperature: DEC(acid)-Char600) tainers without any soil or amendment.1 48.8) CHEacid Flocculation + drainage Acidified 11.2 6. were included Table 2 Characterisation of the soils (A & B) used for incubation Soil Soil texture clay silt sand pH Olsen-Pa CDGTb [w/w%] [w/w%] [w/w%] (in 0.8 5. For the sandy soil with low pH (A). gravimetrically-determined individual water loss was 2014) was applied. Six et al.8 (2. as well as P content in the reference mineral fertiliser Samples Separation method Slurry treatment -Solids -Char400 -Char600 -Ash drying pyrolysis pyrolysis combustion 80 °C 400 °C 600 °C 625 °C mg P g−1 DM−1 mg P g−1 DM−1 yield (w/w% of DM) SCR Screw press Control 7. n=4 for soil B).1 DECacid Decanter centrifuge Acidified 8.0 87. partly covered by a To determine changes in available P over time.01 M CaCl2) [mg P kg−1 soil] [μg PO4-P L−1] A sand 6. standard deviation is given in parentheses b average CDGT of control treatment (non-amended soil) from all sampling times during the incubation period (n=15). 1954) of the non-amended soil (n=3 for soil A. the DGT lid at room temperature (22 °C±3 °C). the available-DGT devices (DGT Research Ltd. The samples were incubated in darkness.0) CHE Flocculation + drainage Control 20. standard deviation is given in parentheses . Once a week.8 155 (56. (2014). been proposed as a better predictor of plant response to All 12 different manure solids. number of amendments was reduced to six different Lancaster.4) (13.0) 262.96 Plant Soil (2016) 401:93–107 Table 1 Phosphorus (P) content in the dry matter (DM) and yield DEC(acid)-Solids-derived char materials at the two pyrolysis tem- (w/w% of feedstock DM. Soil without any application MΩ) to the desired water content for incubation.

5000. Incubation sampling was performed DGT devices were removed.. 3. After another were applied five times during incubation: after 24 h minimum period of 24 h. the gravimetrical (Zhang et al.0 % for the sandy loam during 10−6 cm2 s−1) was provided by the DGT supplier DGT application. soil without any amendment (CON) and soil with sampler (5027. connected to an auto- ments.5 mL of 1 DECacid) and their derived char and ash. The iron- fractions separated by decanting centrifuge (DEC & containing binding gel was put into 1. Subsequently. Denmark). 0.0 % for phosphate in the DGT gel at 22 °C (D = 5. 1999).57 · the sandy soil and 27. FOSS. The control treat.5. The diffusion coefficient for water content was therefore increased to 23. the CDGT from the respective P-treated soil in order to rials. For all the treatments with solid surface with MilliQ-water and opened. before carefully pressing the DGT device onto the The P-fertilising effect of the soil amendment is there- rest of the soil in the incubation container. All P captured in TSP addition were sampled on all five occasions during the binding gel was assumed to be eluted in nitric the incubation period. acid and therefore an elution factor of 1. were very different (Table 2). 1):   μg PO4 −P C DGT ðsoil amended with P sourceÞ−C DGT ðcontrol soilÞ Δ C DGT L ΔC DGT −index ¼ ¼   ð1Þ ΔPtotal mg P total P added kg soil pH measurements in soil-amendment mix Statistics After removing the DGT. in order to facilitate proper application of the present the resulting increase in P availability only. United Kingdom). Radiometer. of thermal treatment were considered as discrete .5 mL purified water (MilliQ) at a ratio of 1:10. After equilibration for a minimum of 30 min. increased to obtain a thin water film on the surface. Denmark). By DGT method (Hooda et al. reduced for the other treatments: the soils amended with Samples were stored refrigerated (5 °C) before PO4- manure fibre fractions (SCR(acid) & CHE(acid)) were P analysis on a Flow Injection Analyser (FIAstar measured in weeks 0. and type as well as temperature (PHM 210 lab pH meter. the dividing by the amount of total P applied. even after amendment of char or ash mate. the gel was removed from (Bweek 0^) and 1 week. After fore expressed as absolute increase in CDGT per P added 24 h’ application time at room temperature. three DGTs molar nitric acid (HNO3) for elution. 2014). The concentration of P in the soil solution at the which is necessary to ensure good contact and hence interface between the DGT filter and soil matrix diffusive transport of P between the soil solution (CDGT) was calculated from the P mass captured in phase and the DGT device. the as ΔCDGT-index (Eq. acidification. pH was measured in the supernatant using a pH meter separation technology. rinsed on the filter destructively over time. the water con. As the CDGT of the two unamended soils (controls) ration (>80 % of water-holding capacity) in all treat. 6 and 12 weeks after set-up.5 mL of the acid was diluted with However. Lancaster. the acid and 0. to secure sufficiently high water contents near satu.01 M CaCl2 solution was Linear models were used to carry out the analysis of added to the wet soil mix to reach a solid–liquid ratio of variances (ANOVA) to evaluate the treatment effects on 1:2. the DGT binding gel and Fick’s law of diffusion vious study (Christel et al. Denmark). they were subtracted from ments. These moisture levels were chosen (DGT Research Ltd.Plant Soil (2016) 401:93–107 97 in the analysis. et al. unpublished results) was used for the calcula- tent in the respective incubation cups had to be tion of P mass recovered in the eluted binding gel.. 1998). treatments (Table 3) were also taken into consideration. where soil. the number of DGT application times was 4. the the ΔCDGT-index and pH. FOSS. 3 and 6 only. As described in a pre. the slight soil was mixed and some soil paste was directly deviations from the target P amendment for the various smeared onto the filter layer of the DGT device.0 (Christel One day before DGT application.

