Evaluation of phosphorus of the struvite as fertilizer in soil with contrasting minerology

L. A. Flores1*; R. García-Ruiz2; V. Aranda3; J. Calero3

1. Benemérita Universidad Autónoma de Puebla, Facultad de Ingeniería Química., Benemérita Universidad Autónoma de Puebla, Benemérita Universidad Autónoma de Puebla, Facultad de Ingeniería Química, Mexico , 2. Universidad de Jaén, Departamento de Ecología., Universidad de Jaén, Universidad de Jaén, Departamento de Ecología, Spain , 3. Universidad de Jaén, Departamento de Edafología y Química Agrícola., Universidad de Jaén, Universidad de Jaén, Departamento de Edafología y Química Agrícola, Spain

Correspondence: *. Corresponding Author: Flores Pérez, Leticia Angélica, Benemérita Universidad Autónoma de Puebla, Facultad de Ingeniería Química, Ciudad Universitaria, Av. Sn. Claudio y 18 sur, Col. Jardines de San Manuel, C.P.72570,Puebla, Puebla, México. Phone: +52(222) 291 0535, E-mail: E-mail:


The production of struvite from urban or livestock wastewater is an important strategy to generate recycled phosphorus (P), especially under a scenario of exhaustion of the primary sources of this nutrient. However, little is known on the availability of P-struvite in soil or the precipitation/solubilisation mechanisms in soils of ifferent properties. The aim of this study was to assess for the solubility and P adsorption in soils of contrasting properties; calcareous soil on marl (pH 8.14) and siliceous soil on granodiorites (pH 6.74), with increasing concentrations of P-struvite and P-superphosphate (0 to 32 μg P mL-1). The results indicate that struvite was more adsorbed reversibly on marls than on granodiorite. In addition, the fraction of P readily available to the plant was almost three times (89 μg P g-1) higher on mark and on granodiorite (31 μg P g-1). Furthermore, 100 % of struvite and superphosphate P adsorbed by soils was found in the most labile fractions (P and P Olsen membrane). We concluded that the struvite is a slow release fertilizer, highly recommended for use in agriculture in general and in the olive in particular.

Received: 2017 November 14; Accepted: 2018 March 14

revbio. 2020 Mar 22; 5: e395
doi: 10.15741/revbio.05.e395

Keywords: Key words: Struvite, superphosphate, phosphorus, granodiorite, marl.


Phosphorus (P) and nitrogen are the essential nutrients for the proper development of plants, however the deficiencies of one of these nutrients limit agricultural productivity. The main source of phosphorus (P) in agricultural systems is superphosphate and its derivatives that come from open mines. Approximately, 90 % of the P extracted is destined to agriculture as fertilizer (Kataki et al., 2016). Population growth and the growing demand for food has caused the intensification of agriculture over the last 50 years and therefore the increase in demand for P. According to the latest estimates, 70 % of the world production of P from natural reserve sources will be exhausted within 100 years, so this poses a risk to the sustainability of agri-food productivity and food security (Huijun et al., 2016).

Actually, both governmental and non-governmental organizations and the scientific community have begun to establish adequate management strategies for P reserves aimed at the efficient and effective use of P, with an impact on the reduction of waste and losses generated during the P cycle, enhancing its recycling (Metson et al., 2016).

Struvite or MAP (Magnesium Phosphate and ammonium hexahydrate-MgNH4PO4∙6H2O) is a compound obtained from various sources of organic waste recycling (urban, industrial and agricultural waste) (Metson et al., 2016; Wang et al., 2016) and it contains a considerable amount of phosphorus (sewage from leather tanning 2.5-8 mg P total L-1, effluent from the packaging of meat products 5.5- 10 mg P total L-1, wastewater from carmine coloring 3490 mg P total L-1, municipal wastewater 21-273 mg P total L-1, yeast industry 17.4 mg P total L-1, human urine 240-460 mg P total L-1 and in general in the dairy industry represents a content of 9.3 g P total kg-1, chicken farm 18 g P total kg-1 and of pigs 39 g P total kg-1) (Kataki & Baruah, 2018). Struvite has low solubility (0.2 g L-1 en agua), contains 5.7 % of N and 12.6 % of P, and it can be found naturally in geochemical and biological systems. At an industrial level, it is found in industrial and urban wastewater treatment plants, as well as in organic waste of various origin (Barak & Stafford, 2006).

