Use of Pulp and Paper Sludge to Improve Performance of Topsoil Layer in a Landfill Capping System Petra Wildauer Dipl. Ing. Chemistry, RWTH Aachen, Abt. Julich (Germany), 1987 Thesis Submitted in Partial Fulfillment of the Requirements for the Degree of Master of Science in Mathematical, Computer, and Physical Sciences (Chemistry) The University o f Northern British Columbia July 2006 © Petra Wildauer, 2006 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 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APPROVAL Name: Petra Wildauer Degree: Master of Science Thesis Title: Use of Pulp And Paper Sludge To Improve Perfonuance Of Topsoil Layer I n A X a n d f i l L r i n n i n n r ------- Examining Committee: Chair: Le^usf"Associate Professor Natural Resources and Environmental Studies Program University of Northern British Columbia Supervisor: Dr. Ron Thnng, rroressoi Mathematical, Computer, and Physical Sciences Program University of Northern British Columbia Committee Member: Dr. Margot Mandy, A s^ciate Professor Mathematical, Computer, and Physical Sciences Program University of Northern British Columbia Committee Memh^f: Dr. Joselito Arocena, Professor Natural Resources and Environmental Studies Program Canada Research Chair. Soil and Environmental Sciences University'fffNorthern jTpfc&i Columbia C^Co^rhfttee Member: Larry Gardner, AScT Environmental Protection Section Head ThompsonJRegion, Ministry of Water, Land and Air Protection CommitteeTVfemfrgf: James Spankie, P.Eng. Mill Environmental Supervisor - Northwood Pulp Mill Canadian Forest Products Ltd. External Examiner: Dr. Michael Rutherford, Associate Professor Natural Resources and Environmental Studies Program University of Northern British Columbia Date Approved: ULL i*), aooi Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. ABSTRACT Sludge is one of the major solid waste products in the pulping process. It consists of wood fibers, fines, some inorganic fillers, and water. Prince George mills produce approximately 11,000 wet tons of sludge annually. Presently, the sludge is either landfilled or incinerated causing potential environmental problems. Pulp mill sludge may be used as soil amendment in the topsoil layer of a landfill cap to enhance plant growth and minimize the formation of cracks, hence reduce erosion and infiltration problems. The objective of this research was to chemically and physically characterize sludge from two different pulping processes and to investigate their suitability as soil amendment in the topsoil layer of a landfill cap. Chemical analysis of both sludge samples revealed that metal concentrations were below maximum allowable concentrations for municipal sewage biosolids. Both sludges have a high C:N ratio and a neutral to alkaline pH. The N immobilization and pH adjustment could be addressed with appropriate fertilization. The type of sludge under consideration will determine the fertilizer composition to enhance plant growth. The high organic content and fibrous structure of the sludges decreased the bulk density of the soil and increased its water holding capacity. Water holding capacity (WHC) was determined by gravity and moisture retention curves were established for sludge and soil samples, various sludge-soil mixtures and sludge-soil layer systems. BCTMP sludge samples had a higher WHC than the soil, resulting in higher water retention and higher amount of plant available water. ii Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Kraft mill sludge samples showed the opposite effect on WHC, water retention and plant available water. Soil amended with increasing amounts of sludge resulted in increasing water retention. Layering systems showed that the soil layers exhibited attributes of constant WHC, while the sludge layers varied depending on their position within the layer system. These attributes of the sludge used in this research would improve the performance of the topsoil layer with less environmental impact than current disposal options. The results and conclusions are not necessarily applicable to any sludge in the pulp and paper industry. iii Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Table of Contents Abstract ii Table of Contents iv List of Tables vi List of Figures x Acknowledgements xii Chapter 1 Introduction 1 1.1 Landfill capping 1 1.2 Pulp and paper sludge 6 1.3 Environmental consideration 12 1.4 Project objectives 18 Chapter 2 Literature review 20 2.1 Sludge disposal alternatives 20 2.2 Case studies of various applications 24 2.3 Landfill applications 27 Chapter 3 3.1 Methods for chemical and physical characterization 31 Materials and methods 32 3.1.1 Sample collection 32 3.1.2 Sample storage 33 3.2 Sludge characterization 33 3.2.1 pH Determination 33 3.2.2 Moisture content 33 3.2.3 Bulk density 34 3.2.4 Porosity 35 3.2.5 Scanning electron microscopy and energy dispersive X-ray 35 3.2.6 Total carbon and total nitrogen 36 3.2.7 Ash content 36 3.2.8 Determination of macro- and micronutrients 37 3.2.9 Electrical conductivity and salinity 38 3.2.10 Effective cation exchange capacity (CECe) 39 3.2.11 Water holding capacity 39 iv Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 3.2.11.1 3.2.11.2 3.2.12 Chapter 4 Gravity or European method 39 Pressure plate experiment 41 Statistical analysis 44 Results and discussion 45 4.1 Baseline characterization 45 4.2 Chemical characterization 48 4.2.1 General properties 48 4.2.2 Macro- and micronutrients 50 Physical characterization 4.3 53 4.3.1 Bulk density and porosity 53 4.3.2 Water holding capacity by gravity 53 4.3.3 Pressure plate experiment 58 Chapter 5 Summary 73 Chapter 6 Recommendations for future work 76 78 References Appendix A Glossary 86 Appendix B Determination of moisture content in sludge samples 88 Appendix C Determination of total C and total N 90 Appendix D Determination of ash content 91 Appendix E Energy dispersive x-ray analysis 92 Appendix F Cation exchange capacity 94 Appendix G Elemental analysis 95 Appendix H Determination of gravimetric water holding capacity 96 Appendix I Pressure plate experiment 112 Reproduced with permission of the copyright owner. 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List of Tables TABLE 1: TABLE 2: TABLE 3: TABLE 4: TABLE 5: TABLE 6: TABLE 7: TABLE 8: TABLE 9: TABLE 10: TABLE 11: TABLE 12: TABLE 13: TABLE 14: TABLE 15: TABLE 16: TABLE 17: TABLE 18: TABLE 19: TABLE 20: TABLE 21: TABLE 22: TABLE 23: TABLE 24: TABLE 25: TABLE 26: Typical materials that comprise a final landfill cover system Quality standards for productive soils Comparison of macronutrient and micronutrient concentrations in and paper sludge and municipal sewage biosolids Plant macro- and micronutrients and their functions Residuals index properties and hydraulic conductivity of sludge used as barrier layer from previous studies Properties of BCTMP and Kraft mill sludge compared with previous data Summary of results of the elemental analysis in oven-dried (105°) mill and BCTMP sludge samples determined by ICP-AES and literature data Bulk density and porosity of BCTMP and Kraft mill sludge Bulk density and gravimetric water holding capacity obtained from original and blended Kraft mill and BCTMP sludge and soil samples Bulk density and gravimetric water holding capacity obtained from various Kraft mill sludge-soil mixtures Bulk density and gravimetric water holding capacity obtained from various BCTMP sludge-soil mixtures Bulk density and gravimetric water holding capacity of 1, 2, and 3 layer systems of Kraft mill sludge Bulk density and gravimetric water holding capacity of 1, 2, and 3 layer systems of BCTMP sludge Volumetric moisture retention curve data with random errors for BCTMP sludge, Kraft mill sludge, and soil Volumetric moisture retention curve data with random errors for BCTMP sludge-soil mixtures Volumetric moisture retention curve data with random errors for Kraft mill sludge-soil mixtures Volumetric moisture content in % and bulk density in g/cm3 of BCTMP sludge-soil mixtures Volumetric moisture content in % and bulk density in g/cm3 of Kraft mill sludge-soil mixtures Total volumetric moisture content of 1,2, and 3 BCTMP sludge-soil layer systems at 0.5, 1.0, and 5.0 bar pressure Total volumetric moisture content of 1,2, and 3 Kraft mill sludge-soil layer systems at 0.5, 1.0, and 5.0 bar pressure Kraft mill sludge dried at 55° C Kraft mill sludge dried at 80° C Kraft mill sludge dried at 105° C BCTMP sludge dried at 55° C BCTMP sludge dried at 55° C BCTMP sludge dried at 55° C 3 13 17 18 24 48 52 53 54 55 55 56 57 59 64 65 66 67 69 69 88 88 88 89 89 89 vi Reproduced with permission of the copyright owner. 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TABLE 27: TABLE 28: TABLE 29: TABLE 30: TABLE 31: TABLE 32: TABLE 33: TABLE 34: TABLE 35: TABLE 36: TABLE 37: TABLE 38: TABLE 39: TABLE 40: TABLE 41: TABLE 42: TABLE 43: TABLE 44: TABLE 45: TABLE 46 TABLE 47: TABLE 48: TABLE 49: TABLE 50: TABLE 51: TABLE 52: TABLE 53: TABLE 54: TABLE 55: TABLE 56: TABLE 57: Total carbon and nitrogen raw data Ash content of sludge and soil samples Elemental analysis of Kraft mill sludge Elemental analysis of BCTMP sludge Effective cation exchange capacity and exchangeable Al, Fe, K, Mg, Mn, and Na for BCTMP and Kraft mill sludge and soil samples Elemental analysis of oven-dried BCTMP and Kraft mill sludge by ICP-AES Raw data for sludge and soil samples Raw data for Kraft mill sludge-soil mixtures Raw data for BCTMP sludge-soil mixtures Total sample mass dry and Db for sludge and soil samples Total sample mass dry and Db for Kraft mill sludge-soil mixtures Total sample mass dry and Db for BCTMP sludge-soil mixtures Raw data for Kraft mill sludge-soil layer systems and Db; 1, 2, and 3 layer systems Raw data for BCTMP sludge-soil layer systems and Db; 1, 2, and 3 layer systems Db and statistics for Kraft mill sludge-soil layer systems; 1, 2, and 3 layer systems Db and statistics for BCTMP sludge-soil layer systems; 1, 2, and 3 layer systems WHCg of sludge and soil samples WHCg of Kraft mill sludge-soil mixtures WHCg of BCTMP sludge-soil mixtures WHCg of Kraft mill sludge-soil layer systems; 1, 2, and 3 layer systems WHCg of BCTMP sludge-soil layer systems; 1, 2, and 3 layer systems Raw data for moisture retention curve of Kraft mill sludge Raw data for moisture retention curve of BCTMP sludge Raw data for moisture retention curve of soil Determination of random errors of bulk density, gravimetric (WHCg) and volumetric moisture content (WHCV) for Kraft mill sludge Determination of random errors of bulk density, gravimetric (WHCg) and volumetric moisture content (WHCV) for BCTMP sludge Determination of random errors of bulk density, gravimetric (WHCg) and volumetric moisture content (WHCV) for soil Raw data for moisture retention curve of Kraft mill sludge Raw data for moisture retentioncurve of blended Kraft mill sludge Raw data for moisture retention curve of Kraft mill sludge-soil mixture 40:10 Raw data for moisture retention curve of Kraft mill 90 91 92 93 94 95 96 96 97 98 99 100 102 103 104 104 105 106 107 108 110 112 113 113 114 114 114 115 115 116 v ii Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. sludge-soil mixture 30:20 Raw data for moisture retention curve of Kraft mill sludge-soil mixture 25:25 TABLE 59 Raw data for moisture retention curve of Kraft mill sludge-soil mixture 20:30 TABLE 60 Raw data for moisture retention curve of Kraft mill sludge-soil mixture 10:40 TABLE 61 Raw data for moisture retention curve of BCTMP sludge TABLE 62 Raw data for moisture retention curve of blended BCTMP sludge TABLE 63 Raw data for moisture retention curve of BCTMP sludge-soil mixture 40:10 TABLE 64 Raw data for moisture retention curve of BCTMP sludge-soil mixture 30:20 TABLE 65 Raw data for moisture retention curve of BCTMP sludge-soil mixture 25:25 TABLE 66 Raw data for moisture retention curve of BCTMP sludge-soil mixture 20:30 TABLE 67 Raw data for moisture retention curve of BCTMP sludge-soil mixture 10:40 TABLE 68 WHCg, Db, W HCV, and random errors of original Kraft mill sludge TABLE 69 WHCg, Db, W HCV, and random errors of blended Kraft mill sludge TABLE 70 WHCg, Db, W HCV, and random errors of Kraft mill sludge-soil mixture 40:10 TABLE 71 WHCg, Db, WHCV, and random errors of Kraft mill sludge-soil mixture 30:20 TABLE 72 WHCg, Db, WHCV, and random errors of Kraft mill sludge-soil mixture 25:25 TABLE 73: WHCg, Db, WHCV, and random errors of Kraft mill sludge-soil mixture 20:30 TABLE 74 WHCg, Db, W HCV, and random errors of Kraft mill sludge-soil mixture 10:40 TABLE 75 WHCg, Db, W HCV, and random errors of original BCTMP sludge TABLE 76 WHCg, Db, W HCV, and random errors of blended BCTMP sludge TABLE 77 WHCg, Db, WHCV, and random errors of BCTMP sludge-soil mixture 40:10 TABLE 78 WHCg, Db, W HCV, and random errors of BCTMP sludge-soil mixture 30:20 TABLE 79: WHCg, Db, WHCV, and random errors of BCTMP sludge-soil mixture 25:25 TABLE 80 WHCg, Db, WHCV, and random errors of BCTMP sludge-soil mixture 20:30 TABLE 81 WHCg, Db, W HCV, and random errors of BCTMP sludge-soil mixture 10:40 116 TABLE 58 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 117 117 118 119 119 120 120 121 121 122 123 123 123 124 124 124 125 126 126 126 127 127 127 128 TABLE 82: TABLE 83: TABLE 84: TABLE 85: TABLE 86: TABLE 87: Raw data for bulk density, WHCg and WHCVdetermination of each sludge and soil layer for Kraft mill sludge Raw data for bulk density, WHCg and WHCVdetermination of each sludge and soil layer for BCTMP sludge Determination of bulk density, gravimetric and volumetric moisture content with random errors and the total WHCVof the sludge-soil layers for Kraft mill sludge Determination of bulk density, gravimetric and volumetric moisture content with random errors and the total WHCVof the sludge-soil layers for Kraft mill sludge Total volumetric moisture content of 1, 2, and 3 Kraft mill sludge-soil layer systems at 0.5, 1.0, and 5.0 bar pressure with random errors Total volumetric moisture content of 1, 2, and 3 BCTMP sludge-soil layer systems at 0.5, 1.0, and 5.0 bar pressure with random errors 141 143 145 146 147 147 ix Reproduced with permission of the copyright owner. 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List of Figures FIGURE 1: FIGURE 2: FIGURE 3: FIGURE 4: FIGURE 5; FIGURE 6: FIGURE 7: FIGURE 8: FIGURE 9: Simplified layout of sludge generation paths Final sludge disposal practices Outline for the sludge-soil layer systems Pressure plate extractor set up BCTMP sludge (1:1) Kraft mill sludge (1:1) SEM micrographs of BCTMP sludge (15x) SEM micrographs of Kraft mill sludge (15x) Moisture retention curves of BCTMP sludge, Kraft mill sludge and soil from -0.1 to -15 bar with random errors FIGURE 10: Moisture retention curves of BCTMP sludge, Kraft mill sludge and soil from -0.1 to -2.5 bar with random errors FIGURE 11: Moisture retention curves for BCTMP sludge-soil mixtures from -0.1 t o -15 bar FIGURE 12: Moisture retention curves for BCTMP sludge-soil mixtures from -0.1 t o -2 .5 bar FIGURE 13: Moisture retention curves for Kraft mill sludge-soil mixtures from -0.1 t o -15 bar FIGURE 14: Moisture retention curves for Kraft mill sludge-soil mixtures from -0.1 t o -2 .5 bar FIGURE 15: Moisture retention curves for Kraft mill sludge, Kraft mill sludge-soil mixtures 40:10, 30:20, and 10:40 from -0.1 to -15 bar FIGURE 16: Moisture retention curves for blended Kraft mill sludge, Kraft mill sludge-soil mixtures 25:25 and 10:40 from -0.1 to -15 bar FIGURE 17: Moisture retention curves for Kraft mill sludge, Kraft mill sludge-soil mixtures 40:10, 30:20, and 10:40 from -0.1 to -2.5 bar FIGURE 18: Moisture retention curves for blended Kraft mill sludge, Kraft mill sludge-soil mixtures 25:25 and 10:40 from -0.1 to -2.5 bar FIGURE 19: Moisture retention curves for Kraft mill sludge, Kraft mill sludge-soil mixtures 40:10, 30:20, and 10:40 with random errors from -0.1 t o -15 bar FIGURE 20: Moisture retention curves for blended Kraft mill sludge, Kraft mill sludge-soil mixtures 25:25 and 10:40 with random errors from -0.1 t o -15 bar FIGURE 21: Moisture retention curves for Kraft mill sludge, Kraft mill sludge-soil mixtures 40:10, 30:20, and 10:40 with random errors from -0.1 t o -2.5 bar FIGURE 22: Moisture retention curves for blended Kraft mill sludge, Kraft mill sludge-soil mixtures 25:25 and 10:40 with random errors from -0.1 t o -2.5 bar FIGURE 23: Moisture retention curves for BCTMP sludge, BCTMP sludge-soil mixtures 40:10, 25:25, and 10:40 from -0.1 to -15 bar FIGURE 24: Moisture retention curves for blended BCTMP sludge, BCTMP Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 11 20 40 42 46 46 47 47 60 60 62 62 63 63 129 130 131 132 133 133 134 134 135 sludge-soil mixtures 20:30 and 30:20 from -0.1 to -15 bar FIGURE 25: Moisture retention curves for BCTMP sludge, BCTMP sludge-soil mixtures 40:10, 25:25, and 10:40 from -0.1 to -2.5 bar FIGURE 26: Moisture retention curves for blended BCTMP sludge, BCTMP sludge-soil mixtures 20:30 and 30:20 from -0.1 to -2.5 bar FIGURE 27: Moisture retention curves for BCTMP sludge, BCTMP sludge-soil mixtures 40:10, 25:25, and 10:40 with random errors from -0.1 t o -15 bar FIGURE 28: Moisture retention curves for blended BCTMP sludge, BCTMP sludge-soil mixtures 30:20 and 20:30 with random errors from -0.1 t o -15 bar FIGURE 29: Moisture retention curves for BCTMP sludge, BCTMP sludge-soil mixtures 40:10, 25:25, and 10:40 with random errors from -0.1 to -2.5 bar FIGURE 30: Moisture retention curves for blended BCTMP sludge, BCTMP sludge-soil mixtures 30:20 and 20:30 with random errors from -0.1 to -2.5 bar 136 137 138 139 139 140 140 xi Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Acknowledgements The author would like to sincerely thank all the people who gave her their encouragement and assistance to conduct this research. In particular, the author would like to recognize: Dr. R. W. Thring, my supervisor, for giving me this opportunity to realize this research and support and guide me through this time. The members of my committee: Dr. J. Arocena, Dr. M. Mandy, L. Gardner, and J. Spankie for their input and guidance. The environmental science, chemistry and central equipment laboratories for lending me equipment and assisting me with sample analysis. The Science Council of British Columbia and its GREAT scholarship for providing the financial support required to complete this thesis. Michele, Eric, Alida, Dave, Svetlana, and Geoffrey for their friendship and boosting me up by telling me “that everything would work out”. My husband for being so patient and encouraging while I completed my degree, for rescuing my data and fixing all the little computer problems. Finally, to my high school chemistry teacher, who not only inspired my interest in chemistry but also helped me to set my career path. I would like to dedicate this project to my friend, Sheri Merchant, whose excitement and passion for the sludge project lifted me over some course work hurdles ( f July 2002). Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Chapter 1 Introduction Municipal solid waste landfills are capped when they reach their disposal capacities. The primary purposes of this cap are to minimize the infiltration of precipitation and to limit the release of landfill gases. Landfill caps combine layers of clay, sand, vegetated topsoil, and, sometimes, synthetic liners. To restore the local environment, it is desirable that the top layer of the cap supports vegetation. Therefore, additional material needs to be blended with the capping material to improve vegetation growth. The objective of this project was to chemically and physically characterize sludge from two different pulping processes and investigate their suitability for use as landfill capping material. Presently, the vast majority of sludge is either landfilled or incinerated. Due to high waste-related disposal costs, increased difficulty and expense of permitting new landfills, and the growing environmental concerns, the pulp and paper industry is searching for technologies that are capable of reusing or recycling this sludge, one of the most difficult wastes to handle or deal with. 1.1 Landfill capping The safe and reliable disposal of municipal and industrial solid waste is an important component of integrated waste management. Landfill is the term used to describe the physical facilities used for the disposal of solid wastes in the surface soils of the earth. Landfill refers to an engineered facility for disposal of municipal solid waste (MSW) designed and operated to minimize public and environmental impacts. Since the turn of the century, the use of landfills, in one form or another, has been the most economical and environmentally acceptable method for disposal of solid wastes throughout the world. Although many landfills have been constructed in the past with 1 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. little or no thought for the long-term protection of public health and the environment, in the last 20 years, practices have changed substantially (Kreith, 1994). Municipal solid waste landfills are capped with a final cover when they reach capacity. The landfill final cover system is designed to control fire, water infiltration, gas, dust, blowing litter, and erosion, and to enhance site appearance. One main function of the final cover system is to minimize infiltration of rainwater into the underlying waste and therefore reduce the amount of leachate generated in the landfill. Most covers incorporate a layered arrangement to minimize the quantity of water entering the landfill. The configuration of the final cover system depends on the site, waste characteristics, regulatory requirements, and future use of the site (GeoSyntec Consultants, 1995). When water percolates through solid wastes that are undergoing decomposition, both biological materials and chemical constituents are leached into solution (Tchobanoglous et al., 1993). As leachate percolates through the underlying strata, many of the chemical and biological constituents originally contained in it will be removed by the filtering and adsorptive action of the material composing the strata. In general, the extent of this action depends on the characteristics of the soil, especially the clay content. Because of the potential risk involved in allowing leachate to percolate to the groundwater, best practice calls for its elimination or containment (Tchobanoglous et al., 1993). The purpose in the design of a final landfill cover system is to minimize the infiltration of leachate into the subsurface soils below the landfill thus reducing the potential for groundwater contamination. A number of cover system designs have been developed to minimize the movement of leachate into the subsurface below the landfill. In general, the final cover system is a combination of different layer types: surface layer, protection layer, drainage layer, barrier layer, gas collection layer, and foundation layer. 2 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Each of the layers has one or more functions and the material typically used to construct them are listed in table 1. Table 1: Typical materials that comprise a final landfill cover system (GeoSyntec Consultants, 1995) Component Surface layer Protection layer Drainage layer Barrier layer Gas collection layer Foundation layer Typical materials topsoil; cobbles, paving material soil; cobbles sand, gravel; geonet, geotextile clay, geomembrane sand, gravel, geotextile, geonet soil, selected waste Purpose support vegetation growth, promote rainwater run-off promote rainwater run-off, prevent penetration by roots limit buildup of hydraulic head on top of barrier layer, reduce infiltration minimize leachate generation collect and transmit generated landfill gas provide subgrade for overlying layers of final cover Thickness min. 6” min. 24” 40 - 60 mil min. 18” min. 12” min. 12” To meet the above mentioned purposes, the final landfill cover system must: a) be able to withstand climatic extremes (e.g., hot/cold, wet/dry, and freeze/thaw cycles), b) be able to resist water and wind erosion, c) have stability against slumping, cracking and slope failure, and downslope slippage or creep, d) resist the effects of differential landfill settlements caused by the release of landfill gas and the compression of the waste and the foundation soil, e) resist failure due to surcharge loads resulting from the stockpiling of cover material and the travel of collection vehicles across completed portions of the landfill, f) resist deformation caused by earthquakes, g) withstand alterations to cover materials caused by constituents in the landfill gas, h) resist the disruptions caused by plants, burrowing animals, worms, and insects (Kreith, 1994). Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. A 1988 study by the U.S. Environmental Protection Agency (EPA) of randomly selected landfills revealed that the vast majority of final landfill cover systems are leaking, and many have caused severe contamination of the groundwater and surrounding ecosystems (Dwyer, 1998). Examining the factors that affect cap performance, it is apparent that hydrologic and erosional processes account for most of the performance-related problems (Duguid, 1977; Jacobs et al., 1980; Hakonson et al., 1982). For example, erosion associated with runoff can breach the cap and expose waste to the biosphere (Nyhan and Lane, 1982; Nyhan et al., 1984). The drastic outcomes motivated a new research area in waste management. The instability of existing cover systems and increasing costs for recommended cover materials required by regulatory authorities suggest a broad variety of research projects on suitable alternative cover materials. The British Columbia Landfill Criteria (MoELP, 1993) set minimum standards for landfill covers, specifying permeability and construction materials. The cover must be configured such that it can be maintained efficiently and be amenable to relatively easy repair. Components of this conventional closure system may be modified if the proposed alternative performs to an equivalent standard. The final vegetative cover is the only mechanism that almost completely controls infiltration independent of site location. The majority of precipitation is unable to infiltrate the landfill because of surface slopes and runoff control. Slope and permeability are two parameters that are largely variable and controllable by various engineering methods. T h e s e p a ra m e te rs d e te rm in e th e qu an tity o f w a te r th a t a ffec t the landfill, a la rg e portion of which is captured by a surface collection system and is diverted away from the landfill. If a dense vegetative cover is present on the landfill, the evapotranspiration of these plants can be considerable. Depending on the local climate and annual precipitation, up 4 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. to 60% of the water may evaporate and, depending on the slope grades, another 5 to 20% can be diverted on the surface (Bilitewski et al., 1994). The function of the surface layer is to cover and protect the barrier layer from water and wind erosion, desiccation, freeze-thaw, and penetration by equipment or burrowing animals, and to support the growth of vegetation. Soils capable of supporting vegetation growth are used in the surface layer. Other materials may also be used in the surface layer such as cobbles and paving materials, although these applications are rare (GeoSyntec Consultants, 1995). The surface layer of the final cover system will be exposed to environmental conditions over the design life of the landfill. During this time period, erosion and sediment control measurements are implemented to minimize soil loss due to rain, runoff, and wind, prevent the development of rills or gullies, protect the underlying layers of the cover system including the barrier layer, and minimize sediment impact to the surrounding environment (GeoSyntec Consultants, 1995). According to the universal soil loss equation (Hillel, 1998), soil loss is related to rainfall intensity, soil type, length and inclination of slope, vegetation, and land management practices. To reduce soil loss, certain criteria for construction material, construction of the surface, plant selection, and maintenance of the surface layer have to be implemented. Soils or other materials used in the surface layer are selected to be of appropriate texture, organic content, salt content, acidity, and nutrient content for plant growth depending on the plant species and climatic conditions at the site. The failures of existing cover systems (from 163 landfills, 146 have groundwater contamination, EPA 1988) and results of several research projects support the need for finding an adequate capping system with regards to ecological and economical aspects based on site specific parameters (e.g. climate, geology, hydrogeology, leachate and landfill gas management, end use) (Dwyer, 1998; Siuru, 1996; Hakonson, 1997). EPA 5 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. recommends a soil tolerance level of 4.4 tons ha'1 yr'1 to prevent deflation of the cover surface over the lifetime of the site. Cover design features that are used to prevent erosion include the establishment of vegetation, the use of mulching techniques, synthetic mats, controlling slope and slope length, and the construction of terraces or benches (Hakonson, 1997). Depending on the capping system, costs range from $400,000 to $500,000 per hectare (Dwyer, 1997). Hence, the landfill is operated on a 'user pay' basis; wherein tipping fees are set to recover these future costs. Late implementation of these costs would end in a drastic increase of the tipping fees. 1.2 Pulp and paper sludge Pulp mill sludge, hereafter referred to as sludge, is a by-product of the pulp and paper industry. The pulp and paper industry in the United States generates 5.3 million metric tons of sludge annually (dry weight) (National Council for Air and Stream Improvement (NCASI), 2000). Quebec and Ontario mills produce an estimated 720,000 metric tons per year (Chong et al., 1988), while a Kraft mill in Prince George produces approximately 10,950 wet tons of sludge per year (Sigfusson, 1999). Presently, the sludge is treated as an industrial waste and either landfilled or incinerated. Sludge disposal poses significant environmental liabilities, logistical problems, and economic burdens. Paper mills spend between $50 and $100 per ton to dispose of the sludge at a typical landfill. Pressured by high waste-related disposal costs, increased difficulty and expense of permitting new landfills, accompanied by growing environmental concerns, the pulp and paper industry is searching for beneficial alternatives to dispose of sludge. Paper making is a three step process. First, the source of cellulose fiber has to be identified. The source can be wood, recovered paper or non-woody plants. In the 6 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. second step, usable cellulose fibers are produced (pulping). In the final step, paper is made after formatting sheets of pulp, pressing and drying. The main processes used in the pulp and paper industry to make pulp are mechanical pulping, semi-mechanical pulping, and chemical pulping. Mechanical (groundwood or refiner) pulping uses physical forces to separate wood fibers, resulting in a high yield pulp that is characterized by shorter fibers and relatively low strength (Mabee, 2001). However, it is a lower cost method compared to producing pulps for other useful applications than from chemical pulping. Also, compared to chemical pulping which only produces about 50% yield of pulp from the starting wood feedstock, mechanical pulping operations typically attain about 100% yields. Groundwood pulps are made by forcing a log against the face of a cylindrical abrasive stone which rotates at high speed. Refiner pulps are made by passing wood chips in water through a set of disc refiners (one or both rotating at high speed) (Walker, 1993). Semi-mechanical pulping techniques include the addition of heat and/or chemicals. Thermomechanical pulps (TMP), chemi-thermomechanical pulps (CTMP), and bleached chemi-thermomechanical pulps (BCTMP) can be produced after the initial mechanical process. Mechanical and semi-mechanical pulps account for only 15% of North America’s total pulp output (Mabee, 2001). The current trend in the industry has been an increase in semi-mechanical and less investment in purely mechanical pulping. Chemical pulping also includes CTMP and BCTMP, as well as alkaline pulping, and sulphite pulping. Alkaline or acidic chemicals are used to dissolve lignin and release individual fibers. This method of pulping can work in both high and low pH ranges, has an increased chemical to wood ratio, uses more severe cooking, and the pulp is readily bleached (Roberts, 1996). The CTMP process produces pulps with short average fiber length, resulting in low paper strength (Mabee, 2001). A CTMP mill generally uses less 7 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. power than the BCTMP process and has pulp yields of 85-90% (MacDonald et al., 1969). Alkaline pulping, also known as Kraft or sulphate process, is the most common method used in the pulp and paper industry, and is responsible for approximately 80% of North American pulp production (Mabee, 2001). Kraft pulping produces pulp in good yields and is consistent with the highest pulp quality and strength (Biermann, 1993). Paper is generally made out of a blend of hardwood and softwood to meet the strength and printing surface demands of the customer. Wood is mostly composed of cellulose, hemicellulose, lignin, and extractives. Cellulose is a highly suitable raw material with wide applications and shows small morphological differences among species of trees (Schuerch, 1989). It consists of long, straight chains of glucose monomers. It forms the skeleton of the plant cell wall and has the most desired properties for making paper. These fibers are long, strong and translucent (Blum, 1996). Hemicelluloses are short, branched polysaccharides from a variety of sugars. This results in a polymer with a lower molecular weight than cellulose. Hemicelluloses fill in space in the plant cell wall and make up 20% of the total wood mass, although this fraction can change between soft and hardwood species. They are more soluble in water and thus are often removed during the pulping process. Lignin is the most complicated wood macro polymer. Unlike cellulose and hemicellulose, lignin is not fibrous, and is composed mostly of aromatics (Glasser et al., 1996). It is an amalgamation of two (or three) principal phenylpropane groups and their derivatives, which combine in countless numbers of ways to produce a very large, am o rp h o u s m o le cu le . Th is th re e dim en sio n al cross-linked p o lym er o f h e te ro g e n e o u s structure generally acts as an interfiber bonding agent, imparting strength and cohesiveness to the physical structure of the tree (Zakis, 1994). The presence of lignin is considered undesirable by the pulp and paper industry, as it hampers the production of 8 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. quality paper and imparts color to the nearly white tone of cellulosic matter. Lignin usually makes up 20% of the total wood mass (Mabee, 2001). Extractives is a collective term referring to extractable components and trace elements found in wood. Some of these substances include fatty acids, resins, tannins, sugars, resenes, turpenes (appendix A), gums, and waxes (Roberts, 1996). These components serve no structural function, and normally form the smallest portion of the total wood mass at approximately 3-8% (Mabee, 2001). Pulp mill sludge represents the waste portion of the pulping process. It contains knotted and separated wood fibers, dirt, and any other materials introduced through the pulping or recycling process. The principle component of sludge is water, which makes up more than half of the total mass of sludge even after dewatering (Mabee, 2001). Sludge is mainly composed of unused cellulose and is produced in various stages of the pulping process (Figure 1). As the wood input, the wood processing and the subsequent effluent treatment varies greatly, so does the composition of the sludge. The physical and chemical characteristics of the sludge of a single mill changes over time, and the sludges from different mills using similar processes will exhibit different properties. A better understanding of the characteristics of sludge is needed to come up with more effective and economically viable means of disposal and/or recycling. As governmental regulations require that at least 10% of manufactured paper must be recycled, more and more paper mills are using recycled paper in the manufacture of paper. Production of paper from recycled materials increases the amount of sludge produced at paper mills (Coburn and Dolan, 1995). Because of recycling, more unusable, short, odd-shaped fibers (cellulose) are generated from post-consumer fibers than from virgin pulp. Sludge or wastewater treatment plant solid residuals are those solid materials, collected in the process of treating water used in the mill prior to release into the 9 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. environment. Typically, these materials consist of solids collected in primary treatment (separation of solids from raw wastewater) and secondary treatment (biological treatment followed by clarification to separate biosolids) (NCASI, 2000). Primary sludge is produced through the physical cleaning of the wastewater stream. It is collected in screens and filters and is fairly clean, consisting of wood fibers, fines, some inorganic fillers, and water (Mabee, 2001). Primary sludge is usually easy to dewater because of the relatively high fiber to fines ratio of the organics and because of the high proportion of woody-organic material in the sludge (Kennedy et al., 1989). The moisture content varies from 30 to 70% depending on the drying process employed. As there is ten times more primary then secondary residual they are combined to facilitate handling. Primary sludge is derived from primary clarification treatment and is comprised predominantly of wood fibers. Because of the high wood fiber content, primary sludge has low nitrogen (N) concentration, ranging from 0.05 to 0.9%, with C:N ratios often ranging from 100:1 to 300:1. Secondary sludge is derived from biological treatment of effluent during which N and P are commonly added. This sludge consist largely of microbial biomass and has higher concentrations of N and P and lower C:N ratios ranging from 5:1 to 20:1. Both primary and secondary sludge can provide significant sources of other macro- and micronutrients, although concentrations of these constituents vary widely (NCASI, 2000). The vast majority of sludge is combined primary and secondary sludge representing 54% of the total residual production (NCASI, 1999b). A simplified layout of sludge generation paths is shown in Figure 1. