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Nutrient and Solids Removal by Lime and Alum Treatment of Flushed Dairy Manure

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PAGE 1

NUTRIENT AND SOLIDS REMOVAL BY LIME AND ALUM TREATMENT OF FLUSHED DAIRY MANURE By HECTOR LAGO JOPSON A THESIS PRESENTED TO THE GRADUATE SCHOOL OF THE UNIVERSITY OF FLOR IDA IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF MASTER OF ENGINEERING UNIVERSITY OF FLORIDA 2004

PAGE 2

Copyright 2004 by Hector Lago Jopson

PAGE 3

This thesis is dedicated to my loving wife Ann and daughter Harriet, my parents, Reyland and Matilde Jopson, and to my sist er Hilda and brother Reyland Jr.

PAGE 4

ACKNOWLEDGMENTS The author would like to thank all of the members of his supervisory committee for their help and ideas throughout this effort. Dr. Roger A. Nordstedt, the committee chair, provided valuable time, guidance, and expertise of the subject. Acknowledgment is extended to Dr. Dorota Z. Haman and Dr. Donald A. Graetz for their insights and guidance. The author would also like to express gratitude to all of those within the Agricultural and Biological Engineering Department, especially Veronica Campbell, Senior Chemist, for lending her time and effort in assisting him with the laboratory experiments. The author would like to acknowledge the Fulbright Commission, Philippine American Educational Foundation, Institute of International Education, Philippine Department of Agriculture, and Western Mindanao State University for granting the opportunity to pursue his graduate studies here in the U.S. The author would like to thank his wife Ann, and daughter Harriet, for the unyielding love, support, prayers, and inspiration they offered him during these two years of being away from them. And lastly, gratitude is owed to the Almighty God, the infinite source of all goodness and love. iv

PAGE 5

TABLE OF CONTENTS page ACKNOWLEDGMENTS.................................................................................................iv LIST OF TABLES............................................................................................................vii LIST OF FIGURES...........................................................................................................ix ABSTRACT.......................................................................................................................xi CHAPTER 1 INTRODUCTION AND OBJECTIVES......................................................................1 Introduction...................................................................................................................1 Objectives.....................................................................................................................6 2 REVIEW OF LITERATURE.......................................................................................7 3 MATERIALS AND METHODS...............................................................................14 Manure Characterization............................................................................................14 Experimental Design..................................................................................................15 Effluent Samples.................................................................................................15 Arrangement of Treatments.................................................................................16 Selection of Chemical Dosage.............................................................................16 Treatment Procedure...........................................................................................18 Data Analysis.......................................................................................................19 4 RESULTS AND DISCUSSIONS...............................................................................21 Manure Characterization............................................................................................21 Preliminary Test on pH with Chemical Treatment.....................................................21 Alum Treatment..........................................................................................................22 BMPQ Treatment........................................................................................................24 Hydrated Lime Treatment With and Without Alum...................................................26 Test for Determining Difference of Treatments from Control...................................30 Curve Fitting Analysis................................................................................................31 v

PAGE 6

5 CONCLUSIONS AND RECOMMENDATIONS.....................................................34 Conclusions.................................................................................................................34 Recommendations.......................................................................................................36 APPENDIX A TABULATED MEANS.............................................................................................37 B STATISTICAL ANALYSIS RESULTS....................................................................39 Dunnet Method for a Comparison of all Treatments with a Control..........................39 Sample Output of SAS 8.2 Regression Analysis........................................................42 C PRODUCT SPECIFICATIONS OF CHEMICAL COAGULANTS.........................43 LIST OF REFERENCES...................................................................................................44 BIOGRAPHICAL SKETCH.............................................................................................48 vi

PAGE 7

LIST OF TABLES Table page 3-1 Chemical dosages.......................................................................................................18 4-1 Wastewater sample characterization results (n=10)...................................................21 4-2 Effects of hydrated lime and 108 mg Al/L of alum on the pH of the wastewater......22 4-3 Effects of alum and of hydrated lime on the pH of the wastewater...........................22 4-4 Effects on nutrients and solids with alum treatment...................................................23 4-5 Effects on nutrients and solids with BMPQ treatment...............................................25 4-6 Effects on nutrients and solids with hydrated lime and 432 mg Al/L treatment........27 4-7 Effects on nutrients and solids with hydrated lime and 108 mg Al/L treatment........29 4-8 Effects on nutrients and solids with hydrated lime treatment....................................29 4-9 A comparison of r2 between linear and quadratic regression for all parameters........32 A-1 Treatment with hydrated lime....................................................................................37 A-2 Treatment with hydrated lime and 108 mg Al/L.......................................................37 A-3 Treatment with hydrated lime and 432 mg Al/L.......................................................37 A-4 Treatment with alum..................................................................................................38 A-5 Treatment with BMPQ..............................................................................................38 B-1 Sample calculation for Dunnet method......................................................................39 B-2 Summary of the test for difference between control and treatments using Dunnet method D(4, 0.05) for treatment with hydrated lime alone......................................40 B-3 Summary of the test for difference between control and treatments using Dunnet method D(4, 0.05) for treatment with hydrated lime and 108 mg/L alum...............40 vii

PAGE 8

B-4 Summary of the test for difference between control and treatments using Dunnet method D(4, 0.05) for treatment with hydrated lime and 432 mg/L alum...............41 B-5 Summary of the test for difference between control and treatments using Dunnet method D(4, 0.05) for treatment with alum.............................................................41 B-6 Summary of the test for difference between control and treatments using Dunnet method D(4, 0.05) for treatment with BMPQ..........................................................41 C-1 Blended metallurgical pulverized quicklime product specification. Product of Chemical Lime Corporation, Forth Worth, Texas...................................................43 C-2 Hydrated lime product specification. Product of Fisher Scientific, Fair Lawn, New Jersey........................................................................................................................43 C-3 Alum product specification. Product of Fisher Scientific, Fair Lawn, New Jersey..43 viii

PAGE 9

LIST OF FIGURES Figure page 1-1 A GIS map of the distribution of dairy farms in Florida, courtesy of Florida Department of Agriculture and Consumer Services (2004).......................................4 3-1 University of Florida Dairy Research Unit.................................................................15 3-2 Agitated feed tank where samples were collected......................................................16 3-3 Simplified schematic diagram of liquid dairy manure treatment system, Riverview, Florida......................................................................................................................18 3-4 Mixing stage...............................................................................................................19 3-5 A closer look during the settling stage.......................................................................20 4-1 The response of pH over time with hydrated lime.....................................................23 4-2 Effect of alum addition on the pH of the wastewater.................................................24 4-3 A comparison of the TP and DRP concentrations after adding alum.........................24 4-4 A comparison of the TP and DRP concentrations after adding BMPQ.....................25 4-5 A comparison of the effects of hydrated lime alone and in combination with alum on TP concentration in three separate experiments.......................................................26 4-6 A comparison of the effects of hydrated lime addition alone and in combination with alum on DRP concentration in three separate experiments......................................27 4-7 A comparison of the reduction levels of TKN with treatment of hydrated lime alone and in combination with 108 mg Al/L and 432 mg Al/L in three separate experiments..............................................................................................................28 4-8 A comparison of the reduction levels of NH3-N with treatment of hydrated lime alone and in combination with 108 mg Al/L and 432 mg Al/L in three separate experiments..............................................................................................................28 4-9 Effects of hydrated lime addition alone and in combination with alum on the pH of the samples...............................................................................................................30 ix

PAGE 10

4-10 A quadratic regression curve fit with the TP data points taken from the treatment with hydrated lime alone. The calculated r2 for this curve was 0.997.....................31 x

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Abstract of Thesis Presented to the Graduate School of the University of Florida in Partial Fulfillment of the Requirements for the Degree of Master of Engineering NUTRIENT AND SOLIDS REMOVAL BY LIME AND ALUM TREATMENT OF FLUSHED DAIRY MANURE By Hector Lago Jopson December 2004 Chair: Roger A. Nordstedt Major Department: Agricultural and Biological Engineering Dairy farms utilizing flushed manure systems deal with voluminous liquid manure on a daily basis. To maintain the effective storage capacity of storage ponds, tanks, and lagoons, an irrigation system is usually employed for land application of wastewater. This repeated application of dairy wastewater on limited cropland can result in high levels of nutrients, especially phosphorus (P), in the soil. Runoff from these areas can potentially increase the risk of eutrophication of nearby surface water and leaching into the groundwater. Presently, solids separators have proven inefficient in removing the solids and nutrients from the liquid dairy manure. An effective and sustainable system must be developed to further reduce the solids and nutrients. The field demonstration project in Riverview, Florida, where hydrated lime slurry and alum were used to remove nutrients and solids from a flushed dairy manure system, was the basis for this laboratory evaluation. This study evaluated the effectiveness of hydrated lime, a commercial quicklime product, alum, and combined hydrated lime and xi

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alum in reducing the levels of solids and nutrients, especially P, in liquid dairy manure after mechanical separation. Preliminary investigation on the effect of hydrated lime and alum on the pH of the wastewater with respect to time was conducted on 100 ml samples. With high dosages of hydrated lime (406 mg Ca/L), the pH stabilized to about 11.4 and 11.5 in about 5 minutes. When 216 mg Al/L of alum was added to untreated wastewater, the pH after 5 minutes decreased rapidly to about 4.4. The combination of each dosage of hydrated lime (135 mg Ca/L, 271 mg Ca/L, 406 mg Ca/L, and 541 mg Ca/L) with 108 mg Al/L of alum resulted in a final pH range of 6.6 to 9.0 after 15 minutes. Laboratory tests of liquid dairy manure containing an average of 0.70% total solids (TS) showed that, when compared to the control (no chemical addition), the addition of hydrated lime combined with alum performed best in reducing the levels of total phosphorus (TP), dissolved reactive phosphorus (DRP), and total Kjeldahl nitrogen (TKN) by 98%, 99%, and 59%, respectively. Treatment with hydrated lime reduced the volatile solids (VS) by about 66.2%, while the addition of only alum reduced VS by about 34%. When the resulting pH of the solution is considered, especially for potential applications on dairy flush systems that recycle the treated wastewater, the combination of hydrated lime (676 mg Ca/L) and alum (432 mg Al/L) performed best by achieving a pH between 7 and 8 and at the same time reducing TP and DRP by about 95% and 98%, respectively. However, the combination of hydrated lime (676 mg Ca/L) and a lesser amount of alum (108 mg Al/L) removed 77.7% of TP. Curve fitting analysis showed that effects on P removal were greatest with removal curves best described by a quadratic polynomial (TP r2 = 0.99 and DRP r2 = 0.97). xii

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CHAPTER 1 INTRODUCTION AND OBJECTIVES Introduction A significant amount of pollutants entering lakes, estuaries, streams, and groundwater in the United States (U.S.) results from agricultural activities. The harmful consequences of farm production on water quality include soil erosion; runoff into lakes, rivers, and streams of fertilizers, animal wastes, and pesticides; and leaching into groundwater of nutrients and pesticides. Pollution from agricultural operations is only one source of water quality problems. Discharges from industrial activities and municipal sewage treatment plants, stormwater runoff, and naturally occurring contaminants are also potential sources of water pollution. However, the U.S. Environmental Protection Agency (EPA) considers nonpoint source pollution from agriculture as the primary contributor to the nations surface water quality deterioration. A 1998 EPA Water Quality Inventory report showed that more than one-third of the river miles, lake acres, and estuary miles are impaired to some degree (U.S. EPA, 2000). Water pollution may be categorized into two types based on sources. Point sources discharge effluent directly into water bodies through an identifiable pipe, ditch, or other conveyance. Industrial and municipal effluents are examples of this category. Non-point source (NPS) pollution comes from diffuse sources such as runoff and leachate from rain or snow melt. Unlike point source pollution, NPS pollution is difficult to regulate because it is not readily identifiable. Nutrients, sediments, pesticides, salts, and pathogens are the major agricultural pollutants contributing to NPS pollution. 1

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2 Nutrients such as nitrogen (N), phosphorus (P), and potassium (K) are essential for plant growth. Of these three nutrients, N and P can cause quality deterioration when they enter water systems. Nitrogen and P accelerate aquatic plant and algal production in receiving surface waters, a condition known as eutrophication. Accelerated eutrophication causes a variety of problems, including fish kills, human health issues, clogged pipelines, and reduced recreational opportunities. Nitrogen is primarily the limiting nutrient in brackish or salt water and P in freshwater. In Florida and many other areas in the U.S., there have been serious concerns over surface water and groundwater pollution from agriculture, especially from animal production facilities. Floridas water resources such as lakes, rivers, springs, and beaches attract millions of tourists annually. But with the threat of diminishing water quality due to eutrophication, this multi-million dollar industry may be adversely affected. In addition, Floridas drinking water supplies come largely from groundwater. Since surface water is ultimately linked to groundwater at some point, N from agricultural operations can leach through underwater systems and become a health problem for those who drink water directly pumped from groundwater. The U.S. national drinking water standard sets a maximum nitrate-N concentration as 10 mg/L. Above this level it is considered harmful, especially to infants, causing a condition called methemoglobinemia (Craun et al., 1981). In recent years, Floridas dairy industry has been striving to meet the needs of the state for milk. Though the number of dairy farms has decreased in Florida, the herd size has increased. Figure 1-1 shows the distribution of dairy farms in the state of Florida. The average herd size in the state is about 693 milk cows per dairy farm, one of the

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3 nations largest (University of Florida Institute of Food and Agricultural Sciences [UF/IFAS], 2001). The Florida Agricultural Statistics Service (FASS) reported that as of January 2004, dairy cow numbers were estimated at 140,000 milk cows and 40,000 replacement cows (FASS, 2004). This translates to a fresh manure production of 9,907 tons/day or 3.6 million tons/year (American Society of Agricultural Engineers [ASAE], 2003). Handling and disposal of these voluminous wastes create additional burdens to the dairy farmers, not to mention the environmental issues these wastes pose. Growing public concerns associated with nutrient losses from manure of large dairy herds as well as other sources have been overwhelming in Florida. The eutrophic condition in Lake Okeechobee (second largest freshwater lake in the continental U.S.) due to P contamination from farm runoff and nitrate-N losses into the groundwater through the sandy soils of the Suwannee River Basin (largest undammed drainage basin in the U.S. Coastal Plain) are causes of these major concerns. Most dairy farms in Florida utilize flushing to a lagoon, storage pond, or storage tank to remove manure from confinement facilities. An irrigation system is usually employed for land application of wastewater. Dairy farm wastewater normally contains a large percentage of solids and nutrients, and one conventional method being used to deal with them is by separating the solids through sedimentation and mechanical solids separators. By separating the solids, less sludge is formed in the lagoon, thus extending its capacity. However, this method has proven to be inefficient because only a small percentage of the solids and nutrients are removed. Most of the solids and nutrients end up in the lagoon or storage pond. When the liquid waste from the lagoon is applied to limited cropland through spray irrigation, more nutrients, especially N and P,

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4 Figure 1-1. A GIS map of the distribution of dairy farms in Florida, courtesy of Florida Department of Agriculture and Consumer Services (personal correspondence, June 15, 2004). accumulate in the soil and increase the risk of surface and ground water contamination. Due to stricter environmental regulations, dairy farms have to implement systems that

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5 incorporate significant levels of new or existing technology to ensure that nutrients are handled efficiently in an environmentally friendly manner. For the past several decades, chemical treatment of municipal wastewater has proven effective in precipitating solids and P. The coagulants most commonly used have been lime, alum, and iron salts. Recently, applications of chemical removal with flocculants and coagulants to treat animal manure have shown promising improvement in solids and P removal compared to physical separation methods only. Since water is the major constituent of liquid manure, it is very expensive to transport off of the farm. If a fairly significant amount of the solids and nutrients can be concentrated into a small portion of the total manure volume, then it may be economical to haul this concentrated portion farther and to land that may not have an oversupply of nutrients. The treated wastewater can then be diverted back to flush tanks for reuse. Since this technology has proven successful in municipal wastewater treatment, it is therefore worth investigating whether this treatment process can increase the removal efficiency of solids and nutrients in liquid dairy manure. Earlier investigations on the use of coagulants to treat various types of animal wastewater have to be re-evaluated in terms of correlation between laboratory and field scale test results. Furthermore, to minimize the cost of chemical treatment, dairy farmers must know how many chemicals are needed to efficiently reduce the nutrients and solids in the wastewater. Adding more chemicals does not necessarily mean that the dairy wastewater treatment system will work more efficiently. Thus, finding the best combination of chemicals in minimum amounts that will satisfactorily meet the desired removal efficiency is highly important for the system to be cost effective.

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6 Objectives The overall objective of this research was to improve solids, nitrogen, and phosphorus removal from a flushed dairy waste management system using alum and lime. Specifically, it aimed to a) evaluate and characterize the liquid dairy manure following mechanical separation, and b) compare the effectiveness of varying concentrations of lime and alum, alone or in combination, in maximizing removal of solids and nutrients from the wastewater.

