Published in J. Environ. Qual. 33:1062-1069 (2004).
© ASA, CSSA, SSSA
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TECHNICAL REPORTS
Waste Management
Laboratory Characterization of Phosphorus in Fresh and Oven-Dried Organic Amendments
B. Ajiboye,
O. O. Akinremi* and
G. J. Racz
Department of Soil Science, University of Manitoba, Winnipeg, MB, R3T 2N2 Canada
* Corresponding author (akinremi{at}ms.umanitoba.ca).
Received for publication February 27, 2003.
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ABSTRACT
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This study was performed to determine the forms of P and to examine the influence of oven-drying on P forms in different organic amendments. Samples of biosolids, beef and dairy cattle manures, and hog manures from sow and nursery barns were used in this study. Both fresh and oven-dried amendments were analyzed for inorganic (Pi), organic (Po), and total phosphorus using a modified Hedley fractionation technique. Water extracted about 10% of total biosolids P and 30 to 40% of total hog and cattle manure P. The amount of P extracted by NaHCO3 ranged from 21 to 32% of total P in all organic amendments except in the dairy cattle manure with 45% of total P. The labile P fraction (sum of H2O- and NaHCO3–extractable P) was 24% of biosolids P, 60% of hog manure P, and 70% of dairy cattle manure P. The residual P was about 10% in biosolids and cattle manures and 5 to 8% in hog manures. Oven-drying caused a transformation in forms of P in the organic amendments. In hog manures, H2O-extractable Po was transformed to Pi, while in the dairy manure NaHCO3–extractable P was converted to H2O-extractable Pi with oven-drying. Therefore, caution should be exercised in using oven-drying for studies that evaluate forms of P in organic amendments. Overall, these results indicate that biosolids P may be less susceptible to loss by water when added to agricultural land.
Abbreviations: BEEF, manure collected from a beef cattle barn • BIO1 and BIO2, biosolids samples • DAIRY, manure from a dairy cattle barn • DRY, oven-dried manure samples • FRESH, thawed manure samples • HOG-NUR, hog manure collected from a nursery barn • HOG-SOW, hog manure collected from a sow barn • OLD-HOG, hog manure collected from an agitated storage lagoon • Pi, inorganic phosphorus • Po, organic phosphorus
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INTRODUCTION
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THE CURRENT METHOD of utilizing organic amendments, be they municipal biosolids or hog or cattle manure, is to apply them to agricultural land, thereby taking advantage of their nutrients. Continuous application of manures to agricultural land to meet N requirements of crops, as currently practiced in the Canadian Prairies, can result in the accumulation of P in soil (Simard et al., 1995; Whalen and Chang, 2001). This build-up of P in the soil could be initially beneficial to crop growth, especially in Manitoba soils that are often P deficient (Johnston and Roberts, 2001). Increased soil P levels could also increase the concentration of dissolved P in surface runoff or lateral subsurface flow (Simard et al., 2001; Sharpley and Moyer, 2000; Sharpley, 1996; Lennox et al., 1997; He et al., 1999), which could lead to eutrophication if excess P gets to water bodies.
Application of manures to agricultural land has been identified as a potential source of underground and surface water pollution (Beauchemin and Simard, 1999; Eghball et al., 1996; Whalen and Chang, 2001). Consequently, application of biosolids (digested sewage sludge) on land has also created concerns about the possibility of polluting nearby surface waters. A recent survey of Manitoba streams indicates an increasing trend in the phosphorus concentration with time (Jones and Armstrong, 2001). Since these streams empty into Lake Winnipeg and Lake Manitoba, there is the possibility of lake eutrophication if this trend continues. A possible strategy of P management in this region is to manage land application of various organic amendments based solely on their P contents or P loading. This would be plausible if the forms of P in the amendments were the same, with similar reactions when added to soil.
