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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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Granular strength was evaluated by placing 5 granules on a flat metal plate and estimating the amount of force required to crush the granule with the compression platens attachment of a TA-XT2 Texture Analyzer equipped with a 500 Newton (Nw) load cell (Texture Tech. Corp., Scarsdale, NY 10583) (Deng and Lin, 1997; McMullen et al., 2005). The attrition study, used to test for friction durability, was conducted by placing 100 g of "as-is" granules onto a 0.85 mm screen. The screen was shaken at 200 rpm for 10 min on an oscillating shaker. Particulates were captured beneath the sieve and weighed to determine the amount of weak granular material out of total test weight (ASABE, 2006).

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Moisture and elemental concentration of dry and wet ingredients used to formulate granules are presented in Tables 4.2a and 4.2b. Moisture content was determined by weighing 10 g subsamples and drying at 110°C for 48 h (Hoskins et al., 2003). Samples were cooled in a desiccator, weighed and moisture content calculated {moisture = [(dry sample weight + container) - (container weight)]/wet sample weight}.

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was weighed and incinerated using a LECO CN2000 combustion analyzer (LECO Corp., St. Joseph, MI 49085) (Colombo and Giazzi, 1982). Total elemental concentration was analyzed using a HNO3 digest (Hoskins et al., 2003). Digestion tubes (100 niL) had 0.25 g of product added and were pre-digested for 16 hr with 2.5 mL of concentrated HNO3.

Tubes were then heated for 45 min at 60°C on a digestion block. Three mLs of 30% H2O2 were added in 1 mL increments and tubes were digested for 1 h at 120°C until approximately 2 mL remained. Digests were brought to 25 mL volume using doubledeionized water, mixed on a vortex mixer, and filtered through Whatman 42 filter paper (Whatman pic, Middlesex, UK) into 25 mL scintillation bottles. Total elements were analyzed using inductively coupled plasma emission spectroscopy (SPECTRO CIROS ICP; SPECTRO Analytical Institute, Kleve, Germany).

Water soluble organic N, inorganic N, and DRP were determined using a PL analysis procedure described by Self-Davis and Moore (2000). Twenty g subsamples were extracted with double deionized water (1:10, w:w) at 200 rpm for 1 hr and centrifuged at 2415 xg for 20 min. Supernatant was vacuum filtered through a 0.45 urn membrane filter. An aliquot for total N, NH4-N and DRP determination was acidified to pH ~2 using 1 drop concentrated HC1 per 10 mL sample while a second non-acidified sample was used for NO3-N analysis. Dissolved reactive P, NH4-N and NO2-N+NO3-N were analyzed on a Sanplus System (SKALAR Inc., Norcross, GA 30071) using the Murphey-Riley colorimetric method (DRP), the modified Berthelot reaction (NH4-N), and the cadmium reduction method (NO2-N+NO3-N) (Murphey and Riley, 1962; Peters et al., 2003). Total N was determined by dry combustion and organic N was calculated by

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This experiment was a completely randomized design in a 2 (BS) x 2 (DCD) x 3 (binding agent) factorial arrangement of treatments; which were all fixed effects. Four replications were used in all procedures, except in the force to crush granules test, where 10 replications were used. Data were analyzed using analysis of variance conducted with the General Linear Model procedure (PROC GLM) in SAS v. 9.1 (SAS, 2003) at the 5% significance level.

Prior to statistical analysis, all elemental concentration values were adjusted to a granule moisture content of 120 g water kg" to alleviate confounding moisture concentrations between binding agents and formulations while density measurements were corrected to 0 g water kg" granule as directed by AS ABE (2006). Fisher's protected least significant difference (LSD) test was used to separate significant means (Steel and Torrie, 1980).

