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Water Air Soil Pollut DOI 10.

1007/s11270-011-0983-6

The Influence of Soil Properties on the Water Pollution (Nitrate, Phosphate and COD) Following a Single Application of Sewage Sludge to 70 Contrasting Agricultural Soils
J. M. Soriano-Disla & I. Gmez & J. Navarro-Pedreo

Received: 12 May 2011 / Accepted: 28 September 2011 # Springer Science+Business Media B.V. 2011

Abstract The aim was to study the influence of soil properties on the leaching of nitrate, phosphate and organic matter (OM) following the application of sewage sludge to contrasting soils. Seventy agricultural soils from different parts of Spain were amended with sewage sludge (50 t dry weight ha1), and a controlled column study was developed. After 2, 4 and 6 months of incubation, distilled water, equivalent to an autumn rainfall event of 25 lm2 in Mediterranean environments, was applied and leachates collected and analysed: pH, electrical conductivity (EC), chemical oxygen demand (COD), phosphate and nitrate. The mean values of pH in the leachates after 2, 4 and 6 months were similar and close to the neutrality. The highest concentrations for the rest of the parameters analysed were found after 2 months of incubation and diminished for 4 and 6 months, especially COD. Soil pH and texture were the most relevant soil properties controlling the leaching of the analysed parameters. The OM mineralization seemed to be enhanced at high values of soil pH, thus increasing the nitrate and reducing the COD leaching. However, phosphate levels were reduced at high values of soil pH. In addition, leaching was promoted
J. M. Soriano-Disla (*) : I. Gmez : J. Navarro-Pedreo Department of Agrochemistry and Environment, University Miguel Hernndez of Elche, Avenida de la Universidad S/N, 03202 Elche, Spain e-mail: jsoriano@umh.es

in sandy soils. Other soil properties influenced phosphate leaching being the equivalent calcium carbonate soil content as the most relevant. Soil organic carbon was negatively related to the EC and nitrate concentration in the leachates but resulting in a weak contribution compared with soil pH and texture. Concerns about nitrate pollution have been confirmed. Keywords Chemical oxygen demand (COD) . Mobility . Nitrate . Phosphate . Sewage sludge . Soil properties

1 Introduction The progressive implementation of the European Directive 91/271/EEC (1991) concerning urban wastewater treatment has dramatically increased the production of sewage sludge. The use of sewage sludge in agriculture provides a means of disposing an unwanted waste product, supplying valuable plant nutrients and organic matter (OM), which can help to meet crop fertilizer requirements and to reclaim degraded soils (Bernal et al. 1998; Smith et al. 1998; Speir et al. 2003). However, the application of sewage sludge can lead to environmental or human health problems via leaching of nutrients, pathogens, heavy metals and organic compounds to groundwater (Vogeler et al. 2006). An increasing awareness exists on the potential risks from nitrate, phosphate and OM leaching. Particularly,

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nitrate is very soluble (Kessavalou et al. 1996) and it is generally considered by far the major, if not the only, N specie leached when sewage sludge and manurial wastes are applied to land (Qiang et al. 2004). Nitrates from agricultural sources are considered to be the main cause of pollution from diffuse sources affecting the European states waters (D EEC/ 91/676 1991). Thus, member states are required to design nitrate vulnerable zones where action programmes must be implemented to limit the risk of nitrate pollution derived from fertilizer application (including sewage sludge). On the other hand, phosphates are relatively immobile in soils; however, they can also result in significant losses to groundwater (Smith et al. 1998; Djodjic et al. 2004). The presence of OM in the leachates (dissolved organic matter (DOM)) is an important factor for determining the water quality and its pollution potential, which can be quantified in terms of chemical oxygen demand (COD) (Camobreco et al. 1996; Santibaez et al. 2007). The DOM has been reported to be very mobile through the soil system (Dunnivant et al. 1992) and to form stable, soluble complexes with heavy metals (e.g. Cd, Cu, Ni, Pb and Zn) (Antoniadis and Alloway 2002; Ashworth and Alloway 2004). It is well known that both the amounts and form of nutrients and OM present in different types of organic wastes will vary and, consequently, may influence nutrient and OM loss (Shepherd 1996; Cooke et al. 2001). However, few have been the attempts to evaluate the influence of soil properties on the mobility of these substances following organic waste applications, always using a reduced set of soils (Siddique et al. 2000; Wong et al. 2000; Kaschl et al. 2002; Barton et al. 2005; Toribio and Romany 2006). The leaching of nutrients and OM after sewage sludge application is controlled by many soil properties (Wong et al. 2000; Yang et al. 2008), consequently, and for a proper management of sewage sludge applications, it is necessary to evaluate the relative influence of soil properties on the nutrient and OM leaching. Thus, the main objective of this article was to study the influence of soil properties on the leaching of nitrate, phosphate and OM following a single sewage sludge application to 70 contrasting agricultural soils in a column assay developed under controlled conditions and determining the possibility of water pollution.