Eq. CHE 60 When comparing the individual DEC treatments. as thermal treatment in itself also mg P kg−1 soil−1 had a significant effect on the ΔCDGT-index. For the loamy soil B. the Tukey rably large standard deviations in week 6 caused the test was used. ments. on the ΔCDGT-index and pH majority of sampling times (weeks 1. a lower ΔCDGT-index of below 0. For any statistical differences to be re- increasing effect to be statistically insignificant. however.1. while incubation time was a quanti- and TSP resulted in a significant increase in the ΔCDGT- tative variable. the in- crease in P availability after char or ash applications SCR 52 was lower than after treatment with solids or TSP. index. factor separation technology. soil B. For multiple comparisons. Char600 and –Ash in both soils). in weeks 1. weeks 3 and 6. ΔCDGT-index between the -Char600 and -Ash-treat- nure solids and the TSP had a higher initial ΔCDGT. All time were also found to have a significant effect on the amendments resulted in a positive ΔCDGT-index. DEC(acid)-Char400 in week 3 in soil B. the effect of the treatment.. .0. but decreased continuously during the initial In the second half of the incubation period (weeks 6– incubation phase. the ΔCDGT-index after addition of DEC(acid)-Solids tive of soil type. dex. additional interactions were identified with the ly different from 0 for all treatments (especially DECacid. ferred to as significant in the text.001). all SCRacid 51 materials derived from the non-acidified fraction (DEC- DECacid 63 77 60 76 Solids/-Char600/-Ash). For the solids. Additionally. the ΔCDGT-index around up to four times greater (Fig. 1) in the amended sandy soil A was generally separated by SCR or CHE however. The ma. 6 and 12 in soil A. al. both time and the different from TSP amendment in both soils. the DEC(acid)-Char400. compared to the non-acidified 2011). the acidified solids (DECacid- CHEacid 61 Solids) and TSP increased the ΔCDGT-index significant- TSP 59 ly throughout the whole incubation period compared to the unamended sandy soil A. Accordingly. R Development Core Team was generally observed.98 Plant Soil (2016) 401:93–107 Table 3 P application rate in comparison to the anticipated 59 mg interaction of time with thermal treatment were found P kg−1 soil−1 (see Table 1 for abbreviations) to be significant factors in the statistical models for the Treatment -Solids -Char400 -Char600 -Ash two soils. very different trends in the ΔCDGT-index solids. only the DEC-Solids. Acidification and its interaction with icant in the ANOVA of the linear model (P<0. espe- DEC 55 61 56 54 cially at the beginning of the incubation. The tendency of lower ΔCDGT-index for materials de- Results rived from acidified slurry was only statistically signif- icant in some cases (DEC(acid)-Solids in week 1 in both ΔCDGT-index soils. The thermally processed materials and DEC-Char400 (only amended to soil B) and resulted in a fairly stable ΔCDGT-index over the whole -Char600 was even higher than or not significantly incubation period. In though for some weeks it was not statistically significant. ΔCDGT-index in both soils in the statistical model. 12). All data were analysed using the statistical the DECacid-Solids and all the materials derived from it software R (Version 3. At the i.05. DEC-Char600 variables (factors). This tendency.e. type of amendment. The effect of the soil was only statistically significant for CHE(acid)-Solids in as a discrete variable was also found to be highly signif. DEC(acid)-Ash The increase in P availability (expressed as ΔCDGT-in. 1-B1 and the non-acidified counterparts. stabilising after 3 to 6 weeks irrespec. no significant differences were observed in for all DEC-derived materials were observed. However. With respect to thermal conversion of the manure Over time. B2) during the experimental period. 1-A1 and A2) was usually higher for the acidified solids compared to compared to the amended sandy loam B (Fig. 3 and 12 in both soils). index in the period from week 1 to week 12. 3 and 12). DEC- was tested in a one-way ANOVA for each sampling time Ash significantly increased ΔCDGT-index. the p-value had to be With slurry acidification. but compa- and soil separately. DEC(acid)- Char600 in weeks 1. independent of soil type or slurry acidification. counterparts (DEC(acid)-Solids in week 3 and -Char400 treatments week 6 in soil B being the only exceptions).