Limited information exists on the forms of phosphorus in biosolids and manures. However, a large variability has been reported on the P content of manures, which depends on the source of manure (type of operation), moisture content, the type of bedding materials, the age of animal, the feed and feed supplements used, and the duration of storage (Barnett, 1994a; Leinweber et al., 1997; Dou et al., 2000). Similarly, there is a large variation in the P contents of P in biosolids, depending on the biosolids treatments methods (aerobic or anaerobic digestion) and nutrient removal (chemical versus biological) processes (Frossard et al., 1996; Maguire et al., 2001; Penn and Sims, 2002). Characterization of soil P into "labile" and "nonlabile" fractions had been used to assess the bioavailability and likelihood of P transport (Qian and Schoenau, 2000; Sui et al., 1999). The complexity of P compounds in the soil makes identification of individual P compounds difficult and a compromise is to operationally define classes of P compounds by the extractant that removes them in a single or sequential extraction procedure.
The sequential fractionation method developed by Hedley et al. (1982) was used to separate soil P into fractions with various physicochemical reactivity and related plant availability (Tiessen and Moir, 1993; Sui et al., 1999). A modification of this technique was successfully applied to different manures and composts (Sharpley and Moyer, 2000) and freeze-dried biosolids samples (Sui et al., 1999). Leinweber et al. (1997) employed the sequential extraction procedure on freeze-dried poultry and hog manures and reported the distribution of total P among residual P (39–41%), recalcitrant H2SO4–extractable P (17–27%), labile P (24–39%), and NaOH-extractable P (3–10%). Similarly, Dou et al. (2000) characterized P in dairy and poultry manures using the sequential extraction scheme involving multiple extractions with various extractants. They found that 70% of total P in dairy manure was extracted by water, 14% by NaHCO3, 6% by NaOH, 5% by HCl, and 5% as residual. In poultry manure, the P fractions extracted were 49% by water, 19% by NaHCO3, 5% by NaOH, 25% by HCl, and 2% as residual. They concluded that dairy manure P, with a high labile concentration of P (sum of H2O-extractable P and NaHCO3–extractable P), may be more susceptible to runoff loss than poultry manure.
Most of the studies on P fractionation of organic amendments involved either biosolids (Frossard et al., 1996; Sui et al., 1999) or manures (Barnett, 1994a, 1994b; Sharpley and Moyer, 2000) alone, and not all the P forms were analyzed. A concurrent fractionation of P in manures and biosolids, as recommended by Maguire et al. (2001), is an important step toward the proper management of organic sources of P. Our hypothesis was that forms of P in organic amendments may influence their reaction in soils. So, fractionation of P in these amendments can be used to evaluate their potential environmental impact. It may also be an important means of comparing organic amendments with respect to the magnitude of their labile P.
A common feature of organic amendments is their high moisture content (Akinremi et al., 2003). In some studies with organic amendments, for example those involving soil microcosms, a large moisture content may not be desirable. Several avenues are available for removing water contained in manures including air-drying (Wu and Ma, 2001), freeze-drying (Sui et al., 1999), and oven-drying (Dou et al., 2000). It is often assumed that these pretreatments have no effect on the phosphorus level and the forms of phosphorus in these organic amendments.
The objective of this study was to characterize the forms of P in organic amendments, including biosolids and cattle and hog manures, as a first step in determining the fate of P in manured soils. We also examined the effect of pretreatment by comparing P fractions in fresh and oven-dried organic amendments, since dry manures are easier to handle compared with fresh forms and laboratory assessments are often performed on dried, ground samples to improve sample homogeneity and analytical precision (Dou et al., 2003).