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CHAPTER 2 REVIEW OF LITERATURE In recent years, there has been tremendous progress in addressing various aspects of water pollution. As a result of the Clean Water Act, point source pollution such as industrial discharges has been controlled by permits, and raw sewage discharges have been reduced by the construction of sewage treatment plants. Nonpoint source pollution (NPS) such as runoff from agricultural operations has become the main focus of extensive scientific research. Nutrients such as nitrogen (N) and phosphorus (P) from fertilizers and animal manure contaminate surface and groundwater, preventing the attainment of the water quality goals stipulated in the Clean Water Act (U.S. EPA, 1988; Parry, 1998). The presence of P in runoff from agricultural land is a significant component of NPS pollution and has been reported to cause surface water eutrophication (Corell, 1998). Eutrophication is the overenrichment of receiving waters with mineral nutrients resulting in excessive production of autotrophs such as algae and cyanobacteria. According to the U.S. Environmental Protection Agency (EPA), major surface water quality deterioration is brought about by increased eutrophication due to anthropogenic activities (U.S. EPA, 1996). Sharpley et al. (1999) reported that the presence of P is especially correlated to or associated with nutrient enrichment of normally oligotrophic surface water. Algal blooms and the growth of thick masses of weeds can limit the use of a water body for recreation, fisheries, and industries. Anoxia, a condition of deficiency of dissolved oxygen due to high bacterial population and high respiration rates, can 7

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8 decimate aquatic animal populations (Corell, 1998). The zone of hypoxia in the Mississippi delta is attributed partly to excessive release of nutrients from agricultural runoff (Fouss et al., 2003). Eutrophication of Chesapeake Bay and North Carolinas estuaries and coastal waters in recent years is a classic example of a public health issue associated with nutrient loadings of surface water. Outbreaks of the toxic dinoflagellate Pfiesteria piscicida resulted in fish kills and short term memory impairment in fishermen and other workers involved with sampling the rivers (Boesch, 2000). Among various sources of P, the most significant threat of accelerated eutrophication of adjacent surface water occurs in watersheds having a large concentration of animal manure production (Duda and Finan, 1983; Daniel et al., 1994; Sharpley et al., 1997). The continuous application of animal wastes based on plant N requirements has caused build up of P in an increasing number of areas, thus increasing the likelihood of excessive P in runoff (McFarland and Hauck, 1995). Sharpley et al. (1999) reported that P levels exceeding 0.02 mg/L have been shown to significantly increase the rate of eutrophication in lakes and streams. States such as Delaware, Maryland, and Virginia have passed nutrient management laws and regulations to reduce P inputs to surface waters (Sims, 2000). Phosphorus applications in agricultural productions are restricted or prohibited in areas where high P soils are tested. For example, in Delaware the Nutrient Management Act of 1999 allows a maximum P application rate to high P soils equivalent to the three year crop removal rate or one application every three years(Sims, 1999). Sandy soils such as those found in Florida require a different approach in terms of management of P. Harris et al. (1996) pointed out that soils with seasonally high water

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9 table and poor P retention capacities are potentially susceptible to P leaching. Most of the large animal production facilities such as beef and dairy operations are situated in the south and central part of Florida where the dominant types of soils are Histosols, Spodosols, and Entisols (Flaig and Reddy, 1995). Excess nutrients, especially P accumulated in soils treated with organic waste (such as animal manure), have the potential to leach into the soil and enter the surface water through lateral transport when clay, Fe, Al, and Ca compounds adsorbing P are absent or low in concentration in the surface horizon (Campbell et al., 1995; Graetz and Nair, 1995). Dairy farms with solids separation systems are still dealing with high concentrations of nutrients and solids in the effluents. This is chiefly a result of the inefficiency of solid separators which remove only a small fraction of the solids (<30%) and about 10 to 20% of organic N and P (Barrow et al., 1997; Vanotti and Hunt, 1999). A study conducted by Moller et al. (2000) concluded that simple mechanical separators can separate dry matter into a solid fraction, however, the efficiency of P removal is low and almost no N is separated. As a result, substantial amounts of N, P and solids are still present in the liquid waste. Storage ponds and lagoons continuously fill up with solids containing P and odorous compounds. Due to the high cost of transporting manure slurry, liquid wastes are often land applied to limited land areas. These repeated liquid waste applications could exceed the crop uptake and the P sorption capacity of soil and increase P leaching and losses through subsurface drainage (Johnson et al., 2004). In order to remove more solids and nutrients from animal liquid waste handling operations, another method should be employed that will eventually meet the desired removal efficiency.

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10 Municipal and industrial wastewater treatment systems using chemical coagulants such as lime, alum, ferric sulfate, and ferric chloride have been commonplace since 1970 (Lind, 2003). Recently, the use of these coagulants and flocculants after solids separation in animal wastes to efficiently reduce solids and P has been reported (Sherman et al., 2000; Chastain et al., 2001). Lime is often used to treat wastewater to remove solids and phosphorus. Control of pathogenic microorganisms in wastewater is also possible when lime is applied due to its high pH which destroys the cell membranes (National Lime Association, 2004). In addition, when pH is high, calcium ions react with odorous sulfur species such as hydrogen sulfide and organic mercaptans, thereby reducing odor (National Lime Association, 2004). When lime is added, it reacts with the natural bicarbonate alkalinity of wastewater forming CaCO3. Above pH 10, calcium ions react with phosphate ions precipitating hydroxylapatite [Ca 10 (PO 4) 6 (OH) 2] (Metcalf and Eddy, 2002). Thus, the alkalinity of wastewater is important in determining the chemical dosage of lime rather than the amount of phosphate present. Metcalf and Eddy (2002) suggest that lime dosage required to precipitate P is about 1.4 to 1.5 times the total alkalinity expressed as CaCO3. A study by Barrow et al. (1997) showed that the addition of hydrated lime to simulated dairy flushwaters reduced total solids by about 70%. In batch level jar tests, Karthikeyan et al. (2002) showed that lime was effective in removing total phosphorus (TP) and dissolved reactive phosphorus (DRP) by 96% and 92%, respectively, for dairy wastewater with 1.6% total solids (TS). Vanotti et al. (2002) reported the removal of almost 100% of P from swine wastewater using lime after a nitrification pre-treatment.

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11 The researchers explained that without a nitrification process the presence of ammonia and alkalinity would exert high buffering capacity which prevented P from precipitating. Alum [Al 2 (SO 4) 3] has been commonly used to chemically treat water and wastewater. Metcalf and Eddy (2002) reported that aluminum metal ions bind with phosphate on a 1:1 molar ratio. However, the reactions are dependent upon several factors such as alkalinity, pH, trace elements and ligands found in wastewater, thus necessitating bench scale and if possible full-scale tests to determine the required dosages (Metcalf and Eddy, 2002). Laboratory tests conducted by Jones and Brown (1999) showed that 99% of ortho-phosphorus (initial concentration was 13.86 mg P/L) was reduced by treating dairy wastewater with a dosage of 3 g/L of alum but beyond this dosage, removal efficiency actually decreased. A similar study by Karthikeyan et al. (2002) reported removal efficiencies of 99%, 92%, and 92% for DRP, total dissolved phosphorus (TDP), and TP, respectively, for a dairy manure with 0.8% TS and dosage rate of 8 mM as Al. The concentrations of DRP, TDP, and TP prior to treatment were 15.5 mg/L, 38.1 mg/L and 255.8 mg/L. A detailed laboratory study by Zhang and Lei (1998) reported that additions of aluminum sulfate effectively enhanced settling of manure solids by promoting coagulation of suspended particles. Moore et al. (1995, 1996) evaluated several chemical additives for broiler litter and concluded that alum was the most effective and economical in reducing soluble P and ammonia volatilization. In a study by Ndegwa et al. (2001) utilizing swine manure, suspended solids (SS) and P were reduced by 96% and 78%, respectively, using a dosage of 1,500 mg/L of alum. However, the authors did not specify the P concentration prior to chemical treatment.

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12 Nutrient removal using chemical additives involves three processes: a) coagulation, b) flocculation, and c) precipitation of the aggregated floc (Francois and Van Haute, 1985). Chemical coagulation entails reactions or processes that facilitate charge neutralization which results in the destabilization of suspended particles, allowing aggregation. Then, aggregated particles can be easily separated by passive or mechanical means. Flocculation refers to the process of particle size increase due to collision. Floc formation can result when a chemical coagulant is added to destabilize the colloidal particles in wastewater. A flocculant is used to enhance the flocculation process. The most common coagulants and flocculants include natural and synthetic polymers, metal salts such as alum, ferric and ferrous sulfate, and prehydrolized metal salts such as polyaluminum chloride and polyiron chloride (Metcalf and Eddy, 2002). The practice of using coagulants has a long history that dates back to ancient times. Alum, alone or in combination with lime, ferric sulfate and ferric chloride, has been used to treat water. As early as 2000 B.C., the Egyptians used crushed almonds to clarify drinking water as well as waters from the Nile River (Faust and Aly, 1998). Alum and lime were reportedly used as coagulants by the early Romans to make bitter water potable (Faust and Aly, 1998). In 1885, the first scientific study on coagulation with the use of alum was conducted by Austen and Wilbur. They reported that alum clarified water, and this type of treatment would not impair the taste or physiological properties of water (Faust and Aly, 1998). Although investigations and others have shown the effectiveness of chemical coagulants and flocculants, the results vary due to a lack of standardization. The concentration of flocculants and coagulants, percentage of total solids (TS) present in

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13 samples, type of solids separator used (screening or sedimentation) are parameters that have to be fully investigated. Bench scale tests are therefore highly recommended to test appropriate dosages of chemical coagulants and flocculants specific to the characteristics of animal wastes and method of solid separation. A more effective system will provide more benefits for animal waste handling facilities, such as reduced solids and P in effluents, less odor problems, easier handling and transport, and more capacity for storage ponds and lagoons.

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CHAPTER 3 MATERIALS AND METHODS Manure Characterization Initial characterization of flushed dairy manure collected from the University of Florida Dairy Research Unit included the following parameters: total solids (TS), volatile solids (VS), total Kjeldahl nitrogen (TKN), ammonia-nitrogen (NH3-N), total phosphorus (TP), dissolved reactive phosphorus (DRP), soluble potassium (K), and pH. Filtered samples were analyzed for DRP using the stannous chloride-based colorimetric method at a wavelength of 690 nm. For TP analysis, samples were digested using the persulfate digestion method prior to colorimetric analysis. Calibration curves prepared from known phosphorus standards were used to determine the concentrations of TP and DRP in mg/L (American Public Health Association [APHA], 1989). For TKN determination, samples were digested and distilled following the semi-micro Kjeldahl procedure (APHA, 1989). Samples analyzed for NH3-N underwent preliminary distillation. Both TKN and NH3-N were measured using the titrimetric method. Soluble potassium was determined using a specific ion electrode (Orion Research Inc., Boston, MA), and pH was determined using a probe (Orion Research Inc., Boston, MA). A calibration curve using known standard solutions of K was used to determine the values in mg/L (APHA, 1989). Total and volatile solids determination of the supernatant and settled solids was done by following the APHA (1989) standard methods. 14

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15 Experimental Design Effluent Samples The University of Florida Dairy Research Unit employs a mechanical separator (Agpro Extractor, Agpro Inc., Paris, TX) followed by a settling basin to separate the solids from the wastewater (Figure 3-1). The samples used in this study were effluents from the mechanical separator and settling basin before the wastewater overflowed into an agitated feed tank for anaerobic digester (Figure 3-2). The wastewater was collected in a 20 L plastic container and transported immediately to the laboratory. The wastewater sample was stored at 4 C for no more than 48 hours to inhibit microbial and chemical transformations. Figure 3-1. University of Florida Dairy Research Unit.

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16 Figure 3-2. Agitated feed tank where samples were collected. Arrangement of Treatments All chemical treatments were added to one liter of wastewater and evaluated as follows: Al as Al2 (SO4)3*18H2O alone at four concentrations Ca as Ca (OH) 2 alone at four concentrations, Ca as CaO alone at four concentrations, Ca as Ca (OH) 2 at four concentrations in combination with two concentrations of Al as Al2 (SO4)3*18H20. A control with no chemical addition was included for each treatment. The source of CaO was blended metallurgical pulverized quicklime (BMPQ) produced by Chemical Lime Corporation, Ft. Worth, Texas. BMPQ contains 32.54% of MgO, SiO2, Fe2O3, Al2O3, and 48.22% Ca (Appendix C). Selection of Chemical Dosage In a demonstration project in Riverview, Florida, the Agricultural and Biological Engineering Department at the University of Florida is involved in a demonstration of

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17 hydrated lime slurry and alum treatment of dairy wastewater after mechanical separation (Figure 3-3). The lime slurry had 35% solids by weight. Once added to the wastewater, the pH significantly increased. Alum solution, which was 48% by weight, was added to the lime-treated wastewater to lower the pH before it was diverted into the flush tanks for reuse. The amount of chemicals added to the wastewater was controlled by a pH controller. Lime was continuously added into the mixing tank as long as the pH was below 11.5. Once this pH was achieved, lime feeding automatically stopped and alum was injected to lower the pH of the wastewater. Since the exact amounts of chemicals being added could not be measured, the chemical dosages for the laboratory test had to be prepared in such a way that the pH of the treated samples was similar to the actual field conditions. Preliminary laboratory tests for pH were conducted using 100 ml samples and the effects of chemical addition were recorded with respect to time. Stocks of chemical solutions were prepared as follows: 133.2 g/L (200 mM) of alum [Al2 (SO4)3*18H2O], 50 g/L (675 mM) of hydrated lime [Ca (OH) 2], 50 g/L (890 mM) of BMPQ. BMPQ was included in the laboratory experiment to determine how it affected the pH, as well as the removal efficiency of solids and nutrients. In some cases Mg has been shown to decrease volume of settled solids (Wu, 2002). The chemical dosages (Table 3-1) for alum were 1.332 g/L (108 mg Al/L), 2.664 g/L (216 mg Al/L), 5.328 g/L (432 mg Al/L), 10.66 g/L (863 mg Al/L), and control (no alum addition). The dosages for hydrated lime were 1.25 g/L (676 mg Ca/L), 2.5 g/L (1,353 mg Ca/L), 5 g/L (2,705 mg Ca/L), 7.5 g/L (4,058 mg Ca/L), and control (no hydrated lime). For BMPQ, the dosages were 1.25g/L (603 mg Ca/L), 2.5 g/L (1,205 mg Ca/L), 5 g/L (2,411 mg

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18 Ca/L), 7.5 g/L (3,616 mg Ca/L), and control (no BMPQ). Each chemical dosage was added to 1 liter of liquid dairy wastewater. Figure 3-3. Simplified schematic diagram of liquid dairy manure treatment system, Riverview, Florida. Table 3-1. Chemical dosages. Alum (mg Al/L) Control 108 216 432 863 Hydrated Lime (mg Ca/L) Control 676 1353 2705 4058 BMPQ (mg Ca/L) Control 603 1205 2411 3616 Hydrated Lime (mg Ca/L) + 108 mg Al/L Alum Control 676 1353 2705 4058 Hydrated Lime (mg Ca/L) + 432 mg Al/L Alum Control 676 1353 2705 4058 Treatment Procedure Jar test experiments were employed to determine the effect of chemical coagulants on nutrients and solids in the wastewater. A 6-paddle Floc Illuminator bench top stirrer (Phipps and Bird, Inc. Richmond, Virginia) was used to mix one liter samples (Figure 3-3). The jar test procedure consisted of 3 steps: rapid mixing, slow mixing, and settling period. The stirrer was set to rapidly mix the samples at 100 rpm for 2 minutes, followed

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19 by 8 minutes of slow mixing at 35 rpm. Finally, the flocs were allowed to settle for 50 more minutes without agitation. The pH of each sample was measured prior to chemical addition and after the settling stage. All chemicals were added at the beginning of the rapid mixing stage. Data Analysis Nutrient and solids reductions were determined by analyzing the supernatant solution and comparing the results to the analyses of the untreated wastewater. The volume of settled solids was measured after the settling period using a graduated cylinder, and subsamples were tested for TS. A sufficient amount of supernatant was collected from each beaker, and solids and chemical analyses were performed Figure 3-4. Mixing stage.

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20 Figure 3-5. A closer look during the settling stage. immediately. Likewise, the difference between TKN, NH3-N, TP, DRP, and soluble K concentrations in the control and their corresponding levels after chemical treatment was used to determine the percent reduction. The Dunnet test (Kuehl, 2000) was used to determine if the results generated from the treated samples were significantly different from the control. Curve fitting analysis using polynomial regression was done to determine which model best described the data.