2 Material and Methods 2.1 Soil and Sewage Sludge Samples Seventy agricultural soils from different parts of Spain were chosen to cover a wide range of soil properties. The soils, sampled from the ploughed layer (030 cm), were air-dried and sieved (2 mm). Selected physical and chemical characteristics of the soils are shown in Table 1: pH (1:2.5 (w/v), distilled water), electrical conductivity (1:5 (w/v), distilled water), equivalent calcium carbonate (CO32) determined using the Bernard calcimeter (Hulseman 1966), soil organic carbon (SOC) determined by potassium dichromate oxidation (Nelson and Sommers 1982), Kjeldahl nitrogen (Bremmer and Mulvaney 1982), exchangeable phosphorus determined by the Burriel Hernando method (Dez 1982), amorphous Fe and Mn (AmMn) extracted by an ammonium oxalate/oxalic acid extraction (Houba et al. 1989) and determined by atomic absorption spectrophotometry (Unicam 969, UK), water holding capacity (WHC) (Forster 1995) and texture determined by the Bouyoucos method (Gee and Bauder 1986). Sewage sludge was obtained from a wastewater treatment plant of Alicante (SE Spain). The main characteristics of this sludge were (in dry weight):

Table 1 Mean values (standard deviation) and ranges of the selected properties of the soils used in this study Parameters pH EC (s cm1) CO32 (%) SOC (g kg1) KjN (g kg1) ExP (mg kg1) AmFe (mg kg1) AmMn (mg kg1) WHC (%) Clay (%) Silt (%) Sand (%) MeanSD 7.91.1 218411 22.922.8 7.44.3 0.70.4 38.9114.7 313223 96122 0.40.1 1910 2513 5619 Range 5.09.1 182,370 <0.178.7 2.120.0 0.21.7 2.1932.3 711,024 7810 0.20.8 153 260 1790

EC electrical conductivity, CO32 equivalent calcium carbonate, SOC soil organic carbon, KjN Kjeldahl nitrogen, ExP exchangeable phosphorus, AmFe amorphous Fe, AmMn amorphous Mn, WHC water holding capacity

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pH 7.8; electrical conductivity, 4.9 ms cm1; organic carbon, 234.2 gkg1; Kjeldahl nitrogen, 58.1 gkg1; and total phosphorous, 22.1 gkg1 (determined after microwave acid extraction, Moral et al. 1996). 2.2 Column Study Soil was mixed with sewage sludge (both air-dried and sieved at 2 mm), at a single dose of 50 t dry weight ha1 (assuming 30 cm of ploughed layer), obtaining homogeneous mixtures that were packed in PVC columns (3012 cm internal diameter) and maintained at 60% of the WHC and room temperature (mean value of 22C) for 6 months. After 2, 4 and 6 months, columns were saturated and 283 ml of distilled water (equivalent to an autumn rainfall event of 25 lm2 in Mediterranean areas) were applied. The leachates were collected in a plastic container 24 h after watering (similar to Navarro-Pedreo et al. 2003 and Qiang et al. 2004) and analysed for pH, EC, COD (APHA 1999), phosphate (Dez 1982) and nitrate (Sempere et al. 1993). The experimental devices were similar to those used by Almendro-Candel et al. (2007). As in the study of Ashworth and Alloway (2004), the sewage sludge application rate was relatively high to ensure that easily detectable concentrations of the analysed parameters were leached through the columns for all the soils and irrigations. The same or higher sewage sludge (or derived compost) application rates were used in others column studies (Antoniadis and Alloway 2002; Jordn et al. 2008).