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MATERIALS AND METHODS
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Collections and Pretreatments of Organic Amendments
Samples of biosolids (anaerobically digested sewage sludge) were collected from the North End Water Pollution Control Centre of the City of Winnipeg Water and Waste Department (Winnipeg, MB, Canada) in February and June 2001 and labeled BIO1 and BIO2, respectively. Hog manures were collected from an agitated storage lagoon of Elite Swine farm (OLD-HOG), and from sow (HOG-SOW) and nursery (HOG-NUR) barns of the University of Manitoba Experimental Farm at Glenlea near Winnipeg. Manures from dairy (DAIRY) and beef (BEEF) cattle barns were also collected from the same location. All samples were frozen immediately upon collection (at –13°C) and thawed just before analysis. Portions of the thawed samples (FRESH) were oven-dried in a Blue M Electric Co. Model EM-243F forced draft oven (Lindberg/Blue M, Asheville, NC) at 105°C for 24 h to determine the moisture content of each amendment. The amendments were digested using the H2SO4–H2O2 method (Akinremi et al., 2003) and total P content was determined colorimetrically. Aluminum, Fe, Ca, and Mg contents of the digests were determined using inductively coupled plasma atomic emission spectrometry (ICP–AES) (Table 1). The oven-dried samples (DRY) were kept in desiccators until sequentially analyzed.
Characterizing Phosphorus in Organic Amendments
A modification of the sequential extraction procedure of Hedley et al. (1982) as described by Dou et al. (2000) was used in this study. Extraction was performed sequentially using deionized water, 0.5 M NaHCO3 (pH 8.5), 0.1 M NaOH, and 1 M HCl. A 0.3-g (on an oven-dry basis) sample of organic amendments was weighed into 30 mL of extractant inside a 50-mL centrifuge tube. The suspension was shaken on an end-to-end shaker at 150 epm (excursions per minute) for 16 h at room temperature. The sample was then centrifuged at 10000 rpm for 15 min and vacuum-filtered using a 0.45-µm cellulose membrane. The phosphorus in the filtrate was determined colorimetrically using the molybdate-blue method (Murphy and Riley, 1962) on a Ultrospec 3100 pro UV/visible spectrophotometer (Biochrom, Cambridge, UK) at a wavelength of 882 nm. This was termed inorganic phosphorus (Pi). To measure the total P in each extract, another portion of the filtrate was digested using the sulfuric acid–hydrogen peroxide method of Akinremi et al. (2003). The pH of the digested solution was adjusted to 6.5 to 7.0 and P measured using the same procedure described for Pi. Organic phosphorus (Po) in each extract was estimated as the difference between total P and Pi. Both Pi and Po were measured in the extract obtained with water, 0.5 M NaHCO3 (pH 8.5), and 0.1 M NaOH while 1 M HCl extract was assumed to contain only Pi. Residual P was determined following sulfuric acid–hydrogen peroxide digestion of the residue remaining after all the extraction steps. The summary of this fractionation technique is shown in Fig. 1
. The same fractionation scheme was used to characterize the oven-dried amendments.
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Fig. 1. Flowchart of the sequential extraction procedure. The terms H2O-P, NaHCO3–P, NaOH-P, and HCl-P represent phosphorus that was extracted by deionized H2O, 0.5 M NaHCO3, 0.1 M NaOH, and 1 M HCl, respectively. Residual P was the phosphorus that could not be extracted by the above extractants.
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All P analyses were performed in triplicate. The extracted P in each fraction was expressed as a percentage of total P in the amendments (Table 1) to provide a means of comparing the various P fractions in the organic amendments. The total inorganic fraction was estimated as the sum of all Pi values including the HCl-P, while the total organic fraction was estimated as the sum of all Po values plus the residual P. Unlike soil, which contained clay fractions capable of occluding P minerals thereby preventing their extraction, we assumed that manure and biosolids residue at the end of the extraction process contained only organic P. As such, the residual P in this study was classified as organic.
Statistical Analyses
The experiment was set up as a 2 x 7 factorial, performed as a completely randomized design. The factors were types of amendments at seven levels (BIO1, BIO2, OLD-HOG, HOG-SOW, HOG-NUR, DAIRY, and BEEF), and pretreatment at two levels (FRESH and DRY). Statistical analysis was performed using the GLM procedure of SAS (SAS Institute, 2002). Analysis of contrast was used to compare differences between organic amendments.