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CHAPTER 4 RESULTS AND DISCUSSIONS Manure Characterization Wastewater samples were collected from a sedimentation tank at the University of Florida Dairy Research Unit after the wastewater had undergone mechanical separation. The liquid manure samples were tested and were found to have TS and VS averages of 0.70% and 69.1%, respectively (Table 4-1). DRP and TP concentrations averaged 18.1 mg/L and 82.4 mg/L, respectively. The effluent samples contained an average of 257 mg/L of TKN. Similarly, the NH3-N level was 175 mg/L. The average soluble K and pH were 976 mg/L and 7.5, respectively. A complete summary of the analyses for the effluent samples is shown in Table 4-1. Table 4-1. Wastewater sample characterization results (n=10). Standard Characteristic Units Mean Deviation TP mg/L 82.4 25.4 DRP mg/L 18.1 1.0 TKN mg/L 257 75.7 NH3-N mg/L 175 13.9 K mg/L 976 6.7 TS % 0.70 0.10 VS % 69.1 2.2 pH 7.5 0.20 Preliminary Test on pH with Chemical Treatment Laboratory experiments were conducted to determine the pH response in terms of varying concentrations of hydrated lime, alum, and a combination of hydrated lime and alum (108 mg Al/L) with respect to time. For the combined treatment, hydrated lime was 21

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22 added first followed by alum after 5 minutes. Results showed that after 15 minutes, higher dosages of lime (>406 mg Ca/L) achieved a final pH of 8 to 9 while at lower dosages (<271 mg Ca/L), the pH was between 6 and 7 (Table 4-2). Treatment with 216 mg Al/L of alum decreased the pH to 4.4 after 10 minutes and remained at 4.3 after 15 minutes, while for hydrated lime, the highest dosage of 541 mg Ca/L caused the pH to increase to 11.4 after 5 minutes and stabilized at 11.5 thereafter (Table 4-3 and Figure 4-1). Determining the pH response time was important for the field demonstration project to make sure that the pH of the wastewater in the lime mixing tank had stabilized before the addition of alum. Table 4-2. Effects of hydrated lime and 108 mg Al/L of alum on the pH of the wastewater. Time (min) Hydrated Lime with 108 mg Al/L (mg Ca/L) 135 271 406 541 0 7.9 7.9 7.9 7.9 5 8.7 10.2 11.3 11.3 10 7.7 8.6 10.2 11.0 15 6.5 6.9 8.3 9.0 Table 4-3. Effects of alum and of hydrated lime on the pH of the wastewater. Time Alum (mg Al/L) Hydrated Lime (mg Ca/L) (min) 27 81 108 216 135 271 406 541 0 7.8 7.8 7.8 7.8 7.3 7.3 7.3 7.4 5 6.6 6.1 5.4 4.4 8.4 9.0 11.3 11.4 10 6.6 6.0 5.2 4.3 8.6 10.7 11.4 11.5 15 6.6 6.0 5.2 4.3 8.8 10.8 11.4 11.5 Alum Treatment Treatment with alum at 432 mg Al/L significantly reduced TP and DRP concentration by 94% and 97.9%, respectively. The levels of TKN, NH3-N, and %TS significantly decreased (Table 4-4). VS decreased by 61.5% at dosage level of 432 mg Al/L. This was also the maximum dosage level before the TP and DRP

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23 0.02.04.06.08.010.012.014.0051015Time (minute)pH 135 mg Ca/L 271 mg Ca/L 406 mg Ca/L 541 mg Ca/L Figure 4-1. The response of pH over time with hydrated lime. concentrations began to increase in the wastewater. Consistent decrease in pH was observed with increasing dosage of alum as shown in Figure 4-2. At pH level below 4.6, P resolubilized bringing about an increase of P concentration in the solution (Fig. 4-3). Appendix A contains the actual measurements for all the parameters. Table 4-4. Effects on nutrients and solids with alum treatment. Alum treatment level (mg Al/L) Control 108 216 432 863 TP mg/L 31.8 3.8 2.1 1.8 14.0 % Removal 88.2 93.4 94.3 56.1 DRP mg/L 29.7 10.3 3.0 0.60 12.4 % Removal 65.4 90.1 97.9 58.3 TKN mg/L 189 108 113 117 111 % Removal 43.0 40.0 37.8 41.5 NH3-N mg/L 112 106 101 99.4 96.6 % Removal 5.0 10.0 11.3 13.8 K mg/L 397 380 362 355 372 % Removal 4.2 9.0 10.5 6.3 TS % 0.49 0.37 0.32 0.37 0.32 % Removal 23.7 33.5 25.0 34.1 VS % 64.3 49.8 32.2 24.8 43.1 % Removal 22.7 50.0 61.5 33.0 pH 7.4 6.5 5.8 4.6 4.0

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24 012345678Control108216432863mg Al/LpH Figure 4-2. Effect of alum addition on the pH of the wastewater. 05101520253035Control108216432863mg Al/LP ( mg/L) TP DRP Figure 4-3. A comparison of the TP and DRP concentrations after adding alum. BMPQ Treatment The average reduction of TP and DRP ranged from 26.6% to 85.8% and 57.5% to 89.4%, respectively. Compared with alum treatment alone, the reduction efficiencies with BMPQ were smaller. As shown in Figure 4-4, the concentrations of TP and DRP decreased with increasing amount of BMPQ, although a slight increase in DRP occurred

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25 at a dosage level of 2,411 mg Ca/L. TKN and NH3-N levels consistently decreased but the reduction efficiencies were below 50% (Table 4-5). VS also decreased by 45.7% at a maximum dosage level of 3,616 mg Ca/L. 010203040506070Control603120524113616mg Ca/LP (mg/L) TP DRP Figure 4-4. A comparison of the TP and DRP concentrations after adding BMPQ. Table 4-5. Effects on nutrients and solids with BMPQ treatment. BMPQ treatment level (mg Ca/L) Control 603 1205 2411 3616 TP mg/L 65.4 48.0 43.0 30.3 9.3 % Removal 26.6 34.4 53.7 85.8 DRP mg/L 15.8 6.7 5.9 10.3 1.7 % Removal 57.5 62.4 34.8 89.4 TKN mg/L 295 273 266 232 175 % Removal 7.6 10.0 21.3 40.8 NH3-N mg/L 188 168 161 151 141 % Removal 10.5 14.2 19.4 24.6 K mg/L 388 376 323 324 361 % Removal 3.0 16.7 16.3 6.8 TS % 0.41 0.37 0.35 0.31 0.35 % Removal 8.2 13.0 24.1 14.7 VS % 58.0 56.7 57.6 56.2 31.5 % Removal 2.2 0.60 3.1 45.7 pH 7.2 9.1 10.0 10.3 11.3

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26 Hydrated Lime Treatment With and Without Alum Comparisons of the effects of hydrated lime alone and in combination with two concentrations of alum on TP and DRP are shown in Figures 4-5 and 4-6, respectively. 020406080100120140Control676135327054058mg Ca/LTP (mg/L) No Alum 108 mg Al/L 432 mg Al/L Figure 4-5. A comparison of the effects of hydrated lime alone and in combination with alum on TP concentration in three separate experiments. The combination of hydrated lime and 108 mg Al/L showed a consistent significant decrease in the concentrations of TP and DRP. Treatment with hydrated lime and 432 mg Al/L resulted in a slight P increase in the solution at a maximum dosage of 4,058 mg Ca/L. DRP reduction of 99.7% occurred from the addition of 2,705 mg Ca/L in combination with 432 mg Al/L. The highest reduction for TP was 98.6%. This was achieved from the addition of 4,058 mg Ca/L and 108 mg Al/L. Treatment with hydrated lime and 432 mg Al/L reduced TKN levels by 59.4% (Table 4-6). Reductions in TKN and NH3-N levels are shown in Figures 4-7 and 4-8. The combination of hydrated lime and 108 mg Al/L reduced the NH3-N level by 18.0% (Table 4-7). A maximum reduction efficiency of 66.2% for VS occurred with treatment of hydrated lime alone (Table 4-8).

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27 For the most part, the volume of settled solids increased with increasing dosages of hydrated lime and alum. Appendix A shows all measurements for all the parameters. 051015202530Control676135327054058mg Ca/LDRP (mg/L) No Alum 108 mg Al/L 432 mg Al/L Figure 4-6. A comparison of the effects of hydrated lime addition alone and in combination with alum on DRP concentration in three separate experiments. Table 4-6. Effects on nutrients and solids with hydrated lime and 432 mg Al/L treatment. Hydrated lime treatment level (mg Ca/L) Control 676 1353 2705 4058 TP mg/L 69.1 3.2 2.5 1.3 1.4 % Removal 95.4 96.3 98.2 98.0 DRP mg/L 27.2 0.59 0.27 0.09 0.10 % Removal 97.8 99.0 99.7 99.6 TKN mg/L 335 186 174 153 136 % Removal 44.4 48.1 54.4 59.4 NH3-N mg/L 181 175 167 150 148 % Removal 3.1 7.8 17.1 17.8 K mg/L 377 330 320 313 367 % Removal 12.6 15.1 17.1 2.8 TS % 0.49 0.43 0.39 0.30 0.38 % Removal 10.5 20.2 38.0 22.1 VS % 65.1 26.9 24.5 38.0 22.2 % Removal 58.7 62.4 41.7 65.9 pH 7.4 7.6 8.3 10.8 11.3

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28 100150200250300350Control676135327054058mg Ca/LTKN (mg/L) No Alum 108 mg Al/L 432 mg Al/L Figure 4-7. A comparison of the reduction levels of TKN with treatment of hydrated lime alone and in combination with 108 mg Al/L and 432 mg Al/L in three separate experiments. 100110120130140150160170180190Control676135327054058mg Ca/L NH3-N (mg/L ) No Alum 108 mg Al/L 432 mg Al/L Figure 4-8. A comparison of the reduction levels of NH3-N with treatment of hydrated lime alone and in combination with 108 mg Al/L and 432 mg Al/L in three separate experiments. The pH of the treated wastewater is a major consideration in the demonstration project in Riverview, Florida. Combined dosage levels of lime and alum which could

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29 Table 4-7. Effects on nutrients and solids with hydrated lime and 108 mg Al/L treatment. Hydrated lime treatment level (mg Ca/L) Control 676 1353 2705 4058 TP mg/L 125.9 28.1 14.0 2.4 1.8 % Removal 77.7 88.9 98.1 98.6 DRP mg/L 16.1 4.5 3.8 0.30 0.30 % Removal 72.1 76.8 98.5 98.5 TKN mg/L 295 249 216 172 160 % Removal 15.6 27.0 41.7 46.0 NH3-N mg/L 171 154 158 143 140 % Removal 9.8 7.4 16.4 18.0 K mg/L 415 399 399 389 409 % Removal 3.8 3.8 6.2 1.3 TS % 0.46 0.39 0.36 0.42 0.43 % Removal 16.4 21.2 9.2 7.4 VS % 62.6 55.8 52.2 30.3 24.2 % Removal 10.8 16.7 51.6 61.3 pH 7.2 8.4 9.2 11.4 11.4 Table 4-8. Effects on nutrients and solids with hydrated lime treatment. Hydrated lime treatment level (mg Ca/L) Control 676 1353 2705 4058 TP mg/L 60.7 38.1 22.5 5.0 2.8 % Removal 37.3 63.0 91.8 95.5 DRP mg/L 27.2 13.1 8.8 1.5 0.70 % Removal 51.7 67.8 94.5 97.6 TKN mg/L 274 253 249 189 185 % Removal 7.7 9.2 31.1 32.7 NH3-N mg/L 179 176 175 165 162 % Removal 1.6 2.3 7.8 9.4 K mg/L 411 359 353 368 377 % Removal 12.6 14.1 10.4 8.1 TS % 0.38 0.34 0.32 0.34 0.37 % Removal 10.9 15.1 10.77 2.90 VS % 55.8 55.5 49.8 25.5 18.9 % Removal 0.50 10.7 54.2 66.2 pH 7.2 9.2 10.8 11.3 11.4 achieve a final pH of 7 to 8, and could reduce considerable amounts of N and P, would be most ideal for the field situation. From Figure 4-9, pH levels of the samples are shown in relation to the different dosages of hydrated lime and alum. At a combined dosage of 676

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30 mg Ca/L and 432 mg Al/L, the pH was about 7.6. Going back to Table 4-6, TP and DRP concentrations were reduced by 95.4% and 97.8%, respectively, at this combined dosage. TKN concentration was reduced by 44.4%, while for NH3-N it was 3.1%. Further increases in the reduction efficiencies were achieved when 1,353 mg Ca/L was combined with 432 mg Al/L. However, at this dosage, the final pH increased to about 8.3. 024681012Control676135327054058mg Ca/LpH No Alum 108 mg Al/L 432 mg Al/L Figure 4-9. Effects of hydrated lime addition alone and in combination with alum on the pH of the samples. Test for Determining Difference of Treatments from Control To determine whether there was a significant difference between the controls and the treatments, the Dunnet test was used (Kuehl, 2000). An assumption that the data points were normally distributed was made. All parameters except K were significantly different [D (4, 0.05)] when treated with alum, BMPQ, and hydrated lime containing 108 mg Al/L. Treatment with BMPQ also showed that VS reduction was not significantly different from the control on the first 3 dosages (603 mg Ca/L, 1,205 mg Ca/L, and 2,410 mg Ca/L). Appendix B shows a summary of the results for the Dunnet test.

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31 Curve Fitting Analysis Using regression analysis in SAS version 8.2 (SAS Inst., Cary, NC), most of the data points were found to have a good fit with a quadratic polynomial model. This result was consistent with the study conducted by Sherman et al. (2000). For the curve in Figure 4-10, the equation y = 4.95-6x2 0.034x + 59.88 estimates TP reduction by the addition of hydrated lime. 0.010.020.030.040.050.060.070.0010002000300040005000mg/L Camg/L TP Data Quadratic Polynomial Curve Figure 4-10. A quadratic regression curve fit with the TP data points taken from the treatment with hydrated lime alone. The calculated r2 for this curve was 0.997. In this procedure, the chemical dosages in mg Ca/L was used as the continuous independent variable (x) and the mg/L of TP, DRP, TKN, and NH3-N, levels of pH, %TS, and %VS as the dependent variables (y). A linear model was also tested, but the results were not significant. A comparison of the SAS generated r2 for the linear and quadratic regression analysis is shown in Table 4-9.

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32 Table 4-9. A comparison of r2 between linear and quadratic regression for all parameters. Linear Regression Quadratic Polynomial Regression r2 r2 TP Hydrated lime 0.857 0.997 Hydrated lime with 108 mg Al/L 0.544 0.866 Hydrated lime with 432 mg Al/L 0.3875 0.752 Alum 0.0425 0.731 BMPQ 0.971 0.967 DRP Hydrated lime 0.794 0.974 Hydrated lime with 108 mg Al/L 0.636 0.894 Hydrated lime with 432 mg Al/L 0.378 0.747 Alum 0.1195 0.897 BMPQ 0.4786 0.847 TKN Hydrated lime 0.919 0.862 Hydrated lime with 108 mg Al/L 0.907 0.997 Hydrated lime with 432 mg Al/L 0.606 0.833 Alum 0.267 0.535 BMPQ 0.969 0.983 NH3-N Hydrated lime 0.961 0.922 Hydrated lime with 108 mg Al/L 0.836 0.875 Hydrated lime with 432 mg Al/L 0.929 0.964 Alum 0.746 0.924 BMPQ 0.903 0.959 K Hydrated lime 0.104 0.612 Hydrated lime with 108 mg Al/L 0.003 0.698 Hydrated lime with 432 mg Al/L 0.065 0.939 Alum 0.225 0.719 BMPQ 0.18 0.641 %TS Hydrated lime 0.438 0.645 Hydrated lime with 108 mg Al/L 0.002 0.545 Hydrated lime with 432 mg Al/L 0.53 0.928 Alum 0.499 0.986 BMPQ 0.542 0.936

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33 Table 4-9. Continued. Linear Regression Quadratic Polynomial Regression r2 r2 %VS Hydrated lime 0.937 0.937 Hydrated lime with 108 mg Al/L 0.9627 0.964 Hydrated lime with 432 mg Al/L 0.332 0.494 Alum 0.187 0.977 BMPQ 0.673 0.954 pH Hydrated lime 0.862 0.999 Hydrated lime with 108 mg Al/L 0.941 0.946 Hydrated lime with 432 mg Al/L 0.90 0.928 Alum 0.881 0.999 BMPQ 0.836 0.942

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CHAPTER 5 CONCLUSIONS AND RECOMMENDATIONS Conclusions This study demonstrated that chemical treatment of dairy wastewater using hydrated lime, BMPQ, and alum is capable of reducing the concentration of P (TP and DRP) and N (TKN and NH3-N), as well as considerable amounts of TS and VS. The combination of hydrated lime and alum performed very well in reducing the levels of TP and DRP in the wastewater. At a combined dosage of 2,705 mg Ca/L and 432 mg Al/L, DRP concentration was reduced by 99.7%. In the case of TP, 98.6% reduction was observed. This was achieved by the combined dosage of 4,058 mg Ca/L and 108 mg Al/L. The combination of hydrated lime and alum that resulted in a final pH range between 7 and 8 was 676 mg Ca/L and 432 mg Al/L. At this dosage, TP and DRP concentrations were reduced by 95.4% and 97.8%, respectively. TKN and NH3-N were reduced by 44.4% and 3.1%, respectively. Also, the combination of 676 mg Ca/L of hydrated lime and 108 mg Al/L of alum removed 77.7% TP. Although these particular combinations did not attain the maximum reduction efficiencies for P, N, and solids, less chemical was needed. The addition of alum alone showed that there is a limit in terms of P reduction, because the solution tended to become very acidic as alum dosage level increased. Phosphorus re-solubilization was observed at a dosage level of 863 mg Al/L when the pH decreased to about 4. However, when the lowest dosages of the chemicals selected for 34

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35 this experiment were compared, alum performed best compared to hydrated lime and BMPQ in reducing TP, DRP, and TKN. With an alum dosage of 108 mg Al/L, the levels of TP, DRP, and TKN were reduced by 88.2%, 65.4%, and 43%, respectively. For the same parameters, the lowest dosage of hydrated lime (676 mg Ca/L) reduced the levels by 37.3%, 51.7%, and 7.7%, respectively. Similarly, BMPQ with the lowest dosage of 603 mg Ca/L, removed 48%, 57.5%, and 7.6% of TP, DRP, and TKN. BMPQ treatment was not as effective in the jar test experiments compared to hydrated lime and alum. The maximum dosage of 3,616 mg Ca/L of BMPQ only removed 85.8%, 89.4%, 40.8%, and 24.6% of TP, DRP, TKN, and NH3-N, respectively. However, BMPQ was slightly more effective than alum in removing VS. BMPQ removed 45.7% of VS, while for alum the removal efficiency was only 43.1% The test for pH response with varying concentrations of hydrated lime showed that at higher dosages pH stabilized after 5 minutes, and for lower dosages it took 10 minutes. For alum, it took only 5 minutes to stabilize the pH for all the dosages. These results were important in relation to the field demonstration project to make sure that hydrated lime had enough time to stabilize the pH before alum was added. Curve fitting analysis showed that removal of nutrients and solids best fit a quadratic polynomial model. Finally, since this laboratory evaluation showed that lower dosages of hydrated lime and alum combination were effective in removing considerable amounts of TP and DRP, using excessive quantities of hydrated lime to achieve unnecessary P removals may not be necessary in actual field conditions. When adequate cropland is available to handle the remaining N and P in the wastewater, then there is no need to apply excessive

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36 amounts of hydrated lime. It will result in a final pH which will be too high and will be too expensive for the dairy farmers. Thus, achieving a final N/P ratio that is closer to fertilization requirements will be more ideal. Recommendations This laboratory evaluation showed that chemical treatment with hydrated lime combined with alum has a potential for field scale application. In line with the demonstration project in Riverview, Florida, consideration should be given to evaluating the amount of chemicals added rather than depending on the prescribed range of pH for disinfection, as the latter maybe more expensive. Lesser amounts of hydrated lime and alum should be investigated in the pilot project, since the laboratory results showed that significant reductions in the concentrations of nutrients and solids from the wastewater took place at even lower dosages. Moreover, further investigation should be done to evaluate the performance of other chemical coagulants such as ferric chloride and aluminum chloride to come up with better cost-effective combinations of dosages. The addition of polymers is also a possibility, since there has been a growing interest in the performance of polymers in municipal wastewater treatment.