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Loose bulk density measurements were obtained to estimate container sizes needed for packaging and shipment. It is important to note that the following bulk density measurements were corrected to 0 g water kg" ; therefore, larger containers for packaging will be needed as moisture concentrations are increased (McMullen et. al., 2005). Triple superphosphate and urea fertilizers were denser than BS and PL (Table 4.3). Poultry litter is half as dense and contains 15 times less N than urea (Tables 4.2a and 4.3). This low N

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formulated products ranged in loose bulk density from 0.44 to 0.59 g cm (Table 4.4);

which was lower than commercially available urea and TSP fertilizers (0.76 and 1.09 g cm", respectively) (Table 4.3). Although the range between our products seems small, statistical differences were observed and slight bulk density changes due to processing will make considerable differences when scaled up to large transport and application vehicles. Loose bulk density measurements indicated that granules with formulations containing BS were denser than other formulations in a BS x DCD x binding agent interaction (Table 4.4). Formulations containing BS were denser since the BS dry ingredient was nearly 2 times as dense as fresh PL (0.70 and 0.37 g cm"3, respectively). In treatments without BS, lignosulfonate and urea formaldehyde produced heavier granules than water bound treatments (Table 4.4). Denser products would allow for more weight to be shipped per volume, reducing shipping cost per kilogram of N or P.

Packed bulk density measurements were 8.1 to 11.3% higher and generally mirrored loose bulk density results in a BS x DCD x binding agent interaction (Table 4.4). Differences between loose and packed bulk density measurements indicated that different rates of package or container settling will occur during shipment. Treatments containing BS and no DCD settled less when water bound versus lignosulfonate or urea formaldehyde binders. Similarly, no BS and DCD treatments had lower settling rates when water bound compared to other binders (Table 4.4). Overall, N-fortified PL and BS granular fertilizers settled more than prilled urea and fresh PL (5.9 and 8.1% for urea and PL, respectively) (Table 4.3).

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attrition test was used. Attrition measured strength of granules when exposed to friction due to shaking. Fines produced due to attrition may cause uneven spreading during application, are susceptible to blowing during windy conditions, and likely mineralize nutrients at different rates than larger particles. We found that various binding agents interacted with additions of BS and DCD to produce granules with varying levels of deterrence to attrition. Granules without BS or DCD and water bound were the weakest products during the attrition study as 3.68% fell through a 0.85 mm screen (Table 4.5).

Hinkle and Rosenthal (1991) found similar results with limestone when water was used as a binding agent. They found other binder agents, such as lignosulfonate, more suitable to the granulation process. Conversely, the same no BS and no DCD treatment had the strongest granules when bound with urea formaldehyde resin (0.34%) (Table 4.5). Water was one of the strongest binding agents when DCD and BS were included in the granule formulation (0.54%). Overall, N-fortified PL and BS granules were not as strong and produced more fines than TSP and urea (0.02 and 0.01%). Manufacturing, hauling, storing, and applying granules may require less forceful moving equipment than traditionally used with fertilizers, such as belts to move products instead of augers.

Crush tests to quantify product strength were conducted to determine the amount of force required to crush the granule between two metal plates. In a BS x binding agent interaction, averaged over DCD treatments, water bound treatments without BS had the weakest granule as 336 Nw was needed to crush the granule (Table 4.6). All other formulations with different binding agents were statistically similar. However, even the weakest granules required more force to crush than TSP and urea (260 and 238 Nw,

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Water extracted TN had isolated effects in a DCD x binding agent interaction, averaged over BS treatments (Table 4.7). The no DCD formulation bound with urea formaldehyde had more dissolved TN extracted (63.0%) than the urea formaldehyde bound granules with DCD (49.3%) or the water bound granules without DCD (49.3%) (Table 4.7). The TN in solution was mostly organic N (98.1%) with inconsequential concentrations of NH4-N (1.8%) and NO3-N (0.1%). However, we suspect that most organic N was dissolved urea and would be plant available within 3 to 7 d (Knud-Hansen andPautong, 1993).

A BS x binding agent interaction indicated highest percentages of TP present as DRP when no BS were added to formulations, averaged over DCD treatments (Table 4.8). Decreases in DRP as a percentage of TP in BS are attributed to the addition of metal salts during the wastewater treatment process and a long C chain charge neutralization polymer added during dewatering to assist in solids flocculation (ECO130LH, Ecotech Enterprises, Inc., Little Rock, AR 72223). Reduction of the DRP fraction may facilitate reducing DRP losses in rainfall events after fertilizer application. Similarly, additions of lignosulfonate and urea formaldehyde reduced the fraction of DRP present as TP compared to water bound granules (Table 4.8).