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RESULTS
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Phosphorus Fractions in Fresh Organic Amendments
The total P content varied significantly between the organic amendments used in this study, ranging from 0.25% in beef cattle manure to 4.5% (dry matter basis) in hog manure from a sow barn (Table 1). There was variability in P content between the two biosolids samples collected from the same location (Table 1).
There were also significant differences (p < 0.05) in the forms of P between the different amendments (Table 2).
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Table 2. Mean squares values of the analysis of variance of the effects of amendments and pretreatments on the P fractions.
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In the fresh amendments, water extracted about 10% of total P in biosolids (BIO1 and BIO2), 20% in DAIRY, and between 35 and 43% in BEEF and hog manures (OLD-HOG, HOG-SOW, and HOG-NUR) (Fig. 2a)
. About 50% of the total P from DAIRY and 20% from the BEEF was extracted by NaHCO3, complementing the amount previously extracted by water (Fig. 2b). There was less variation in the amount of P extracted by NaHCO3 from biosolids and hog manures (15–25%). A stronger extractant, NaOH, extracted a significantly higher percentage of total P from biosolids (38%) than from hog and cattle manures (5–22%). Hydrochloric acid also extracted a significantly higher proportion of P (about 30% of total P) from biosolids and OLD-HOG, and less than 10% from cattle manures (Fig. 2d). The residual P that could not be extracted by this procedure was less than 10% of total P in all the amendments (Fig. 2e). The amount of P accumulated with successive extraction of the fresh amendments is shown in Fig. 3
. The labile P fractions (P accumulated up to the NaHCO3 extraction) were significantly smaller in biosolids (24%) compared with other amendments (55–70%).
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Fig. 2. Phosphorus fractions in fresh and oven-dried amendments. (a) Phosphorus extracted by deionized H2O, (b) P extracted by 0.5 M NaHCO3 (pH 8.5), (c) P extracted by 0.1 M NaOH, (d) P extracted by 1 M HCl, and (e) residual P. **Significant at the 0.01 probability level. ***Significant at 0.01 probability level. The whiskers represent standard errors of the means of three replicates. BEEF, manure collected from beef cattle barn; BIO1 and BIO2, biosolids samples; DAIRY, manure from dairy cattle barn; HOG-NUR, hog manure collected from a nursery barn; HOG-SOW, hog manure collected from a sow barn; OLD-HOG, hog manure collected from an agitated storage lagoon.
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Fig. 3. Cumulative P fractions extracted in various amendments. BEEF, manure collected from beef cattle barn; BIO1 and BIO2, biosolids samples; DAIRY, manure from dairy cattle barn; HOG-NUR, hog manure collected from a nursery barn; HOG-SOW, hog manure collected from a sow barn; OLD-HOG, hog manure collected from an agitated storage lagoon.
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Pretreatment Effects on Phosphorus Fractions
There was a significant effect of pretreatment on the P fractions (Table 2). The water-extractable P fractions in the DRY amendments were similar to those in FRESH amendments except in DAIRY, with 45% of the total P compared with 20% in the FRESH DAIRY (Fig. 2a). The effect of oven-drying on H2O-extractable P in DAIRY was not observed in other amendments, and was responsible for the significant pretreatment by amendment interaction in the H2O-extractable Pi and Po (Table 2). The amount of P extracted by NaHCO3 was significantly less in oven-dry DAIRY, HOG-SOW, and HOG-NUR compared with the fresh form of these amendments (Fig. 2b). Similar to the results for NaHCO3, P fractions extracted by NaOH were significantly smaller in DRY biosolids and cattle manures compared with their fresh counterparts. In contrast, oven-drying significantly increased NaOH-extractable P in hog manures (Fig. 2c). The HCl-extractable P in biosolids and cattle manures was also significantly increased by oven-drying (Fig. 2d). However, oven-drying significantly decreased residual P in biosolids and cattle manures (Fig. 2e).