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APPENDIX A TABULATED MEANS Table A-1. Treatment with hydrated lime. Parameters Control (No Lime) 676 mg Ca/L 1352 mg Ca/L 2705 mg Ca/L 4058 mg Ca/L TP (mg/L) 60.7 38.1 22.5 5.0 2.8 DRP (mg/L) 27.2 13.1 8.8 1.5 0.70 TKN (mg/L) 274 253 249 189 185 NH3-N (mg/L) 179 176 175 165 162 K (mg/L) 411 359 353 368 377 pH 7.2 9.2 10.8 11.3 11.4 TS (%) 0.38 0.34 0.32 0.40 0.42 VS (%) 55.6 55.5 49.8 25.5 18.9 Volume of Settled Solids (ml/L) 85.0 105 161 166 176 TS (Settled Solids) (%) 9.16 15.5 18.5 28.2 30.9 VS (Settled Solids) (%) 77.4 53.2 46.8 40.2 22.0 Table A-2. Treatment with hydrated lime and 108 mg Al/L. Parameters Control (No Lime) 676 mg Ca/L 1352 mg Ca/L 2705 mg Ca/L 4058 mg Ca/L TP (mg/L) 125.9 28.1 14.0 2.4 1.8 DRP (mg/L) 16.1 4.5 3.8 0.30 0.30 TKN (mg/L) 295 249 216 172 160 NH3-N (mg/L) 171 154 158 143 140 K (mg/L) 415 399 399 389 430 pH 7.2 8.4 9.2 11.4 11.4 TS (%) 0.46 0.39 0.36 0.42 0.43 VS (%) 62.6 55.8 52.2 30.3 24.2 Volume of Settled Solids (ml/L) 40.0 120 115 172 185 TS (Settled Solids) (%) 2.5 3.9 3.3 4.0 4.7 VS (Settled Solids) (%) 75.3 36.6 39.3 32.2 13.0 Table A-3. Treatment with hydrated lime and 432 mg Al/L. Parameters Control (No Lime) 676 mg Ca/L 1353 mg Ca/L 2705 mg Ca/L 4058 mg Ca/L TP (mg/L) 69.1 3.2 2.5 1.3 1.4 DRP (mg/L) 27.2 0.59 0.27 0.09 0.10 TKN (mg/L) 335 186 174 153 136 37

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38 Table A-3. Continued. Parameters Control (No Lime) 676 mg Ca/L 1353 mg Ca/L 2705 mg Ca/L 4058 mg Ca/L NH3-N (mg/L) 181 175 167 150 148 K (mg/L) 377 329 320 313 367 pH 7.4 7.6 8.3 10.8 11.3 TS (%) 0.49 0.43 0.39 0.30 0.38 VS (%) 65.1 26.9 24.5 38.0 22.2 Volume of Settled Solids (ml/L) 44.0 110 127 182 184 TS (Settled Solids) (%) 2.9 7.4 8.3 9.0 9.64 VS (Settled Solids) (%) 75.0 50.0 44.3 32.6 28.3 Table A-4. Treatment with alum. Parameters Control (No Alum) 108 mg Al/L 216 mg Al/L 432 mg Al/L 863 mg Al/L TP (mg/L) 31.8 3.76 2.1 1.8 14.0 DRP (mg/L) 29.7 10.3 2.95 0.62 12.4 TKN (mg/L) 189 108 113 118 111 NH3-N (mg/L) 112 106 101 99.4 96.6 K (mg/L) 397 380 362 355 372 pH 7.4 6.5 5.8 4.6 4.0 TS (%) 0.49 0.37 0.32 0.37 0.32 VS (%) 64.3 49.8 32.2 24.8 43.1 Volume of Settled Solids (ml/L) 46.0 80.0 155 150 152 TS (Settled Solids) (%) 3.4 3.3 6.8 6.3 8.5 VS (Settled Solids) (%) 72.9 72.6 72.5 69.5 73.1 Table A-5. Treatment with BMPQ. Parameters Control (No BMPQ) 603 mg Ca/L 1205 mg Ca/L 2411 mg Ca/L 3616 mg Ca/L TP (mg/L) 65.4 48.0 43.0 30.1 9.3 DRP (mg/L) 15.8 6.7 5.9 10.3 1.7 TKN (mg/L) 295 273 266 232 175 NH3-N (mg/L) 188 168 161 151 141 K (mg/L) 387 376 323 324 361 pH 7.2 9.1 10.0 10.3 11.3 TS (%) 0.41 0.37 0.35 0.31 0.35 VS (%) 58.0 58.1 58.9 56.2 31.5 Volume of Settled Solids (ml/L) 52.0 86.0 79.0 116 133 TS (Settled Solids) (%) 4.3 5.8 7.2 5.3 4.9 VS (Settled Solids) (%) 77.4 57.9 46.8 50.7 46.9

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APPENDIX B STATISTICAL ANALYSIS RESULTS Dunnet Method for a Comparison of all Treatments with a Control The formula for the Dunnet criterion to compare k treatments to the control is: D (k, ) =d,k,v rs22 where: k = number of treatment s2 = variance r = replicates E = 0.05 If |yi-yc| exceeds D (4,0.5) = 1.39770, then the treatment mean is significantly different from the control (Table B-1). The value for D is taken from Table VI (Kuehl, 2000). Table B-1. Sample calculation for Dunnet method. Observation yi (yi-yc)2 Controla 31.953 31.824 0.01656 Controlb 31.696 0.01656 T1a 3.77 3.757 0.00023 T1b 3.742 0.00023 T2a 2.099 2.103 0.00002 T2b 2.107 0.00002 T3a 1.833 1.804 0.00085 T3b 1.775 0.00085 T4a 14.592 13.971 0.38562 T4b 13.350 0.38562 SSE = 0.80657 D = 3.48 MSE = s2 = 0.16131 D(k, )= 1.39770 df = 5 r = replicates = 2 39

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40 Table B-1. Continued. 95% SCI Treatment Mean yi-yc Lower Upper |yi-yc| Different From Control Control 31.824 T1 3.757 -28.068 28.068 28.068 28.068 yes T2 2.103 -29.721 31.119 29.721 29.721 yes T3 1.804 -30.020 31.418 30.020 30.020 yes T4 13.971 -17.854 19.251 17.854 17.854 yes Table B-2. Summary of the test for difference between control and treatments using Dunnet method D(4, 0.05) for treatment with hydrated lime alone. Control (No Lime) 676 mg Ca/L 1353 mg Ca/L 2705 mg Ca/L 4058 mg Ca/L TP yes yes yes yes DRP yes yes yes yes TKN yes yes yes yes NH3-N yes yes yes yes K yes yes yes no pH yes yes yes yes %TS yes yes yes yes %VS no yes yes yes Table B-3. Summary of the test for difference between control and treatments using Dunnet method D(4, 0.05) for treatment with hydrated lime and 108 mg/L alum. Control (No Lime) 676 mg Ca/L 1353 mg Ca/L 2705 mg Ca/L 4058 mg Ca/L TP yes yes yes yes DRP yes yes yes yes TKN yes yes yes yes NH3-N yes yes yes yes K no no no no pH yes yes yes yes %TS yes yes yes yes %VS yes yes yes yes

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41 Table B-4. Summary of the test for difference between control and treatments using Dunnet method D(4, 0.05) for treatment with hydrated lime and 432 mg/L alum. Control (No Lime) 676 mg Ca/L 1353 mg Ca/L 2705 mg Ca/L 4058 mg Ca/L TP yes yes yes yes DRP yes yes yes yes TKN yes yes yes yes NH3-N yes yes yes yes K yes yes yes no pH yes yes yes yes %TS yes yes yes yes %VS yes yes yes yes Table B-5. Summary of the test for difference between control and treatments using Dunnet method D(4, 0.05) for treatment with alum. Control (No Alum) 108 mg Al/L 216 mg Al/L 432 mg Al/L 863 mg Al/L TP yes yes yes yes DRP yes yes yes yes TKN yes yes yes yes NH3-N yes yes yes yes K no no no no pH yes yes yes yes %TS yes yes yes yes %VS yes yes yes yes Table B-6. Summary of the test for difference between control and treatments using Dunnet method D(4, 0.05) for treatment with BMPQ. Control (No BMPQ) 603 mg Ca/L 1205 mg Ca/L 2411 mg Ca/L 3616 mg Ca/L TP yes yes yes yes DRP yes yes yes yes TKN yes yes yes yes NH3-N yes yes yes yes K no no no no pH yes yes yes yes %TS yes yes yes yes %VS no no no yes

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42 Sample Output of SAS 8.2 Regression Analysis TP with Hydrated lime alone The REG Procedure Model: MODEL1 Dependent Variable: y Analysis of Variance Sum of Mean Source DF Squares Square F Value Pr > F Model 2 4676.37109 2338.18555 991.26 <.0001 Error 7 16.51162 2.35880 Corrected Total 9 4692.88271 Root MSE 1.53584 R-Square 0.9965 Dependent Mean 25.78782 Adj R-Sq 0.9955 Coeff Var 5.95568 Parameter Estimates Parameter Standard Variable DF Estimate Error t Value Pr > |t| Intercept 1 59.88392 0.96397 62.12 <.0001 x 1 -0.03407 0.00126 -27.11 <.0001 x2 1 0.00000495 2.953355E-7 16.77 <.0001

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APPENDIX C PRODUCT SPECIFICATIONS OF CHEMICAL COAGULANTS Table C-1. Blended metallurgical pulverized quicklime product specification. Product of Chemical Lime Corporation, Forth Worth, Texas. PARAMETER NORMAL RANGE Sizing 0 x #18 mesh Bulk density 58 lb./ft.3 average L.O.I. 2.0% max. 1.5% average MgO 26% +/2% SiO2 2.5% max. 1.5% average Fe2O3 1.0% max. 0.35% average Al2O3 1.0% max. 0.55% average S 0.035% max. 0.018% average Note: Total CaO may be determined by difference of the sum of L.O.I. (Loss on Ignition), MgO, SiO2, Fe2O3, and Al2O3. In this case, CaO is 67.46%. Table C-2. Hydrated lime product specification. Product of Fisher Scientific, Fair Lawn, New Jersey. PARAMETER ACTUAL LOT ANALYSIS Chloride (Cl) 0.02% Heavy metals (as Pb) 0.001% Insoluble in HCl 0.01% Iron (Fe) 0.05% Mg and alkali salts 0.8% Sulfur compounds (as SO4) 0.02% Table C-3. Alum product specification. Product of Fisher Scientific, Fair Lawn, New Jersey. PARAMETER ACTUAL LOT ANALYSIS Assay (as 18H2O) 101.6% Chloride 0.004% Heavy metals (as Pb) 0.0008% Insoluble matter 0.008% Iron (Fe) 0.0016% 43

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LIST OF REFERENCES American Society of Agricultural Engineers (ASAE). 2003. Manure production and characteristics. In ASAE Standards. St. Joseph, Mich.: ASAE. American Public Health Association (APHA). 1989. Standard Methods for the Examination of Water and Wastewater, 17th ed. Washington, D.C.: American Public Health Assoc. Barrow, J. T., H. H. Van Horn, D. L. Anderson, and R. A.Nordstedt. 1997. Effects of Fe and Ca additions to dairy wastewaters on solids and nutrient removal by sedimentation. Applied Engineering in Agriculture 13(2): 259-267. Boesch, D. F. 2000. Measuring the health of the Chesapeake Bay: toward integration and prediction. Environ. Res. 82:134-142. Campbell, K. L., J. C. Capece, and T. K. Tremwel. 1995. Surface/subsurface hydrology and phosphorus transport in the Kissimmee River Basin, Florida. Ecol. Eng. 5:301-330. Chastain, J. P., M. B. Vanotti, and M. M. Wingfield. 2001. Effectiveness of liquid-solid separation for treatment of flushed dairy manure: a case study. Transactions of the ASAE 42(6):1833-1840. Corell, D. L. 1998. The role of phosphorus in the eutrophication of receiving waters: a review. J. Environ. Qual. 27:261-266. Craun, G. F., D. G. Greathouse, and D. H. Gunderson. 1981. Methaemoglobin levels in young children consuming high nitrate well water in the United States. Int. J. Epidemiol. 10(4): 309-317. Daniel, T. C, A. N. Sharpley, D. R. Edwards, R. Wedepohl, and J. L. Lemunyon. 1994. Minimizing surface water eutrophication from agriculture by phosphorus management. J. Soil Water Cons. 49:30-38. Duda, A. M. and D. S. Finan. 1983. Influence of livestock on nonpoint source nutrient levels of streams. Transactions of the ASAE 26:1710-1716. Florida Agricultural Statistics Service (FASS). 2004. Livestock. Retrieved May 26, 2004 from http://www.nass.usda.gov/fl/ 44

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45 Faust, S. D. and O. M. Aly. 1998. Chemistry of Water Treatment, 2nd ed. Chelsea, Michigan. Ann Arbor Press Inc,. Flaig, E. G., and K. R. Reddy. 1995. Fate of phosphorus in the Lake Okeechobee watershed, Florida, USA: overview and recommendations. Ecol. Eng. 5:127. Fouss, J. L., D. A. Bucks, and B. C. Grigg. 2003. The agricultural drainage management systems task force: decreasing nutrient export through the Mississippi drainage basin. In Total Maximum Daily Load (TMDL) Environmental Regulations II, ed. A. Saleh. St. Joseph, Mich.: ASAE. Francois, R. J. and A. A. Van Haute. 1985. The role of rapid mixing time on a flocculation process. Wat. Sci. Tech. 17:1091-1101. Graetz, D. A. and V. D. Nair. 1995. Fate of phosphorus in Florida Spodosols contaminated with cattle manure. Ecol. Eng. 5:163-181. Harris, W. G., R. D. Rhue, G. Kidder, R. B. Brown, and R. Little. 1996. Phosphorus retention as related to morphology of sandy coastal plain soil materials. Soil Sci. Soc. Am. J. 60:1513. Johnson, A. F., D. M. Vietor, F. M. Rouquette, Jr., and V. A. Haby. 2004. Fate of phosphorus in dairy wastewater and poultry litter applied on grassland. J. Environ. Qual. 33:735-739. Jones, R. M., and S. P. Brown. 2000. Chemical and settling treatment of dairy wastewater for solids separation and phosphorous removal. In Animal, Agricultural and Food Processing Wastes, ed. J. A. Moore, 1321. St. Joseph, Mich.: ASAE. Karthikeyan, K. G., M. Z. Tekeste, M. Kalbasi, and K. Gungor. 2002. Chemical treatment of dairy manure using alum, ferric chloride and lime. ASAE Meeting Paper No. 024093. St. Joseph, Mich.: ASAE. Kuehl, R. 2000. Design of Experiments: Statistical Principles of Research Design and Analysis, 2nd ed. Pacific Grove, California: Duxbury Press. Lind, C. B. 2003. Precipitation of phosphorus in wastewater, lakes, and animal wastes. In Total Maximum Daily Load (TMDL) Environmental Regulations II, ed. A. Saleh, 107-117. St. Joseph, Mich.: ASAE. McFarland, A., and L. Hauck. 1995. Livestock and the environment: scientific underpinnings for policy analysis. Rep. 1. Texas Inst. for Applied Environ. Res. Stephenville, TX.: Tarleton State University. Metcalf and Eddy, Inc. 2002. Wastewater Engineering: Treatment and Reuse, 4th ed. New York, NY: McGraw-Hill.