only the following treatments compared to the DEC(acid)-Solids. The soil pH.Plant Soil (2016) 401:93–107 99 Fig. but rather at the same level or even higher amendments. statistically separation (CHEacid-Solids) was not significantly significant differences between the manure-derived lower. However. all the chars and ashes are shown on the right (A2.and pH. for treatment abbreviations see Table 1 The manure solids. Note the different y-axis scaling for the two soils. the ΔCDGT-index af. manure-derived treatments caused the pH to rise in both ter amendment of the acidified fraction after CHE soils A and B. a decrease in soil incubation (see Fig. B2). sandy soil (A). In soil A. With respect to the effect of soil amendment on ΔCDGT-index after amendment of SCR(acid). On the other hand. 2) and time was also identified as the factor in processing. DECacid-Char600 and the DEC(acid)-Solids-treatments (insignificant). In contrast. over the incubation period relative to the amendment of total P Only DEC(acid)-Solids. no change was observed after amendment with TSP CHE(acid)-Solids was generally in the same range as compared to the non-amended control. The factor separation pH was observed within the first few weeks of incuba- technology. also showed a generally decreasing trend of the ΔCDGT-index within the first 6 weeks of the Irrespective of soil type or treatment. ashes) to the (A) sandy soil (pH~5) and the (B) sandy loam Error bars represent the standard deviation of the mean (n=3). chars. also in interaction with time or thermal tion (Fig. 1-B1). but there were no consistent. had a significantly higher pH at the given times: DEC- the amendment of the CHE. separated by the SCR or CHE pH of the amended soils during incubation technique. DEC-Solids in resulted in a lower ΔCDGT-index in comparison to week 1 as well as DEC-Solids. was found to have a significant effect on the linear models having the most significant effect on the ΔCDGT-index in the linear model for soil B. 1. B1). −Char600 and -Ash were amended to the (ΔCDGT-index) in the form of the manure fraction products (solids. DECacid-Ash in week 3.and SCR(acid)-Solids Solids and DEC-Char600 in week 0. For (pH~7): the manure solids and TSP treatments are shown on the left calculation refer to Eq. 1 Increase in P CDGT (relative to the unamended control soil) (A1. all the DEC(acid)-Solids. .

as the soil had not been pre-incubat. but this acidi- fication effect disappeared over time (a significant effect of acidification in interaction with time in the statistical mod. nificantly. The pH mean (n=3). B1).1 initially (week 0). no significant pH differences could be determined in soil A. For treatment abbreviations see Table 1 of the unamended control soil is displayed in all figures as the For the sandy soil A (Fig. all DEC. 2 Soil pH (in 0. Error bars represent the standard deviation of the derived chars and ashes are shown on the right (A2. based on a CHEacid-Solids in weeks 3 and 6. compared to a pH of el). This drop in pH could possibly be an Char600 treatments were able to increase soil pH sig- effect of nitrification.7 tion technology and acidification in the statistical mod- for the unamended control treatment. 2-B1 and B2) decreased by approximately 0. . Note the different y-axis scaling solids and TSP treatments are shown on the left (A1. soil pH Solids in week 3 (significant effect of the factor separa- stabilised after 6 weeks’ incubation at approximately 4. stabilising at around In this study changes in soil available P over time was pH 6.5. compared to the control and TSP treatment in ed. Only DEC(acid)-Solids. After 12 weeks’ incubation. B2). Discussion el). In weeks 6 and 12. −Char600 and Ash were materials to the (A) sandy soil and the (B) sandy loam: the manure amended to the sandy soil (A).100 Plant Soil (2016) 401:93–107 Fig. for the two soils. as well as SCR. number of recent studies. The review by Degryse et al. 2-A1 and A2). Soil phosphorus availability testing by the DGT The pH of the control treatment of the loamy soil B technique (Fig. acidified slurry was (insignificantly) lower.01CaCl2) after amendment of the manure reference. Initially the pH in soil amended with materials from soil B. only the DEC(acid)- 5.7 pH units within the first 3 weeks. The only exceptions to the general liming effect quantified by the DGT technique (Davison and Zhang of the manure-derived materials were the treatments 2012) as a proxy for plant P availability.