Transformation of Phosphorus Fractions with Oven-Drying
There was a significant pretreatment by amendment interaction on the entire P fraction in the organic amendments (Table 2). This was caused by a significant effect of oven-drying on some forms of P in the organic amendments but not in others (Fig. 2). In the hog and DAIRY manures, for example, oven-drying resulted in the transformation of one form of P to another. This transformation is better visualized as the arithmetic difference between DRY and FRESH forms of P in these two manures (Fig. 4)
. In the hog manures, there was a significant transformation of P from Po into Pi within the water extract as a result of oven-drying (Fig. 4a, 4b, 4c). In DAIRY, however, NaHCO3–extractable Pi and Po were converted into water-soluble Pi following oven-drying (Fig. 4d).
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Fig. 4. Transformation of P fractions with oven-drying of the amendments. (a) Hog manure collected from an agitated storage lagoon (OLD-HOG), (b) hog manure from a sow barn (HOG-SOW), (c) hog manure from a nursery barn (HOG-NUR), and (d) manure from a dairy barn (DAIRY). The whiskers represent standard errors of the means of three replicates. The terms H2O-Pi and H2O-Po are water-extractable inorganic and organic phosphorus, NaHCO3–Pi and NaHCO3–Po are NaHCO3–extractable inorganic and organic phosphorus, NaOH-Pi and NaOH-Po are NaOH-extractable inorganic and organic phosphorus; and HCl-P is HCl-extractable phosphorus.
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Organic and Inorganic Phosphorus Fractions in the Amendments
Apart from BEEF, all organic amendments contained predominantly inorganic P (55–77% of total P). The BEEF samples had the highest proportion of Po (50%) compared with other amendments, whose values ranged from 29 to 45% of total P (Table 3). The distribution of Pi differed among amendments (Table 3). For example, 6 to 8% of total P in biosolids was H2O-extractable Pi compared with 11 to 22% and 13 to 22% in cattle and hog manures, respectively. In contrast, most of the inorganic P in DAIRY (66%) was extracted by NaHCO3. Similar proportions of Pi (33–38%) from biosolids were soluble in NaOH and HCl. However, HCl extracted a greater proportion of Pi in all hog manures except HOG-NUR. Most of the Po in hog manures was soluble in water (46–64% of total Po) and NaHCO3 (24–32% of total Po). In cattle manures, NaOH extracted a relatively higher Po (30–37%) and similar proportions of Po were extracted by water, NaHCO3, and HCl. The distribution of Po in biosolids was similar to that of Pi: least in water-soluble forms and most in NaOH- and HCl-extractable forms.
Similar to the FRESH amendments, most of the P in DRY amendments was inorganic. However, the proportion of total P in the Pi form was higher in DRY compared with FRESH amendment (55–77% for fresh versus 75–89% for oven-dried samples). There was a concomitant reduction in Po (11–24% of total P) in DRY manure compared with FRESH (Tables 3 and 4).
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DISCUSSION
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Phosphorus Fractions and Solubilities
The variability in the P content of the organic amendments used for this study confirmed the results from previous studies (Barnett, 1994a; Dou et al., 2000). The H2O-extractable P in the cattle manures was within the range of 15 to 47% reported by Sharpley and Moyer (2000) for several dairy and composted manures. The observed dominance of NaHCO3–extractable P in DAIRY is similar to the results obtained by Dou et al. (2000) with dairy and poultry manure. Qian and Schoenau (2000) also reported that 70% of the total P in liquid hog manure was in a labile form. The total inorganic P fraction of DAIRY and BEEF (Table 3) is similar to the values of 50 and 70% reported by Barnett (1994b) for beef and dairy cattle manures, respectively. The predominance of Pi in all the organic amendments except BEEF may be due to the large amount of straw mixed with feces and urine in the beef cattle manure. A mild extractant like water removed proportionally smaller fractions of P from biosolids compared with a stronger extractant like HCl. This indicates that biosolids P is in the more recalcitrant fraction and less is in the labile fraction compared with other amendments. The relatively small content of H2O-extractable P may be due to the Fe, Al, and Ca contents of biosolids (Table 1). The combined effect of anaerobic digestion and higher Fe, Al, and Ca contents of biosolids might partly explain the smaller labile P fractions in biosolids compared with other amendments (Table 2). Elliott et al. (2002) reported that there was only a small proportion of P in the labile fraction of activated and anaerobically digested sewage sludge treated with large amounts of Fe and Al. Application of inorganic chemicals to wastewater and sludge has also been reported to reduce P availability (Häni et al., 1981; Kyle and McClintock, 1995). The use of polymer to flocculate the biosolids used in our study may be responsible for the greater contents of Fe, Al, and Ca, and hence relatively small content of labile P compared with manures. It is important to note that the polymer was only used to flocculate the solid material in the wastewater and not for P removal. In general, these results show that biosolids P may be less likely to be transported in surface runoff compared with other amendments (Fig. 3). The smaller amount of plant-available (labile) P in biosolids compared with other amendments also suggests that biosolids P may not be as readily available for plant uptake as that in hog and cattle manures.