PAGE 58

46 Moller, H., I. Lund, and S. Sommer. 2000. Solid-liquid separation of livestock slurry: efficiency and cost. Bioresour. Technol. 74: 223-229. Moore Jr., P. A., T. C. Daniel, D. R. Edwards, and D. M. Miller. 1995. Effect of chemical amendments on ammonia volatilization from poultry litter. J. Environ. Qual. 24: 293-300. Moore Jr., P. A., T. C. Daniel, D. R. Edwards, and D. M. Miller. 1996. Evaluation of chemical amendments to reduce ammonia volatilization from poultry litter. Poultry Sci. 75: 315-320. National Lime Association. 2004. Retrieved May 24, 2004 from http://www.lime.org/ENV02/Animal Ndegwa, P. M., J. Zhu, A. C. Luo. 2001. Effects of solid levels and chemical additives on removal of solids and phosphorus in swine manure. J. Environ. Eng. Div. (ASCE) 127(12): 1111-1115. Parry, R. 1998. Agricultural phosphorus and water quality: a U.S. Environmental Protection Agency Perspective. J. Environ. Qual. 27: 258-261. Sharpley, A. N., T. C. Daniels, J. T. Sims, J. L. Lemunyon, R. Stevens, and R. Parry. 1999. Agricultural phosphorus and eutrophication. U.S. Dep. of Agri. ARS. ARS-149. Natl. Technical Information Serv. (NTIS), Port Royal Rd, Springfield, VA. Sharpley, A. N., J. J. Meisinger, A. Breeuwsma, T. Sims, T. C. Daniel, and J. S. Schepers. 1997. Impacts of animal manure management on ground and surface water quality. In Effective Management of Animal Waste as a Soil Resource, ed. J. Hatfield, 1-50. Boca Raton, Fla: Lewis Pub. Sherman, J. J., H. H. Van Horn, and R. A. Nordstedt. 2000. Use of flocculants in dairy wastewaters to remove phosphorus. Applied Engineering in Agriculture 16(4): 445-452. Sims, J. T. 2000. The role of soil testing in environment risk assessment for phosphorus. In Agriculture and phosphorus management: the Chesapeake Bay, ed. A.N. Sharpley. Boca Raton, Fl.: Lewis Pub. Sims, J. T. 1999. Delawares state nutrient management program: overview of the 1999 Delaware Nutrient Management Act.: College of Agri. and Nat. Resour., Univ. of Delaware, Newark. University of Florida Institute of Food and Agricultural Sciences (UF/IFAS). 2001. The Florida Dairy Industry. Retrieved May 26, 2004 from http://www.animal.ufl.edu/dairy/dairyindustry.htm

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47 U.S. Environmental Protection Agency (EPA). 1988. Nonpoint source pollution in the U.S.: Report to Congress. Office of Water, Criteria, and Standards Division, U.S. EPA, Washington, D.C. U.S. Environmental Protection Agency (EPA). 1996. Environmental indicators of water quality in the United States. U.S. EPA Rep. 841-R-96-002. U.S. EPA, Office of Water, Washington, D.C.: U.S. Gov. Print. Office. U.S. Environmental Protection Agency (EPA). 2000. National Water Quality Inventory: 1998 Report to Congress. EPA841-F-00-006. U.S. EPA, Office of Water, Washington, D.C. Vanotti, M. B., and P. G. Hunt. 1999. Solids and nutrient removal from flushed swine manure using polyacrylamides. Transactions of the ASAE 42: 1833. Vanotti, M. B., A. A. Szogi, and P. G. Hunt. 2002. Extraction of soluble phosphorus from swine wastewater. ASAE Meeting Paper No. 024098. St. Joseph, Mich.: ASAE. Wu, Q. 2002. Potential applications of magnesium hydroxide for municipal wastewater treatment: sludge digestion enhancement and nutrient removal. Ph.D. diss., University of Cincinnati. Zhang, R. H., and F. Lei. 1998. Chemical treatment of animal manure for solidliquid separation. Transactions of the ASAE 41: 1103.

PAGE 60

BIOGRAPHICAL SKETCH Hector Lago Jopson was born in May 14, 1971, in Zamboanga City, Philippines, to Reyland and Matilde Jopson. He received his undergraduate degree in agricultural engineering at Xavier University, Philippines, in 1993. In 1999, he married Ann Rochelle Arranguez and the following year became a proud father of Harriet. He is presently on study leave from Western Mindanao State University where he works as a member of the faculty of the Department of Agricultural Engineering. In 2002, he became a recipient of the Fulbright-Philippine Agriculture Scholarship Program to pursue graduate studies in the U.S. After the completion of his masters work, he will return to the Philippines to share his knowledge to help improve the agricultural sector and continue his service at Western Mindanao State University. 48


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NUTRIENT AND SOLIDS REMOVAL BY LIME AND ALUM TREATMENT OF
FLUSHED DAIRY MANURE















By

HECTOR LAGO JOPSON


A THESIS PRESENTED TO THE GRADUATE SCHOOL
OF THE UNIVERSITY OF FLORIDA IN PARTIAL FULFILLMENT
OF THE REQUIREMENTS FOR THE DEGREE OF
MASTER OF ENGINEERING

UNIVERSITY OF FLORIDA


2004

































Copyright 2004

by

Hector Lago Jopson
































This thesis is dedicated to my loving wife Ann and daughter Harriet, my parents, Reyland
and Matilde Jopson, and to my sister Hilda and brother Reyland Jr.















ACKNOWLEDGMENTS

The author would like to thank all of the members of his supervisory committee for

their help and ideas throughout this effort. Dr. Roger A. Nordstedt, the committee chair,

provided valuable time, guidance, and expertise of the subject. Acknowledgment is

extended to Dr. Dorota Z. Haman and Dr. Donald A. Graetz for their insights and

guidance. The author would also like to express gratitude to all of those within the

Agricultural and Biological Engineering Department, especially Veronica Campbell,

Senior Chemist, for lending her time and effort in assisting him with the laboratory

experiments. The author would like to acknowledge the Fulbright Commission,

Philippine American Educational Foundation, Institute of International Education,

Philippine Department of Agriculture, and Western Mindanao State University for

granting the opportunity to pursue his graduate studies here in the U.S. The author would

like to thank his wife Ann, and daughter Harriet, for the unyielding love, support,

prayers, and inspiration they offered him during these two years of being away from

them. And lastly, gratitude is owed to the Almighty God, the infinite source of all

goodness and love.
















TABLE OF CONTENTS

page

A C K N O W L E D G M E N T S ................................................................................................. iv

LIST OF TA BLE S .................. ............ .................. ....... ............ .. vii

LIST OF FIGURES ......... ......................... ...... ........ ............ ix

ABSTRACT .............. ......................................... xi

CHAPTER

1 INTRODUCTION AND OBJECTIVES ....................................... .................

In tro d u ctio n .................................................................................. 1
O bjectiv e s ................................................................... ................................. . .6

2 R EV IEW O F LITER A TU R E .......................................................................... ......7

3 M ATERIALS AND M ETHOD S ........................................ ......................... 14

M anure C haracterization .................................................. .............................. 14
E xperim mental D design ........................ .. ........................ .. ........ .. ...... .. .. 15
E affluent Sam ples .......................................... ................... .. ...... 15
A rrangem ent of T reatm ents.................................................................................16
Selection of Chem ical D osage................................................. ............... 16
T reatm ent Procedure ..................... .. .... ................... .... .. ........... 18
D ata A n aly sis ................................................................................ 19

4 RESULTS AND DISCU SSION S......................................... .......................... 21

M anure Characterization ................................ ......... ........... ............... 21
Preliminary Test on pH with Chemical Treatment................. .............................21
A lu m T reatm ent.......... .................................................................... ........... .. 22
BM PQ Treatm ent......................... ........ ...................... ................24
Hydrated Lime Treatment With and Without Alum...................................................26
Test for Determining Difference of Treatments from Control .................................30
Curve Fitting Analysis........... ...... ................. ..... ........31




v









5 CONCLUSIONS AND RECOMMENDATIONS ............................................... 34

C o n clu sio n s.................................................... .................. 3 4
Recommendations........ ........ ........ .. ................. ........ 36

APPENDIX

A T A B U L A TE D M E A N S .................................................................. .....................37

B STATISTICAL ANALYSIS RESULTS ...... .................................. ... ..............39

Dunnet Method for a Comparison of all Treatments with a Control..........................39
Sample Output of SAS 8.2 Regression Analysis............................................ 42

C PRODUCT SPECIFICATIONS OF CHEMICAL COAGULANTS.........................43

L IST O F R E F E R E N C E S ........................................................................ .....................44

BIOGRAPH ICAL SKETCH ...................................................... 48
















LIST OF TABLES


Table page


3-1 Chem ical dosages. .................................... .. .. ...... .. ............18

4-1 Wastewater sample characterization results (n=10). .............................................21

4-2 Effects of hydrated lime and 108 mg Al/L of alum on the pH of the wastewater......22

4-3 Effects of alum and of hydrated lime on the pH of the wastewater. ..........................22

4-4 Effects on nutrients and solids with alum treatment.................................................23

4-5 Effects on nutrients and solids with BMPQ treatment. ............................................25

4-6 Effects on nutrients and solids with hydrated lime and 432 mg Al/L treatment........27

4-7 Effects on nutrients and solids with hydrated lime and 108 mg Al/L treatment........29

4-8 Effects on nutrients and solids with hydrated lime treatment. ...................................29

4-9 A comparison of r2 between linear and quadratic regression for all parameters........32

A -i Treatm ent w ith hydrated lim e........................................................ ............... 37

A-2 Treatment with hydrated lime and 108 mg A/L. ................... ............................. 37

A-3 Treatment with hydrated lime and 432 mg A/L. ................... ............................. 37

A -4 T reatm ent w ith alu m .............................. ......... ...... ...............................................3 8

A -5 Treatm ent w ith B M PQ .................................................................... ...................38

B-1 Sample calculation for Dunnet method.................................. ........................ 39

B-2 Summary of the test for difference between control and treatments using Dunnet
method D(4, 0.05) for treatment with hydrated lime alone................................40

B-3 Summary of the test for difference between control and treatments using Dunnet
method D(4, 0.05) for treatment with hydrated lime and 108 mg/L alum ..............40









B-4 Summary of the test for difference between control and treatments using Dunnet
method D(4, 0.05) for treatment with hydrated lime and 432 mg/L alum .............41

B-5 Summary of the test for difference between control and treatments using Dunnet
method D(4, 0.05) for treatment with alum ................................. ..................41

B-6 Summary of the test for difference between control and treatments using Dunnet
method D(4, 0.05) for treatment with BM PQ. ..................................... ............... 41

C-1 Blended metallurgical pulverized quicklime product specification. Product of
Chemical Lime Corporation, Forth Worth, Texas. .............................................43

C-2 Hydrated lime product specification. Product of Fisher Scientific, Fair Lawn, New
J e rs e y ............................................................................ 4 3

C-3 Alum product specification. Product of Fisher Scientific, Fair Lawn, New Jersey..43
















LIST OF FIGURES


Figure pge

1-1 A GIS map of the distribution of dairy farms in Florida, courtesy of Florida
Department of Agriculture and Consumer Services (2004)..............................4..

3-1 University of Florida Dairy Research Unit ...............................................15

3-2 Agitated feed tank where samples were collected................... .................................16

3-3 Simplified schematic diagram of liquid dairy manure treatment system, Riverview,
F lorida. ....................................................................18

3 -4 M ix in g stag e ................................................................................................19

3-5 A closer look during the settling stage. ........................................... ............... 20

4-1 The response of pH over time with hydrated lime. .................................................23

4-2 Effect of alum addition on the pH of the wastewater................... ...................24

4-3 A comparison of the TP and DRP concentrations after adding alum....................24

4-4 A comparison of the TP and DRP concentrations after adding BMPQ. ....................25

4-5 A comparison of the effects of hydrated lime alone and in combination with alum on
TP concentration in three separate experiments.................................................... 26

4-6 A comparison of the effects of hydrated lime addition alone and in combination with
alum on DRP concentration in three separate experiments.............................. 27

4-7 A comparison of the reduction levels of TKN with treatment of hydrated lime alone
and in combination with 108 mg Al/L and 432 mg Al/L in three separate
experim ents. ....................................................... ................. 2 8

4-8 A comparison of the reduction levels of NH3-N with treatment of hydrated lime
alone and in combination with 108 mg Al/L and 432 mg Al/L in three separate
experim ents. ....................................................... ................. 2 8

4-9 Effects of hydrated lime addition alone and in combination with alum on the pH of
the sam ples. .......................................... ............................ .. 30









4-10 A quadratic regression curve fit with the TP data points taken from the treatment
with hydrated lime alone. The calculated r2 for this curve was 0.997 ...................31















Abstract of Thesis Presented to the Graduate School
of the University of Florida in Partial Fulfillment of the
Requirements for the Degree of Master of Engineering

NUTRIENT AND SOLIDS REMOVAL BY LIME AND ALUM TREATMENT OF
FLUSHED DAIRY MANURE

By

Hector Lago Jopson

December 2004

Chair: Roger A. Nordstedt
Major Department: Agricultural and Biological Engineering

Dairy farms utilizing flushed manure systems deal with voluminous liquid manure

on a daily basis. To maintain the effective storage capacity of storage ponds, tanks, and

lagoons, an irrigation system is usually employed for land application of wastewater.

This repeated application of dairy wastewater on limited cropland can result in high

levels of nutrients, especially phosphorus (P), in the soil. Runoff from these areas can

potentially increase the risk of eutrophication of nearby surface water and leaching into

the groundwater. Presently, solids separators have proven inefficient in removing the

solids and nutrients from the liquid dairy manure. An effective and sustainable system

must be developed to further reduce the solids and nutrients.

The field demonstration project in Riverview, Florida, where hydrated lime slurry

and alum were used to remove nutrients and solids from a flushed dairy manure system,

was the basis for this laboratory evaluation. This study evaluated the effectiveness of

hydrated lime, a commercial quicklime product, alum, and combined hydrated lime and









alum in reducing the levels of solids and nutrients, especially P, in liquid dairy manure

after mechanical separation.

Preliminary investigation on the effect of hydrated lime and alum on the pH of the

wastewater with respect to time was conducted on 100 ml samples. With high dosages of

hydrated lime (>406 mg Ca/L), the pH stabilized to about 11.4 and 11.5 in about 5

minutes. When 216 mg Al/L of alum was added to untreated wastewater, the pH after 5

minutes decreased rapidly to about 4.4. The combination of each dosage of hydrated

lime (135 mg Ca/L, 271 mg Ca/L, 406 mg Ca/L, and 541 mg Ca/L) with 108 mg Al/L of

alum resulted in a final pH range of 6.6 to 9.0 after 15 minutes.

Laboratory tests of liquid dairy manure containing an average of 0.70% total solids

(TS) showed that, when compared to the control (no chemical addition), the addition of

hydrated lime combined with alum performed best in reducing the levels of total

phosphorus (TP), dissolved reactive phosphorus (DRP), and total Kjeldahl nitrogen

(TKN) by 98%, 99%, and 59%, respectively. Treatment with hydrated lime reduced the

volatile solids (VS) by about 66.2%, while the addition of only alum reduced VS by

about 34%. When the resulting pH of the solution is considered, especially for potential

applications on dairy flush systems that recycle the treated wastewater, the combination

of hydrated lime (676 mg Ca/L) and alum (432 mg Al/L) performed best by achieving a

pH between 7 and 8 and at the same time reducing TP and DRP by about 95% and 98%,

respectively. However, the combination of hydrated lime (676 mg Ca/L) and a lesser

amount of alum (108 mg Al/L) removed 77.7% of TP. Curve fitting analysis showed that

effects on P removal were greatest with removal curves best described by a quadratic

polynomial (TP r2 = 0.99 and DRP r2 = 0.97).














CHAPTER 1
INTRODUCTION AND OBJECTIVES

Introduction

A significant amount of pollutants entering lakes, estuaries, streams, and

groundwater in the United States (U.S.) results from agricultural activities. The harmful

consequences of farm production on water quality include soil erosion; runoff into lakes,

rivers, and streams of fertilizers, animal wastes, and pesticides; and leaching into

groundwater of nutrients and pesticides. Pollution from agricultural operations is only

one source of water quality problems. Discharges from industrial activities and

municipal sewage treatment plants, stormwater runoff, and naturally occurring

contaminants are also potential sources of water pollution. However, the U.S.

Environmental Protection Agency (EPA) considers nonpoint source pollution from

agriculture as the primary contributor to the nation's surface water quality deterioration.

A 1998 EPA Water Quality Inventory report showed that more than one-third of the river

miles, lake acres, and estuary miles are impaired to some degree (U.S. EPA, 2000).

Water pollution may be categorized into two types based on sources. Point sources

discharge effluent directly into water bodies through an identifiable pipe, ditch, or other

conveyance. Industrial and municipal effluents are examples of this category. Non-point

source (NPS) pollution comes from diffuse sources such as runoff and leachate from rain

or snow melt. Unlike point source pollution, NPS pollution is difficult to regulate

because it is not readily identifiable. Nutrients, sediments, pesticides, salts, and

pathogens are the major agricultural pollutants contributing to NPS pollution.









Nutrients such as nitrogen (N), phosphorus (P), and potassium (K) are essential for

plant growth. Of these three nutrients, N and P can cause quality deterioration when they

enter water systems. Nitrogen and P accelerate aquatic plant and algal production in

receiving surface waters, a condition known as eutrophication. Accelerated

eutrophication causes a variety of problems, including fish kills, human health issues,

clogged pipelines, and reduced recreational opportunities. Nitrogen is primarily the

limiting nutrient in brackish or salt water and P in freshwater.

In Florida and many other areas in the U.S., there have been serious concerns over

surface water and groundwater pollution from agriculture, especially from animal

production facilities. Florida's water resources such as lakes, rivers, springs, and beaches

attract millions of tourists annually. But with the threat of diminishing water quality due

to eutrophication, this multi-million dollar industry may be adversely affected. In

addition, Florida's drinking water supplies come largely from groundwater. Since

surface water is ultimately linked to groundwater at some point, N from agricultural

operations can leach through underwater systems and become a health problem for those

who drink water directly pumped from groundwater. The U.S. national drinking water

standard sets a maximum nitrate-N concentration as 10 mg/L. Above this level it is

considered harmful, especially to infants, causing a condition called methemoglobinemia

(Craun et al., 1981).

In recent years, Florida's dairy industry has been striving to meet the needs of the

state for milk. Though the number of dairy farms has decreased in Florida, the herd size

has increased. Figure 1-1 shows the distribution of dairy farms in the state of Florida.

The average herd size in the state is about 693 milk cows per dairy farm, one of the









nation's largest (University of Florida Institute of Food and Agricultural Sciences

[UF/IFAS], 2001). The Florida Agricultural Statistics Service (FASS) reported that as of

January 2004, dairy cow numbers were estimated at 140,000 milk cows and 40,000

replacement cows (FASS, 2004). This translates to a fresh manure production of 9,907

tons/day or 3.6 million tons/year (American Society of Agricultural Engineers [ASAE],

2003). Handling and disposal of these voluminous wastes create additional burdens to

the dairy farmers, not to mention the environmental issues these wastes pose. Growing

public concerns associated with nutrient losses from manure of large dairy herds as well

as other sources have been overwhelming in Florida. The eutrophic condition in Lake

Okeechobee (second largest freshwater lake in the continental U.S.) due to P

contamination from farm runoff and nitrate-N losses into the groundwater through the

sandy soils of the Suwannee River Basin (largest undammed drainage basin in the U.S.