Gichangi et al. Furthermore. confirmed both the DGT ranking but also the propor. 2010) and maize (Six observed a reduced P adsorption after the addition of an et al. which will be discussed in activity of soil extracts differed significantly from that of more detail in the following section about the effect of soil plant P. DGT was a better predictor agreement with the decrease in P availability after amend- than extraction (Olsen P. 2012). water soluble) and resin tech. 2006. immobilisation of labile P in soil microbial biomass soil P that is plant accessible (Mason et al. Roboredo et al. which highlights the relevance of the co-applied organic tion which is accessible to plants. which was expected to be boxylate anions. 2012). TSP. since the specific matter. studies that the DGT technique samples the soil P frac. organic P proach as in the current study. which caused a pattern of P avail- with various manure types (poultry. 2013) and of P uptake by barley (Tandy 1999). indicating that extracts only partly measure the type. the ability of the DGT method to predict decreased in all the above-mentioned studies in the first soil P availability and plant uptake has been evaluated in few weeks after soil incorporation. the high initial availability might amendment with the solid fractions was in accordance have been due to a high proportion of easily available P with a number of other studies. as P speciation according to their modified Hedley fraction- Effect of time during incubation ation did not differ significantly between the first and final sampling. tionation (Hedley et al. correlated with CDGT to some extent (Christel et al. but ment. 2014). 2015). (2012) conclude that highly concentrated. no generally valid effect of time was by studying P in different fractionation classes in the observed in the case of the thermally-processed . 2013. if diffusion. whereas added labile inorganic P study from our group (Lemming. In this study the plant P uptake clearly lated formation of organic P forms in soils. initial incubation phase. the temporal pattern of P availability after applica. He et al. The solubilisation such as the exudation of protons or car. However. pers. Several studies have et al. the results of the present study did not As already reported in a previous study (Christel et al. Roboredo et al. phosphorus availability. Consequently Malik et al. 2009. cattle. (2012) also indicate a (re-)mineralisation of intermediately tional P availability level of amendments. wheat (Mason et al. These results are in a number of recent studies. 1999. 1998). Santner et al. caused by the addition of the manure solid fractions. Nevertheless. Gichangi et al. Reddy et al. or better than. rice (Six et al. The pronounced increase in P availability after (12 weeks). mainly we have good indications that C DGT is valid for labile and non-labile organic P was formed during 8 weeks predicting plant P availability from a yet unpublished of soil incubation. 1982) was used to detect changes ity test. 2014). 2014. water-extractable inorganic P. ment of the manure solids and the TSP observed within the niques of relative yield P response of tomato (Menzies first 3 weeks in the current study.Plant Soil (2016) 401:93–107 101 (2009) showed conclusively that DGT performs as well amended soils. is controlling nutrient supply. 2011).) where (KH2PO4) was primarily converted into non-labile inor- we tested how thermal drying of sewage sludge affected ganic P (Malik et al. but not of wetland organic P source (Ohno and Crannell 1996. 2009. Waldrip-Dail et al. suggest a return to the high initial level of P availability 2014). and not mass flow or active P in inorganic and organic P pools of decreasing lability. After the addition of other such data are not present in the current study. immobilised P after a total of 26 weeks’ incubation. in which soil was amended (Christel et al. comm. goat and pig) ability similar to the pattern observed after amendment of (Reddy et al. application of goat manure with or without TSP amend- ity. but also including a pot sources may release P slowly over time due to the stimu- trial with barley. whereas no such effect on P sorption in soil could et al. followed by a decline. but tion of the dried solids differed from thermally processed then the incubation duration was also less than half as long fractions. batch extractions as a soil P availabil. in order to validate whether our time increase in microbial biomass P within the first 4 weeks of courses of CDGT are valid as index for plant P availabil. significantly different in most soils. Six may contribute to reducing the easily extractable P in the et al. while the specific Other than abiotic mechanisms. It has also been shown by isotope dilution be observed after TSP addition (Nziguheba et al. plant growth trials would have to be performed. However. 2012). Therefore the initial ΔCDGT-index values for the activity of plant and DGT P were found to be not TSP treatment may well be lower than for manure solids. The In contrast to the amendment of soil with manure authors investigated the resulting change in P availability solids or TSP. 2005). organic P sources (compost or plant residues). applying the same DGT ap. In these studies (a modified) Hedley frac- as. (2009) found an However. 2013.

