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«A dissertation submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Crop, Soil, and Environmental Sciences ...»

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Snyder, C.S., S.L Chapman, W.H. Baker, W.E. Sabbe, and Y.S. McCool. 1993. Changes in Arkansas' sampled acreage testing low and high in soil test phosphorus over the last 30 years. Soils and Fert. Inf. Article 1-93. Univ. of Arkansas Coop. Ext.

Serv., Little Rock.

Tabler, G.T. and I.L. Berry. 2003. Nutrient analysis of poultry litter and possible disposal alternatives. Avian Advice 5:1-3.

Tiessen, H. and J.O. Moir. 1993. Characterization of available P by sequential extraction, p. 75-86. In M.R. Carter (ed.) Soil sampling and method of analysis. Lewis Pub., Boca Raton, FL.

Tobert, H.A., T.C. Daniel, J.L. Lemunyon, and R.M. Jones. 2002. Relationship of soil test phosphorus and sampling depth to runoff phosphorus in calcareous and noncalcareous soils. J. Environ. Qual. 31:1380-1387.

Wang, H.D., W.G. Harris, and K.R. Reddy. 1995. Stability of phosphorus forms in dairyimpacted soils under simulated leaching. Ecol. Eng. 5:209-227.

Wood, C.W. 1998. Agricultural phosphorus and water quality: An overview, p. 5-12. In J.T. Sims (ed.) Soil testing for phosphorus - Environmental uses and implications.

South. Coop. Ser. Bull. 389. Univ. of Delaware, Newark.

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Veryhigh 334.6 a 8.9 b 1630.7a 43.3a 31.7c 0.8 d 479.7 a 12.7b 1192.9a 31.7a tSoluble and loosely bound-P (SLB-P), Al bound P (Al-P), Fe bound P (Fe-P), reductant soluble P (RS-P), and Ca bound P (Ca-P).

{Percentage of P in each fraction out of total soil P.

§For each column, means followed by the same letter are not significantly different at/?0.10 for each soil series.

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Fig. 3.1. Correlation of runoff dissolved reactive P (DRP) as a function of Mehlich-3 and water extractable soil test P concentrations for Captina, Frederick and Hoberg silt loam soils. Arrows represent critical points where DRP plateaus or declines as Mehlich-3 and water extractable P continued to increase.

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• • •. • <

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3.2. Relationship between Mehlich-3 extractable soil test P concentrations and percentage of Mehlich-3 extractable P as water extractable P (water extractable P + Mehlich-3 P x 100) for silt loam soils. Arrows represent asymptotes of Mehlich-3 P and runoff dissolved reactive P relationships from Fig. 3.1. The/? and r values were derived from linear regression by taking the natural log of both axis.

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Fig. 3.4. Relationship between Mehlich-3 extractable soil Ca concentration and percentage of Mehlich-3 extractable P as water extractable P (water extractable P

-*- Mehlich-3 P x 100) for silt loam soils. Arrows represent asymptotes of Mehlich-3 P and runoff dissolved reactive P relationships from Fig. 3.1 calculated in regression equations established between Mehlich-3 extractable P and Mehlich-3 extractable Ca in Fig. 3.3. The/? and r2 values were derived from linear regression by taking the natural log of both axis.

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Northwest Arkansas (NWA) is a region of high density confined animal feeding operations (CAFO) that produces annual surpluses of poultry litter (PL) and municipal biosolids (BS) that can be used in organic fertilizer formulations. The objective of this study was to evaluate the effect of various binding agents and a nitrification inhibitor [dicyandiamide (DCD)] on granule physical strength and nutrient water solubility. We produced 4 different granule formulations using agglomeration techniques with a pin mixer in a 2 x 2 x 3 factorial arrangement. Treatments included granules with and without BS, with and without DCD, and bound with lignosulfonate, urea formaldehyde, or water. These 12 granular products were tested for bulk density, physical strength and water soluble N and P. Overall, granulated products were bulkier (0.48 to 0.64 g cm") than commercial urea fertilizer and BS (0.81 and 0.76 g cm", respectively), but had a higher bulk density than fresh PL (0.40 g cm"3). Compared to urea and triple super phosphate (TSP) fertilizers, granules were more resistant to crumbling during force crush tests but degraded faster during attrition tests. Generally, the heat dependent granulation process increased granule DRP concentrations by up to 278% compared to unprocessed ingredients. Based on ingredient and production costs, granules can be produced for $0.82 to $1.24 per kilogram of N, similar to commercially available urea ($0.99 kg"1 N).