Coastal Plain) are causes of these major concerns.

Most dairy farms in Florida utilize flushing to a lagoon, storage pond, or storage

tank to remove manure from confinement facilities. An irrigation system is usually

employed for land application of wastewater. Dairy farm wastewater normally contains a

large percentage of solids and nutrients, and one conventional method being used to deal

with them is by separating the solids through sedimentation and mechanical solids

separators. By separating the solids, less sludge is formed in the lagoon, thus extending

its capacity. However, this method has proven to be inefficient because only a small

percentage of the solids and nutrients are removed. Most of the solids and nutrients end

up in the lagoon or storage pond. When the liquid waste from the lagoon is applied to

limited cropland through spray irrigation, more nutrients, especially N and P,


















































Figure 1-1. A GIS map of the distribution of dairy farms in Florida, courtesy of Florida
Department of Agriculture and Consumer Services (personal correspondence,
June 15, 2004).


accumulate in the soil and increase the risk of surface and ground water contamination.

Due to stricter environmental regulations, dairy farms have to implement systems that









incorporate significant levels of new or existing technology to ensure that nutrients are

handled efficiently in an environmentally friendly manner.

For the past several decades, chemical treatment of municipal wastewater has

proven effective in precipitating solids and P. The coagulants most commonly used have

been lime, alum, and iron salts. Recently, applications of chemical removal with

flocculants and coagulants to treat animal manure have shown promising improvement in

solids and P removal compared to physical separation methods only. Since water is the

major constituent of liquid manure, it is very expensive to transport off of the farm. If a

fairly significant amount of the solids and nutrients can be concentrated into a small

portion of the total manure volume, then it may be economical to haul this concentrated

portion farther and to land that may not have an oversupply of nutrients. The treated

wastewater can then be diverted back to flush tanks for reuse.

Since this technology has proven successful in municipal wastewater treatment, it

is therefore worth investigating whether this treatment process can increase the removal

efficiency of solids and nutrients in liquid dairy manure. Earlier investigations on the use

of coagulants to treat various types of animal wastewater have to be re-evaluated in terms

of correlation between laboratory and field scale test results. Furthermore, to minimize

the cost of chemical treatment, dairy farmers must know how many chemicals are needed

to efficiently reduce the nutrients and solids in the wastewater. Adding more chemicals

does not necessarily mean that the dairy wastewater treatment system will work more

efficiently. Thus, finding the best combination of chemicals in minimum amounts that

will satisfactorily meet the desired removal efficiency is highly important for the system

to be cost effective.






6



Objectives

The overall objective of this research was to improve solids, nitrogen, and

phosphorus removal from a flushed dairy waste management system using alum and

lime. Specifically, it aimed to a) evaluate and characterize the liquid dairy manure

following mechanical separation, and b) compare the effectiveness of varying

concentrations of lime and alum, alone or in combination, in maximizing removal of

solids and nutrients from the wastewater.














CHAPTER 2
REVIEW OF LITERATURE

In recent years, there has been tremendous progress in addressing various aspects

of water pollution. As a result of the Clean Water Act, point source pollution such as

industrial discharges has been controlled by permits, and raw sewage discharges have

been reduced by the construction of sewage treatment plants. Nonpoint source pollution

(NPS) such as runoff from agricultural operations has become the main focus of

extensive scientific research. Nutrients such as nitrogen (N) and phosphorus (P) from

fertilizers and animal manure contaminate surface and groundwater, preventing the

attainment of the water quality goals stipulated in the Clean Water Act (U.S. EPA, 1988;

Parry, 1998). The presence of P in runoff from agricultural land is a significant

component of NPS pollution and has been reported to cause surface water eutrophication

(Corell, 1998).

Eutrophication is the overenrichment of receiving waters with mineral nutrients

resulting in excessive production of autotrophs such as algae and cyanobacteria.

According to the U.S. Environmental Protection Agency (EPA), major surface water

quality deterioration is brought about by increased eutrophication due to anthropogenic

activities (U.S. EPA, 1996). Sharpley et al. (1999) reported that the presence of P is

especially correlated to or associated with nutrient enrichment of normally oligotrophic

surface water. Algal blooms and the growth of thick masses of weeds can limit the use of

a water body for recreation, fisheries, and industries. Anoxia, a condition of deficiency

of dissolved oxygen due to high bacterial population and high respiration rates, can









decimate aquatic animal populations (Corell, 1998). The zone of hypoxia in the

Mississippi delta is attributed partly to excessive release of nutrients from agricultural

runoff (Fouss et al., 2003). Eutrophication of Chesapeake Bay and North Carolina's

estuaries and coastal waters in recent years is a classic example of a public health issue

associated with nutrient loadings of surface water. Outbreaks of the toxic dinoflagellate

Pfiesteriapiscicida resulted in fish kills and short term memory impairment in fishermen

and other workers involved with sampling the rivers (Boesch, 2000).

Among various sources of P, the most significant threat of accelerated

eutrophication of adjacent surface water occurs in watersheds having a large

concentration of animal manure production (Duda and Finan, 1983; Daniel et al., 1994;

Sharpley et al., 1997). The continuous application of animal wastes based on plant N

requirements has caused build up of P in an increasing number of areas, thus increasing

the likelihood of excessive P in runoff (McFarland and Hauck, 1995). Sharpley et al.

(1999) reported that P levels exceeding 0.02 mg/L have been shown to significantly

increase the rate of eutrophication in lakes and streams. States such as Delaware,

Maryland, and Virginia have passed nutrient management laws and regulations to reduce

P inputs to surface waters (Sims, 2000). Phosphorus applications in agricultural

productions are restricted or prohibited in areas where high P soils are tested. For

example, in Delaware the Nutrient Management Act of 1999 allows a maximum P

application rate to high P soils equivalent to the three year crop removal rate or one

application every three years(Sims, 1999).

Sandy soils such as those found in Florida require a different approach in terms of

management of P. Harris et al. (1996) pointed out that soils with seasonally high water









table and poor P retention capacities are potentially susceptible to P leaching. Most of

the large animal production facilities such as beef and dairy operations are situated in the

south and central part of Florida where the dominant types of soils are Histosols,

Spodosols, and Entisols (Flaig and Reddy, 1995). Excess nutrients, especially P

accumulated in soils treated with organic waste (such as animal manure), have the

potential to leach into the soil and enter the surface water through lateral transport when

clay, Fe, Al, and Ca compounds adsorbing P are absent or low in concentration in the

surface horizon (Campbell et al., 1995; Graetz and Nair, 1995).

Dairy farms with solids separation systems are still dealing with high

concentrations of nutrients and solids in the effluents. This is chiefly a result of the

inefficiency of solid separators which remove only a small fraction of the solids (<30%)

and about 10 to 20% of organic N and P (Barrow et al., 1997; Vanotti and Hunt, 1999).

A study conducted by Moller et al. (2000) concluded that simple mechanical separators

can separate dry matter into a solid fraction, however, the efficiency of P removal is low

and almost no N is separated. As a result, substantial amounts of N, P and solids are still

present in the liquid waste. Storage ponds and lagoons continuously fill up with solids

containing P and odorous compounds. Due to the high cost of transporting manure

slurry, liquid wastes are often land applied to limited land areas. These repeated liquid

waste applications could exceed the crop uptake and the P sorption capacity of soil and

increase P leaching and losses through subsurface drainage (Johnson et al., 2004). In

order to remove more solids and nutrients from animal liquid waste handling operations,

another method should be employed that will eventually meet the desired removal

efficiency.









Municipal and industrial wastewater treatment systems using chemical coagulants

such as lime, alum, ferric sulfate, and ferric chloride have been commonplace since 1970

(Lind, 2003). Recently, the use of these coagulants and flocculants after solids separation

in animal wastes to efficiently reduce solids and P has been reported (Sherman et al.,

2000; Chastain et al., 2001).

Lime is often used to treat wastewater to remove solids and phosphorus. Control of

pathogenic microorganisms in wastewater is also possible when lime is applied due to its

high pH which destroys the cell membranes (National Lime Association, 2004). In

addition, when pH is high, calcium ions react with odorous sulfur species such as

hydrogen sulfide and organic mercaptans, thereby reducing odor (National Lime

Association, 2004). When lime is added, it reacts with the natural bicarbonate alkalinity

of wastewater forming CaCO3. Above pH 10, calcium ions react with phosphate ions

precipitating hydroxylapatite [Ca 10 (PO 4) 6 (OH) 2] (Metcalf and Eddy, 2002). Thus, the

alkalinity of wastewater is important in determining the chemical dosage of lime rather

than the amount of phosphate present. Metcalf and Eddy (2002) suggest that lime dosage

required to precipitate P is about 1.4 to 1.5 times the total alkalinity expressed as CaCO3.

A study by Barrow et al. (1997) showed that the addition of hydrated lime to simulated

dairy flushwaters reduced total solids by about 70%. In batch level jar tests, Karthikeyan

et al. (2002) showed that lime was effective in removing total phosphorus (TP) and

dissolved reactive phosphorus (DRP) by 96% and 92%, respectively, for dairy

wastewater with 1.6% total solids (TS). Vanotti et al. (2002) reported the removal of

almost 100% of P from swine wastewater using lime after a nitrification pre-treatment.









The researchers explained that without a nitrification process the presence of ammonia

and alkalinity would exert high buffering capacity which prevented P from precipitating.

Alum [Al 2 (SO 4) 3] has been commonly used to chemically treat water and

wastewater. Metcalf and Eddy (2002) reported that aluminum metal ions bind with

phosphate on a 1:1 molar ratio. However, the reactions are dependent upon several

factors such as alkalinity, pH, trace elements and ligands found in wastewater, thus

necessitating bench scale and if possible full-scale tests to determine the required dosages

(Metcalf and Eddy, 2002). Laboratory tests conducted by Jones and Brown (1999)

showed that 99% of ortho-phosphorus (initial concentration was 13.86 mg P/L) was

reduced by treating dairy wastewater with a dosage of 3 g/L of alum but beyond this

dosage, removal efficiency actually decreased. A similar study by Karthikeyan et al.

(2002) reported removal efficiencies of 99%, 92%, and 92% for DRP, total dissolved

phosphorus (TDP), and TP, respectively, for a dairy manure with 0.8% TS and dosage

rate of 8 mM as Al. The concentrations of DRP, TDP, and TP prior to treatment were

15.5 mg/L, 38.1 mg/L and 255.8 mg/L. A detailed laboratory study by Zhang and Lei

(1998) reported that additions of aluminum sulfate effectively enhanced settling of

manure solids by promoting coagulation of suspended particles. Moore et al. (1995,

1996) evaluated several chemical additives for broiler litter and concluded that alum was

the most effective and economical in reducing soluble P and ammonia volatilization. In a

study by Ndegwa et al. (2001) utilizing swine manure, suspended solids (SS) and P were

reduced by 96% and 78%, respectively, using a dosage of 1,500 mg/L of alum. However,

the authors did not specify the P concentration prior to chemical treatment.









Nutrient removal using chemical additives involves three processes: a) coagulation,

b) flocculation, and c) precipitation of the aggregated floc (Francois and Van Haute,

1985). Chemical coagulation entails reactions or processes that facilitate charge

neutralization which results in the destabilization of suspended particles, allowing

aggregation. Then, aggregated particles can be easily separated by passive or mechanical

means. Flocculation refers to the process of particle size increase due to collision. Floc

formation can result when a chemical coagulant is added to destabilize the colloidal

particles in wastewater. A flocculant is used to enhance the flocculation process. The

most common coagulants and flocculants include natural and synthetic polymers, metal

salts such as alum, ferric and ferrous sulfate, and prehydrolized metal salts such as

polyaluminum chloride and polyiron chloride (Metcalf and Eddy, 2002).

The practice of using coagulants has a long history that dates back to ancient times.

Alum, alone or in combination with lime, ferric sulfate and ferric chloride, has been used

to treat water. As early as 2000 B.C., the Egyptians used crushed almonds to clarify

drinking water as well as waters from the Nile River (Faust and Aly, 1998). Alum and

lime were reportedly used as coagulants by the early Romans to make bitter water potable

(Faust and Aly, 1998). In 1885, the first scientific study on coagulation with the use of

alum was conducted by Austen and Wilbur. They reported that alum clarified water, and

this type of treatment would not impair the taste or physiological properties of water

(Faust and Aly, 1998).

Although investigations and others have shown the effectiveness of chemical

coagulants and flocculants, the results vary due to a lack of standardization. The

concentration of flocculants and coagulants, percentage of total solids (TS) present in






13


samples, type of solids separator used (screening or sedimentation) are parameters that

have to be fully investigated. Bench scale tests are therefore highly recommended to test

appropriate dosages of chemical coagulants and flocculants specific to the characteristics

of animal wastes and method of solid separation.

A more effective system will provide more benefits for animal waste handling

facilities, such as reduced solids and P in effluents, less odor problems, easier handling

and transport, and more capacity for storage ponds and lagoons.














CHAPTER 3
MATERIALS AND METHODS

Manure Characterization

Initial characterization of flushed dairy manure collected from the University of

Florida Dairy Research Unit included the following parameters: total solids (TS), volatile

solids (VS), total Kjeldahl nitrogen (TKN), ammonia-nitrogen (NH3-N), total phosphorus

(TP), dissolved reactive phosphorus (DRP), soluble potassium (K), and pH. Filtered

samples were analyzed for DRP using the stannous chloride-based colorimetric method at

a wavelength of 690 nm. For TP analysis, samples were digested using the persulfate

digestion method prior to colorimetric analysis. Calibration curves prepared from known

phosphorus standards were used to determine the concentrations of TP and DRP in mg/L

(American Public Health Association [APHA], 1989).

For TKN determination, samples were digested and distilled following the semi-

micro Kjeldahl procedure (APHA, 1989). Samples analyzed for NH3-N underwent

preliminary distillation. Both TKN and NH3-N were measured using the titrimetric

method. Soluble potassium was determined using a specific ion electrode (Orion

Research Inc., Boston, MA), and pH was determined using a probe (Orion Research Inc.,

Boston, MA). A calibration curve using known standard solutions of K was used to

determine the values in mg/L (APHA, 1989).

Total and volatile solids determination of the supernatant and settled solids was

done by following the APHA (1989) standard methods.









Experimental Design

Effluent Samples

The University of Florida Dairy Research Unit employs a mechanical separator

(Agpro Extractor, Agpro Inc., Paris, TX) followed by a settling basin to separate the

solids from the wastewater (Figure 3-1). The samples used in this study were effluents

from the mechanical separator and settling basin before the wastewater overflowed into

an agitated feed tank for anaerobic digester (Figure 3-2). The wastewater was collected

in a 20 L plastic container and transported immediately to the laboratory. The

wastewater sample was stored at 4 oC for no more than 48 hours to inhibit microbial and

chemical transformations.


Figure 3-1. University of Florida Dairy Research Unit.

































Figure 3-2. Agitated feed tank where samples were collected.

Arrangement of Treatments

All chemical treatments were added to one liter of wastewater and evaluated as

follows: Al as Al2 (S04)3*18H20 alone at four concentrations, Ca as Ca (OH)2 alone at

four concentrations, Ca as CaO alone at four concentrations, Ca as Ca (OH) 2 at four

concentrations in combination with two concentrations of Al as Al2 (S04)3*18H20. A

control with no chemical addition was included for each treatment. The source of CaO

was blended metallurgical pulverized quicklime (BMPQ) produced by Chemical Lime

Corporation, Ft. Worth, Texas. BMPQ contains 32.54% ofMgO, SiO2, Fe203, A1203,

and 48.22% Ca (Appendix C).

Selection of Chemical Dosage

In a demonstration project in Riverview, Florida, the Agricultural and Biological

Engineering Department at the University of Florida is involved in a demonstration of









hydrated lime slurry and alum treatment of dairy wastewater after mechanical separation

(Figure 3-3). The lime slurry had 35% solids by weight. Once added to the wastewater,

the pH significantly increased. Alum solution, which was 48% by weight, was added to

the lime-treated wastewater to lower the pH before it was diverted into the flush tanks for

reuse. The amount of chemicals added to the wastewater was controlled by a pH

controller. Lime was continuously added into the mixing tank as long as the pH was

below 11.5. Once this pH was achieved, lime feeding automatically stopped and alum

was injected to lower the pH of the wastewater. Since the exact amounts of chemicals

being added could not be measured, the chemical dosages for the laboratory test had to be

prepared in such a way that the pH of the treated samples was similar to the actual field

conditions. Preliminary laboratory tests for pH were conducted using 100 ml samples

and the effects of chemical addition were recorded with respect to time.

Stocks of chemical solutions were prepared as follows: 133.2 g/L (200 mM) of

alum [A12 (SO4)3*18H20], 50 g/L (675 mM) of hydrated lime [Ca (OH) 2], 50 g/L (890

mM) ofBMPQ. BMPQ was included in the laboratory experiment to determine how it

affected the pH, as well as the removal efficiency of solids and nutrients. In some cases

Mg has been shown to decrease volume of settled solids (Wu, 2002). The chemical

dosages (Table 3-1) for alum were 1.332 g/L (108 mg Al/L), 2.664 g/L (216 mg Al/L),

5.328 g/L (432 mg Al/L), 10.66 g/L (863 mg Al/L), and control (no alum addition). The

dosages for hydrated lime were 1.25 g/L (676 mg Ca/L), 2.5 g/L (1,353 mg Ca/L), 5 g/L

(2,705 mg Ca/L), 7.5 g/L (4,058 mg Ca/L), and control (no hydrated lime). For BMPQ,

the dosages were 1.25g/L (603 mg Ca/L), 2.5 g/L (1,205 mg Ca/L), 5 g/L (2,411 mg










Ca/L), 7.5 g/L (3,616 mg Ca/L), and control (no BMPQ). Each chemical dosage was

added to 1 liter of liquid dairy wastewater.