2.3 Statistical analysis The mean values (standard deviation) and ranges of the different parameters analysed in the leachates after 2, 4 and 6 months in the amended soils were calculated. The values of the parameters throughout the experimental period were compared with the soil properties by stepwise multiple linear regressions (SMLR). The regression equations, ordered by their regression coefficient (r2) and the standard error of estimate, followed P the general model y a bn xn where y is the mean value of the different parameters analysed in the leachates after 2, 4 and 6 months of incubation, a and bn are coefficients and xn represents soil properties. For the development of the statistical procedures, SPSS v.15.0 and Microsoft Excel 2003 were used.

3 Results Table 2 shows the mean values and ranges of the different parameters analysed in the leachates after 2, 4 and 6 months of incubation. Table 3 shows the SMLR where soil parameters were compared with the mean values of the different parameters analysed in the leachates over the incubation period in order to have an assessment of the influence of soil properties on the leaching of the different parameters over the 6-month column assay. The mean pH values observed for the three leachates were similar and close to the neutrality. The predicting equation obtained from the SMLR for pH in the leachates consisted of soil pH and silt,

Table 2 Mean values (standard deviation) and ranges of the analysed parameters in the leachates after 2, 4 and 6 months

Leachate

pH

EC (ms cm1)

COD (mg O2 l1)

Phosphate (mg l1)

Nitrate (mg l1)

2 months MeanSD Range 4 months MeanSD Range 6 months MeanSD 7.30.9 5.48.4 6.52.1 1.811.5 289154 75800 27.236.7 2.5155.9 3,4721,276 7566,220 7.30.8 4.98.6 8.12.8 2.916.7 430279 1091,697 33.045.1 3.3221.9 4,1781,535 9838,158 7.20.7 4.98.5 9.92.6 5.117.0 799636 2183,523 48.653.5 5.5241.1 4,9751,510 2,1647,889

EC electrical conductivity, COD chemical oxygen demand

Range

Water Air Soil Pollut Table 3 Stepwise multiple regression equations (p<0.001) for the mean values of the analysed parameters in the leachates throughout the experimental period as function of soil properties Step pH 1 2 EC (ms cm1) 1 2 3 LogCOD (mg O2 l1) 1 2 LogPhosphate (mg l1) 1 2 3 4 5 Nitrate (mg l1) 1 2 3 56.327+544.028 soil pH 494.938+651.823 soil pH55.391 silt 242.840+729.266 soil pH49.136 silt69.086 SOC 0.22/1,160 0.52/918 0.56/884 1.6260.013CO32 2.6850.008CO32 0.148 3.2360.010CO32 0.197 2.7460.007CO32 0.190 2.8310.008CO32 0.182 pH pH0.001 AmMn soil pH0.001 AmMn+0.006 sand soil pH0.001 AmMn+0.005 sand0.0002 soil EC 0.48/0.31 0.58/0.28 0.69/0.24 0.75/0.22 0.77/0.21 2.069+0.010 sand 2.712+0.009 sand0.074 soil pH 0.59/0.16 0.70/0.14 1.179+0.886 soil pH 2.007+1.048 soil pH0.083silt 1.485+1.208 soil pH0.070 silt0.143 SOC 0.20/2.0 0.43/1.7 0.49/1.6 2.647+0.589 soil pH 2.531+0.567 soil pH+0.012 silt 0.75/0.4 0.78/0.4 Soil propertiesa r2/SE

SOC soil organic carbon (in g kg1 ), CO32 equivalent calcium carbonate (in %), AmMn amorphous Mn (in mg kg1 ), EC electrical conductivity (in s cm1 ), SE standard error, COD chemical oxygen demand
a

Sand and silt in %

presenting a high level of correlation (r2 =0.78, p< 0.001) with the soil pH having the largest effect on the prediction. High values were observed in general for the EC in the leachates, reaching the maximum in the first leachate (mean value of 9.92.6). In the following leachates, a reduction of the EC values was observed (mean value of 6.52.1 after 6 months). The values of EC observed were highly influenced by the nitrate leaching, presenting a good linear correlation when the mean values of both parameters were compared (r2 =0.93, p<0.001). For this reason, the soil factors explaining the leached values of soluble salts were similar to those of nitrates. The SMLR showed that 49% (p<0.001) of the variations in EC concentrations in the leachates could be accounted by a linear combination of pH, silt and SOC. Similar to EC, the highest values of COD were found in the first leachate and reduction was observed throughout the incubation time. The variations