Organic, granular fertilizers also contain other macro and micronutrients that adds additional value to the formulations not accounted for in this study. Using the granulation process, significant amounts of PL and BS could economically be transported out of sensitive nutrient surplus watersheds in NWA to areas suffering from nutrient deficiencies.

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AS ABE, American Society of Agricultural and Biological Engineers; BS, municipal biosolids; CAFO, confined animal feeding operation; DCD, dicyandiamide;

DRP, dissolved reactive P; LS, lignosulfonate; LSD, least significant difference; Nw, Newton; NWA, Northwest Arkansas; PL, poultry litter; PLU, poultry litter + urea;

PLUB, PLU + BS; PLUBDCD, PLUB + DCD ; PLUDCD, PLU + DCD; rpm, rotations per minute; STP, soil test P; TSP, triple superphosphate; UF, urea formaldehyde; W, water.

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Northwest Arkansas, a region of high density CAFOs, produces annual surpluses of broiler litter (Slaton et al., 2004) and municipal BS (Northwest Arkansas Conservation Authority, 2003). Approximately 1.2 billion broilers (Gallus gallus domesticus) are produced annually in Arkansas, resulting in 1.7 million Mg of litter which is land applied to cool- and warm-season pastures (National Agricultural Statistics Service, 2006). With 28% of total state poultry production confined to 4 counties in NWA that represents only 6.3% of total land area (National Agricultural Statistics Service, 2004; USA Census Bureau, 2007), limited land is available for PL application, which leads to a buildup of excessive soil test P (STP) concentrations and contributes to runoff P (Edwards and Daniel, 1993; Slaton et al., 2004). The region is also experiencing unparalleled economic growth as evidenced by NWA being identified in 2005 as the 8th top regional economy in the USA by the Milken Institute (DeVol et al., 2006). Such economic potential translates into rapid regional population growth (15% of state population in NWA) (USA Census Bureau, 2007), increased production of municipal sewage BS and decreased available

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major municipalities of NWA (Northwest Arkansas Conservation Authority, 2003) and land application is not practiced due to the perceived risk of P loss and potential liability (DeLaune et al, 2006).

Fortunately, given some modification, environmentally stable uses of surplus PL and BS exist. Numerous studies have cited PL and BS as excellent fertilizer sources useful on the vast row crop production areas in eastern Arkansas operating on P and N deficient soils (Reynolds, 1926; Shorthall and Liebhardt, 1975; Bitzer and Sims, 1988;

Sistani et al., 1988). In addition to fertility, studies by Miller and coworkers (1990, 1991) showed restorative qualities of using PL on precision leveled soils while Brye and coworkers (2004) found positive influences on soil properties such as bulk density.

Equally important to agricultural production is the urban market which remains virtually untapped, awaiting the development of a formulation that meets urban needs.

Pelletizing PL and BS is a common industrial practice (AgriRecycle, 2007;

Milorganite, 2007); however, concerns exist regarding cost of production and end-user acceptance. Granulation, a process which produces small dense spherical particles (~3 mm) through centrifugal force and binding agent additions, was used successfully for decades to agglomerate powdery substances for ease in handling and storage. However, granulation of organic materials such as PL is a new approach by the fertilizer industry to address emerging environmental and production needs (Robert Hinkle, 2004; Lee Harris, 2004; personal communications). The granulation process produces a cheaper product than pelletized PL and BS ($21.25 t"1 vs. $24.89 t"1 for granulation and steam/pressure pellets, respectively), requires less capital cost ($123,200 vs. $2,720,000 for a granulator

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combined with municipal BS tipping fees, has the potential to be competitive economically (Wolfe et al., 2002).

Forming granules from PL and BS allows the incorporation of additives to enhance fertilizer performance both physically and nutritionally. Nitrogen additions would improve the current fertilizer N:P:K analysis of fresh PL and BS from 3:2:2 to 9:1:1 to closely match nutrient removal by crops. Southeast agricultural crops remove nutrients in ratios ranging from 4:1 (N:P) to 23:1 for corn (Zea mays) and tobacco (Nicotiana tabacum), respectively (International Plant Nutrition Institute, 2007).

Nitrification inhibitors, such as DCD, have potential to reduce N loss that is attributed to denitrification and leaching. Cabrera and coworkers (1993) indicated that the greatest loss of inorganic N from PL is correlated to NO3-N concentration. Inhibiting NH4-N from undergoing nitrification by using DCD would reduce N losses and increase fertilizer efficiency.