Although the recovery and application of struvite and other phosphates with fertilizing potential is now a reality (Johnston & Richards, 2003; González-Poncer & García-López, 2007; Massey et al., 2007; Plaza et al., 2007; Pastor et al., 2008; Cabeza et al., 2011), its real value as a fertilizer in specific crops is not yet known in depth, as is the case of the olive grove, and especially in soils of different properties.

The objective of this work was to determine the solubility and quantify the availability of P for struvite and superphosphate in soils with proven mineralogy; siliceous soil on granodiorite and carbonated soil on marl.

Material y Methods

Samples were taken from the topsoil (first 30 cm) of the two types of soil (on marl at basic pH and on granite at acidic pH) in commercial olive trees in the province of Jaén (37º 49’ 58.25” N y 3º 46’ 06.05” W) and Córdoba (38º 09’ 01.10” N y 4º 54’ 17” W). The soil samples were sifted (<2mm) and the main properties are presented in Table 1.

Table 1.

Properties of siliceo soil on granodiorite and carbonate soil on marl

Classification of texture Physical properties
Sample Classification Permeability
Sandy % Silt (%) Clay % USDA D.A. (g/co) F.C. (%) W.P. (%) A.W. (%) W.S. (%) (mm/h)
Granite 63 23 13 Fr-Sandy 1.55 18.4 9.0 9.4 41.6 31.6
Marl 28 40 23 Franco 1.43 31.2 15.3 15.9 46.2 9.3
Chemical properties
N% Base of change
IA2 % Saturation pH
E.C.3 O.M.
C/N Caliza
(CA+Mg)K CaK CaMg MgK
P1 K Ca Mg Na K Mg Ca Na Base H2O KCl %
Granite 0.05 7 43 548 109 36 10 6 1 9 27 2 39 6.74 6.05 0.184 1.35 17.2 <1 33 25 3 8
Marl 0.08 31 348 2744 156 64 19 3 5 7 72 1 85 8.14 7.44 0.219 2.05 14.7 75 17 15 11 1

TFN11: Olsen Phosphorus; 2: Units meg/100g; 3: Relation 1:5 to 25oC (mS/cm); DA: Density apparent; C.C. Field Capacity; W.P.: Wilting Point; A.W.: Available Water; W.S.: Water Saturation; IA: Interchange acid in meg/100g; C.E.C.: Cation Exchange Capacity; E.C.: Electrical Conductivity; O.M.: Organic Matter; C/N: Relationship between Carbon Nitrogen.

For the solubility and adsorption tests, the method of Daly et al. (2015). Concentration solutions were prepared 0, 3, 6, 10, 17 and 31 μg P mL-1 in the form of struvite (Struvite Crystal Green® de Ostara Nutrient Recovery Technologies Inc.) and of superphosphate (SS) (FERTYSEM Agro Special SL) which were placed in 50 L alcon tubes. In the adsorption tests, 3 g of soil were added (siliceous soils on granite and/or carbonated soils on marl). The solutions were stirred at a rate of 42 U min-1 during 72 h at room temperature. Finally, the centrifugation (4000 rpm) was carried out for 5 min for the solubility tests and 10 min for the adsorption tests. The characteristics of struvite and SS are detailed in Table 2. The concentration of phosphate was determined in the supernatant, in which the colorimetric method with ascorbic acid was used (Murphy & Riley, 1962). Once the phosphate concentration was determined and on the pellet, the sequential fractionation of P was carried out (Hedley et al., 1982) in those samples that received a concentration of 10 μg P mL-1 of struvite and SS. The procedure consisted in determining the P-membrane using anion exchange membranes (5x2.5 cm2 type 204-U-386 Ionics Inc., Watertown, MA, USA; loaded with LiCl 0.5 M). The solutions with the charged membranes were shaken to 42 U min-1 during 24 h, subsequently, the membranas were washed with distilled water and transferred to falcon tubes with 30 mL of 0.5 M HCl, which were shaken for 16 h. The phosphate content was determined on the resulting solution. Thirty mL of 0.5 M NaHCO3 was added to thesoil pellets contained in the falcon tubes and the mixture was stirred for 16 h. After that time, the phosphate was centrifuged and analyzed in the supernatant. This form of phosphorus is known as P Olsen. The most labile fraction of organic P was estimated by difference between the total P extracted with NaHCO3 and the P Olsen. Later, 30 mL of 0.5 M NaOH were added to the resulting pellet after extraction with NaHCO3 and the procedure was as in the case of NaHCO3. The phosphorus analyzed in the NaOH extract is considered the inorganic P associated with Fe and Al and the organic phosphorus linked to Fe and Al secondary minerals was obtained by difference between the total P of this extract and the inorganic P linked to Fe and Al. Finally, 30 mL of 1 M HCl was added to the pellet obtained after extraction of NaOH and it was stirred for 16 h to determine the inorganic P associated with carbonatebound Ca. The organic P linked to these minerals was determined by the difference between the total P and the Pi-HCl. The supernatants resulting from the fractionation are neutralized with a pHmeter GLP 21/CRISON for the determination of P.