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Centrifugal Cleaners (Varying Consistencies) Mechanical Pulping/ Chemical Pulping/ Recycling Screens (Varying P ressu res/ C onsistencies) Raw Materials Flotation Deinking Refiners/ Fiberizers/ Dispensers Secondary Treatment: ActivatedSludge/ Aerated Lagoon Pulp Headbox Paper Machine PRIMARY SLUDGE SECONDARY SLUDGE "1 { j —© ▼ PRO D UC T Sludge Press Mixed Sludge Figure 1: Sim plified layout o f s ludge g eneration paths after M a b e e , 2001 A to D : Recovered sludge sources Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. The sludge is also generally low in potential environmental contaminants. In recent years the reduction of metal concentrations in ink, analysis of raw materials and processing chemicals led to lower metal concentrations in the sludge. Nevertheless, chemical characterization is important as the metal concentrations in sludge wood fibers are largely derived from the manufacturing process. 1.3 Environmental considerations The high organic matter content of sludge represents a valuable resource as soil amendment (Bellamy et al., 1995; Bowen et al., 1996; Edwards, 1997; Carpenter and Fernandez, 2000) when soils are depleted or subject to erosion. Sludge is also rich in macro- and micronutrients. The organic matter and nutrients are the two main elements that make the use of this kind of waste on agricultural land as fertilizer and organic soil amendment suitable. Although attractive for use as soil amendment, there can be potentially harmful effects from the sludge depending on its constituents. The most significant environmental concerns associated with the land application of sludge are the potential for constituent movement - either down and out of the soil profile potentially entering surface or groundwater, or the assimilation into plants and associated food chain effects. This is largely dependent on the volume of material applied, concentrations of trace elements, mobility and toxicity of elements from the materials, and incorporation of the elements into living organisms (Barker et al., 2000; Mullen, 2002). Sludge properties such as percent organic matter, pH, cation exchange capacity, texture, and timelines for microbial modification are expected to influence short and long term metal and nutrient mobility. In terms of soil quality, the British Columbian Landscape Association (BCLA, 2001) has set quality criteria for boron (B), total nitrogen (N), phosphorus (P), potassium 12 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. (K), calcium (Ca), and magnesium (Mg) besides C:N ratio, organic matter concentration and pH. These standards are listed in Table 2. Table 2: Quality standards for productive soils (BCLNA, 2001). Constituent Units Range C:N Organic matter Acidity Boron Total N Phosphorus Potassium Calcium Magnesium ratio % PH ppm % ppm ppm ppm ppm < 40 3-5 6-7 <1 0.2-0.6 20-100 50-250 1500-2000 175-250 Nitrogen (N) content often limits the effectiveness of sludge as a soil amendment (Edwards, 1997; O’Brien, 2001). Only secondary sludge contains significant quantities of N. Because of their low N concentrations and high C:N ratios, primary sludge can induce N deficiencies in vegetation when land applied. As with most organic material, soil microorganisms utilize both C and N during decomposition of sludge applied to soil. Since the C:N ratio of the sludge is much higher than that of microbial cells (roughly 7:1), soil microorganisms must utilize inorganic N (i.e., NH4+ and N 0 3") from the surrounding soil matrix during sludge decomposition. The immobilized N is not lost from the system, but is synthesized into organic forms that are unavailable for plant uptake until the microbes die and decompose themselves. This process can reduce N leaching when high N sludges are applied, but is also the cause of potential N deficiencies in vegetation when low N sludges are used. Depending on the N concentration in the surrounding soil, primary sludge may have to be applied in limited quantities or external sources of N added to prevent such deficiencies in the soil sludge system. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. As secondary sludge contains mainly microbial biomass and nutrients (primarily N and P) the properties of the combined sludges depend on the proportion of primary and secondary sludge in the mix, and the type of products being produced by the mill. Secondary sludge can thus provide a valuable source of N for vegetation, but there is also more potential for N leaching and runoff if high application rates are used (NCASI, 200 0 ). Organic matter, such as sludge, has a direct effect on water retention because of its hydrophilic nature, and an indirect effect because of the modification of the soil structure that may be affected due to the presence of the organic matter. Porous media like soil consist of solid material and void or pore space. Air and water and possibly nonaqueous phase liquids occupy the pore space. The spatial arrangement of the soil particles relate to both the size and shape of the components and their arrangement in aggregates. There are two broad categories of aggregates. Microaggregates are less than 250 pm in diameter and macroaggregates more than 250 pm. Pore diameters in microaggregates mainly range from 0.2 to 6 pm; in macroaggregates from 25 to 100 pm. Pore size determines the hierarchy at which pores remain water-filled at differing soil water potentials (Paul et al. 1996). The relation between the soil water content and the soil water suction (matric potential) is a fundamental part of the characterization of the hydraulic properties of a soil. The water retention function relates a capacity factor, the water content, to an intensity factor, the energy state of the soil water. The term soil water is used for the solution or liquid phase of the soil (Klute, 1986). A soil is composed of 25% water, 25% air, 47% minerals and 3% organics (Klocke et al., 1996). The amount of water in the soil influences many processes, including gas exchange with the atmosphere, diffusion of nutrients to plant roots, soil temperature, and the speed with which solutes move through the root zone during irrigation or rainfall. The force with which water is retained by the 14 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. soil matrix also affects the amount of drainage occurring under gravity, and the extent of upward movement of water and solutes against gravity (Gardner et al., 1991). The soil water characteristic curve (also called moisture characteristic, matric potential, or water retention curve) shows the relationship between water content and soil suction in the vadose zone (Burckhard et al., 2000). The terms matric potential, matric suction, and soil water suction are used interchangeably. Soil suction is defined as the negative gauge pressure, relative to the external gas pressure on soil water. It describes the soil’s ability to store and release water. If the soil water retention curve is known then it is possible to estimate the amount of water available to plant roots. The upper soil moisture limit for plant available water is considered to be at field capacity. The micropores are still filled with water and can supply plants with needed water. The matric potential will vary from soil to soil but is generally in the range of -10 to -30 kPa (Brady et al., 1999). The lower soil moisture limit for plant available water is the permanent wilting point (PWP). There is only some water remaining in the smallest of the micropores as a thin film. By convention the permanent wilting point is the amount of water retained by the soil when the water potential is -1500 kPa. Moisture retention curves of soil samples are determined in the laboratory by using a pressure plate apparatus. This equipment allows the application of successive suction values and repeated measurement of the equilibrium soil wetness at each suction. Sludge as an organic amendment affects soil structure by increasing soil aggregation and stability. In well-aggregated soil, the interaggregate macropores drain very quickly, while the intra-aggregate micropores tend to retain their moisture against gravity. On the other hand, a dispersed or compacted soil has few macroaggregates and drains very slowly. Air entry and oxygen diffusion are thereby affected. Depending on the amount of organic matter present, soil organic matter can contribute to the retention of soil moisture. The moisture retention or water holding capacity represents the temporary 15 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. internal drainage or redistribution of water in the soil, responsible for maintaining an amount of moisture for plants to survive during periods between rains or irrigations. Organic matter increases soil aggregation and stability, reduces bulk density, and increases water-holding capacity and retention (Khaleel et al., 1981; Metzger and Yaron, 1987; Tester, 1990; Hill and James, 1995). The increased soil aggregation is also due to increased microbial activity, which increases soil porosity (Hill and James, 1995). Over time microorganisms incorporate carbon into soil organic matter (Camberato et al., 1997). As sludge decomposes, carbon is lost to the atmosphere as carbon dioxide, which gradually decreases the C:N ratio and increases the availability of nitrogen for plant growth. The concentration of organic matter in soil is mainly responsible for water and ion retention and supplying both to plants. High and low concentrations of organic matter limit soil productivity. Metal and nutrient availability in part depend on the soil acidity. Soil acidity is affected by low pH as well as the effects the pH has on metal and micronutrient availability. The U.S. EPA has established metal loading limits for land-applied municipal sewage sludge, which generally have high metal concentrations compared to paper mill sludge (Table 3). In British Columbia the metal contents in soils used for specific sites such as agricultural, urban park, residential, commercial and industrial lands are regulated under the Contaminated Sites Regulation. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Table 3: Comparison of macro- and micronutrient concentrations in pulp and paper sludge a and municipal sewage biosolids d (NA SCI, 2000). NCASI 54 Mill Survey bc range Municipal sewage biosolidsd median range median Macronutrients (g/kg) N 0.51 -87.5 P 0.01 -25.4 K 0 .1 2 -1 0 0 .2 8-210 Ca Mg 0 .2 -1 9.0 S 0 .2 -2 0 .0 8.98 2.35 2.2 14 1.55 4.68 < 1.0-210 < 1.0-150 0.2 - 650 1 .0-250 0 .3 -2 5 .0 6 .0 -1 5 32.0 14.0 2.3 27.0 4.0 11.0 Micronutrients/Metals (mg/kg) <0.1 - <11 Ag Al 590 - 59000 As <0.07-8.3 B <1 -491 Ba 17.9-1800 Cd <0.09 - 56 Cl <0.06 - 8500 Co 0 -9 .7 Cr 3.0 - 2250 Cu 3 .9 -1590 97.1 - 10800 Fe 0.0009 - 3.52 Hg Mn 13-2200 <2.5-14.0 Mo 300 - 66700 Na Ni 1 .3 -1 33 Pb <0.05 - 880 Se <0.01 -<31 Sn <70.6 Ti 3100-76000 Zn 13 -3780 0.55 13400 1.2 25.0 160.0 1.2 383 NA 42.0 52.0 1540 0.35 155.0 NA 2200 18.3 28 0.21 NA NA 188.0 NA 1000- 13500 0 .3-315.6 4 -1 0 0 0 <0.01 - 9000 0.7 - 8220 NA 1 -260 2.0 - 3750 6 .8 -3120 1000- 15400 0 .2 -4 7 .0 32 - 9870 2.0 - 67.9 100-30700 2.0 - 976 9 .4 -1 67 0 0 .5 -7 0 .0 40 - 700 NA 38 - 68000 NA 4000.0 6 33 200 7 NA 10 40 463 1700 4 260 11 2400 29 106 5 150 NA 725 a Concentrations o f som e m etals in sludge have declined in recent years due to reductions in m etal concentrations in inks and more careful scrutiny o f raw m aterials and processing chem icals. For this reason, m etal concentrations in sam ples collected prior to 1990, particularly m axim um values, m ay be higher than those in present day sludges and should be interpret with a high degree of caution. bAn assortm ent of primary, secondary & com bined sludge. 0 N C A SI 1984 N A = not available d McG overn et al. 1983 17 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. The total trace element content of a soil may not relate to the plant growth; as only a portion of the total metal is available to the plant through absorption from the soil solution (Pais and Jones, 1997). As different plant species have different elemental needs, this would be another consideration in the suitability of using sludge. Table 4 lists typical ranges of the plant macro- and micronutrients required for plant growth and their primary function in plants. Table 4: Plant macro- and micronutrients and their functions (W hitehead, 2000). Constituent Typical Range Primary Function Macronutrients N P 2.0-3.5% 0.2-0.5% S Ca Mg K 0.15-0.60% 0.6-0.8% 0.25-0.30% 1.0-3.5% required for protein synthesis transfer of energy through A D P to A TP for energy storage form amino acids which are incorporated into proteins cell wall stabilization and osmotic regulation photosynthesis and protein synthesis open/close stomata and transport photosynthate Micronutrients B Cu Fe Mn Mo Zn 8-15 ppm 10-15 ppm 150-175 ppm 70-100 ppm 0.1-4.0 ppm 35-40 ppm cell wall synthesis and membrane function photosynthesis and nitrogen fixation Constituent of proteins involved in redox reactions electron transfer and detoxification of free radicals N metabolism (conversion of ammonium to nitrate) enzyme catalyst Since the late 1980s, dioxins have been an environmental concern with sludge derived from chlorine-based bleaching processes. Over the last decade; however, new technologies have reduced dioxin concentrations in bleaching mill effluents and residuals (sludge) (NCASI, 2000). Although concentrations of metals and potential organic contaminants in sludge are generally low, elevated concentrations can occur in some situations and should be determined prior to establishing a recycling path. 1.4 Project objectives The focus of this research was to evaluate the moisture retention properties of 18 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. sludge amended soil in a laboratory set up in order to determine the usefulness of sludge as landfill cover. The moisture retention influences the available amount of water for plants. Organic matter increases water holding capacity. As the water holding capacity affects the water uptake by plants, it is important for the final layer of a landfill capping system. The final layer is also exposed to water related damage resulting in soil loss and further infiltration. Sludge amendment could result in higher absorption of water, thus reducing infiltration to the barrier layer. 19 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Chapter 2 Literature Review Currently, 67% of sludge produced in North America is landfilled or incinerated, neither of which utilizes the potentially valuable properties of this paper mill by-product (Carpenter and Fernandez, 2000). Only 13% of the sludge is reused or recycled. The pulp and paper industry has sought alternatives to sludge disposal since the early 80’s. At the same time, individual pulp companies privately owned over 50% of landfills used in the pulp and paper industry. This figure is declining, due to increasingly stringent requirements for siting and construction (Glowacki, 1994). 2.1 Sludge disposal alternatives Since sludge is mainly composed of organic fibers other disposal options are incineration, land application, and recycling/reusing the fiber-rich material. The sludge disposal practices are shown in Figure 2. Figure 2 summarizes a survey conducted by NCASI representing 98% of the sludge generated by 204 mills in the U.S. in 1995. L a n d A p p lic a tio n 12% B u rn ' L a n d fill/ O th e r Lagoon B e n e fic ia l U s e 51% 5 .5 % R e c y c le / R e u s e 5 .6 % 3.9 Million Tons - Total Sludge Production Figure 2: Final sludge disposal practices (NCASI, 1999). 20 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. In 1995, according to NCASI, the pulp and paper industry produced a total of 3.9 million dry tons of sludge. Of this, 51% were landfilled, 26% incinerated, and 23% were beneficially used. These numbers are slightly different from Carpenter and Fernandez (2000) publication as they come from different sources and years. Incineration of sludge serves the purpose of disposing the material to recover energy for the paper making process. Unfortunately, the high moisture and ash content of sludge make total combustion difficult. Modification of traditional incinerator technology and mixing sludge with high amounts of bark is necessary in order to totally incinerate the organic material. Before combustion, the moisture content of the material needs to be reduced. A great deal of heat is necessary to burn sludge when it has high moisture content (Mabee, 2001). Other, but less economical alternatives to incineration include ethanol production by indirect combustion and pelletizing sludge as an alternative fuel source. Recycling options are based on the chemical or physical characteristics of the sludge. Because sludge is a significant source of organic matter and nutrients, early research focused on land application for enhancing growth of trees and crops. Land application of sludge is the most popular disposal alternative for the pulp and paper industry in countries such as the United States, Sweden, Finland, India, Brazil and Canada (Alberta, British Columbia, Ontario, Quebec). The main problem identified in the earliest trials was the low fertilization value associated with the sludge (NCASI, 1984a). This problem was addressed by numerous pilot projects using discrete materials mixed with sludge to be of beneficial use as soil amendment. Another option to increase the fertilization value was composting mixed sludges, most utilizing the aerated static pile method (Biofine Inc., 1998). Composting lowers the 21 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. C content, which combined with high N feedstock decreases the C:N ratio. Several composting facilities include wood ash in their feedstock mixture to decrease the moisture content and increase the mineral content of the mix (Kunzler, 2001). However, composting can be quite expensive (upwards of $30/ton) and thus economic success is dependent upon market conditions (Pickell and Wunderlich, 1995). Further recycling technologies are based on the physical characteristics of sludge. The fibrous material can be used in the manufacture of ceramic and building materials, such as cement, bricks and concrete. If sludge is used as filler or aggregate in cement or concrete, the tensile strength increases. Sludge-amended material will not crack as easily under freezing and thawing conditions. It could be used to construct highways, buildings and bridges, providing a longer lifespan (Canning, 1999). Sludge has been used beneficially as absorbent materials for industrial cleanups, hydromulch, and animal beddings. Land-applied sludge is a source of organic matter affecting physical properties of the soil like aggregation, stability, bulk density, water holding capacity, and water retention. Organic matter plays a fundamental role in the stabilization of soil and the formation of pores (Khaleel et al. 1981; Metzger and Yaron, 1987; Tester, 1990; Hill and James, 1995). These attributes are of importance in land reclamation and construction projects. Sludge has been used beneficially in several land reclamation projects in the UK and U.S. Recovery of unusable land is enhanced by sludge application to areas where plant growth is non-existent or limited, often due to previous industrial activities that have introduced or brought to