Flush
Tanks Feed Barn Liquid Manure Tank Solids
Tanks eed Barnepaato
/ Separator


Mixing and Aeration Tanks
r I r-i


Solids Exported from Farm

Treated Wastewater Recycled Back to Flush Tanks


Excess Treated Wastewater to Storage Pond


Figure 3-3. Simplified schematic diagram of liquid dairy manure treatment system,
Riverview, Florida.

Table 3-1. Chemical dosages.
Alum (mg Al/L) Control 108 216 432 863
Hydrated Lime (mg Ca/L) Control 676 1353 2705 4058
BMPQ (mg Ca/L) Control 603 1205 2411 3616
Hydrated Lime (mg Ca/L)
+ 108 mg A/L Alum Control 676 1353 2705 4058
Hydrated Lime (mg Ca/L)
+ 432 mg Al/L Alum Control 676 1353 2705 4058

Treatment Procedure

Jar test experiments were employed to determine the effect of chemical coagulants

on nutrients and solids in the wastewater. A 6-paddle Floc Illuminator bench top stirrer

(Phipps and Bird, Inc. Richmond, Virginia) was used to mix one liter samples (Figure 3-

3). The jar test procedure consisted of 3 steps: rapid mixing, slow mixing, and settling

period. The stirrer was set to rapidly mix the samples at 100 rpm for 2 minutes, followed









by 8 minutes of slow mixing at 35 rpm. Finally, the flocs were allowed to settle for 50

more minutes without agitation. The pH of each sample was measured prior to chemical

addition and after the settling stage. All chemicals were added at the beginning of the

rapid mixing stage.

Data Analysis

Nutrient and solids reductions were determined by analyzing the supernatant

solution and comparing the results to the analyses of the untreated wastewater. The

volume of settled solids was measured after the settling period using a graduated

cylinder, and subsamples were tested for TS. A sufficient amount of supernatant was

collected from each beaker, and solids and chemical analyses were performed


Figure 3-4. Mixing stage.
































Figure 3-5. A closer look during the settling stage.


immediately. Likewise, the difference between TKN, NH3-N, TP, DRP, and soluble K

concentrations in the control and their corresponding levels after chemical treatment was

used to determine the percent reduction. The Dunnet test (Kuehl, 2000) was used to

determine if the results generated from the treated samples were significantly different

from the control. Curve fitting analysis using polynomial regression was done to

determine which model best described the data.














CHAPTER 4
RESULTS AND DISCUSSIONS

Manure Characterization

Wastewater samples were collected from a sedimentation tank at the University of

Florida Dairy Research Unit after the wastewater had undergone mechanical separation.

The liquid manure samples were tested and were found to have TS and VS averages of

0.70% and 69.1%, respectively (Table 4-1). DRP and TP concentrations averaged 18.1

mg/L and 82.4 mg/L, respectively. The effluent samples contained an average of 257

mg/L of TKN. Similarly, the NH3-N level was 175 mg/L. The average soluble K and pH

were 976 mg/L and 7.5, respectively. A complete summary of the analyses for the

effluent samples is shown in Table 4-1.

Table 4-1. Wastewater sample characterization results (n=10).
Standard
Characteristic Units Mean Deviation
TP mg/L 82.4 25.4
DRP mg/L 18.1 1.0
TKN mg/L 257 75.7
NH3-N mg/L 175 13.9
K mg/L 976 6.7
TS % 0.70 0.10
VS % 69.1 2.2
pH 7.5 0.20

Preliminary Test on pH with Chemical Treatment

Laboratory experiments were conducted to determine the pH response in terms of

varying concentrations of hydrated lime, alum, and a combination of hydrated lime and

alum (108 mg Al/L) with respect to time. For the combined treatment, hydrated lime was









added first followed by alum after 5 minutes. Results showed that after 15 minutes,

higher dosages of lime (>406 mg Ca/L) achieved a final pH of 8 to 9 while at lower

dosages (<271 mg Ca/L), the pH was between 6 and 7 (Table 4-2). Treatment with 216

mg Al/L of alum decreased the pH to 4.4 after 10 minutes and remained at 4.3 after 15

minutes, while for hydrated lime, the highest dosage of 541 mg Ca/L caused the pH to

increase to 11.4 after 5 minutes and stabilized at 11.5 thereafter (Table 4-3 and Figure 4-

1). Determining the pH response time was important for the field demonstration project

to make sure that the pH of the wastewater in the lime mixing tank had stabilized before

the addition of alum.

Table 4-2. Effects of hydrated lime and 108 mg Al/L of alum on the pH of the
wastewater.
Time Hydrated Lime with 108 mg Al/L
(min) (mg Ca/L)
135 271 406 541
0 7.9 7.9 7.9 7.9
5 8.7 10.2 11.3 11.3
10 7.7 8.6 10.2 11.0
15 6.5 6.9 8.3 9.0

Table 4-3. Effects of alum and of hydrated lime on the pH of the wastewater.
Time Alum (mg Al/L) Hydrated Lime (mg Ca/L)
(min) 27 81 108 216 135 271 406 541
0 7.8 7.8 7.8 7.8 7.3 7.3 7.3 7.4
5 6.6 6.1 5.4 4.4 8.4 9.0 11.3 11.4
10 6.6 6.0 5.2 4.3 8.6 10.7 11.4 11.5
15 6.6 6.0 5.2 4.3 8.8 10.8 11.4 11.5

Alum Treatment

Treatment with alum at 432 mg Al/L significantly reduced TP and DRP

concentration by 94% and 97.9%, respectively. The levels of TKN, NH3-N, and %TS

significantly decreased (Table 4-4). VS decreased by 61.5% at dosage level of 432 mg

Al/L. This was also the maximum dosage level before the TP and DRP











14.0
12.0
10.0
8.0
6.0
4.0
2.0
0.0


-u-135 mg Ca/L
--271 mg Ca/L
--- 406 mg Ca/L
-- 541 mg Ca/L


5 10
Time (minute)


Figure 4-1. The response of pH over time with hydrated lime.


concentrations began to increase in the wastewater. Consistent decrease in pH was

observed with increasing dosage of alum as shown in Figure 4-2. At pH level below 4.6,

P resolubilized bringing about an increase of P concentration in the solution (Fig. 4-3).

Appendix A contains the actual measurements for all the parameters.

Table 4-4. Effects on nutrients and solids with alum treatment.
Alum treatment level (mg Al/L)
Control 108 216 432 863
TP mg/L 31.8 3.8 2.1 1.8 14.0
% Removal 88.2 93.4 94.3 56.1
DRP mg/L 29.7 10.3 3.0 0.60 12.4
% Removal 65.4 90.1 97.9 58.3
TKN mg/L 189 108 113 117 111
% Removal 43.0 40.0 37.8 41.5
NH3-N mg/L 112 106 101 99.4 96.6
% Removal 5.0 10.0 11.3 13.8
K mg/L 397 380 362 355 372
% Removal 4.2 9.0 10.5 6.3
TS % 0.49 0.37 0.32 0.37 0.32
% Removal 23.7 33.5 25.0 34.1
VS % 64.3 49.8 32.2 24.8 43.1
% Removal 22.7 50.0 61.5 33.0
pH 7.4 6.5 5.8 4.6 4.0











8
7
6
5
I4
3
2
1
0


Control


216
mg AI/L


Figure 4-2. Effect of alum addition on the pH of the wastewater.


- TP


--DRP


Control 108 216 432 863
mg AI/L


Figure 4-3. A comparison of the TP and DRP concentrations after adding alum.

BMPQ Treatment

The average reduction of TP and DRP ranged from 26.6% to 85.8% and 57.5% to

89.4%, respectively. Compared with alum treatment alone, the reduction efficiencies

with BMPQ were smaller. As shown in Figure 4-4, the concentrations of TP and DRP

decreased with increasing amount of BMPQ, although a slight increase in DRP occurred









at a dosage level of 2,411 mg Ca/L. TKN and NH3-N levels consistently decreased but

the reduction efficiencies were below 50% (Table 4-5). VS also decreased by 45.7% at a

maximum dosage level of 3,616 mg Ca/L.


- TP


--DRP


Control 603 1205 2411 3616
mg Ca/L


Figure 4-4. A comparison of the TP and DRP concentrations after adding BMPQ.

Table 4-5. Effects on nutrients and solids with BMPQ treatment.


TP mg/L
% Removal
DRP mg/L
% Removal
TKN mg/L
% Removal
NH3-N mg/L
% Removal
K mg/L
% Removal
TS %
% Removal
VS %
% Removal


Control
65.4

15.8

295

188

388

0.41

58.0


BMPQ treatment level (mg Ca/L)
603 1205 2411
48.0 43.0 30.3
26.6 34.4 53.7
6.7 5.9 10.3
57.5 62.4 34.8
273 266 232
7.6 10.0 21.3
168 161 151
10.5 14.2 19.4
376 323 324
3.0 16.7 16.3
0.37 0.35 0.31
8.2 13.0 24.1
56.7 57.6 56.2
2.2 0.60 3.1
9.1 10.0 10.3


3616
9.3
85.8
1.7
89.4
175
40.8
141
24.6
361
6.8
0.35
14.7
31.5
45.7
11.3










Hydrated Lime Treatment With and Without Alum

Comparisons of the effects of hydrated lime alone and in combination with two

concentrations of alum on TP and DRP are shown in Figures 4-5 and 4-6, respectively.


--- No Alum --- 108 mg AI/L --- 432 mg AI/L


140

120

100

S80

S 60
I-
40

20
n


Control 676 1353 2705 4058
mg Ca/L


Figure 4-5. A comparison of the effects of hydrated lime alone and in combination with
alum on TP concentration in three separate experiments.


The combination of hydrated lime and 108 mg Al/L showed a consistent significant

decrease in the concentrations of TP and DRP. Treatment with hydrated lime and 432

mg Al/L resulted in a slight P increase in the solution at a maximum dosage of 4,058 mg

Ca/L. DRP reduction of 99.7% occurred from the addition of 2,705 mg Ca/L in

combination with 432 mg Al/L. The highest reduction for TP was 98.6%. This was

achieved from the addition of 4,058 mg Ca/L and 108 mg Al/L. Treatment with hydrated

lime and 432 mg Al/L reduced TKN levels by 59.4% (Table 4-6). Reductions in TKN

and NH3-N levels are shown in Figures 4-7 and 4-8. The combination of hydrated lime

and 108 mg Al/L reduced the NH3-N level by 18.0% (Table 4-7). A maximum reduction

efficiency of 66.2% for VS occurred with treatment of hydrated lime alone (Table 4-8).










For the most part, the volume of settled solids increased with increasing dosages of

hydrated lime and alum. Appendix A shows all measurements for all the parameters.


---108 mg AI/L


1353
mg CalL


---432 mg AI/L


2705


4058


Figure 4-6. A comparison of the effects of hydrated lime addition alone and in
combination with alum on DRP concentration in three separate experiments.

Table 4-6. Effects on nutrients and solids with hydrated lime and 432 mg Al/L treatment.
Hydrated lime treatment level (mg Ca/L)
Control 676 1353 2705 4058
TP mg/L 69.1 3.2 2.5 1.3 1.4
% Removal 95.4 96.3 98.2 98.0
DRP mg/L 27.2 0.59 0.27 0.09 0.10
% Removal 97.8 99.0 99.7 99.6
TKN mg/L 335 186 174 153 136
% Removal 44.4 48.1 54.4 59.4
NH3-N mg/L 181 175 167 150 148
% Removal 3.1 7.8 17.1 17.8
K mg/L 377 330 320 313 367
% Removal 12.6 15.1 17.1 2.8
TS % 0.49 0.43 0.39 0.30 0.38
% Removal 10.5 20.2 38.0 22.1
VS % 65.1 26.9 24.5 38.0 22.2
% Removal 58.7 62.4 41.7 65.9
pH 7.4 7.6 8.3 10.8 11.3


-*-No Alum


30

25

2 20

15
0.
o 10

5

0


Control











-- No Alum --- 108 mg AI/L


350


300
_1
) 250
E
z
z 200
I-

150


100


Control


676


1353


2705


4058


mg CalL


Figure 4-7. A comparison of the reduction levels of TKN with treatment of hydrated lime
alone and in combination with 108 mg Al/L and 432 mg Al/L in three separate
experiments.


- No Alum --- 108 mg A, L


Control


676


1353


-- 432 mg AI/L


2705


4058


mg CalL


Figure 4-8. A comparison of the reduction levels of NH3-N with treatment of hydrated
lime alone and in combination with 108 mg Al/L and 432 mg Al/L in three
separate experiments.


The pH of the treated wastewater is a major consideration in the demonstration

project in Riverview, Florida. Combined dosage levels of lime and alum which could


A


-- 432 mg AI/L










Table 4-7. Effects on nutrients and solids with hydrated lime and 108 mg Al/L treatment.
Hydrated lime treatment level (mg Ca/L)
Control 676 1353 2705 4058
TP mg/L 125.9 28.1 14.0 2.4 1.8
% Removal 77.7 88.9 98.1 98.6
DRP mg/L 16.1 4.5 3.8 0.30 0.30
% Removal 72.1 76.8 98.5 98.5
TKN mg/L 295 249 216 172 160
% Removal 15.6 27.0 41.7 46.0
NH3-N mg/L 171 154 158 143 140
% Removal 9.8 7.4 16.4 18.0
K mg/L 415 399 399 389 409
% Removal 3.8 3.8 6.2 1.3
TS % 0.46 0.39 0.36 0.42 0.43
% Removal 16.4 21.2 9.2 7.4
VS % 62.6 55.8 52.2 30.3 24.2
% Removal 10.8 16.7 51.6 61.3
pH 7.2 8.4 9.2 11.4 11.4

Table 4-8. Effects on nutrients and solids with hydrated lime treatment.
Hydrated lime treatment level (mg Ca/L)
Control 676 1353 2705 4058
TP mg/L 60.7 38.1 22.5 5.0 2.8
% Removal 37.3 63.0 91.8 95.5
DRP mg/L 27.2 13.1 8.8 1.5 0.70
% Removal 51.7 67.8 94.5 97.6
TKN mg/L 274 253 249 189 185
% Removal 7.7 9.2 31.1 32.7
NH3-N mg/L 179 176 175 165 162
% Removal 1.6 2.3 7.8 9.4
K mg/L 411 359 353 368 377
% Removal 12.6 14.1 10.4 8.1
TS % 0.38 0.34 0.32 0.34 0.37
% Removal 10.9 15.1 10.77 2.90
VS % 55.8 55.5 49.8 25.5 18.9
% Removal 0.50 10.7 54.2 66.2
pH 7.2 9.2 10.8 11.3 11.4

achieve a final pH of 7 to 8, and could reduce considerable amounts of N and P, would be

most ideal for the field situation. From Figure 4-9, pH levels of the samples are shown in

relation to the different dosages of hydrated lime and alum. At a combined dosage of 676









mg Ca/L and 432 mg Al/L, the pH was about 7.6. Going back to Table 4-6, TP and DRP

concentrations were reduced by 95.4% and 97.8%, respectively, at this combined dosage.

TKN concentration was reduced by 44.4%, while for NH3-N it was 3.1%. Further

increases in the reduction efficiencies were achieved when 1,353 mg Ca/L was combined

with 432 mg Al/L. However, at this dosage, the final pH increased to about 8.3.



-- No Alum -- 108 mg Al/L -- 432 mg AI/L
12

10

8

CL 6
4

2

0
Control 676 1353 2705 4058
mg CalL


Figure 4-9. Effects of hydrated lime addition alone and in combination with alum on the
pH of the samples.

Test for Determining Difference of Treatments from Control

To determine whether there was a significant difference between the controls and

the treatments, the Dunnet test was used (Kuehl, 2000). An assumption that the data

points were normally distributed was made. All parameters except K were significantly

different [D (4, 0.05)] when treated with alum, BMPQ, and hydrated lime containing 108

mg Al/L. Treatment with BMPQ also showed that VS reduction was not significantly

different from the control on the first 3 dosages (603 mg Ca/L, 1,205 mg Ca/L, and 2,410

mg Ca/L). Appendix B shows a summary of the results for the Dunnet test.










Curve Fitting Analysis

Using regression analysis in SAS version 8.2 (SAS Inst., Cary, NC), most of the data

points were found to have a good fit with a quadratic polynomial model. This result was

consistent with the study conducted by Sherman et al. (2000). For the curve in Figure 4-

10, the equation y = 4.95-6X2 0.034x + 59.88 estimates TP reduction by the addition of

hydrated lime.



Data
Quadratic Polynomial Curve
70.0
60.0 4
50.0
i 40.0
S30.0
20.0
10.0
0.0
0 1000 2000 3000 4000 5000
mglL Ca


Figure 4-10. A quadratic regression curve fit with the TP data points taken from the
treatment with hydrated lime alone. The calculated r2 for this curve was
0.997.

In this procedure, the chemical dosages in mg Ca/L was used as the continuous

independent variable (x) and the mg/L of TP, DRP, TKN, and NH3-N, levels of pH,

%TS, and %VS as the dependent variables (y). A linear model was also tested, but the

results were not significant. A comparison of the SAS generated r2 for the linear and

quadratic regression analysis is shown in Table 4-9.