Table 2.

Main properties of the struvite and superphosphate (SS).

Struvite/Nutrient Content (%) SS/Nutrient Content (%)
N ammoniacal 5 P2O5 neutral ammonium citrate-soluble 18
P2O5 total/P2O5 available 28 P2O5 soluble in water 12 12
MG 10 SO3 28

The total P was determined by taking 10 mL of the solutions from each of the fractionation treatments of P, which were added in digester tubes in which 5 mL of the mixture of HClO4:HNO3; 3:5 v/v were added. Digestion was done in the digester SELECTA/BLOC DIGEST μ40 in two phases; 130 ºC during 90 min and 204 ºC during 75 min. After digestion, 30 mL of distilled wáter were added to the digester tubes and the phosphate concentration was determined by the AOAC method (1997), phosphorous section.

For this study, the applied terminology of fractionation of P was used based on the literature of experiments performed with the Hedley method and summarized in Table 3.

Table 3.

Main fractions of P in the sequential P fractionation procedure used in this study.

Classification Hedley Fractionation method Description
Resin Pi Resin Labile Pi (mg P kg-1).
Bicarbonate Pi (Olsen P) NaHCO3 0.5 M Labile Pi (mg P kg-1).
Hydroxide Pi NaOH 0.5 M Secondary mineral Pi adsorbed to surfaces of Al and Fe oxides (mg P kg-1).
Apatite P or P-Ca HCl 1 M Apatite P or P-Ca (mg P kg-1).
Residue P HClO4:HNO3 (3:5) Occluded P (mg P kg-1).
Bicarbonate Po NaHCO3 0.5 M Labile Po, easily mineralized (mg P kg-1).
Hydroxide Po NaOH 0.5 M Stable Po, involved with long term transformation of P in soils (mg P kg-1).

The results were statistically treated using a descriptive statistical analysis and the normality and homocedasticity test of all the measured variables, using numerical transformations. The one- and two-way analysis of variance (ANOVA) and Fisher’s a posteriori test were also used to check the differences among the means of the variables of the different treatments (type of soil, type of fertilizer and P concentrations added). In all the statistical analyzes, the IBM SPSS Statistics 22 program was used.

Results y Discussion

Solubility of struvite phosphate and superphosphate

There were no significant differences in the solubility of P in water due to the two forms of phosphorus. However, it was observed that the phosphate concentration was higher with the SS (15 ppm) than with the struvite (10 ppm). As expected, there were significant differences (p<0.05) in phosphate levels due to the dose especially for doses lower than 17 ppm (Figure 1). This shows a clear tendency of saturation that was more evident in struvite than for SS.

[Figure ID: f1] Figure 1.

Solubility of the P-struvite and P-superphosphate at in creasing P concentration.

Adsorption of P in soils with contrasted pH

Typification of adsorption isotherms.Figure 2 shows the adsorption isotherms obtained for the two soils and the two fertilizers used. In both types of soil, the adsorption of P was greater when it was added in the form of struvite than in the form of SS, especially at high concentrations (32 ppm), which contrasts with the greater solubility in water observed in the SS.