the surface substances which are unfavorable to plant growth. In the UK and U.S., sludge has been applied to spoil mounds from abandoned coalmines. Such locations tend to generate acidic run-off (as low as pH 3-4 in some 22 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. cases) due to oxidation of pyrites in the colliery spoil (Webb, 2000). That means that the absorptive activity and the buffering capacity of any calcium carbonate in the sludge is particularly valuable. Sludge also has a much higher affinity to adsorb heavy metals than typical kaolinite clay because of its high organic content. This characteristic is used in another research project in the U.S. where sludge was utilized to build a slurry wall around an old processing plant where zinc and lead contamination endangered groundwater (Canning, 1999; Brown etal., 2003). The clay like behavior of sludge is also of interest for landfill capping. The NCASI has investigated the use of sludge as cover material on a daily, intermediate, and final cover of varying thickness on industrial, municipal, and industrial/municipal waste landfills. The most important physical property affecting the suitability of sludge as material for the barrier layer is hydraulic conductivity. It describes the ratio of the flux to the potential gradient of water (volume per time) (Hillel, 1998). Field hydraulic conductivity studies were conducted at barrier layer test plots over eight years. At the effective stress of approximately 5 kPa existing during the service life of the test plots, sludge had a hydraulic conductivity of 4x1 O'8 cm/sec. The clay test plots had a hydraulic conductivity of 1x1 O'6 cm/sec. The test results also showed that the barrier layers made with paper mill sludge underwent no deterioration in performance during their service life. After the eight year study sludge in the test plots appeared identical to fresh sludge, which also suggests that the sludge had not degraded. In addition to the hydraulic conductivity measurements, a dye tracer study was conducted. The study showed that only one preferential flow pattern existed in the sludge barriers, and this flow path appeared to be in a construction defect. In contrast, the clay barrier layers were riddled with preferential flow paths, and thus had much higher hydraulic conductivity than the paper mill sludge (NASCI, 1997). Some of the earth normally used to cap the daily inputs can be replaced by sludge. The observation that sludge has properties similar to 23 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. some clay soils has created particular interest in using sludge as landfill liner material and as the hydraulic barrier layer in landfill covers. Results from previous studies are summarized in Table 5. Table 5: Residuals index properties and hydraulic conductivity of sludge used as barrier layer from previous studies (NCASI, 2002). Source Andersland and Laza (1972) Kraus et al. (1997) Zimmie and Moo Young (1993-1997) NCASI (1989) Benson and Wang (1996) W ater Content1 Organic Content (% ) Ash Content (% ) Solids Content Specific Gravity Hydraulic Conductivity3 (cm/s) - 49-84 28-50 2.22.36 8.1x1 O'5 8.1x1 O'6 1.4x10'3 2.8x1 O'8 150-260 44-56 “ “ " 150-268 - 35-60 29-40 1.8-2.0 121-409 10-62 - 20-45 1.6-2.4 - - - (%) - - 7.4x1 O'7 1,1x10'8 4 .2x 1 0'4 5.8x1 O'8 8 .3x10'7 9.9x1 O'9 Residuals Type Sorted Organic Residual Primary and combined Primary and combined Primary and combined Primary and combined2 1water content = (wet mass-dry mass)/dry mass 2tests conducted at effective stresses ranging from 5 kPa to 60 kPa 3sludge compacted similar to compacted clay 2.2 Case studies o f various applications Sludge from paper manufacturing has been applied to agricultural and forestry land to increase net primary productivity for decades. Numerous studies throughout North America and Europe have highlighted the benefits associated with utilization of sludge as soil amendment. Intensive agriculture and nursery culture in the Niagara area of Ontario have resulted in a high demand for organic soil amendments. Besides manures and peat moss, organic-rich paper sludge and sludge-based composts could serve as substitute soil amendments. In several studies, crop yield was investigated in relation to sludge application (Bellamy et al., 1995). Tomatoes, cucumbers, and peppers were grown with 24 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. separate and mixed primary, secondary and deinking sludge components. All growth responses were related to N content in the sludges. Inhibited growth was observed with primary and deinking sludge, which are low in N content. Secondary sludge, which is rich in N, produced excessive growth. A blend of primary and secondary sludge enriched with N fertilizer had a beneficial effect on vegetable growth in the greenhouse. In a second greenhouse experiment with shrubs and an additional field experiment with corn the growth of the species was correlated to the percent of N in the sludge soil mixture. In conclusion, sludge utilization is constrained by N immobilization in sludge-treated growing media or field soils, resulting in N deficiencies in plants. This could be overcome by adding appropriate quantities of N fertilizer (Bellamy et al., 1995). In Spain, three organic residues (olive mill sludge, municipal solid waste compost, paper mill sludge) were used in a 3-year field experiment involving orange production (Madejon et al., 2003). The application of compost and paper mill sludge increased orange yield. Moreover, total carbon and humic substances significantly increased in soils treated with all the organic amendments. Positive correlations between enzymatic activities and total organic carbon were found for all treatments. However, a clear inhibition of phosphatase activity was observed in soils treated with sludge. This result indicates that repeated application of moderate amounts of organic amendments has positive effects on the chemical and biochemical properties of the soil, as well as on the orange yield (Madejon et al., 2003; Gagnon et al., 2001). Sludge amendment promotes microbial growth and activity in the soil by improving carbon and water availability. A measurable indicator for bacterial growth is the enzyme phosphatase, which accelerates the hydrolysis and synthesis of organic esters of phosphoric acid and the transfer of phosphate groups to other compounds. Phosphatase activates the mineralization of organic phosphorous, releasing phosphate, which would otherwise not be available. 25 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. In Atlantic Canada, the amendment of sludge to organic-matter-depleted potatoproducing soils was investigated. One year after incorporating sludge at rates equivalent to 0.5, 1.0, 2.0, and 4% organic matter in the plow layer of a gravelly loam soil, bulk density had decreased with increasing rates of organic matter addition, while saturated hydraulic conductivity and specific moisture content increased. The beneficial effects of the organic matter treatment include 2.1 times delay in runoff initiation, and 23 and 71% reduction in runoff and soil loss. Although the beneficial effects in soil and water conservation are apparent, a minor drawback appears to be lower field soil moisture content, which could be controlled by sludge application rates (Chow et al., 2003). Forest land application is a particularly attractive use for this material because many companies own forest lands that are in close proximity to mill sites where the sludge is generated and would be consistent with the concepts of sustainable forestry (NCASI, 2000). In one study, growth and yield of lodgepole pine and white spruce grown on sludge-treated soil were measured. Primary and secondary sludge mixed in the ratio of 1:2 was applied to marginal forestland at a rate of 80 t/ha per year. The resulting seedling growth showed significant increases of up to 250% in both height and diameter compared to control sites (Macyk, 1999; Mabee, 2001). Effects of land-applied sludges on forest productivity have been shown to depend to a great extent on their N content and availability. A study on productivity of cottonwood, Douglas fir, Noble fir, and white pine seedlings grown in nursery beds showed direct dependency on the C:N ratio (Henry, 1986). Growth responses to sludge were positive with C:N ratios up to 20:1. Positive tree growth responses have been reported for sludges having C:N ratios of 100:1 to 150:1 (Henry, 1991). While the contribution of organic matter from sludge is often confounded by effects on N availability, the importance of sludge as a source of organic matter has been demonstrated on some sites. One study showed that land application of primary 26 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. sludge (C:N 213) on a fertile alluvial site in Oregon increased initial cottonwood height growth 41% above fertilized, control plots (Shields et al., 1986). Although greater initial growth increases (68%) were obtained with a higher nutrient, primary:secondary sludge mixture, respective increases in height growth after three years were 31% and 38% for primary and mixed sludge treatments. This suggests that site factors related to organic matter were more limiting than nutrients. Surface-applied sludge can also enhance soil moisture retention and alter soil temperature due to its mulching effect. Positive effects of surface-applied sludge increased tree growth were attributed to improved moisture retention on a site in the Pacific Northwest (Henry, 1991). A study in Maine showed reduced growth of red pine, Japanese larch, and black spruce seedlings due to lower soil temperature brought about by surface-applied sludge (Kraske, 1992; NCASI, 2000). 2.3 Landfill applications In numerous laboratory and field studies, some paper mill sludges have been shown to possess engineering properties similar to clays. The use of paper mill sludge in landfill construction was initially investigated by Stoffel and Ham (1979) and Pepin (1984). Based on these promising studies, significant research has been done by NCASI and others using sludges for construction of barrier layers in landfill final covers (NCASI, 1989; Genthe, 1993; Floess et al., 1995; Moo-young and Zimmie, 1996; NCASI, 1997). These studies indicate that the hydraulic performance of barrier layers constructed with sludge will be as good as, or better than, the performance of barriers with clay. The e arlies t reported d a te for a sludge incorporated into a landfill c o v e r w a s 1990. This disposal alternative has the potential to use large quantities of sludge, and may be particularly advantageous to landfill operators in regions where paper mills exist and clay sources are scarce or costly (NCASI, 1997). 27 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Hydraulic conductivity tests were conducted on 15 paper mill sludges of various origins (NCASI, 1989). After compaction of the specimens at their as-received water contents (120-409%) using standard Proctor procedures (ASTM D 698), rigid-wall compaction-mold permeaters were used for hydraulic conductivity testing. The resulting hydraulic conductivities ranged from 4.2x1 O'6 to 5.8x10"10 m/s. The low hydraulic conductivity obtained for some of the paper mill sludges suggested that some sludges may be viable for use in constructing barrier layers, which generally are required to have hydraulic conductivities less than 1x1 O'9 m/s (Kraus et al., 1997). Since 1990, more then 14 landfills in the U.S. have been closed with sludge as the hydraulic barrier material. Landfill size ranges from 1.21 ha municipal landfill to a 12.1 ha industrial landfill. The combined sludges contained approximately 5% to 15% secondary sludge. Barrier layer thickness ranged from 0.6 to 1.2 meter. In some cases, the sludge was placed 25% thicker than the target thickness to account for consolidation. Hydraulic conductivity ranges from 10'5 to 10'9 cm/sec. Overburden thickness ranged from 0.08 to 0.6 meter. In several cases synthetic soil was used as overburden material. This manufactured soil was made from low-quality local soil as the base material. Sludge added to the soil improved desired soil characteristics such as water retention and the ability to support vegetative growth (NCASI, 1997). In Massachusetts, the Hubbardston municipal sanitary landfill used sludge as a substitute low-permeability material for the final cap. The sludge applied to the landfill originated from a small mill processing 100% waste paper, typically pre- and post consumer ground-free ledger and book paper. The annual 12,000 dry tons of sludge contain a high percentage of clay resulting in hydraulic conductivity of 6x1 O'7 cm/s. Based on the results of the pilot study the design of the final cap was approved and a 0.76 meter layer of sludge was substituted for the normal 0.46 meter low-permeability soil layer in the cap (Floess et al., 1995). 28 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. In Michigan, MEAD Publishing Paper Division operates an integrated pulp and paper mill producing approximately 400 t/day of dewatered combined sludge. Instead of disposing the sludge at the company-owned industrial landfill, it was utilized as hydraulic barrier material for the closure of Mead’s 3.64-ha Phase 2 landfill (Malmstead et al., 1999). Recent studies focus on geotechnical, biochemical and microbiological properties of soil organic matter as sludge seems to have applications beyond landfill barrier layers. It has been used as a topsoil amendment in the municipal landfill caps for the towns of Wilton and Hadley (N.Y.). These projects indicate that the sludge amended topsoil readily absorbs large quantities of rainfall, reducing infiltration to the barrier layer and also holding water for vegetation growth during dry periods (Floess et al., 1995). Being at the surface, cover systems exhibit the greatest change in temperature, moisture and atmospheric pressure. On the other hand, the stability of the soil pore system is one of the important properties that affect the ability of the soil to store and transmit air, water, and solutes. Sudden wetting is an important factor that can modify the number, shape, continuity, and size distribution of the soil (Gregorich et al., 1993). Rapid wetting of a structurally unstable soil results in filling of the interaggregate pores by microaggregates, reduced porosity, changes in the pore-size distribution, and a decreased infiltration rate (Nemati et al. 2000). Organic matter plays a fundamental role in the stabilization of soil and the formation of pores (Bolt et al., 1986; Chow, 2003) and bulk density (Martens, 1992). When subjected to sudden wetting, sludge application can improve the resistance of the amended soil to the destructive action of rapid wetting. On comparatively smooth soil surfaces, the beating action of raindrops causes most of the detachment. Where water is concentrated into channels, the cutting action of turbulent flowing water detaches soil particles. As dispersed material dries, it may develop hard crusts, which will prevent the emergence of seedlings and will encourage runoff from 29 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. subsequent precipitation (Brady and Weil, 1999). These steps are the mechanics of water erosion resulting in soil loss. Sludge has the potential to protect the soil during critical periods of vegetation establishment and to prevent erosion on steep side slopes. The processes of depletion and replenishment of soil moisture have received considerable attention from agricultural scientists because of the dependence of plant growth on soil moisture supply. The maximum amount of moisture that can be stored in soil in the field and the degree of dryness to which plants can reduce the moisture content of soil are the limits that determine the range of moisture available to plants (Richards and Weaver, 1944). The effect of organic matter on soil moisture retention became more and more an issue as soil and water quality and quantity became a growing environmental concern. The consequences of soil amended with organic matter were mainly studied in long term field experiments over the last decade. As the case studies show, the research focus was on determining optimum application rates of various organic amendments, including sludge, to improve soil conditions for plant growth. There is no literature available on the effect of organic matter on soil moisture retention investigated in laboratory experiments. Laboratory experiments allow research of various parameters under defined conditions. They can be performed on a small scale, in less time, and in a controlled environment. This environment provides more flexible and cost efficient research without negatively impacting the actual application site. The influence of each parameter on the outcome can be adjusted in the lab and the consequences can be determined which has the advantage of optimizing procedures for field conditions. The result can then be applied to those field conditions and eventually lead to field applications. 30 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Chapter 3 Chemical and Physical Characterization The chemical and physical characteristics of sludge vary with the manufacturing process, and the type of effluent treatment employed. This research was designed to evaluate the feasibility of utilizing two different sludges as soil amendments on a clay topsoil layer in a landfill capping system, amendments designed to support vegetation without causing an adverse environmental impact. The first step in conducting the experimental part was to obtain a clay sample, representative of the Prince George area. Two sludge samples have been obtained: One from a Kraft pulping process and one from a bleaching chemo-thermo-mechanical process (BCTMP). Sludge and soil samples have been distributed in smaller portions and stored in a walk-in-freezer to prevent alterations. The structural composition of the sludge samples was determined visually and with the scanning electron microscope. To chemically characterize the sludge, pH, moisture content, ash content, C:N ratio, cation exchange capacity, electrical conductivity, and salinity were determined. Selected elements were quantitatively determined after closed vessel microwave acid digestion by ICP-AES. Carbon and nitrogen were determined by total combustion. For physical characterization bulk density, porosity, and water holding capacity were determined. Water holding capacity was determined by gravity for three different treatments: original sludge and soil samples, sludge-soil mixtures for BCTMP and Kraft mill sludge samples (10:40, 20:30, 25:25, 30:20, 40:10), and sludge-soil layer systems for BCTMP and Kraft mill sludge samples (1,2,3 layer systems). All samples were utilized as received. Moisture retention curves were established for all three treatments using the pressure plate experiment. Statistical analysis has been performed on all obtained data. 31 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Because sludge is composed mainly of organic fibers, standard procedures for chemical analysis and methods for organic soils were applied. Methods and procedures are outlined in this chapter. Results are summarized and discussed in chapter 4. 