Table 4-9. A comparison of r2 between linear and quadratic regression for all parameters.
Quadratic
Linear Polynomial
Regression Regression
r2 r2
TP
Hydrated lime 0.857 0.997
Hydrated lime with 108 mg Al/L 0.544 0.866
Hydrated lime with 432 mg Al/L 0.3875 0.752
Alum 0.0425 0.731
BMPQ 0.971 0.967
DRP
Hydrated lime 0.794 0.974
Hydrated lime with 108 mg Al/L 0.636 0.894
Hydrated lime with 432 mg Al/L 0.378 0.747
Alum 0.1195 0.897
BMPQ 0.4786 0.847
TKN
Hydrated lime 0.919 0.862
Hydrated lime with 108 mg Al/L 0.907 0.997
Hydrated lime with 432 mg Al/L 0.606 0.833
Alum 0.267 0.535
BMPQ 0.969 0.983
NH3-N
Hydrated lime 0.961 0.922
Hydrated lime with 108 mg Al/L 0.836 0.875
Hydrated lime with 432 mg Al/L 0.929 0.964
Alum 0.746 0.924
BMPQ 0.903 0.959
K
Hydrated lime 0.104 0.612
Hydrated lime with 108 mg Al/L 0.003 0.698
Hydrated lime with 432 mg Al/L 0.065 0.939
Alum 0.225 0.719
BMPQ 0.18 0.641
%TS
Hydrated lime 0.438 0.645
Hydrated lime with 108 mg Al/L 0.002 0.545
Hydrated lime with 432 mg Al/L 0.53 0.928
Alum 0.499 0.986
BMPQ 0.542 0.936









Table 4-9. Continued.
Quadratic
Linear Polynomial
Regression Regression
r2 r2
%VS
Hydrated lime 0.937 0.937
Hydrated lime with 108 mg Al/L 0.9627 0.964
Hydrated lime with 432 mg Al/L 0.332 0.494
Alum 0.187 0.977
BMPQ 0.673 0.954
pH
Hydrated lime 0.862 0.999
Hydrated lime with 108 mg Al/L 0.941 0.946
Hydrated lime with 432 mg Al/L 0.90 0.928
Alum 0.881 0.999
BMPQ 0.836 0.942














CHAPTER 5
CONCLUSIONS AND RECOMMENDATIONS

Conclusions

This study demonstrated that chemical treatment of dairy wastewater using

hydrated lime, BMPQ, and alum is capable of reducing the concentration of P (TP and

DRP) and N (TKN and NH3-N), as well as considerable amounts of TS and VS.

The combination of hydrated lime and alum performed very well in reducing the

levels of TP and DRP in the wastewater. At a combined dosage of 2,705 mg Ca/L and

432 mg Al/L, DRP concentration was reduced by 99.7%. In the case of TP, 98.6%

reduction was observed. This was achieved by the combined dosage of 4,058 mg Ca/L

and 108 mg Al/L.

The combination of hydrated lime and alum that resulted in a final pH range

between 7 and 8 was 676 mg Ca/L and 432 mg Al/L. At this dosage, TP and DRP

concentrations were reduced by 95.4% and 97.8%, respectively. TKN and NH3-N were

reduced by 44.4% and 3.1%, respectively. Also, the combination of 676 mg Ca/L of

hydrated lime and 108 mg Al/L of alum removed 77.7% TP. Although these particular

combinations did not attain the maximum reduction efficiencies for P, N, and solids, less

chemical was needed.

The addition of alum alone showed that there is a limit in terms of P reduction,

because the solution tended to become very acidic as alum dosage level increased.

Phosphorus re-solubilization was observed at a dosage level of 863 mg Al/L when the pH

decreased to about 4. However, when the lowest dosages of the chemicals selected for









this experiment were compared, alum performed best compared to hydrated lime and

BMPQ in reducing TP, DRP, and TKN. With an alum dosage of 108 mg Al/L, the levels

of TP, DRP, and TKN were reduced by 88.2%, 65.4%, and 43%, respectively. For the

same parameters, the lowest dosage of hydrated lime (676 mg Ca/L) reduced the levels

by 37.3%, 51.7%, and 7.7%, respectively. Similarly, BMPQ with the lowest dosage of

603 mg Ca/L, removed 48%, 57.5%, and 7.6% of TP, DRP, and TKN.

BMPQ treatment was not as effective in the jar test experiments compared to

hydrated lime and alum. The maximum dosage of 3,616 mg Ca/L of BMPQ only

removed 85.8%, 89.4%, 40.8%, and 24.6% of TP, DRP, TKN, and NH3-N, respectively.

However, BMPQ was slightly more effective than alum in removing VS. BMPQ

removed 45.7% of VS, while for alum the removal efficiency was only 43.1%

The test for pH response with varying concentrations of hydrated lime showed that

at higher dosages pH stabilized after 5 minutes, and for lower dosages it took 10 minutes.

For alum, it took only 5 minutes to stabilize the pH for all the dosages. These results

were important in relation to the field demonstration project to make sure that hydrated

lime had enough time to stabilize the pH before alum was added.

Curve fitting analysis showed that removal of nutrients and solids best fit a

quadratic polynomial model.

Finally, since this laboratory evaluation showed that lower dosages of hydrated

lime and alum combination were effective in removing considerable amounts of TP and

DRP, using excessive quantities of hydrated lime to achieve unnecessary P removals may

not be necessary in actual field conditions. When adequate cropland is available to

handle the remaining N and P in the wastewater, then there is no need to apply excessive









amounts of hydrated lime. It will result in a final pH which will be too high and will be

too expensive for the dairy farmers. Thus, achieving a final N/P ratio that is closer to

fertilization requirements will be more ideal.

Recommendations

This laboratory evaluation showed that chemical treatment with hydrated lime

combined with alum has a potential for field scale application. In line with the

demonstration project in Riverview, Florida, consideration should be given to evaluating

the amount of chemicals added rather than depending on the prescribed range of pH for

disinfection, as the latter maybe more expensive. Lesser amounts of hydrated lime and

alum should be investigated in the pilot project, since the laboratory results showed that

significant reductions in the concentrations of nutrients and solids from the wastewater

took place at even lower dosages. Moreover, further investigation should be done to

evaluate the performance of other chemical coagulants such as ferric chloride and

aluminum chloride to come up with better cost-effective combinations of dosages. The

addition of polymers is also a possibility, since there has been a growing interest in the

performance of polymers in municipal wastewater treatment.















APPENDIX A
TABULATED MEANS


Table A-1. Treatment with hydrated lime.
Control
Parameters (No Lime)
TP (mg/L) 60.7
DRP (mg/L) 27.2
TKN (mg/L) 274
NH3-N (mg/L) 179
K (mg/L) 411
pH 7.2
TS (%) 0.38
VS (%) 55.6


Volume of
Settled Solids (ml/L)
TS (Settled Solids) (%)
VS (Settled Solids) (%)


85.0
9.16
77.4


676
mg Ca/L
38.1
13.1
253
176
359
9.2
0.34
55.5

105
15.5
53.2


Table A-2. Treatment with hydrated lime
Control
Parameters (No Lime)
TP (mg/L) 125.9
DRP (mg/L) 16.1
TKN (mg/L) 295
NH3-N (mg/L) 171
K (mg/L) 415
pH 7.2
TS (%) 0.46
VS (%) 62.6


Volume of
Settled Solids (ml/L)
TS (Settled Solids) (%)
VS (Settled Solids) (%)


40.0
2.5
75.3


Table A-3. Treatment with hydrated lime
Control
Parameters (No Lime)
TP (mg/L) 69.1
DRP (mg/L) 27.2
TKN (mg/L) 335


and 108 mg
676
mg Ca/L
28.1
4.5
249
154
399
8.4
0.39
55.8

120
3.9
36.6


and 432 mg
676
mg Ca/L
3.2
0.59
186


1352
mgCa/L
22.5
8.8
249
175
353
10.8
0.32
49.8


161
18.5
46.8


2705
mg Ca/L
5.0
1.5
189
165
368
11.3
0.40
25.5

166
28.2
40.2


4058
mg Ca/L
2.8
0.70
185
162
377
11.4
0.42
18.9

176
30.9
22.0


Al/L.
1352
mg Ca/L
14.0
3.8
216
158
399
9.2
0.36
52.2


115
3.3
39.3


Al/L.
1353
mg Ca/L
2.5
0.27
174


2705
mg Ca/L
2.4
0.30
172
143
389
11.4
0.42
30.3

172
4.0
32.2


2705
mg Ca/L
1.3
0.09
153


4058
mg Ca/L
1.8
0.30
160
140
430
11.4
0.43
24.2

185
4.7
13.0


4058
mg Ca/L
1.4
0.10
136









Table A-3. Continued.
Control 676 1353 2705 4058
Parameters (No Lime) mg Ca/L mg Ca/L mg Ca/L mg Ca/L
NH3-N (mg/L) 181 175 167 150 148
K (mg/L) 377 329 320 313 367
pH 7.4 7.6 8.3 10.8 11.3
TS (%) 0.49 0.43 0.39 0.30 0.38
VS (%) 65.1 26.9 24.5 38.0 22.2
Volume of
Settled Solids (ml/L) 44.0 110 127 182 184
TS (Settled Solids) (%) 2.9 7.4 8.3 9.0 9.64
VS (Settled Solids) (%) 75.0 50.0 44.3 32.6 28.3

Table A-4. Treatment with alum.
Control 108 216 432 863
Parameters (No Alum) mg Al/L mg Al/L mg A/L mg Al/L
TP (mg/L) 31.8 3.76 2.1 1.8 14.0
DRP (mg/L) 29.7 10.3 2.95 0.62 12.4
TKN (mg/L) 189 108 113 118 111
NH3-N (mg/L) 112 106 101 99.4 96.6
K (mg/L) 397 380 362 355 372
pH 7.4 6.5 5.8 4.6 4.0
TS (%) 0.49 0.37 0.32 0.37 0.32
VS (%) 64.3 49.8 32.2 24.8 43.1
Volume of
Settled Solids (ml/L) 46.0 80.0 155 150 152
TS (Settled Solids) (%) 3.4 3.3 6.8 6.3 8.5
VS (Settled Solids) (%) 72.9 72.6 72.5 69.5 73.1

Table A-5. Treatment with BMPQ.
Control 603 1205 2411 3616
Parameters (No BMPQ) mg Ca/L mg Ca/L mg Ca/L mg Ca/L
TP (mg/L) 65.4 48.0 43.0 30.1 9.3
DRP (mg/L) 15.8 6.7 5.9 10.3 1.7
TKN (mg/L) 295 273 266 232 175
NH3-N (mg/L) 188 168 161 151 141
K (mg/L) 387 376 323 324 361
pH 7.2 9.1 10.0 10.3 11.3
TS (%) 0.41 0.37 0.35 0.31 0.35
VS (%) 58.0 58.1 58.9 56.2 31.5
Volume of
Settled Solids (ml/L) 52.0 86.0 79.0 116 133
TS (Settled Solids) (%) 4.3 5.8 7.2 5.3 4.9
VS (Settled Solids) (%) 77.4 57.9 46.8 50.7 46.9















APPENDIX B
STATISTICAL ANALYSIS RESULTS

Dunnet Method for a Comparison of all Treatments with a Control

The formula for the Dunnet criterion to compare k treatments to the control is:


D (k, aE) =da,v -2s2


where: k = number of treatment

s2 = variance

r = replicates

(E = 0.05

If lyi-ycl exceeds D 4,0.5) = 1.39770, then the treatment mean is significantly

different from the control (Table B-l). The value for D is taken from Table VI (Kuehl,

2000).


Table B-1.

Control
Control
Tla
Tlb
T2a
T2b
T3a
T3b
T4a
T4b


Sample calculation for Dunnet method.
Observation yi (yi-yc)2
31.953 31.824 0.01656
31.696 0.01656
3.77 3.757 0.00023
3.742 0.00023
2.099 2.103 0.00002
2.107 0.00002
1.833 1.804 0.00085
1.775 0.00085
14.592 13.971 0.38562
13.350 0.38562
SSE = 0.80657 D=
MSE = s2= 0.16131 D(k, aE)=
df= 5
r = replicates = 2


3.48
1.39770











Table B-1. Continued.
95% SCI
Different
Treatment Mean yi-yc Lower Upper |yi-yc| From
Control
Control 31.824 -
Tl 3.757 -28.068 28.068 28.068 28.068 yes
T2 2.103 -29.721 31.119 29.721 29.721 yes
T3 1.804 -30.020 31.418 30.020 30.020 yes
T4 13.971 -17.854 19.251 17.854 17.854 yes


Table B-2. Summary of the test for difference between control and treatments using
Dunnet method D(4, 0.05) for treatment with hydrated lime alone.
Control 676 1353 2705 4058
(No Lime) mg Ca/L mg Ca/L mg Ca/L mg Ca/L
TP -yes yes yes yes
DRP yes yes yes yes
TKN yes yes yes yes
NH3-N yes yes yes yes
K yes yes yes no
pH yes yes yes yes
%TS yes yes yes yes
%VS no yes yes yes

Table B-3. Summary of the test for difference between control and treatments using
Dunnet method D(4, 0.05) for treatment with hydrated lime and 108 mg/L
alum.
Control 676 1353 2705 4058
(No Lime) mg Ca/L mg Ca/L mg Ca/L mg Ca/L
TP yes yes yes yes
DRP yes yes yes yes
TKN yes yes yes yes
NH3-N yes yes yes yes
K no no no no
pH yes yes yes yes
%TS yes yes yes yes
%VS yes yes yes yes










Table B-4. Summary of the test for difference between control and treatments using
Dunnet method D(4, 0.05) for treatment with hydrated lime and 432 mg/L
alum.


Control
(No Lime)


TP
DRP
TKN
NH3-N
K
pH
%TS
%VS


676
mg Ca/L
yes
yes
yes
yes
yes
yes
yes
yes


1353
mg Ca/L
yes
yes
yes
yes
yes
yes
yes
yes


2705
mg Ca/L
yes
yes
yes
yes
yes
yes
yes
yes


4058
mg Ca/L
yes
yes
yes
yes
no
yes
yes
yes


Table B-5. Summary of the test for difference between control and treatments using
Dunnet method D(4, 0.05) for treatment with alum.
Control 108 216 432 863
(No Alum) mg Al/L mg Al/L mg Al/L mg Al/L
TP yes yes yes yes
DRP yes yes yes yes
TKN yes yes yes yes
NH3-N yes yes yes yes
K no no no no
pH yes yes yes yes
%TS yes yes yes yes
%VS yes yes yes yes

Table B-6. Summary of the test for difference between control and treatments using
Dunnet method D(4, 0.05) for treatment with BMPQ.
Control 603 1205 2411 3616
(No BMPQ) mg Ca/L mg Ca/L mg Ca/L mg Ca/L
TP yes yes yes yes
DRP yes yes yes yes
TKN yes yes yes yes
NH3-N yes yes yes yes
K no no no no
pH yes yes yes yes
%TS yes yes yes yes
%VS no no no yes








42



Sample Output of SAS 8.2 Regression Analysis

TP with Hydrated lime alone

The REG Procedure
Model: MODEL1
Dependent variable: y


Source

Model
Error
Corrected Total


Analysis of Variance

Sum of Mean
Squares Square

4676.37109 2338.18555
16.51162 2.35880
4692.88271


F Value Pr > F

991.26 <.0001


Root MSE
Dependent Mean
Coeff Var


1.53584
25.78782
5.95568


R-square 0.9965
Adj R-Sq 0.9955


Parameter

Parameter
Estimate

59.88392
-0.03407
0.00000495


Estimates

Standard
Error

0.96397
0.00126
2.953355E-7


variable

Intercept
x
x2


t Value

62.12
-27.11
16.77


Pr > Itl

<.0001
<.0001
<.0001














APPENDIX C
PRODUCT SPECIFICATIONS OF CHEMICAL COAGULANTS

Table C-1. Blended metallurgical pulverized quicklime product specification. Product of
Chemical Lime Corporation, Forth Worth, Texas.
PARAMETER NORMAL RANGE
Sizing 0" x #18 mesh
Bulk density 58 lb./ft.3 average
L.O.I. 2.0% max. 1.5% average
MgO 26% +/- 2%
Si02 2.5% max. 1.5% average
Fe203 1.0% max. 0.35% average
A1203 1.0% max. 0.55% average
S 0.035% max. 0.018% average
Note: Total CaO may be determined by difference of the sum of L.O.I. (Loss on
Ignition), MgO, Si02, Fe203, and A1203. In this case, CaO is 67.46%.

Table C-2. Hydrated lime product specification. Product of Fisher Scientific, Fair Lawn,
New Jersey.
PARAMETER ACTUAL LOT ANALYSIS
Chloride (Cl) 0.02%
Heavy metals (as Pb) 0.001%
Insoluble in HCI 0.01%
Iron (Fe) 0.05%
Mg and alkali salts 0.8%
Sulfur compounds (as SO4) 0.02%

Table C-3. Alum product specification. Product of Fisher Scientific, Fair Lawn, New
Jersey.
PARAMETER ACTUAL LOT ANALYSIS
Assay (as 18H20) 101.6%
Chloride 0.004%
Heavy metals (as Pb) 0.0008%
Insoluble matter 0.008%
Iron (Fe) 0.0016%















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BIOGRAPHICAL SKETCH

Hector Lago Jopson was born in May 14, 1971, in Zamboanga City, Philippines, to

Reyland and Matilde Jopson. He received his undergraduate degree in agricultural

engineering at Xavier University, Philippines, in 1993. In 1999, he married Ann

Rochelle Arranguez and the following year became a proud father of Harriet. He is

presently on study leave from Western Mindanao State University where he works as a

member of the faculty of the Department of Agricultural Engineering. In 2002, he

became a recipient of the Fulbright-Philippine Agriculture Scholarship Program to pursue

graduate studies in the U.S. After the completion of his master's work, he will return to

the Philippines to share his knowledge to help improve the agricultural sector and

continue his service at Western Mindanao State University.