either occlusion of inorganic phosphates might only be relevant for the conventionally managed in or condensation of organic P compounds (Uchimiya soil A. products. dominated by more aromatic structures in the loamy soil B compared to the sandy soil A. 2012. may be very different. Thermal process- soil is governed by abiotic and biotic mechanisms. (2014). 2011. 2012. be assigned to the much longer combustion time in this Waldrip-Dail et al. Cantrell et al. management of 600 °C and would require further testing before practices and under more natural conditions.102 Plant Soil (2016) 401:93–107 treatments. 2011. occurring during pyrolysis or combus- by approximately 0. organic matter content. availability of oxygen during thermal treatment did not son for the proportionally more pronounced increase in affect the P availability from the final char and ash the ΔCDGT-index in soil A. however. 1998. valid. sandy soil A after amendment of a comparable molecule structure reduces the availability of P. precipitation as well as products. 2014). 2012). (2006) added dairy manure 2014). The set of decanter centrifuge-separated dried solid samples importance of the processing temperature. either texture or pH. increasing the pH and P speciation. It is gen. discussed in more detail (Christel et al. 2012). but they did not considerably differ in In agreement with earlier findings (Christel et al. A high extractability of P in a index between the soils amended with char and ash and weak organic acid (2 % citric acid). and 600 °C reported in these studies. Cantrell et al. separation. 2009. Gichangi et al. further tion. and inorganic fertiliser to two soils where the main especially shortly after soil incorporation. but in all cases positive effect Effect of thermal processing on P availability in the amended soils indicates that they may have potential as slow-release P fertilisers. into two soils. He et al. shown that the formation of highly insoluble apatite Frossard et al. for a thermal processing temperature varying in texture. pyrolised at 400 °C than after treatment at 600 °C . 2013). has previously been Christel et al. (2009) incorporated poultry manure present study. content in the loamy soil B. which had an acidic pH. During combustion of pig manure solids. a general decrease in P availability was observed. as well as its history of P The reason for decreased P availability after pig manure depletion. which can et al. Undoubtedly. in which the comparable manure. (2011) have soil microorganisms (Barrow 1983. Huang et al. even for the processed at 600 °C. It may therefore be concluded that thermally-processed treatments. Malik et al. and mobilisation by or immobilisation in Møller et al. (1999) assigned low P adsorption to repeated Tsai et al. 2014).5 pH-units. might be another rea. The observation that the ΔCDGT-index investigate the effect of soil type on P availability from was generally higher after amendment of DEC-char (organic) amendments. Their constant.g. Reddy et al. A similar pattern of higher P availability from the and Hiradate 2014) into the increasingly complex char low pH. although the alterations in chemical structure even after the addition of treatments. both during and derived char and ash has already been reported by combustion and pyrolysis. making their set-up not ing Bintensity^ of thermal processing of the solids after directly comparable with the present study’s. which in the current study carbonisation. Azuara et al. dissolution. 2007. This observation is only studies are needed with a larger number of soil types. (2007) and Thygesen et al. Roboredo yield was slightly lower (Christel et al. desorption from decrease the easily available P fraction in both and occlusion in soil particles. 2000). whereas the ash 1999. During application of manure P. 1999. Hansen et al. The temperature-dependent total P contents of all ther- mally processed materials derived from non-acidified Effect of soil manure were consistent with values available in litera- ture (Møller et al. in order to generalisation. The considerably higher clay minerals and similar compounds decreases availability. et al. Most studies in which organic P fertilisers have been 2012. most of them being rather depleted in P. derived amendments with different extraction methods There was no significant difference in the ΔCDGT- were also characterised. The char yields were in very incubated over a comparably long period have only used good agreement with the respective char yield at 400 one soil type (e. even though this trend was neither consistent erally accepted that P availability after amendment to nor statistically significant in all cases. were expected to result in a higher adsorption pyrolysis has been assigned to changes in biochemical to the greater number of (non-occupied) P-binding sites composition. Nziguheba et al. the ing to produce chars and ashes has been reported to most predominant being adsorption to. with increas- difference was the silt content. Reddy with increasing pyrolysis temperature (Cao et al.