3 .1 M a te ria ls a n d m e th o d s 3.1.1 Sample collection A clay type soil sample, representative of the Prince George area, was taken in June 2002 at Tyner Boulevard/Ospika. The soil is similar to the Aleza Lake 1 - Orthic Luvic Gleysol (Arocena and Sanborn, 1999). After removing the dried top layer from a soil stockpile samples were taken from three different spots in the pile. The soil sample was collected in a 20-liter bucket with lid and stored in the walk-in cooler (4°C) at UNBC. Before usage the soil was mixed well in the bucket. The two sludge samples are solid wastes from two different pulp and paper mills. One sludge is from a Kraft pulping process and one from a bleaching chemo-thermomechanical pulping process (BCTMP). Both sludge samples were taken directly from the filter press output. The sludge samples are representative samples from a pile of sludge that was produced at that time. As pulping process conditions change the chemical and physical sludge composition will vary. The pulp mill sludge from the BCTMP was obtained on December 19, 2001. This sludge sample was collected in two 20-liter buckets. Each of the buckets was half filled. The sludge sample from these two buckets was then evenly distributed among four buckets. After closing and labeling, the four buckets were placed in the -20° C walk-in freezer at the University of Northern British Columbia (UNBC). The pulp mill sludge from the Kraft process was obtained on January 23, 2002. This sludge sample was also collected in two 20-liter buckets. Each bucket was half filled with sludge and the material evenly distributed among four buckets. After closing 32 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. and labeling, the four buckets were placed in the -20° C walk-in freezer at UNBC together with the BCTMP samples (Merchant, 2001). 3.1.2 Sample storage For further experiments, smaller amounts of the original sludge samples are needed. Thus, 10 samples of each sludge of approximately 10 g were placed into ZipLock sandwich bags. The 20 bags were put together in a labeled box and stored in the -20° C walk-in freezer at UNBC alongside with the sludge samples in the buckets until needed. 3 .2 S lu d g e c h a ra cterizatio n 3.2.1 pH Determination For pH determination with a pH-meter, a 1:4 sludge-to-liquid (wet weight/volume) mixture was used. The liquid was distilled water. In a 250 ml beaker 5 grams of each sludge sample was weighed and 20 ml of distilled water added. The sludge-water mixtures were left for 30 minutes to equilibrate. After vacuum filtration the pH of the milky, beige filtrate was measured with a pH-meter, ORION, model 420 A (Kalra and Maynard, 1994). 3.2.2 Moisture content The moisture content of both sludge samples was determined by weighing the original sample in an aluminum dish, followed by drying the sludge in an oven and then reweighing. The loss in weight (water) is expressed as a percentage of ovendried weight (Kalra and Maynard, 1994). Drying of the wet sludge samples was conducted at three different temperatures: 55 °C, 80 °C, 105 °C overnight, for a period of no less than 24 33 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. hours. At higher temperatures, some components of organic matter may be volatilized. If the sludge samples contain significant amounts of volatile compounds, the drying temperature would be a source of variation in the results. For the BCTMP and Kraft mill sludge the water content was conducted on 8 trials for the three temperatures. Data obtained from the moisture content determination are listed in appendix B. C alcu lation s: (1) Wd = Wt - W A, where Wd is the weight of the dry sludge sample in g, Wt represents the weight of the dry sludge sample and the weighing dish in g, and WAi represents the weight of the weighing dish in g. (2) /■> weight of sample wet (Ww) - weight of sample dry (Wd) — ----- - x l 0 0 % weight of sample dry (Wd) 0 = -------2-------------- ----------- ------- --------- 2-------------- where 0 is the moisture content in percent, Ww represents the mass of the wet sample and Wd represents the mass of the dry sample. The mass wetness (Ww), also called gravimetric wetness, is the ratio of the weight loss in drying to the dry weight of the sample (mass and weight being proportional) (Hillel, 1998). 3.2.3 Bulk density The bulk density was determined for each treatment in the water holding capacity and pressure plate experiment. The bulk density for each sample is obtained by dividing the total dry mass over the total volume. The results for the original sludge and soil samples are listed in Table 8. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Calculation: (3) Db Wd weight of oven - dried sludge [g] Vs volume of sludge [cm ] = -----= ------ - ----------------------------- — . „ t . r , ,, = bulk density [g/cm3] where Db is the bulk density in g/cm3, Wd represents the weight of the oven-dried sludge in g and Vs represents the volume of the sludge in cm3 (Brady and Weil, 1999). This calculation was applied to all experimental parts where bulk density was determined. 3.2.4 Porosity With the bulk density, the porosity can be calculated. Knowing the porosity permits interpretation of the sludge behavior in terms of infiltration. Calculation: ... (4) _ . Db bulk density [Mg/m3] P= 1 = 1-------------------------- 2 ----- - porosity [ ] DP particle density [Mg/m ] Where, P is porosity; Db represents bulk density and Dp represents soil particle density. Assumption: Dp = 1.51 Mg/m3; particle density for organic soil (McGill, 2002) 3.2.5 Scanning Electron Microscopy and Energy Dispersive X-ray System The scanning electron microscope (SEM) uses a beam of highly energetic electrons to examine objects on a very fine scale. This examination can yield to information as to structure and composition of the sludge samples. Each of the two oven-dried sludge samples (105 °C) was fixed to an aluminum peg with silver epoxy glue and sputter coated with a thin layer of gold (McGill, 2002). 35 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. The sludge samples were observed under different enlargements to describe the sludge appearance and compare the structure of the two samples. Semi-quantitative elemental analysis was also provided on both sludge samples by using the energy dispersive X-ray system (EDX) of the SEM (Philips Electron Optics, Philips XL 30). The results of the elemental analysis depend on the spot in the sample analyzed. 3.2.6 Total Carbon and total Nitrogen (%C and %N) For the determination of total carbon and nitrogen in the Kraft mill sludge and the BCTMP sludge the oven-dried (105 °C) and ground samples (100 mesh) were used. The method used to determine the carbon to nitrogen ratio is total combustion (Brooks et al., 1989). It is based on the principle of oxidation of the carbon and nitrogen in the sample to carbon dioxide, water, and nitrogen. The analysis has been carried out with an elemental analyzer (Fisons Instruments, Fisons NA1500 NC) by A. Esler, UNBC. The weight of the samples used was 2-3 mg. 3.2.7 Ash content The ash content of the original sludge and soil samples was determined by combustion at 525 °C (TAPPI standard test method T 211 om-93). Three replicates of each sludge sample and the soil samples were weighed in crucibles and ignited in a muffle furnace until the weight of the ash was constant. C alculation: (5) ash % = (mass of ash [g] / mass of dry sample [g]) x 100% Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 3.2.8 Elemental Analysis of selected inorganic components The inorganic composition of BCTMP sludge and Kraft mill sludge was characterized by using inductively coupled plasma atomic emission spectroscopy (ICP-AES; Leeman, Labs PS1000-UV spectrometer). For the ICP analysis of BCTMP and Kraft mill sludge, oven-dried (105°C) samples of each of the sludges were used. Three replicates of each sludge sample were analyzed for macro- and micronutrients. Sludge is mainly composed of organic matter. The sludge fibers are digested by acid oxidation. Digestion of the sludge samples weighing approximately 0.2 g each was accomplished by microwave acid digestion with 6 ml of HN03 (approximately 68% concentration) and 1.5 mi H20 2 (approximately 37% concentration). This procedure for organic matter digestion was developed at UNBC. The procedure gives a homogeneous solution which is transferred to a 50 ml volumetric flask. The total volume of 50 ml was made up with nanopure water. The samples were stored in Nalgene containers at 4°C. Inductively coupled plasma - atomic emission spectroscopy (ICP-AES) was used for elemental analysis of aluminum, boron, calcium, cadmium, cobalt, chromium, copper, iron, lead, magnesium, manganese, molybdenum, nickel, phosphorus, potassium, sodium, and zinc in the digested sludge samples. ICP-AES is a multi-element analysis technique that will dissociate a sample into its constituent atoms and ions and cause them to emit light at a characteristic wavelength by exciting them to a higher energy level. This is accomplished by the use of an inductively coupled plasma source, usually argon. A monochromator can separate specific wavelengths of interest, and a detector is used to measure the intensity of the emitted light. This information can be used to calculate the concentration of that particular element in the sample. 37 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. As there were no elemental analysis data available for the Kraft mill and BCTMP sludge, the data from NCASI Sludge analysis (NCASI, 2002) was the basis for estimating the concentration ranges for the standard calibration curves. Determination of the concentration of each element in the sludge sample relies on the standard calibration curve. Knowledge of possible concentration ranges of the element in the sludge sample helps to determine appropriate standard concentrations. For each element three different concentrations of calibration standards were made up in 5% nitric acid (H N03). Samples of 5% nitric acid were used as blanks to perform background corrections (appendix G). 3.2.9 Electrical conductivity and salinity The 1:5 soil-to-water extraction method was used to determine electrical conductivity and salinity of the BCTMP sludge, Kraft mill sludge, and soil sample (Kalrad and Maynard, 1994). Fifteen grams of air-dried sludge and soil was transferred to a 250 ml Erlenmeyer flask and 75 ml of de-ionized water added. The stoppered flasks were put on a reciprocating shaker, (Eberbach Corporation, Ann Arbor, Michigan) and the mixtures shaken for 1 hour. The filtrates obtained after vacuum filtration were centrifuged for 5 minutes at 10,000 rpm/16,000 g (centrifuge model: Flermle, Z382K). Electrical conductivity and salinity was determined from the clear, pale yellow decanted filtrates of the sludge samples and the clear, colorless decanted filtrate of the soil samples. The pale yellow color of the sludge filtrates is induced by lignin. The conductivity instrument, YSI Model 3100, was calibrated with 0.01 M KCI solution at 25 °C. The cell constant was set to 1 at a measuring range of 0 - 49.99 mS/cm. For the conductivity measurements the mode temperature compensated was chosen. Conductivity and salinity were determined for three replicates of each sludge sample and the soil sample. 38 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 3.2.10 Effective cation exchange capacity (CECe), exchangeable cations The barium chloride method was used to determine the exchangeable cations and the effective cation exchange capacity for the BCTMP sludge, Kraft mill sludge, and soil samples (Gillman and Sumpter, 1986). The soil sample was analyzed directly, but the 2 sludge samples were milled using a Cyclotec mill and homogenized before analysis to enable representative sampling. The soil sample was extracted at a ratio of 1.5 g to 15 ml extracting solution as per mineral soils. The BCTMP sludge was extracted at 0.6 g to 15 ml as per high organic soils. The Kraft mill sludge sample had to be extracted at 0.6 g to 30 ml extractant due to its very fibrous and absorbent nature (Clive R. Dawson, 2003). The analysis was performed by the British Columbia Ministry of Forests Research Branch Laboratory, Analytical Chemistry Section. Triplicate analysis was conducted (appendix F). 3.2.11 Water holding capacity The water-holding capacity (WHC) of sludge and soil samples can be determined by a “soak and drain” method where water in saturated samples is extracted by gravity. Water can also be extracted from saturated samples over a water potential range of 0 to -1 0 kPa using a pressure plate (Tempe cells) or a tension table apparatus (Carter, 1993). 3.2.11.1 Gravity or European Method To determine the water-holding capacity plastic columns of 7.0 centimeters height with a diameter of 6.9 centimeters were used. One end of the column was covered with 2-3 layers of cheese cloth. The column was filled % with sample and tapped gently to compact the sample. The prepared columns were weighed empty and when filled with sample. The height of the sample was also determined. The column 39 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. enclosing the sample was placed in a vessel containing enough water to saturate the sample. When the sample was saturated (24 hours), the vessel was removed and the sample allowed to drain for 24 hours. The top of the column was covered loosely with parafilm to minimize evaporation and a couple of small holes (needle) permit airflow. When drainage was complete, duplicate samples were removed from the central portion of each column for moisture content determination. These samples were dried in an oven at 105 °C for 24 hours. This moisture content is approximately equal to waterholding capacity (Gomez et al., 1997; Harding et al., 1964). The above described set up was used for three different treatments: a) original sludge and soil samples b) sludge-soil mixtures for the BCTMP and Kraft mill sludge samples c) sludge-soil layer systems for the BCTMP and Kraft mill sludge samples. The number of replicates varied depending on the experiment. The columns were filled with original samples and various sludge-soil mixtures to a height of approximately 4 centimeters. For the sludge-soil layer systems, a total height of 6 cm was maintained for the 1, 2, and 3 layer system. The height of each sludge and soil layer was selected to maintain the same total height within the various sludge-soil layer systems. sludge 3rd layer H H 0 soil H height 2nd layer 1st layer Figure 3: Outline for the sludge-soil layer systems. 40 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. First, the bulk density and the water-holding capacity of the original sludge and soil samples were examined. The original data are used for comparison. The same procedure was applied to various mixtures of sludge and soil (10:40, 20:30, 25:25, 30:20, 40:10). The sludge was mixed with soil in a blender, Proctor Silex, 7 Blend Master, on pulsation. The control sludge samples were treated in the same manner. This procedure was also applied to sludge-soil layer systems, where each sludge and soil layer has a different height, but the total height of the sample in the column stays the same. Calculations: (6) Sample volume: V = (t t / 4 ) x d 2 x h where d is the diameter of the column, 6.9 cm, and h is the height of the entire sample in cm in the column. The sample volume is given in cm3. (3) Bulk density: Db = [g/cm3] Vs where Db is the bulk density in g/cm3, Wd represents the weight of the oven-dried sludge in g and Vs represents the volume of the sludge in cm3 (Brady and Weil, 1999). (7) Gravimetric water-holding capacity at equilibrium (Gomez et al., 1997): _ weight of sample wet - weight of sample dry ^ 9 weight of sample dry 3.2.11.2 Pressure Plate Experiment Through the application of pressure plate extractors the characteristic moisture retention curve can be developed for each soil type. The curves relate the soil suction, at which moisture is held by the soil, to its moisture content. This relationship is important 41 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. in studies of soil moisture movement and of quantity and availability of soil moisture for plant growth (Soilmoisture Equipment Corp., 2001). To determine the moisture retention curves, the sample preparation described under 3.2.11.1 was used. The column was filled with sample to a height of 1 cm. The sample was gently compacted with the bottom of a beaker and the height remeasured. The prepared columns were weighed empty and when filled with sample. The column enclosing the sample was placed directly on the ceramic plate and placed in a vessel containing enough water for 24 hours to saturate sample and ceramic plate. Saturated ceramic plate and sample are placed in the pressure plate extractor and left until equilibrated at the desired pressure. Gravimetric moisture content was determined after drying the sample in an oven at 105 °C for 24 hours. d) 1600G1 5 -B a r P re ssu re P la te E x tra c to r 0776L60 C o n n e c tin g H ose ^y/ C o n n e c tin g H o s e 1500G 1 1 5 -B a r P re ssure P la te E x tra c to r Jj 0 779G 1 C o n n e c tin g H ose 0500FG _ C o m p re s s o r F igure 4: P re s s u re p la te e x tra c to r s e t up (S o ilm o is tu re E q u ip m e n t C o rp ., 2 0 0 1 ). For the moisture retention curves of the original sludge and soil samples, the moisture content of 11 pressure points was determined (0.1 ;0.2;0.3 ;0.4;0.5;0.7;1.0;2.0; 42 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 5.0; 10.0;15.0 bar). For each run, one Kraft mill, BCTMP sludge and soil sample was placed on the pressure plate. A 1 bar ceramic plate was used for pressures up to 1 bar. For the pressures 1.0 and 2.0 bar a 3 bar ceramic plate was used. A 15 bar ceramic plate was used for 5.0, 10.0, and 15 bar pressure. Moisture content was determined from the entire sample when equilibrium was reached. Calculations: (8) Volumetric water-holding capacity at equilibrium (Brady and Weil, 1999): weight of sample wet - weight of sample dry 5-----------------weight of sample dry WHCV= ----- - ------------- (9) ^ xD b x 100% Available water (Brady and Weil, 1999): field capacity water content (0.3 bar) - wilting point water content (15.0 bar) = available water The above described set up was also used for sludge-soil mixtures using BCTMP and Kraft mill sludge samples. The mixtures were prepared as described in 3.2.11.1. For the moisture retention curves of the sludge-soil mixtures the moisture content of 9 pressure points was determined (0.1;0.3;0.5;0.7;1.0;5.0;10.0;15.0 bar). At 0.3 and 15 bar, three replicates of each of the mixtures were measured, and from the average the available water was calculated. Two trials for each mixture were performed at 1.0 bar. Using the same set up as before, the moisture retention curves for sludge-soil layer systems for the BCTMP and Kraft mill sludge samples were determined. The same layer systems as described in 3.2.1.1 were prepared. The pressure points analyzed 43 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. were 0.5, 1.0, and 5.0 bar. When equilibrium was reached each layer was split in half for moisture content determination. 