[Figure ID: f2] Figure 2.

Adsorption isotherms of the P-struvite and P-superphosphate in calcareous (on marl; pH 8.1) and siliceous (on granite; pH 6.7) soils. The continuous lines show the best fitted models.

Significant differences have been found (p<0.01) in the adsorption of P depending on the type of soil for the highest concentration of P tested, being higher in soil rich in carbonates than in soil of siliceous nature. Likewise, the values of statistical significance associated to the variations of P adsorbed in equilibrium for the different doses of added P, indicate a saturation process similar to that found for water solubility, the saturation effect being more evident at higher concentrations (17 to 32 ppm). The effects due to the interaction type of soil x P type was not significant (two-way ANOVA). However, the interaction type of soil x dose of P had a significant effect (p<0.01) (Table 4), which suggests the strong effect of fertilizer concentration on the adsorption of P.

Table 4.

Two-way ANOVA analysis on the effects of type of fertilizer (F), soil type (S) and the concentration of added P (C), and the different interactions (FxS, FxC and SxC) on adsorbed P.

P fraction Fertilizera
Resin Pi 37/37 28/24
Olsen P 80/53 31/89***
NaOH Pi 17/9 7/13
HCl Pi 3/3 3/4*
NaHCO3 Po 22/2 5/11
NaOHPo (μg P g-1) 81/66 87/52**
HCl Po (μg P g-1) 3/6 0/7***

TFN2Significant: p<0.05 *, p<0.01**, p<0.001**

Effects of fertilizer P and the type of soil in the different fractions of inorganic P

No significant differences were found in the concentration of the most labile form of phosphorus (phosphorus retained in anion exchange membranes) between carbonated soil (24 ppm) and acid (28 ppm) (Table 5). Neither the source of phosphorus (37 ppm in struvite and SS) nor the source interaction of P x type soil had significant effects on this fraction of P (Table 6).

Table 5.

Mean P concentration (mg P g-1) of the analysed P fractions for the two types of P fertilisers and soil.

P fraction Fertilizera
Resin Pi 37/37 28/24
Olsen P 80/53 31/89***
NaOH Pi 17/9 7/13
HCl Pi 3/3 3/4*
NaHCO3 Po 22/2 5/11
NaOHPo (μg P g-1) 81/66 87/52**
HCl Po (μg P g-1) 3/6 0/7***

TFN3aSignificant of Student test for two grups: *<0.05, **<0.01, ***<0.001.

TFN4SS: Superphosphate simple

Table 6.

Two-way ANOVA analysis on the effects of type of fertilizer (F) and soil type (S) and the interactions (FxS) on P fractions.

P fractions Fertilizer-Soil
Resin Pi 0 1 2
Olsen P 6* 24** 2
NaOH Pi 2 0.5 0.4
HCl Pi 0.3 3 4
NaHCO3Po 2 0.4 0.1
NaOHPo 1 5 2
HCl Po 8* 146*** 8*

TFN5Significant: p<0.05 *, p<0.01**, p<0.001***

TFN6F: Fertilizer (struvite and Superphosphate simple); S: Soil of pH 6.74 and 8.14.

However, the effects were significant on the Olsen P (p<0.001). The carbonated soil (89 ppm) had a concentration of P Olsen significantly higher than the acid soil (31 ppm). However, as in the soluble fraction, no significant differences were found with respect to the type of fertilizer studied (80 ppm in struvite and 53 ppm in SS). In spite of not being significant, it is noteworthy that the assimilable P values were higher when struvite was added (Table 5). No interactions were detected in two-way ANOVA (Table 6).

A significant difference was detected in the inorganic P extracted with NaOH (P linked to secondary minerals of Fe and Al) due to the type of soil, although the average on marls (13 ppm) was almost double compared in on granite (7 ppm) (Table 5). Although P-chemisorbed values by labile bonds (complexes of Fe and Al monodentates) was lower than comparable P, there is some property of the soil that affects this fraction. Likewise, no significant difference was detected in this form of P due to the source of soluble phosphorus (17 for struvite and 9 ppm in SS), nor due to the interaction type of soil x source of P. This fraction was, in general, higher in soils of pH 8.14 when struvite was added (Table 6).