. With a lower mineralisation rate of lar. Low-temperature chars in particu. these assumptions should be rate in soils amended with acidified slurry fractions. a higher P availability from the benefits of char application (e. but not for DEC- stimulates the microbial turnover of P as much as (fresh) separated solid fractions. (2012) conclude that cording to Ohno and Crannell (1996) are expected to acidification might have inhibited P immobilisation. suggest- ing that in the long run. 2012). it can be con.. Whereas char opposite trend of the ΔCDGT-index of DEC-Solids be- may provide a habitat for soil microbes (Atkinson et al. ing greater than that of DECacid-Solids might be a sig- 2010) and hence favour their activity close to the nificant increase in particle size in the acidified slurry amendment. However. as discussed earlier. nitri- containing rice-straw biochar and ferrihydrite (Cui et al. Moreover. not been acidification. 2006. Hence. 2011). 2010. investigated before. As reported by Sommer et al. acidified solid fraction would be expected. fraction (67 % in DEC-Solids vs. 2010. 2014). as both the as the solid fraction contains less total P. less P would be partly mineralised (Bruun et al. Regarding the become available after soil incorporation of the organic decrease in P adsorption after organic P source addition matter in the short term. Roboredo et al.Plant Soil (2016) 401:93–107 103 supported the relevance of the choice of temperature liquid fraction after separation of acidified slurry. Waldrip et al. Spokas et al. chars can be assigned to a higher proportion of organic P after and ashes has. it still remains line with the present study’s findings for the solid frac- to be investigated whether manure-derived char addition tions after SCR or CHE-separation. 2015). Consequently a higher total P content is found in the Downie et al. retained is likely to be the organic and insoluble inor- peared in weeks 6 and 12. Based on the change in P speciation of solid release of considerable amounts of dissolved organic pig slurry fractions. This is in line with the present study’s findings that after 6 weeks of incubation no significant effect of acidifica- Effect of slurry acidification tion could still be observed in the loamy soil B. lower P content. the ΔCDGT-index after amendment ortho-phosphate (ortho-P) in pig slurry. 2011). 2011). stock material were conserved during pyrolysis (e. (2015). A plausible P into the liquid slurry phase. when the ΔCDGT-index was ganic forms (Sommer et al. counterparts. considerable moisture content in the separated solid Char compared to DEC-Solids or TSP. which is observed to occur at a faster available P. Moreover the application of already described. Nevertheless. and the P that is effect of pyrolysis and pyrolysis temperature disap. Uchimiya et al. the dissolved ortho-P-share the suitability of manure-derived char as a slow-release of total P is also higher in the solid fraction of acidified P fertiliser compared with the raw manure solids. may also larger particles (Ambus and Jensen 1997). which ac. slurry ΔCDGT-index of all materials derived from acidified acidification did not impede the P availability in soils manure compared to their respective non-acidified amended with manure solid fractions. when pH is decreased to reason could be that the physical properties of the feed- 5. which facilitated the separation its salinity may inhibit microbial activity close to it process. Lehmann et al. a comparable interaction has already acidified (cattle) slurry has been shown to decrease been observed in a controlled watery solution system microbial activity with respect to soil respiration.5 (Hjorth et al. fication and microbial biomass-C (Fangueiro et al. but also resulted in a coarser solid fraction with (Nayak et al. Apart manure (Sommer et al. subjected to further studies. the decrease in P availability from the derived thermally-processed materials. 2009) and consequently the chars derived .g. (2013) report the 2013). the mineral composition of ash and hence (Hjorth et al. One possible reason for the manure application. In the great majority of materials acidification causes a significant increase in dissolved investigated here. 88 % in CHEacid- cluded that (low-temperature) pyrolysis will not reduce Solids. where- during thermal processing. either acidified prior to separation carbon (DOC) from low-temperature chars. after adaptation of the microbial There are a number of explanations for the lower community to the lower pH and coarser substrate. or non-acidified. due to a not significantly lower after amendment of any DEC. which have not been completely pyrolised. to the authors’ knowledge. which is in Atkinson et al. 2015). Where the soil was amended with the The effect of slurry acidification on P availability manure solid fractions. Nevertheless. mainly soil physical and chemical of total P is applied. but decrease P sorption in soil and hence provide more not mineralisation. Dissolution of with ash or char derived from acidified slurry was lower occluded P and Calcium-associated P will transfer more than that derived from non-acidified slurry.g. wet-weight-based). 2015). if a constant rate from the numerous.