3.2.12 Statistical Analysis Statistical analyses were performed on all data except the semi-quantitative results from the energy dispersive x-ray analysis. Microsoft Excel was used to determine average, standard error, and standard deviation. Error analysis was carried out by using the method of propagation of random errors for the gravimetric and volumetric water holding capacity data. Random or statistical errors are unpredictable errors resulting from limited precision of the measuring instrument and minor uncontrollable variations in the operation of the equipment (Am, Ad, Ah). However, random error is not correctable and the degree of uncertainty in measurements is indicated by derivations of the experimental results. The errors expressed as ± ADb, ± AWHCg and ± AWHCV represent the uncertainty in the quantity of interest in terms of confidence limits. Random error is reduced by good tools and a large sample size. Calculation: (10) For F = axyz (or axy/z or ax/yz or a/xyz), A2( F ) _ A2(x) F2 x2 A2(y ) A2(z) y2 z2 where a,x,y,z are actual values and F represents the uncertainty in the final result (Shoemaker et al., 1996). Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Chapter 4 Results and Discussion The two major aspects for reusing sludge are its chemical and physical characteristics. Sludge samples from BCTMP and Kraft mill processing were compared and their water holding effect on a clay type of soil examined. Analysis was conducted following the methods described in chapter 3. 4.1 Baseline characteristics The BCTMP sludge sample in Figure 5 appeared as soft pellets and clumps of fibers of medium to dark brown color. The sludge pellets contained smaller pieces of white-yellowish wood fibers (0.5-1 cm length). The Kraft mill sludge in Figure 6 appeared in lumps of fibers in a bi'own-beige color and contained fewer but larger pieces of darker brown wood fibers (2-3 cm length). The micrographs in Figure 7 and 8 show the sludge samples on an enlarged scale. The Kraft mill sludge sample appears to be more homogeneous in its fiber structure. The BCTMP sludge sample is composed of a broader variety of fibers and wood pieces. The difference in structure and aggregation of the sludge and soil samples were visually inspected. The soil sample had a finer texture than the sludge samples. The Kraft mill sludge sample has the coarsest texture. This is reflected in the bulk density and porosity results (Table 8). Both sludge samples have a lower bulk density than the soil. Bulk density indicates how easily a soil will till, how easily water will infiltrate, how it will hold water, and its suitability for growing plants. There is more pore space available to be filled with water in the sludge samples than in the soil. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. FIGURE 5: BCTMP sludge (1:1) FIGURE 6: Kraft mill sludge (1:1) Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. F IG U R E 7: SEM micrograph of BCTM P sludge (15x). F IG U R E 8: SEM micrograph of Kraft mill sludge (15x). 47 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. When preparing the sludge soil mixtures, the original sludge and soil structure was changed by using a blender. The sludge and soil particles were separated into more individual aggregates. The arrangement of aggregates gives the soil its structure. However; soil particles filled the void space in the sludge samples. This is partially due to the original sludge moisture content and the blending. After soaking and draining the soil sludge layer samples, it was observed that the soil particles on the interface filled the void pore space of the sludge. This change in aggregates increased the degree of stability. When the sludge soil layer samples were taken out of the plastic columns, they resisted sliding and crumbled less than the original soil sample. Increasing stability of the topsoil layer is especially desirable at the site slopes. 4.2 Chemical characterization 4.2.1 General properties A variety of properties are used to characterize sludge, including pH, moisture content, ash content, C:N ratio, cation exchange capacity, electrical conductivity, and salinity. The results are summarized in Table 6 and compared to previous studies. Table 6: Properties of B C TM P and Kraft mill sludge compared with previous data. component n unit BCTMP Kraft mill literature pH 2 - 6.95 8.25 6.43 a moisture content 8 % 164 ± 1.78 165 ±3.41 121 - 409 b ash content 3 % 4.40 ±0.15 4.40 ± 0.23 10 - 62 b C:N 4 - 52:1 43:0 100:1; 300:1 c C EC 3 cmol+/kg 35.25 ±0.12 19.70 ±0.04 NAd electrical conductivity 3 pS/cm 1466 241 1120 a salinity 3 ppt 0.8 0.1 NAd aThe data were indirectly calculated based on a 3:1 primary to secondary sludge ratio (Clear Lake Ltd., 1993). bNCASI, 2002; cNCASI, 2000; dNA = not available 48 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. With a pH of 6.95 the BCTMP sludge is neutral. The Kraft mill sludge with a pH of 8.25 is basic. The calculated literature value is slightly acidic with a pH of 6.43 (Clear Lake Ltd., 1993). The moisture content represents the average of 8 samples, oven-dried at 55°C, 80°C, and 105° C for 24 h until constant weight (± 0.2 g). The BCTMP sludge sample at 80° C represents the average of 6 samples. Raw data, standard deviation and standard error are presented in Table (21-23) for Kraft mill and Table (24-26) for BCTMP sludge (appendix B). The difference in moisture content determination at three different temperatures for both sludge samples was small, which indicates the low presence of volatile compounds. The larger standard errors for the Kraft mill sludge sample (± 3.41 at 105° C) compared to the BCTMP sludge sample (± 1.78 at 105° C) indicates a broader variance around the average. This is a result of a less homogeneous sample. The moisture content of both samples is alike and falls into the lower range of the literature value. The ash content for both sludge samples is 4.40% and represents the average of three samples. The standard error for the BCTMP sludge is ± 0.15%, and ± 0.23% for the Kraft mill sludge (Table (28), appendix D). Compared to the soil with 95.5% ash content the sludge samples are high in organic matter expressed in the low percentage of ash content. The reference range of the ash content is 10 to 62%. The sludge samples are under the minimum value, which means, they are higher in organic matter. Raw data are presented in Table (28), appendix D. The C:N ratio for BCTMP sludge is 52:1 by mass. For Kraft mill sludge it is 43:0.1 by mass. Raw data are presented in Table (27), appendix C. The actual nitrogen content in the BCTMP sludge could enhance vegetation growth on the final cover layer of a landfill. However, because of the very small amounts of nitrogen present in the sludge, 49 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. the soil-type of sludge mixture is important at as well as additional fertilization possibilities to promote plant growth in landfill cover amended with sludge. The cation exchange capacity for BCTMP sludge is 35.35 cmol+/kg and 19.70 cmol+/kg for Kraft mill sludge (Table 6). There is almost double the amount of exchangeable cations available in BCTMP sludge. In the soil sample the CEC is 15.25 cmol+/kg. Raw data are presented in Table (31), appendix F. Normal CEC ranges in soils would be from < 3 cmol+/kg to > 25 cmol+/kg (Ross, 2003). Cations retained electrostatically are easily exchangeable with other cations in the sludge/soil solution and are thus easily available for plant uptake. The CEC is pH dependent. Addition of sludge material will likely increase the soil’s CEC. The electrical conductivity of BCTMP sludge (1466 pS/cm) is 31% higher than the literature value with 1120 pS/cm (Table 6). The conductivity of the Kraft mill sludge is 78% lower than the literature value. The electrical conductivity is a measurement of a solution’s ability to conduct electric current. As the ability of a solution to conduct electric current depends upon ions, there are more ions in the BCTMP than in the Kraft mill solution. Conductivity is also an indirect measurement of salt content. The measured salinity of BCTMP is 0.8 ppt and of Kraft mill sludge 0.1 ppt. These results are consistent with the conductivity measurements. 4.2.2 Elemental analysis The main elements found in both sludge samples by energy dispersive x-ray analysis (Table 29 and 30, appendix E) are carbon and oxygen as they are the skeleton of the cellulose fibers. The carbon to oxygen ratio of Kraft mill sludge is 2.65:1, and 1.53:1 for the BCTMP sludge. The section of the BCTMP sludge analyzed under the microscope showed that it contains sodium, silicon, sulfur, potassium, and calcium. The section of the Kraft mill sludge analyzed under the microscope showed that it contains 50 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. neither sulfur nor potassium. Kraft mill sludge contains double the amount of sodium than BCTMP sludge. BCTMP sludge contains approximately four times more calcium than Kraft mill sludge. These results are semi-quantitative and represent only a section of the sludge sample on the peg. In both sludge samples, the levels of macro- and micronutrients were established. In each sludge sample, 17 elements were quantitatively determined after closed vessel microwave acid digestion by ICP-AES. These elements include the macronutrients K, Ca, Mg, and P. The other macronutrients S and N were not determined by ICP-AES. All of the micronutrients were determined except chloride. Results are summarized in Table 7 (Table 32, appendix G). The resulting concentrations for all elements are in the lower range of the concentrations determined by NCASI (NACSI, 2000). These results support the findings from NCASI that pulp and paper mill sludge is in general low in potential environmental contaminants. Both types of sludge can provide the nutrients for plant growth. The Kraft mill sludge has lower concentrations of B, K, Mg, Mo, and P than required for plant growth (Barak, 1999). The concentrations for Ca, Co, Fe, Mn, Ni, and Zn are higher than the typical requirements for plant growth. BCTMP sludge differs from Kraft mill sludge. The concentrations of B, K, Na, Ni, P, and Pb are higher in BCTMP sludge while concentrations of Cu, Mg, and Mn are lower in BCTMP sludge (Table 7). Micronutrients are as important for plant growth as macronutrients but in lower concentrations. Whether a macronutrient or micronutrient, the most growth-limiting nutrient will limit growth, no matter how favorable the nutrient supply of other elements is. All essential elements are absorbed by the plants from soil solutions, as either cations or anions, thus soil pH is an important factor to determine, as the ionic charge of the elements depends on the surrounding pH. 51 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Table 7: Summary of results for the elemental analysis in oven-dried (105°C ) Kraft mill and B C TM P sludge samples determined by IC P-A ES and literature data. Element Symbol Kraft Mill [mg/kg] BCTMP [mg/kg] NCASI1 [mg/kg] Nutrients 2 [mg/kg] n/a 20 5,000 Aluminum Al 702 295 590 - 59,000 Boron Calcium Cadmium Cobalt 0.672 5931 0.088 0.582 4.97 62.0 7936 0.232 1.491 13.52 <1 -4 9 1 2 8 0 -2 1 0 ,0 0 0 <0.09 - 56 0 -9 .7 Chromium B Ca Cd Co Cr 3 .0 - 2 ,2 5 0 n/a n/a Copper Co 7.87 Iron Fe K 14.51 587 3 .9 - 1 ,5 9 0 97.1 - 10,800 6 100 1 2 0 - 10,000 Potassium Magnesium 72.8 1795 478 2 0 0 - 19,000 10,000 2,000 28.6 *BDL 1 3 - 2 ,2 0 0 < 2 .5 - 1 4 .0 0.1 162 904 1.819 8.088 300 - 66,700 1 .3 - 1 3 3 0.1 932 *BDL 28.4 1 0 - 2 5 ,4 0 0 <0.05 - 880 1 3 - 3 ,7 8 0 2,000 n/a 20 Mg Mn Mo 89.0 *BDL Nickel Na Ni Phosphorus Lead Zinc Pb Zn 41.2 4.09 30.5 Manganese Molybdenum Sodium P 312 277 n/a 50 n/a 1 NCASI 54 Mill survey (NACSI, 2000) 2 Typical concentrations sufficient for plant growth (Barak, 1999) * B elow de te ctio n lim it n/a = not a p p lica b le The limiting growth factor of sludge is the low level of nitrogen. The nitrogen concentrations in pulp mill sludge are ranging from 1.1 g/kg to 59 g/kg (NCASI, 2000). Extensive research has been conducted in the past to overcome this disadvantage of the sludge amendment. Compounds rich in organic nitrogen like manure, compost, and biosolids were mixed with sludge and applied to agricultural land. Some of these studies are mentioned in chapter II. Most landfills use compost produced onsite as fertilizer for vegetation growth. The growth and appearance of plants varies considerably from one species to another and even within species, depending on the environment. Alfalfa utilizes 272 kg of nitrogen and yields 25.4 t/ha. Clover-grass utilizes only 136 kg of nitrogen and yields 15.3 t/ha (Tisdale et al., 1985). In accordance with the vegetation 52 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. applicable to landfill restoration plans and site climate, nitrogen sources need to be added in quantities that will meet the requirements of the plants. 4.3 Physical characterization 4.3.1 Bulk density and porosity BCTMP sludge has a higher bulk density with 0.094 Mg/m3 than Kraft mill sludge with 0.054 Mg/m3. The different aggregation of the two sludge samples causes different results in porosity. Kraft mill sludge has a coarser texture than BCTMP sludge. This results in lower bulk density and higher porosity. The clay type soil has the highest bulk density with 0.827 Mg/m3 and the lowest porosity. Data are summarized in Table 8. Table 8: Bulk density and porosity of BCTMP and Kraft mill sludge. Assumption: Dp = 1.51 Mg/m3; particle density for organic soil (McGill, 2002). sample Bulk density [Mg/m3] Porosity Kraft mill 0.054 0.964 BCTMP 0.094 0.937 Soil 0.827 0.452 These results support the observations under 4.1. 4.3.2 Water holding capacity by gravity Data obtained from the bulk density and water holding capacity determination for Kraft mill and BCTMP sludge and soil are listed in appendix H. In Table 9, the average of the moisture content determination (=WHCg) of the duplicates of all dried samples is summarized. The Kraft mill and BCTMP sludge samples have a bulk density approximately one order of magnitude lower than the clay type soil sample. The bulk density determined for the blended sludge samples is lower than for the original samples. 53 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Table 9: Bulk density and gravimetric w ater holding capacity obtained from original and blended Kraft mill and BCTMP sludge and soil sample. sample Kraft mill, blend BCTM P, blend Kraft mill BCTM P Soil bulk density [g/cm3] (n=5) ± se 0.033 0.063 0.054 0.095 0.827 0.006 0.002 0.001 0.002 0.005 WHCg ± se [%] 710 520 509 (n=5) 393 32 9.64 4.10 6.68 6.90 0.61 The gravimetric water holding capacity is lowest for the soil sample and highest for the blended Kraft mill sludge sample. The BCTMP sludge sample has approximately 12 times and the Kraft mill sludge sample approximately 16 times more water holding capacity than the soil sample. The data obtained in this part of the experiment demonstrate that different structures and pore size distributions result in very different water holding capacity. In Table 10 and 11 the bulk density and moisture content on a weight basis (=WHCg) average of dried samples of various sludge-soil mixtures is summarized. Data obtained from the bulk density and water holding capacity determination for Kraft mill and BCTMP sludge-soil mixtures are listed in appendix H. The original sludge sample was mixed with 10, 20, 25, 30, and 40 mass percent of soil using a blender (Table 10 and 11). The original sludge was blended and used as reference. For both sludge samples, the bulk density increased with higher percentage of soil in the sludge-soil mixtures. The water holding capacity decreased with higher amounts of soil in the mixture. The BCTMP sludge-soil mixture 10:40 has the highest bulk density and the lowest water holding capacity. By comparing the sludge-soil mixtures the 25:25 mixture doubles in water holding capacity compared to the 10:40 mixtures. Comparing the sludge-soil mixtures with the lowest amount of sludge added (10:40) and the water Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. holding capacity of the clay type soil, the water holding capacity doubles with Kraft mill sludge and increases by two thirds with BCTMP sludge. Table 10: Bulk density and gravimetric water holding capacity obtained from various Kraft Mill sludge-soil mixtures. sample Kraft mill/soil 10:40 Kraft mill/soil 20:30 Kraft mill/soil 25:25 Kraft mill/soil 30:20 Kraft mill/soil 40:10 Kraft mill blend bulk density ± se WHCg ± se [g/cm3] (n=3) [%] (n=6) 0.343 0.157 0.145 0.098 0.055 0.033 0.005 0.015 0.006 0.004 0.001 0.001 65 139 145 251 447 710 4.74 11.95 11.73 17.31 19.44 9.64 Table 11: Bulk density and gravimetric water holding capacity obtained from various BC TM P sludge-soil mixtures sample BCTMP/soil 10:40 BCTMP/soil 20:30 BCTMP/soil 25:25 BCTMP/soil 30:20 BCTMP/soil 40:10 B C TM P blend bulk density ± se WHCg ± se [g/cm3] (n=3) [%] (n=6) 0.499 0.311 0.256 0.181 0.117 0.063 0.008 0.016 0.011 0.006 0.003 0.002 52 87 107 178 294 521 1.19 5.48 3.67 6.03 7.77 4.10 Data obtained in this part of the experiment demonstrate the effect of the sludge amendment. Adding higher amounts of sludge results in decreasing bulk densities and increasing water holding capacities. The same effects were found when sludge at different rates was amended to gravelly loam soil in a field study (Chow et al., 2003). In this study, results on water-stable aggregates revealed that the organic matter in the pulp fib er com bined s m a lle r a g g re g a te s to form la rg e r a g g re g a te s , resulting in a la rg er proportion of macropores as compared to micropores. The original sludge samples (Table 8) have a higher bulk density and a lower water holding capacity compared to the blended samples. Blending the sludge affects the fiber structure, resulting in different bulk density and water holding capacity. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Another alternative to examining sludge-soil mixtures was to look at packing sludge and soil in layers (Figure 4). By keeping the total height of the sample the same, the height of each sludge and soil layer varied between the 1, 2 and 3 layer systems. In Table 12 and 13, the average of the gravimetric moisture content determination (=WHCg) of dried samples of sludge-soil layer systems are summarized. Data obtained from the bulk density and water holding capacity determination for Kraft mill and BCTMP sludge-soil layer systems are listed in appendix H. The water holding capacity of the bottom layer of sludge increased for the 2 and 3 layer system compared to the 1 layer system. For the 1 layer system, the water holding capacity for the sludge is approximately 10 times higher than in the soil. The same effect can be observed for the soil layer in the 2 and 3 layer systems. This is consistent with reduced water transmission being induced by surrounding sludge layers. The water holding capacity of the soil layer stays between 36 and 39% in all three systems. Table 12: Bulk density and gravimetric water holding capacity of 1, 2, and 3 layer systems of Kraft mill sludge. Bulk density ± se WHCg ± se [g/cm3] (n=3) [%] (n=6) Sludge 1 Soil 1 weighted average 0.084 0.916 0.014 0.016 332 39 42.0 0.60 Sludge 1 Soil 1 Sludge 2 Soil 2 weighted average 0.061 0.840 0.073 0.941 Sludge 1 Soil 1 Sludge 2 Soil 2 Sludge 3 Soil 3 weighted average 0.077 0.677 0.114 0.810 0.095 1.019 sample Kraft mill 1 layer Kraft mill 2 layer Kraft mill 3 layer 185 0.002 0.050 0.004 0.059 487 38 494 39 16.5 0.59 11.4 0.23 264 0.006 0.009 0.012 0.024 0.003 0.099 486 36 380 38 431 38 8.60 0.65 15.9 0.67 26.9 0.36 235 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Table 13: Bulk density and gravimetric w ater holding capacity of 1, 2, and 3 layer systems of BCTMP sludge. Bulk density ± se WHCg ± se [g/cm3] (n=3) [%] (n=6) Sludge 1 Soil 1 weighted average 0.094 0.897 0.001 0.011 378 40 3.69 0.46 Sludge 1 Soil 1 Sludge 2 Soil 2 weighted average 0.097 0.681 0.126 0.795 Sludge 1 Soil 1 Sludge 2 Soil 2 Sludge 3 Soil 3 weighted average 0.121 0.850 0.121 0.790 0.134 0.742 sample B CTM P 1 layer B CTM P 2 layer BCTM P 3 layer 209 0.006 0.009 0.005 0.010 476 41 434 40 44.9 0.53 14.6 0.55 248 0.001 0.034 0.013 0.009 0.009 0.007 394 42 356 42 424 41 7.23 0.62 13.2 0.51 17.6 0.63 217 Comparing the total water holding capacity calculated by weighted average, the 2 layer system has the highest water holding capacity with 264 % for Kraft mill sludge and 248 % for BCTMP sludge. The 3 layer system has a total water holding capacity of 235 % for Kraft mill sludge and 217 % for CTMP sludge, and the 1 layer system is lowest with 185 % for Kraft mill sludge and 209 % for BCTMP sludge. Adding a third layer of sludge and soil resulted in a lower total water holding capacity than in the 2 layer system. This could be due to each layer decreasing in layer thickness to maintain the same total height. The increase in water holding capacity in the sludge layer in all three layer systems refers to the sludges capability to retain water. In the three layer system the second sludge layer has a lower water holding capacity than the first and third layer. This second sludge layer is enclosed by soil layers. The soil particles filled some of the voids in the sludge reducing water holding capacity of the sludge. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. The water holding capacity in the layer systems is similar to the 30:20 sludge-soil mixtures and lower than the original sludge samples. The slightly higher bulk density in the second sludge layer of the 2 and 3 layer system are due to soil particle attached to the sludge fibers. 4.3.3 Pressure plate experiment When equilibrium was reached water holding capacity or moisture content was determined for the sludge and soil samples at different pressures. Data obtained for bulk density, moisture content and error analysis are listed in appendix I. The water holding capacity is expressed on a volume basis using equation (8). For 11 samples of BCTMP sludge and for 11 samples of Kraft mill sludge the average bulk density is 0.14 g/cm3. The average bulk density for 10 samples of soil is 1.37 g/cm3. Compared to the original samples (Table 8) bulk densities determined in the pressure plate experiment are higher. A summary of the volumetric moisture content data with random errors is presented in Table 14. BCTMP sludge can hold the highest amount of water. It includes the available, unavailable, and gravitational water. The soil holds the lowest amount of water. The observed water holding capacity is similar to the general literature value of 52% for clay loams (Klocke, 1996). At field capacity, BCTMP sludge has moisture retention of 53.7%, Kraft mill sludge has 36.7%, and soil has 39.2%. The water held between field capacity and wilting point available water is most important for vegetation. Plants can use approximately 50 percent of the available water without stress, as the water is retained by capillary forces. The total amount of available water in BCTMP sludge is 4 times higher than in soil and Kraft mill sludge is 7 times lower than in soil. This water storage Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. capacity of BCTMP sludge can be used beneficially to increase the water holding capacity in soils. The moisture retention curves obtained for the sludge and soil samples are shown in Figure 9 and 10. Table 14: Volumetric moisture retention curve data with random errors for B C TM P sludge, Kraft mill sludge, and soil (n=1). pressure Field capacity BCTMP 0.1 49.6 0.2 52.8 0.3 0.4 53.7 0.5 0.7 1 2 Wilting point Available water moisture % vol. [barl x (-1) 49.5 46.1 45.5 45.4 5 10 46.5 48.9 40.2 15 37.2 16.5 ± A WHCV Kraft mill ± A WHCV 1.01 1.08 1.10 1.01 0.94 0.93 0.93 0.95 1.00 0.82 0.76 58.8 42.3 36.7 38.5 33.5 33.4 32.1 30.4 38.1 35.6 36.1 0.6 1.20 0.86 0.75 0.79 0.68 0.68 0.66 0.62 0.78 0.73 0.74 Soil ± 4 WHCV 52.2 1.07 0.92 0.80 0.92 0.65 0.72 0.78 0.74 0.82 0.72 0.71 45.1 39.2 4 4.9 31.8 35.3 38.0 36.3 40.3 35.0 34.7 4.5 The pressure plate experiment was used to determine moisture retention curves for soil samples. The soil is different in structure from the two sludge samples. The sludge samples are less homogeneous and a broader variety of pore sizes is involved. The various pores are distributed unevenly. This affects the sample preparation and is expressed in the random errors. As the experimental process to obtain a data set for one pressure takes 4 days, no replicates have been conducted. The above information is used for comparison with sludge-soil mixtures and sludge-soil layer systems. 59 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. BCTMP Kraft mill Soil pressure [bar] x (-1) Figure 9: Moisture retention curves for BCTM P sludge, Kraft mill sludge and soil from 0.1 to 15 bar x (-1) with random errors. BCTMP Kraft mill Soil 0.5 2.5 pressure [bar] x (-1) Figure 10: Moisture retention curves for BC TM P sludge, Kraft mill sludge and soil from 0.1 to 2.5 b a rx (-1) with random errors. 60 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Examination of the moisture retention curves of the sludge-soil mixtures support the findings from several field experiments, that organic matter increases the water retention in soil (Foley and Cooperband, 2002). BCTMP sludge-soil mixture 25:25 and Kraft mill sludge-soil mixture 30:20 have the highest volumetric moisture retention at -0.1 bar. The sludge-soil mixture 20:30 for BCTMP sludge, and the original Kraft mill sludge have the lowest volumetric moisture retention at -0.1 bar (Figures 11 to 14). Compared to the soil sample at field capacity (39%) and permanent wilting point (35%) Kraft mill sludge-soil mixtures increased volumetric moisture retention more than BCTMP sludge-soil mixtures. Wei et al. (1985) showed that biosolids additions increased water retention at low tensions in a silty clay loam soil, suggesting an increase in larger pores. Recently, Zibilske et al. (2000) showed that multiple applications of paper mill residuals significantly increased soil moisture holding capacity. Municipal solid waste compost addition to sandy soil increased water retention, but did not change plant available water (Turner et al., 1994). Volumetric moisture content and random errors are summarized in Table 15 for BCTMP sludge-soil mixtures and in Table 16 for Kraft mill sludge-soil mixtures. Data for bulk density, moisture content, and error analysis are provided in appendix I. Bulk density of soil decreases with increasing amounts of sludge added. Overall the BCTMP and Kraft mill sludge-soil mixture bulk densities are similar (Tables 54 to 67, appendix I). Both sludge samples have through all sludge-soil mixtures an outlier at 0.5 or 0.7 bar. The original sludge and soil samples show an outlier at 0.4 bar (Figure 9 and 10). This is not referring to a change of pressure plates as the experiment was conducted with a 1 bar ceramic plate up to and including 1 bar. At this point data collected are not sufficient to provide an explanation for the outliers. Further experiments with smaller pressure increments are necessary to explain the outliers. 61 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. — • — original — □— blend X 40:10 — A — 30:20 •--X--- 25:25 — •-- 2 0 :3 0 XX g . .. ... Q- 0.0 10.0 4.0 2.0 12.0 14.0 16.0 pressure [bar] x (-1) F IG U R E 11: Moisture retention curves for BCTM P sludge-soil mixtures from 0.1 to 15 bar x (-1). original blend A 30.20 X 25:25 •-- 2 0 :3 0 .60 H 10:40 £50 ♦ 0.0 0.5 2.0 2.5 pressure [bar] x (-1) F IG U R E 12: Moisture retention curves for BCTM P sludge-soil mixtures from 0.1 to 2.5 bar x (-1). (Enlarged graphs with error bars see appendix I, Figure 27 - 30) Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. — 4 — original — □— blend — X — 40:10 A 30:20 X 25:25 -• --2 0 :3 0 H 0.0 4.0 2.0 6.0 10.0 10:40 14.0 12.0 16.0 pressure [bar] x (-1) F IG U R E 13: Moisture retention curves for Kraft mill sludge-soil mixtures from 0.1 to 15 b a rx (-1). ♦ — original □ — blend X — 40:10 X 25:25 • -- 2 0 :3 0 B 0.0 0.5 2.0 10:40 2.5 pressure [bar] x (-1) F IG U R E 14: Moisture retention curves for Kraft mill sludge-soil mixtures from 0.1 to 2.5 b a rx (-1). (Enlarged graphs with error bars see appendix I, Figure 19 - 22) 63 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Moisture-retention-curves for BCTMP sludge-soil-mixtures Table 15: Volumetric moisture retention curve data with random errors for B C TM P sludge-soil mixtures. pressure [bar] FC 0.1 0.3 0.5 0.7 1.0 2.0 PW P 5.0 10.0 15.0 moisture % vol. original ± A WHCV blend ± A WHCV 40:10 ± A WHCV 30:20 ± A WHCV 25:25 + A WHCV 20:30 ± A WHCV 10:40 ± A WHCy 37 0.94 0.86 0.78 0.82 0.79 0.78 0.74 0.75 0.75 5; 0.80 46 42 38 40 39 38 38 37 44 45 43 1.11 0.96 0.91 0.89 0.89 0.92 0.89 0.92 0.88 4 0.93 55 47 45 44 44 45 48 46 44 48 1.18 1.10 0.96 0.99 0.99 0.92 1.05 1.04 0.98 6 1.02 58 54 47 49 49 45 51 51 64 47 43 0.99 0.93 0.90 0.94 0.90 0.88 0.91 0.91 0.88 35 37 1.31 0.97 0.73 0.73 0.75 0.74 0.72 0.71 0.74 3 0.92 10 0.82 46 45 43 45 45 36 36 37 36 35 36 0.81 0.88 0.69 0.69 0.71 0.71 0.77 0.80 0.74 43 43 42 41 41 1.10 0.99 0.90 0.84 0.87 0.88 0.85 0.83 0.85 7 0.75 8 0.90 40 43 34 34 35 35 38 39 54 49 44 41 FC = Field Capacity; PW P = Permanent Wilting Point; A W = Available W ater 64 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Moisture-retention-curves for Kraft mill sludge-soil-mixtures Table 16: Volumetric moisture retention curve data with random errors for Kraft mill sludge-soil mixtures. pressure [bar] FC PW P moisture % vol. original ± A WHCV blend ± A WHCV 40:10 0.1 50 0.3 0.5 0.7 1.0 2.0 39 36 38 33 32 5.0 10.0 36 34 15.0 32 1.02 0.80 0.73 0.77 0.68 0.66 0.73 0.70 0.66 7 0.75 38 1.28 0.94 0.86 1.02 0.90 0.78 0.80 0.92 0.78 I 11 0.92 63 46 42 50 44 38 39 45 ± A WHCV 30:20 ± A WHCV 25:25 ± A WHCV 20:30 ± A WHCv 10:40 ± A WHCv 34 1.17 0.89 0.80 0.89 0.81 0.73 0.81 0.69 0.69 9 0.83 57 43 39 44 40 36 40 34 37 1.38 0.98 0.89 1.01 0.88 0.77 0.75 0.71 0.76 h i I 0.90 68 48 44 49 43 38 37 35 36 1.26 0.95 0.92 0.75 0.83 0.74 0.77 0.75 0.74 11 0.86 62 47 45 37 41 36 38 37 33 35 31 1.13 0.90 0.82 0.73 0.80 0.65 0.67 0.71 0.63 13 0.78 55 44 40 36 39 32 57 47 40 39 38 36 34 33 36 11 1.16 0.97 0.81 0.97 0.78 0.73 0.70 0.67 0.73 0.81 FC = Field Capacity; PW P = Perm anent Wilting Point; A W = Available W ater 65 Bulk density decrease with addition of organic matter was reported in other studies (Chow et al., 2003; Foley and Cooperband, 2002; Nemati, 2000). With increasing organic matter, the bulk densities decreased and the porosity increased, thus the water retention at field capacity was greater. At the wilting point, the water retained is slightly lower, but exhibit similar trend. Foley and Cooperband (2002) reported a similar relationship between bulk density and water retention in soil from field experiments. The increase in water held at 0.3 bar is related to increased soil porosity, which allows the soil to hold more water. However, the increase in small pores improved the soil’s ability to retain water at 15 bar (Foley and Cooperband, 2002). Plant available water slightly increased for BCTMP sludge-soil mixtures 25:25, 20:30, and 40:10 compared to the original sludge sample (Table 15). Plant available water increased for all Kraft mill sludge-soil mixtures compared to the original sludge sample (Table 16). Evidence of greater pore-size distribution and a shift toward smaller pores is given by experimental findings from Bauer and Black (1992), suggesting that greater moisture retention at field capacity might be offset by greater moisture retention at the wilting point. These findings would support the plant available water results determined in the laboratory. Table 17: Volumetric moisture content in % and bulk density in g/cm3 of BCTM P sludge-soil mixtures. 0.3 [bar] = FC 15.0 [bar] = PW P BCTM P moisture % vol. Db [g/cm3] moisture % vol. D b [g/cm3] original 42 0.16 37 0.15 blend 47 0.18 43 0.18 40:10 54 0.33 48 0.33 30:20 46 0.42 43 0.45 25:25 47 0.55 37 0.48 20:30 43 0.57 36 0.58 10:40 49 0.95 41 0.97 66 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Table 18: Volumetric moisture content in % and bulk density in g/cm3 of Kraft mill sludge-soil mixtures. 0.3 [bar] = FC 15.0 [bar] = PW P Kraft moisture % vol. D b [g/cm3] moisture % vol. D b [g/cm3] original 39 0.13 32 0.14 blend 46 0.17 38 0.16 40:10 43 0.26 34 0.26 30:20 48 0.41 37 0.42 25:25 47 0.52 36 0.50 20:30 44 0.58 31 0.58 10:40 47 0.92 36 0.93 In this part of the experiment, the moisture content at 0.1 bar is an average of two replicates, and 0.3 and 15 bar are averages of three replicates. The available water is slightly higher for Kraft mill sludge and sludge-soil mixtures than for BCTMP sludge and sludge-soil mixtures. For Kraft mill sludge plant available water is highest (13%) with a sludge-soil mixture of 20:30. For BCTMP sludge it is highest (9%) with a 25:25 sludgesoil mixture. The volumetric moisture content of the original sludge and soil samples measured first (Table 14) are slightly higher for both sludge samples than when measured with the sludge-soil mixtures (Table 15 and 16). BCTMP and Kraft mill sludge are similar in their overall ability to hold water. Nevertheless, BCTMP sludge has higher moisture content at field capacity for most sludge-soil mixtures except the mixtures 30:20 and 20:30. Volumetric moisture content decreases most over the entire pressure range compared to Kraft mill sludge. Preparing the samples in the column is the most crucial part of the experiment due to the different textures of the samples. This is probably reflected in the different results of the two trials. 67 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. The pressure plate experiment was also applied to sludge-soil layer systems. The samples were prepared following the description in 3.2.11.1 (Figure 3). As the overall height of the sample for the layer treatment was 6 cm instead of 1 cm used for original samples and sludge-soil mixtures. As the time required to reach equilibrium varies according to the square of the sample height, the layer systems never reached equilibrium. Gravimetric moisture content was determined after 14 days for 0.5, 1.0, and 5.0 bar. Results for the moisture content are summarized in Table 19 for BCTMP sludgesoil layer systems and in Table 20 for Kraft mill sludge-soil layer systems. Data for bulk density, moisture content, and error analysis are provided in appendix I (Table 82 to 85). Layers of BCTMP sludge or layers of Kraft mill sludge have higher volumetric moisture content than the soil layer. In the layer systems, the BCTMP sludge layer has double the water holding capacity of soil. The Kraft mill sludge layer has a slightly higher or same water holding capacity compared to the soil layer. In the layer systems BCTMP sludge layer has more water holding capacity than Kraft mill sludge. Increasing the amount of layers is not affecting the overall moisture content. For both sludge samples volumetric moisture content remains similar throughout the sludge-soil layer systems. The soil layer surrounded by sludge layers in the 2 and 3 layer systems has similar moisture content as the first layer. This leads to the conclusion that water transmission was induced by surrounding sludge and soil layers. There is less change in moisture content of the soil layers than in the sludge layers. As the equilibrium moisture content was not determined the data represent only a trend. T h e volum etric m oisture c on ten t in the BCTMP slu dg e-so il la y e r s y s te m s is h ig h er in the sludge layers at -0.5 bar compared to various sludge-soil mixtures and the original sludge samples. It is higher in the BCTMP sludge-soil layer systems than in the Kraft mill sludge-soil layer systems. 68 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Table 19: Total volumetric moisture content of 1, 2, and 3 BCTM P sludge-soil layer systems at 0.5, 1.0, and 5.0 bar pressure. pressure 0.5 WHCV bar total WHCV [%] 48 [%] sludge soil 30 39.2 BCTM P sludge 1 sludge 2 51 47 48 46 2 layers soil 1 25 24 BCTM P 1 layer BCTM P 3 layers 1.0 bar WHCV total WHCV [%] 51 24 [%] 37.5 5.0 bar WHCV total WHCV [%] 46 [%] 29 37.2 46 51 24 soil 2 33 sludge 1 42 53 sludge 2 39 43 36 sludge 3 soil 1 soil 2 soil 3 38 30 36 40 29 33 40 26 32 38.9 36.2 24 25 35.5 29 37.4 40 37.3 33 28 34.0 Table 20: Total volumetric moisture content of 1, 2, and 3 Kraft mill sludge-soil layer systems at 0.5, 1.0, and 5.0 bar pressure. pressure Kraft mill 1 layer Kraft mill 2 layers Kraft mill 3 layers 0.5 bar WHCV total WHCV [%] 35 [%] sludge soil 28 31.8 sludge 1 38 34 1.0 WHCv bar total WHCV 5.0 WHCv bar total WHCV [%] 27 [%] [%] 30 28.4 [%] 26 28 35 31 23 sludge 2 soil 1 soil 2 21 sludge 1 sludge 2 sludge 3 35 36 25 33 28 38 29 28 24 soil 1 soil 2 soil 3 27 27 30 26 31 27 25 24 28 30.3 30.1 29 26.7 31 26 24 29.4 30.6 29 26 26.8 26.0 Water holding capacity determined by two different methods (i.e., soak and drain method and pressure plate experiment) show the same trends for all 3 sludge-soil treatments. The plain sludge samples have properties such as much lower bulk density and higher porosity than the soil sample. This results in higher water holding capacity in 69 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. the sludge samples. For the sludge-soil mixtures either method showed, that with increasing organic matter, bulk density decreased and moisture retention increased. The experimental set-up of the pressure plate equipment has its limitations in the sample height. To analyze sludge-soil layer systems using the soak and drain method allows keeping the sample height the same throughout the entire experiment. Water holding capacity results can be compared. The pressure plate experiment is difficult and requires runs of more than one week duration with samples greater than 1 cm in height. The soak and drain method is less time consuming and replicates can be added more easily. More specific information, such as percent of plant available water, can be determined with the pressure plate experiment. The most crucial part of the experiment is the packing of the columns. Soil and sludge are very different in structure. Soil being composed of smaller and more uniform particles than sludge can be packed in the column evenly. Sludge being composed of different types of fibers is more difficult to pack without defined compaction. This is reflected in the error analysis for bulk density determination. The topsoil or vegetative layer is part of a landfill capping system. The main purpose of this system is to prevent infiltration and build the basis for environmental restoration of the landfill area. The vegetative layer is exposed to heavy rainfalls, desiccation, and freeze/thaw cycles. These events can cause severe damage to the cover. The top layer is most vulnerable during germination and seedling growth time. Sludge amended to soil could improve the performance of the topsoil layer. The experimental findings show, that organic matter decreases bulk density and increases porosity. The sludge amendment changes the soil structure by increasing the amount of macropores, resulting in higher water retention capacity (Foley and Cooperband, 2002). The changes in pore-size distribution increase the soil stability and resistance to environmental impacts, especially heavy rainfalls (Nemati, 