The distribution of P in hog manures in this study may be due to the P formulation in the animals' diet. Barnett (1994a) attributed the higher proportion of "acid soluble organic P" in hog manure compared with existing literature values to differences in diet. Sharpley and Moyer (2000) also suggested that the difference in the P fractions of swine manures in their study, compared with those obtained by Zhang et al. (1994), may have been due to differences in mineral supplementation of animals' diet. The greater value of labile P in cattle manures compared with biosolids (Tables 3 and 4) may also reflect the effect of dietary P supplementation. The lower total P in beef cattle manure reported by Barnett (1994b) compared with the published data at that time was attributed to lower supplementation of inorganic sources in the diets of cattle involved in the study and in feedstuff. Ebeling et al. (2002) reported that the high P diet of dairy cattle achieved by supplementing with monosodium phosphate resulted in a two- to threefold increase in water-soluble P, bioavailable P (Sharpley, 1993), and total P concentrations in the manure compared with low dietary P.
Phosphorus Transformation with Oven-Drying
The transformation of the H2O-extractable Po into H2O-extractable Pi in the hog manures following oven-drying (Fig. 4a, 4b, 4c) indicated possible hydrolysis of organic P fractions into inorganic P fractions facilitated by the high water content of hog manures (Table 1). While the transformation of hog manures by oven-drying was restricted to forms of P within a given extract (H2O), the transformation of DAIRY by oven-drying was from one extractant form to another, that is, NaHCO3–extractable P to H2O-extractable Pi. The second extractant, NaHCO3, was designed to remove surface-sorbed P through ligand exchange with the bicarbonate anion. The boiling process involved with oven-drying could cause, in addition to the hydrolysis of NaHCO3–extractable Po, the desorption of P that is held on the surfaces of organic and inorganic colloids in the dairy manure. This desorbed P will then appear in the water-extractable fraction of the oven-dry sample. Similar effects of pretreatment on P fractions were reported by Barnett (1994b), who observed that freeze-dried manure sieved with a 2-mm screen produced a higher lipid P than finely ground (0.25 mm) material even though this fraction (lipid P) constituted only 2% of the total P. Akinremi et al. (2003) also observed a higher total P in fresh than in oven-dried poultry manure.
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CONCLUSIONS
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Results from this study clearly show that most of the P in biosolids was in a recalcitrant form. However, P in hog and cattle manures was mainly in labile forms that were soluble in water and NaHCO3. Inorganic P predominated in biosolids and hog and dairy cattle manures but not in beef cattle manure. The fact that a higher proportion of P in biosolids was soluble in stronger extractants like NaOH and HCl suggests that biosolids P may be less vulnerable to runoff loss compared with other amendments when applied to agricultural lands. Though dry manures are easier to handle compared with fresh forms, results from this study indicate that caution should be exercised in using pretreatments (such as oven-drying) for manure P studies.
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ACKNOWLEDGMENTS
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The funding for this study was provided by the City of Winnipeg Water and Waste Department and Canada-Manitoba Agri-Food Research and Development Initiatives (ARDI).
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TOP
ABSTRACT
INTRODUCTION