Binding agents are commonly used in the pelletizing industry to change pellet physical characteristics. Lignosulfonate, a by-product of paper manufacturing, showed beneficial binding characteristics for numerous powdery products such as ground alfalfa (Medicago sativa), limestone, and graphite (Hinkle and Rosenthal, 1991; Tabil et. al., 1997). Hinkle and Rosenthal (1991) found that lignosulfonate formed stronger granules than water alone but lignosulfonate may not be the strongest binder available (Tabil et al., 1997; Veverka and Hinkle, 2001). Neyman and Derr (2002) proposed using urea formaldehyde as a pellet binder due to its inherent adhesive properties when blending dry fertilizers while Tabil and coworkers (1997) used a lignosulfonate and urea formaldehyde

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binding agent used in granule and pellet production, has shown promise for powdery substances, and is the cheapest binder alternative (Hinkle and Rosenthal, 1991). Limited research is available concerning the use of nitrification inhibitors with organic amendments and the impacts of using different binding agents in the granulation process on their chemical, physical and nutrient water solubility.

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Poultry litter was collected from the Applied Broiler Research Unit at the University of Arkansas Experiment Station located in Savoy, AR. The bedding material consisted of 50% rice (Oryza sativa) hulls and 50% wood shavings, feces from 6 flocks of production broilers, and contained no litter treatment additives. Bird diet and environmental conditions were standard as prescribed by Simmons Foods, Inc. (Siloam Springs, AR 72761). To foster granulation, collected litter was ground until it passed a

5.8 mm screen and thoroughly mixed using a New Holland 352 feed mill mixer (CNH Global N.V., Lake Forest, IL 60045).

Biosolids were obtained from Stuttgart Municipal Water Works in Stuttgart, AR which were dried using a SludgeMASTER RK Indirect Sludge Dryer (Fen-Tech Environmental Inc., Brownwood, TX 76801) after aerobic wastewater digest. Biosolids were heated in temperature increments for 3 h. Initially, BS were heated to 343°C and then the temperature was lowered to 227°C as BS moved through the dryer. Dried BS were ground to pass a 1 mm screen by Pulva Corporation (Saxonburg, PA 16056).

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(Agrotain Int., LLC, Collierville, TN 38017) were weighed in appropriate ratios (Table 4.1) to give a final granular fertilizer mean analysis of 152 g N, 15 g P, 19 g K, and 303 g C. Dry ingredients were blended together in a rotary cement mixer for 30 min prior to granulation. The PL, BS and additives mixture was fed into a bench scale granulator (8D32L Pin Mixer, Mars Mineral, Mars, PA 16046) running at 1400 rotations per minute (rpm) using a vibrating screw feeder (1015 Series Volumetric Screw Feeder, Acrison Inc., Moonachie, NJ 07074) at a rate of 2.09 kg mixed dry product min"1. Binding agents were added through a 6502 nozzle (Spraying Systems Co., Wheaton, IL 60189) set at

0.276 MPa. Binding agents were tap water, lignosulfonate (Norlig G-58%, LignoTech USA, Inc., Bridgewater, NJ 08807), and urea formaldehyde (Resin 730D98, GeorgiaPacific Resins, Inc., Decatur, GA 30035) (Table 4.1). Urea formaldehyde was mixed on a 1:44 ratio (catalysturea formaldehyde resin, w:w basis) with a sulfuric acid and triethylamine catalyst to assist in thermosetting (Catalyst 4590, Georgia-Pacific Resins, Inc., Decatur, GA 30035) (Table 4.1). Granule samples used for evaluation were collected only after representative granules were being produced. After granulation, products were dried at 191 °C for 3.5 h until average water concentration was reduced to 120 g water kg"1 (McMullen et al., 2005).

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Loose bulk density measurements were calculated by pouring "as-is" fertilizer granules through a funnel from a 610 mm height into a 1000 mL graduated cylinder and the final weight recorded (American Society of Agricultural and Biological Engineers (ASABE), 2006). Packed bulk density readings were taken after the cylinder was lightly

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2006). The settling rate was calculated by subtracting loose bulk density measurements from packed bulk density readings.

Granule strength and durability were estimated by force and attrition tests designed to evaluate granular resistance to degradation due to friction and force exerted during manufacturing, hauling, storage, and application. Granules were compared to two commonly used benchmark granular fertilizers; urea and TSP. Granules used were prescreened to pass through a 4.75 mm sieve, while being retained on a 0.85 mm sieve.

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