In the case of inorganic P extracted with HCl (inorganic P associated with carbonates) significant differences were found (p<0.05) due to the soil, being on marls where the slightly higher concentrations were found (4 ppm). In principle, this difference, although significant, is very small for what could be expected depending on the pH of the soils, which a priori would suggest that this fraction is much higher in the case of carbonated soil (pH 8.14), (Table 5). The concentrations found according to the type of soluble fertilizer (3 ppm on average for both soils) or in the interactions were not significant (Table 6).

Effects of the fertilizer of P and the type of soil in the different fractions of organic P

The amount of organic phosphorus in the most labile P fraction was very low, which is reasonable considering the low organic matter content of both soil types. There were no significant effects due to the type of soil and the type of fertilizer (Table 5).

The stable labile organic fraction (that extracted with NaOH) of P was higher than inorganic (average value of 70 ppm versus 60 ppm). There were significant differences (p<0.01) due to soil type (87 and 52 ppm in marl and soil on granite mother rock, respectively). On the other hand, no significant effect was found due to the type of fertilizer used, although the values tended to be higher when struvite was added (81 vs. 66 ppm, in the case of SS). The interaction in two-way ANOVA was also not significant (Table 5 and 6).

Finally the concentration of organic P extracted with HCl was very low and undetectable in those samples with soil on granite. The values were higher in the soil on marl, although the value obtained (7 ppm on average) was low taking into account the basic pH of this soil and the percentage of active limestone (13 %) (Table 6). Like the previous fraction, there were no significant effects due to the fertilizer type, although the values were slightly higher when SS was added (6 vs. 3 ppm in SS and struvite, respectively).


Solubility and adsorption of struvite phosphorus

The P of the struvite presented a relative low solubility in water under room temperature conditions (0.01 g mL-1). This value does not resemble with what was reported by Le Corre et al. (2009), because it is practically half the value of 0.018 g mL-1. This low solubility gives it the characteristic of slow reléase of phosphorus, very suitable a priori for agricultura (Lee et al., 2009; Plaza et al., 2007). Low solubility is an important requirement in the new generations of agrochemicals (slow release fertilizers), because thus the possible losses of P by leaching are reduced and, therefore, less is the possible environmental impact produced by the processes of eutrophication (Jha et al., 2017) and greater the advantage on the part of the plant (Cadahía et al., 2005), which can be translated into a higher efficiency of use of P. Also, in this study it has been found that the solubility factor lies on the concentration used and that it was independent of the type of fertilizer.

The soils on marl showed a great capacity of adsorption of P (maximum of 250 and 200 μg P g-1 for SS and struvite, respectively), whereas the retention of P was relatively low in that soil on granitic mother rock (maximum of P 140 μg P g-1 and 99 μg P g-1 for SS and struvite, with evident effects of desorption in equilibrium at concentrations higher than 10 μg P mL-1 in the latter). The pH of the soil on granodiorite is comparable with that reported in the literature -from slightly acidic to neutral- (Massey et al., 2009; Plaza et al., 2007) which shows the efficiency of the assimilation of P in plants of Triticum aestivum L. from struvite and SS. Although in these trials they obtained a greater assimilability for struvite than for SS, which could be correlated in some way with the adsorption capacity of the soil, the soils that were used were fine textured (loam clay and clay), so that the results can not be directly comparable with those tested in this study, of similar pH, but with a thicker texture (sandy loam). This could indicate the importance of soil surface properties in the adsorption of P, capable of modulating the pH as a bioavailability factor of P.