observed for COD were the largest among the analysed parameters, with reductions of 54% and 36% in the mean values obtained in the second and third leachates, respectively, comparing with the first one. The COD tended to be determined primarily by the sand content showing a positive relationship, and secondly by the soil pH, negatively related. The leaching patterns of phosphates were similar to those of COD and EC. However, the mean values after the second and third irrigation were very similar. Many soil properties influenced phosphate leaching (Table 3) with the CO32 content having the largest effect on the prediction of this parameter. In addition, also soil pH, AmMn, sand and EC appeared in the model, accounting for a high percentage of the variation (r2 =0.77, p<0.001). The high relationship between EC and nitrate in the leachates explained the leaching patterns observed for both parameters. As the reported for phosphates and COD, the highest concentrations were found in

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the first leachate. However, weaker reductions were observed in the following leachates, especially in the second. The SMLR showed that 56% (p<0.001) of the variations in nitrate leaching could be accounted by a linear combination of soil pH, silt and SOC, presenting positive relationships with soil pH and negative with silt and SOC, with no other soil property significantly related.

4 Discussion 4.1 Leachates Characteristics In general, it was in the first leachate where the highest values of the analysed parameters were observed (except for the pH), values that diminished after 4 and 6 months. When sewage sludge is applied to soil, a large proportion of labile OM is available for mineralization, amount that is reduced within this process. The large differences among irrigations for COD seemed to imply a mineralization of the OM, reflected in the amounts of phosphate and nitrate collected in the leachates. The higher values of these anions in the first leachate suggested that the OM mineralization was more intense at the beginning of the experiment. However, and comparing the values of these anions found in the first leachate (after 2 months) with the values found in the second and third leachate (4 and 6 months), reductions were proportionaly higher for phosphates. This may indicates that although a mineralization is occurring and phosphates and nitrates are released, the capacity of soils for retaining phosphates is higher and less amount of phospahte is leached. Considering the levels of N and P contained in the sewage sludge and the quantities of nitrate and phosphate collected in the leachates, it seems evident that the mobility of nitrate was far higher than the observed for phosphate, evidencing the awareness about nitrate pollution of waters from amended soils and the low capacity of soils to retain this anion. Nitrate is easily leached through the soil profile, in fact, a study where a domestic effluent was applied to four soil types showed that the amount of N recovered can be greater than the amount applied, thus showing a net mineralization of the native soil N (Barton et al. 2005). Similarly, in our study, for some soils having high and low values of soil pH and silt, respectively,

the nitrate losses exceeded the quantities applied with sewage sludge suggesting a net mineralization of the native soil N. This enhanced mineralization following the application of organic matter sources (in our case raw sewage sludge) is known as priming effect (Dalenberg and Jager 1989). Relatively large values were observed in general for the analysed parameters in the leachates. It should be remembered that the column study was developed under theoretical optimal conditions of temperature and humidity for OM mineralization, using a high rate of a raw organic waste with high OM, nutrient and salt contents. In addition, plant influence was not considered and three irrigations spaced in time were applied. These facts undoubtedly influenced the high concentrations reached for the different parameters in the leachates. 4.2 Influence of the Soil Properties on the Leaching of the Different Parameters Soil pH and texture were the most important properties controlling the leaching of the different parameters, appearing in all the prediction models. The OM mineralization is generally favoured with increasing pH values, although it is reduced when considerable high values are reached (Luo and Zhou 2006). This is in agreement with the negative correlation found between soil pH and COD and the positive between soil pH and nitrate. For COD, high mineralization rates at high soil pH levels would reduce the soluble OM contents thus reducing the COD contents in the leachates. In addition, a high soil pH can also lead to the decrease in the COD values via precipitation with Ca2+. This has been proved in the work of Rmkens et al. (1996) where increasing levels of Ca2+ led to a decrease in the DOM concentration due to sorption of Ca2+ bound DOM. Soil pH is the major factor regulating the nitrification process with the optimum around 8.5 (Sahrawat 2008). Moreover, acidic conditions have been reported to suppress N mineralization (Funakawa et al. 2009). These facts could explain the positive relationship between soil pH and nitrate leaching. However, a negative relationship was observed between soil pH and phosphate leaching, in agreement with Cooke et al. (2001). The large effect of calcium carbonate (CaCO3) in the retention of phosphate suggests that the negative correlation