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The granulation process changed concentrations of inorganic N and P fractions that were readily extractable during the water shake study compared to pre-granulation

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be in each formulation based upon fresh ingredient concentrations in Table 4.2a and the ratio of each ingredient mixed together from Table 4.1. Assuming that binding agents impacted nutrient extractable concentrations during the water shake study, formulations should have a 0% change [(actual - calculated)/calculated concentration* 100] if all nutrients were extracted as calculated (assuming the binding agent had no effect and no N or P was lost in the granulation process), a negative value if N was lost through NH3 volatilization during the granulation process or granule stability held onto inorganic fractions during the water extract, or a positive value if mineralization of N or P from organic sources occurred.

A BS x binding agent interaction, averaged over DCD treatments, showed a loss of NH4-N in all granule formulations (Table 4.9). Urea formaldehyde bound granules had 74% less NH4-N extracted than amounts calculated from dry ingredients prior to granulation in treatments with BS (Table 4.9). Conversely, water bound granules with BS only had a reduction of 28% of calculated NH4-N. Treatments without BS had about half of the calculated NH4-N as water extractable forms regardless of binding agent. Loss of NH3 from BS and PL products during high heat granulation processes may account for some NH4-N reduction (Van Kessel et al., 1999); however, we cannot separate these NH4-N losses from responses of binding agents due to measurements taken. Regardless of binding agent or BS treatment, less NH4-N was readily released from granulated PL and BS fertilizers than fresh BS and PL ingredients. Less inorganic N decreases plant availability but also decreases risk of readily algae available forms in runoff, at least in the short-term until mineralization ensues.

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processes than inorganic N. In a BS x DCD x binding agent interaction, a range of 106 to 278% more DRP was extracted from granules than the maximum concentration we hypothesized to be available based on dry ingredient concentrations (Table 4.10).

Haggard and coworkers (2005) found 2 times more DRP in pelleted products compared to fresh PL when extracted on a 1:10 ratio (sample:water, w:w); similar to Toor and coworkers (2007) whom suggested 2.5 to 5 times higher concentrations of DRP after PL was granulated and pelletized. Pressure and heat during the granulation process possibly lysed microbial cells and released P previously not water soluble (Skipper and Westermann, 1973; Ferriss, 1984). Therefore, granular formulations are a source of higher plant available P concentrations compared to fresh PL and BS that could lead to increased P in runoff if surface applied to soils and not incorporated (Sharpley et al., 1986; Pote et al., 1996). Water-bound granules may pose a higher environmental risk since they mineralized and released more DRP than other binding agents while urea formaldehyde treatments had similar or less DRP released than lignosulfonate (Table 4.10). Formulations without BS consistently had more DRP released when DCD was added compared to no DCD treatments, an indication of weaker granules that readily dissolved and released nutrients when exposed to water.

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Cost to produce fortified granular fertilizers will ultimately decide the fate of this product. Required ingredients for these formulations ranged from $ 1.101" for tap water to $2651.511"1 for DCD (Table 4.11). Cost for ingredients in Table 4.11 includes shipping cost from their origin to the granulator facility (80 km). Necessary weights

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costs in Table 4.11 to give total ingredient cost. Variable costs represent labor, operation (electricity, gas, dryer, etc.), maintenance, and depreciation of a granulator plant producing 18 t of fertilizer per hour, 16 hours per day, 24 days per month for total production of-83,0001 fertilizer yr'1, equaling a cost of $21.23 t" (Robert Hinkle, personal communication, 2006). When adding ingredient and fixed costs of production, total costs to produce these formulations ranged from $124.77 t"1 for PLUB bound with water to $186.091"1 for PLUDCD bound with urea formaldehyde. Figured on a cost per kg N, PLU with any binder was the cheapest to produce ($0.82 kg N"1), while PLUBDCD bound with urea formaldehyde was the most expensive ($1.24 kg"1). Overall, granular products without DCD were produced with comparable cost per kg N as prilled urea ($0.99 kg N"1; based on 10 -yr price of urea and adjusted for inflation to base year 2007;

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