The positive effect of carbonated soil on adsorption could be explained, therefore, by its greater surface area, as well as the higher calcium saturation of this soil, capable of reversibly binding the solubilized phosphate to the calcium exchange bridging complex (labile fraction). It should be noted that, although there are comparative studies of the effectiveness of struvite as a fertilizer, these studies do not take into account soils of basic pHs, such as those soils on marl. Taking into account that more than 50 % of olive groves in the province of Jaén are located on marls materials (Aguilar et al., 1987), this can understand the relevance of this study. These results will set new research guidelines for basic soils with pH values higher than 7, since there are few studies on this and most are oriented to studies of struvite solubility in soils with pH below 3 and above 4, or the studies focus on the production of biomass in soil cultures with a pH of around 8 (Johnston & Richards, 2003; Massey et al., 2009; Plaza et al., 2007; Vogel et al., 2015; Antoniadis et al., 2016; Frédéric, 2016; Ehmann et al., 2017).

In general, except in the case of struvite in granodiorites, the adsorption isotherms were conveniently adjusted to the Langmuir logarithmic model. Several studies (Holford et al., 1974; Holford & Mattingly, 1975; Indiati et al., 1999; Hooda et al., 1999; Daly et al., 2015) have demonstrated the suitability of the Langmuir model to describe the adsorption of phosphate by the soil. This model, as opposed to others (linear, Freundlich, etc.), has the advantage of allowing the calculation of soil P buffering capacity (PBC), which is the capacity of a soil to moderate changes in soluble P when adding or extract P from it (Moody, 2007). In general, higher PBC implies higher adsorption of P and higher anual fertilization demands to verify a significant response of the crop, but also that the soil compensates for a longer time the same extraction rate, or higher extraction rates in equivalent intervals of time (McGechan, 2002). Although from a qualitative point of view - because in this work the PBC has not been estimated numerically - the greater adsorption in marl at high concentrations of fertilizer would imply a higher PBC and, consequently, greater amounts of struvite or superphosphate would have to be added to these soils at the beginning of the crop, these soils would retain more P. The complex shape of the struvite isotherm in granodiorite soil did not fit any of the models described. The negative inflection point detected at 10 ppm, which implies desorption at higher concentrations, can be interpreted in practical terms as a point of premature saturation (McGechan, 2002). The consequence is that this combination of soil and fertilizer has the lowest possible adsorption potential of all the samples tested. Therefore, the physicochemical conditions of the soil, whether pH or surface properties, are critical for the adsorption of struvite. The adsorption of SS, also, seems relatively independent of such conditions, although it is slightly lower in acidic soil.

Sequential fractionation of phosphorus

The fractionation of P into its labile and nonlabile forms represented differences in its availability, conditioned mainly by the texture and mineralogical properties of the soil. The differences are very marked in the fraction P Olsen and the sodium hydroxide in its inorganic and organic phases, although in general this study showed a greater increase of P of the struvite than with the SS in all the fractions. The greater availability of P Olsen in marl, especially for struvite, is due to its clay texture and its smectite mineralogy, which endows it with greater colloidal properties: total change capacity, clay change capacity and specific surface. These parameters indicated the great capacity that carbonated soils may have in the olive groves for the use of P from struvite, given that the largest fraction of P is in the inorganic form assimilable by the plant.

Regarding this, the studies indicate that similar values of P Olsen (80 ppm) to those found in this study represent an 85 % efficiency in the crops (Roberts & Edward, 2015). The high availability, as well as the high PBC, that can be derived from the study of isotherms help explain why the P is not a critical element in the productivity of most of the olive groves of the province of Jaén (Barranco et al., 2008), located on carbonated materials. Given the low organic matter content of the soils studied, the organic fractions probably represent less than 50 % of the theoretical total available for the plants. Once again, the role played by the colloidal properties of the soil as fundamental parameters for evaluating fertility in terms of available P olives is noteworthy. The quantification of the P fractionation of the struvite in the two types of soils studied shows how viable it is in agriculture for olive production and its good use would maintain the agricultural sustainability of the Jaén olive industry.


The fractionation of phosphorus in its labile and non-labile form, represented differences in its availability, conditioned mainly by the texture and soil mineral properties.

The phosphorus content of struvite, in the two types of soil studied, demonstrates the viability of this material for use in agriculture.

fn1Cite this paper: Flores, L. A., García-Ruiz, R., Aranda, V., Calero, J. (2018). Evaluation of phosphorus of the struvite as fertilizer in soil with contrasting minerology. Revista Bio Ciencias 5, e395. doi: https://doi.org/10.15741/revbio.05.e395


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