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between soil pH and this anion was related with the increased precipitation with this mineral at high pH (Tisdale et al. 1993). Soil texture is related to porosity, which in turn determines soil WHC, water movement and gas diffusion in the soil (Luo and Zhou 2006). Large pores and a low presence of adsorption sites are characteristics of sandy-textured soils, in contrast with silty or clayey-textured soils. These characteristics undoubtedly affected the leaching of the analysed parameters. Thus, the leaching of soluble salts, nutrients and organic matter was promoted in sandy soils (compared with heavier-textured soils) due to their lower retention capacity. In addition, heaviertextured soils are expected to have lower mineralization rates (Franzluebbers 1999). This fact could be explained by a lower proportion of large pores thus reducing the oxygen availability and by the protection effect of the OM from the mineralization by the soil adsorption sites (Wang et al. 2003). Apart from the contribution of soil pH and texture, many other soil properties controlled the phosphate leaching (Table 3). This fact and the low relatively levels found for this comparing with nitrate, shows the strong capacity of soils to restrict the movement of this anion. The precipitation with CaCO3 and the presence of soil colloid like Fe/Mn oxides are wellknown block factors of phosphate migration (Amer et al. 1991; James et al. 1996; Chen et al. 2003). Soil organic carbon was negatively related with the EC and nitrate values in the leachates probably due to the sorption capacity of SOC for cations but resulting in a weak contribution compared with soil pH and texture. It has been well reported that ammonia can be chemically fixed to the SOC (Johansson 1998) thus limiting nitrate formation. Previous studies about organic wastes application on soils have demonstrated the single contribution of soil properties on the leaching of the parameters analysed in this study. For instance, Toribio and Romany (2006) in a study where sewage sludge was applied to one acid and two basic soils showed that the newly added OM leached more readily in the acid soil than in both basic soils. Wong et al. (2000) reported higher retention capacity of soluble salts and nitrates in a sandy loam soil than in a sandy soil after the application of sewage sludge to these two contrasting textural soils. Kaschl et al. (2002), in a study where municipal solid waste compost was

added to two sandy and one loamy soil, observed that the leaching of OM and nitrate was reduced in the heavier soil due to the abundance of adsorption sites. Siddique et al. (2000) studied the leaching P potential from five acid loam soils with different native soil P status following application of different sources of P, finding that the leached P increased at higher native soil P and the degree of P sorption saturation above a so-called change point. Our study has hence affirmed some of the reported single contribution of soil properties on the leaching of the different parameters analysed with comparatively larger number of soils. When multiple factors are involved, it is always difficult to separate the interactions, and the influence of some factors can be masked by the influence of others. However, this was precisely the challenge of this study, knowing the relative contribution of the soil properties when multiple soils are considered.

5 Conclusions The influence of some soil properties on the pH, EC, OM, phosphate and nitrate leaching following the application of sewage sludge to several contrasting agricultural soils was studied and the results suggest that soil pH and texture were the most relevant soil properties controlling the leaching and potential pollution of waters as these soil properties appeared in all the regression models, having a large influence. The positive correlation of soil pH with nitrate and EC and the negative with COD seems to indicate that increasing levels of soil pH favoured OM mineralization. However, the phosphate leaching was reduced at high values of pH. In addition, other soil properties (AmMn and EC) influenced the mobility of this anion with the equivalent calcium carbonate content as the main factor. The leaching of the analysed parameters was promoted in sandy soils compared with heaviertextured soils. Soil organic carbon was negatively related to the EC and nitrates in the leachates but resulting in a weak contribution compared with soil pH and texture. In general, it was in the first leachate where the highest values of the analysed parameters were observed (except for the pH). In the following leachates, a diminution in the concentration of the analysed parameters was observed, especially for COD, showing the mineralization of the OM, more

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intense at the beginning of the experiment. This study also evidenced the large differences in the leaching of the different parameters among soils, especially phosphate, and the awareness about the nitrate leaching due to the high amounts collected in the leachates contrasting with the relative immobility of phosphate. This result reinforced the idea of the nitrate as a pollutant for waters derived from the agricultural addition of sewage sludge.
Acknowledgements This work was supported by the Spanish Ministry of Environment (number of expedient: 021/2006/24.2). Jos M. Soriano gratefully acknowledges the Spanish Ministry of Science and Innovation for a research fellowship (AP2005-0320).

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