significant effect on carbon or nitrogen dynamics during soil incubation. However. (SCRacid and CHEacid) also produced a lower pH than ical SCR technology.104 Plant Soil (2016) 401:93–107 from acidified slurry had a larger particle size. Consequently the pro. with oxidation of C. In a comparison of five – only of minor importance whether the increase in soil different separation techniques. Consequently the slurry separation tech- nology would not be expected to have a major effect on Conclusions microbial P turnover either. from this study it cannot be concluded . the transfer of the most labile P fractions into the solid Moreover. while P availability in As the amendment of all manure-derived materials soils amended with the corresponding acidified DEC caused a change in soil pH. Since P is mostly bound in the their non-acidified counterparts. over the incubation period. availability could not be attributed solely to a release of However. Generally. the observed pH increase would before. first three to 6 weeks after soil amendment. both soils at most sampling times. (2013) were still observed.e. the pH effect could not be the only have documented that not only total P removal. P bound to sesquioxides ashes. the DECacid-Ashes showed a sig. Especially in the could impede P mineralisation. present in the soil would be likely to be mobilised due nificantly lower ΔCDGT-index than the DEC-Ash in to the liming effect of the amendment addition. P availabil- ity decreased substantially for both solids and TSP. Furthermore. compared to the simple mechan. not only for the amended tures of the derived chars and the mineral speciation of P soils. Therefore the decrease smaller slurry particulate matter and DEC and CHE are in soil P availability over time could also be attributed to more efficient in separating the small particles into the (re-)fixation of soil-borne P or P introduced with the solid fraction (Peters et al. This in the ashes. Fangueiro et al. Consequently. some of the acidified solids niques DEC and CHE. and hence the physical disturbance during mixing as well as the re-wetting resulted in a Effect of slurry separation technology mineralisation of both soil organic matter (in case of the control soils) and the organic compounds in the respec- Although not always statistically significant. of the experiment. but great differences in resulting P availability small particles. the application of the separated solid fractions abiotic and biotic processes governing P dynamics in of pig slurry or TSP increased soil P availability in the soil after amendment of manure solids. but this hypothesis should be subjected to further studies. Nevertheless. but also the unamended control treatments. a decreasing trend in soil pH was observed the effect of acidification on the physicochemical struc. operation of mineral fertiliser (such as TSP). further studies on the chemical speciation phenomenon could most likely be attributed to the fact and physical structure of the chars and ashes would be that the soils had not been pre-incubated before the start needed. the extent of Overall. such techniques. as soil pH after amendment of the P availability could potentially be higher as more P various thermally-treated materials did not differ signif- could desorb from the larger specific surface area of the icantly. this argument would not hold true in be expected to have an impact on the lability of native the case of full combustion of the manure solids to soil P-pools. 2012). Popovic et al. ΔCDGT-indices were generally observed for the treat. 2011. nitrification of ammonium in amendments) releasing ments derived from the more efficient separation tech. fertiliser (pellets) are in any case one of the modes of ed with flocculating polymers. However. including simple P availability is caused by the release of P from a passive and more advanced active separation fertilising product or by other co-occurring effects. char and ash amended soils to a similar extent. Moreover. but also governing factor for P availability in the amended soils. However. as already discussed acidic sandy soil A. Kumaragamage et al. it is – from a plant nutritional perspective with smaller particle sizes. S and N (i. the observed increase in P solids (DEC acid -Solids) was lower in both soils. within the should be addressed in future studies. protons.. portion of easily soluble P is higher in the solid fractions Consequently. The pH effects on P availability in the amended soils highest P availability was found after soil amendment with non-acidified DEC-solids. higher tive amendments. amendment. (local) pH effects favouring P release from fraction is improved when the slurry is chemically treat. which P from the added P-rich materials. In order to investigate Generally. (2014) did not observe a as induced pH changes in the soil.

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