2000). Erosion and soil loss problems caused by heavy rainfalls and stormwater runoff could be reduced as the 70 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. sludge amended soil increases the water storage. Under simulated rainfall the beneficial effects of a 4% organic matter treatment with a gravelly loam soil include 2.1 times delay in runoff initiation, and 23 and 71% reduction in runoff and soil loss (Chow et al., 2003). The most concentrated location of erosive forces on landfills occurs in the structures that convey water from the top of the cap to the base of the side slopes (Cabalka, 1996). Desiccation cracking and deterioration due to freeze/thaw cycles could also be minimized by the change in the aggregation of the soil. Sludge could replace the hydraulic mulch typically applied that offers a short-term (four- to eight-week) service life to assist germination and seedling growth. Despite the advantages of the physical properties of sludge amended soils, other amendments like compost, biosolids, or manure need to be considered to provide nitrogen. Ecological and economical evaluation of sludge amendment depends on regional conditions. Costs for implementing the topsoil layer in general includes topsoil mixing and placing, hydroseeding, and erosion control matting are approximately CAD 10.00/m2. One quarter of this price is spent on erosion control matting. The Prince George Regional District Landfill has a surface cover area of 49,886 m2. The top layer has a minimum thickness of 60 cm. The construction, maintenance and after closure costs of a landfill can be minimized, by using adequate alternative materials, which are locally available. Reduction of the deposition of organic wastes is one of the main goals of a municipal solid waste landfill. Organic wastes account for most of the landfill gas and le a c h a te pro b lem s as w ell a s s ettlem e n t pro b lem s. A fte r the clo su re o f a landfill, the settlement problems affect the cover system including the top layer. Beyond financial concerns, the reuse of sludge would reduce the input of organic matter to the landfill, and save ever-shrinking landfill space. Sludge requires only basic equipment like a manure spreader and bulldozer for placement. The high moisture content is ideal for 71 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. placing and spreading. Cap construction with sludge can proceed under a broader range of weather conditions. Sludge amended soils readily absorb large quantities of rainfall reducing infiltration to the protective layer and storing water for vegetation growth during dry periods. All field studies were long-term experiments persisting between 1 and 7 years. Even though more parameters like depth of water penetration and percolation time can be determined in field experiments, the laboratory results of the moisture retention determination are a concise alternative to predict amending effects in soil. A number of functional forms were considered to describe the relationship between water content and matric potential. None of the current functions adequately describe the data. An acceptable function should provide minimum order of polynomial with a maximum accuracy. 72 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Chapter 5 Summary The objective of this study was to chemically and physically characterize sludge from two different pulping processes to investigate their suitability as a substitute or amendment in the topsoil layer of a landfill capping system. The purposes of the topsoil layer are to enhance plant vegetation, moisture retention, and minimize infiltration and chances of cracks followed by erosion and associated with infiltration problems. Pulp mill sludge represents the waste portion of the pulping process. As the wood input, the wood processing and the subsequent effluent treatment varies greatly, so does the composition of the sludge. To identify potential environmental impacts, elemental analysis was performed and the results compared to literature data from a mill survey (NACSI, 2000) and typical nutrient concentrations sufficient for plant growth (Barak, 1999). The BCTMP and Kraft mill sludge samples analyzed are low in potential environmental contaminants. These results support previous findings. Both sludge samples have high C:N ratios. The low nitrogen content often limits the effectiveness of sludge as soil amendment. The N limitation could be alleviated with appropriate fertilization and application rates. The type of sludge under consideration will determine the fertilizer composition to enhance plant growth. As the pH controls more or less nutrient availability, the neutral pH of BCTMP sludge and alkaline pH of Kraft mill sludge could cause a deficiency for micronutrients, eg. Fe, Zn that are important for plant growth. The pH could be altered by mixing sludge with other material or determining appropriate loading rates. Mixtures of compost, or biosolids, or boiler ash with sludge have been used successfully as forestry soil amendment (NACSI, 2000). 73 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Sludge is composed mainly of organic matter. Various studies found that organic amendments increase soil aggregation and stability, reduce bulk density, and increase water holding capacity. This contribution of organic matter was investigated. Soil has the highest bulk density, followed by BCTMP and Kraft mill sludge. The original sludge samples have a higher bulk density than the blended samples. Blending the sludge affects the fibre structure, resulting in lower bulk density. Water holding capacity was determined by gravity and moisture retention curves were established for original sludge and soil samples, various sludge-soil mixtures and sludge-soil layer systems. In both experiments the blended sludge samples had the highest water holding capacity and soil had the lowest. The sludge-soil mixtures demonstrated increasing water holding capacity with increasing amounts of sludge added to soil. The water holding capacity in the sludge-soil layer systems is lower in the sludge layers than in the sludge-soil mixtures and the original sludge samples. The moisture retention curves of BCTMP and Kraft mill sludge are similar in their overall ability to hold water. BCTMP sludge, however, has higher moisture content at field capacity and its moisture content decreases most over the entire pressure range compared to Kraft mill sludge. The BCTMP sludge has the most plant available water. The pressure plate experiment could not be applied successfully to the sludge-soil layer system as with increasing sample height, the time to reach equilibrium increases exponentially. Laboratory experiments are a short-time, concise alternative to field studies and the results can assist predicting the effect of sludge amendment to soil. The laboratory findings should be validated by field studies to determine their application to real world conditions. Kraft mill sludge and soil have similar water holding capacities. Compared to Kraft mill sludge BCTMP sludge has a higher water holding capacity, resulting in high water retention and higher amount of plant available water. Increasing organic matter 74 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. amendment reduces soil bulk density and increases soil microbial activity, which increases soil porosity. This alteration in soil physical properties is a consequence of the pore size distribution of sludge and soil particles. These attributes of the sludge are improving the performance of the topsoil layer with less environmental impact than the current disposal options. Sludge could provide coverage for landfill cap erosion control and vegetation needs. Another advantage for construction is the nature of the sludge, no further treatment or special equipment is needed. Such use would reduce expenses on mill and landfill budgets while conserving significant amount of valuable landfill space. The results and conclusions from this study are not necessarily applicable to any sludge in the pulp and paper industry. Based on this work it is recommended that any end user contemplating using sludge in a landfill capping system should consider chemical and physical characteristics of the sludge under consideration. The most important parameter is the economic feasibility. 75 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Chapter 6 Recommendations for future work Sludge amendments have the potential to protect the soil during critical periods of vegetation establishment, thus reducing on-site damages and costs as well as reducing off-site impacts on water quality. 1. Samples should be collected over a longer period of time, and mixed to have a more representative sample for the experiments of interest. 2. Organic matter plays a fundamental role in the stabilization of soil structure and the formation of pores. Other physical properties of interest to further realize the potential of sludge as soil amendment are the effects of freezing and thawing cycles and shear strength of the samples. 3. Field experiments should be implemented to confirm laboratory results on water holding capacity (WHC) including important parameters like time and depth of water infiltration after a wetting event. 4. Different treatments of sludge (mixtures and layer systems) should be investigated in field studies to determine the most effective application of sludge. Future studies should include various sludge application rates, as well as other amendments to increase plant available N. The process in a pulp mill can change daily to effect the properties of sludge produced. The type of sludge determines the fertilizer composition. 5. Investigations on sludge decomposition and changes in C:N ratios over time should be conducted to assess consequences of sludge amendments. 76 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 6. Mathematical retention functions could be applied to express the relationship of moisture content and matric potential and predict retention characteristics of sludge. 7. The time to reach equilibrium is a crucial factor for the sludge-soil layer systems. Future laboratory experiments should investigate whether different physical set ups for the samples could reduce the time for equilibrium. Factors such as using plastic columns with smaller diameter and compacting the sample under defined conditions could be explored. 8. To get a better understanding of the pore-size distribution in sludge-soil mixtures, samples of the mixtures should be observed under different magnifications under the scanning electron microscope (SEM). Aggregation size could be determined and compared to original sludge and soil samples. 9. The success of plant growth in the topsoil layer depends on various factors such as soil quality, climate, and plant species. Research on various plant species should be conducted to determine adequate species for successful long-term revegetation. 77 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. References Arocena, J.M. and Sanborn, P. 1999. Mineralogy and genesis of selected soils and their implications for forest management in central and northeastern British Columbia. Canadian Journal of Soil Science 79 (4), p. 571-592 Nov. 1999. Barak, P. http://www.soils.wisc.edu/~barak/soilscience326/essentl.htm. University of Wisconsin-Madison, Dept, of Soil Science, 1999; viewed May 2003. Barker, A.V., Stratton, M.L., and Rechcigl, J.E. 2000. Soil and by-product characteristics that impact the beneficial use of by-products. In Land application of agricultural, industrial, and municipal by-products - SSSA Book Series no. 6 Edited by J.F. Power and W.A. Dick. Soil Science Society of America, Inc. Madison, Wl, pp. 169-213 Bauer, A. and Black, A.L. 1992. Organic carbon effects on available water capacity of three textural groups. Soil Sci. Soc. Am. J. 56, p. 248-254. Bellamy, K.L., Chong, C., and Cline, R.A. 1995. Paper sludge utilization in agriculture and container nursery culture. Journal of Environmental Quality 24: 1074-1082. BCLA, 2001. British Columbia Landscape Standard (1997 edition, updated 2001). British Columbia Society of Landscape Architects and the British Columbia Nursery Association. 108 pp. Biermann, C.J., 1993. Essentials of Papermaking. Academic Press Inc., California, USA. 1993. Bilitewski, B.; Haerdtle, G. and MaMarek, K. 1994. Waste Management. Springer-Verlag Berlin Heidelberg; chapter 5, p. 273-322. Biofine Inc. 1998. Markets for paper waste and papermill sludge. Biocycle, Vol. 39, Issue 1, p. 19, 1/4p, JP Press, Inc., Emmaus, January 1998. Bolt, G.H.; De Boodt, M.F.; Hayes, M.H.B.; McBride, M.B.; Destrooper, E.B.A. 1986. Interactions at the soil colloid-soil solution interface. Kluwer Academic, Boston, p. 410-463. Bowen, B.D., Wolkowski, R.; Hansen, G. 1996. Comparison of the effects of fresh and composted paper mill sludge on potato growth. P. 523-527. In TAPPI Proceedings, Environ. Conf. TAPPI Press, Atlanta, Ga. Brady, N. C.; Weil, R. R.1999. The Nature and Properties of Soils. Prentice Hall, 12th edition. Brooks, P.D., Stark J.M., Mclnteer, and Preston T. 1989. Diffusion method to prepare soil extracts for automated nitrogen-15 analysis. Soil Sci. Soc. Am. J. 53, p. 1707-1711. 78 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Brown, S.L.; Henry C.L.; Chaney, R.; Compton, H.; and DeVolder, P.S. 2003. Using municipal biosolids in combination with other residuals to restore metal contaminated mining areas. Plant and Soil, Feb. 2003, vol. 249, no. 1, p. 203-215. Burckhard, S. R., Pirkl, D., Schaefer, V. R. , Kulakow, P, Leven, B. 2002. Proceedings of the 2000 Conference on Hazardous Waste Research. A study of soil waterholding properties as affected by TPH contaminations. Cabalka, D. 1996. Landfill cap erosion: Severe conditions and dramatic solutions. Public Works, vol. 127, no. 10. Camberato, J.J., Vance, E.D., and Someshwar, A.V. 1997. Composition and land application of paper manufacturing residuals. In Agricultural Uses of By-Products and Wastes, ACS Symposium Series 668, ed. J.E. Rechcigl and H.C. MacKinnon, 185-202, Washington, D.C., American Chemical Society. Canning, K. 1999. Innovations address industry waste streams. Pollution Engineering, Newton. Autumn 1999 Carpenter, A.F., and Fernandez, I.J. 2000. Pulp mill sludge as a component in manufactured topsoil. Journal of Environmental Quality. 29(2), p. 387-397. Carter, M.R., 1993. Soil Sampling and Methods o f Analysis. Canadian Society of Soil Science. Lewis Publishers, p. 450-451. Chong, C., R.A. Cline, and D.L. & Rinker, 1988. Use of Papermill sludge in container crop culture. Landscape Trades. 10(7) p. 17-18. Chow, T. L.; Rees, H. W.; Fahmy, S. H.; Monteith, J. O. 2003. Effects of pulp fibre on soil physical properties and soil erosion under simulated rainfall. Canadian Journal of Soil Science 83 (1): 109-119. Clear Lake Ltd. 1993. Proceedings: Pulpmill Waste Utilization in the Forest, a conference held in Edmonton, Alberta, 1993. Coburn, R.; Dolan, G. 1995. Industry/government partnership works to solve New York environmental issues. Pulp & Paper 69 (10), p. 59-63. Duguid, J.O., 1977. Assessment of DOE low-level radioactive solid waste disposal storage activities. Battelle Memorial Institute, Columbus, Ohio. Dwyer, S. 1997. Conference Proceedings: Landfill capping in the semi-arid west: Problems, perspectives, and solutions. Large-scale field study of Landfill covers at Sania National Laboratories, p. 87-107. Dwyer, S. "Alternative landfill covers pass the test". Civil Engineering, 'Sep1998, Vol.68 Issue 9, p.50. Edwards, J.H. 1997. Application of uncomposted waste paper and other organics. P. 163-184. In J.E. Rechcigl and H.C. Mackinnon. Agricultural Uses of By-Products 79 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. and Wastes, ACS Symposium Series 668, American Washington, D.C. Chemical Society, Floess, C., Smith, R., Hitchcock, K. 1995. Capping with fiber clay. Civil Engineering 8:62-63. Foley, B.J. and Cooperband, L.R. 2002. Paper mill residuals and compost effect on soil carbon and physical properties. J. Environ. Qual. 31: 2086-2095. Gardner, W. R.; Gardner W. H.; Jury W. A. 1991. Soil Physics. 5th edition, John Wiley & Sons, Inc. Gagnon, B.; Lalande, R.; Fahmy, S.H. 2001. Organic matter and aggregation in a degraded potato soil as affected by raw and composted pulp residue. Biol. Fertil. Soils. 2001, vol. 34, p. 441-447. Genthe, D. 1993. Shear strength of two pulp and paper mill sludges with low solids content. Master’s Thesis, University of Wisconsin, Madison. GeoSyntec Consultants, 1995. Final Cover System Guidance Document. Municipal Solid Waste Landfills, p. 3-7, p. 59-62. Gillman, G.P., Sumpter, E.A. 1986. Modification to the compulsive exchange characteristics of soils. Aust. J. Soil Res. 24:61-66. Glasser, W.G. and Heinze, T.G. 1996. Cellulose Derivatives: Modification, Characte­ rization, and Nanostructures. ACS Symposium Series: 688, Oxford University Press. 1996. Glowacki, Jeremy. 1994. Landfilling of sludge remains most viable, but new options on horizon. Pulp & Paper 68(9): 95-97. Gregorich, E.G.; Reynolds, W.D.; Culley, J.L.B.; McGovern, M.A.; Curnoe, W.E. 1993. Changes in soil physical properties with depth in a conventionally tilled soil after no-tillage. Soil Tillage Res. 26, p. 289-299. Gomez, C.C., Jans-Hammermeister, D.C., and McGill, W.B. 1997. Soil microbiology and biochemistry. Soils 430 Laboratory Manual. University of Alberta. Edmonton, Alberta. Hakonson, T.E., L.J Lane, J.G. Steger, and G.L. DePoorter, 1982a. Some interactive factors affecting trench cover integrity on low-level waste sites, in Proc. Low-level waste disposal: Site characterization and monitoring, Arlington, Virginia, NUREG/CP-0028, CONF-820674, Vol. 2. Hakonson, T.E."Capping as an alternative to landfill closures: Perspectives and approaches". Conference Proceedings: Landfill capping in the semi-arid west: Problems, perspectives, and solutions. May 1997, p. 1. 80 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Harding, E and D.J. Ross. Some factors in low-temperature storage influencing the mineralizable-nitrogen of Soils. J. Sci. Fd Agric., 1964, Vol. 15, December. Henry, C. L. 1986. Growth response, mortality, and foliar nitrogen concentrations of four tree species treated with pulp and paper and municipal sludges. In The Forest Alternative for Treatment and Utilization of Municipal and Industrial Wates, ed. D.W. Cole, C.L. Henry, and W.L. Nutter, 258-265. Seattle, WA: University of Washington Press. Henry, C. L. 1991. Nitrogen dynamics of pulp and paper sludge amendments to forest soils. Water Science and Technology 24: 417-425. Hill, R.L., and James, B.R. 1995. The influence of waste amendments on soil properties, p. 311-325. In Soil Amendments and Environmental Quality, ed. J.E. Rechcigl, 311-325. Boca Raton, FL: Lewis Publishers. Hillel, D. Environmental Soil Physics. Academic Press. 1998. Jacobs, D.G., J.S. Epler, and R.R. Rose, 1980. Identification of technical problems encountered in the shallow land burial of low-level radioactive wastes. Oak Ridge National Laboratory/SUB-80/136/1, Oak Ridge, Tennessee. Kalra, Y.P. and Maynard, D.G. 1994 Methods manual for forest soil and plant analysis. Northwest Region. Information Report NOR-X-319. Forestry Canada 1994, p. 19-25. Kennedy, J.F., G.O. Philips, P.A. Williams. 1989. Wood Processing and Utilization. Ellis Horwood Limited, England. 1989. Khaleel, R., Reddy, K.R., and Overcash, M.R. 1981. Changes in soil physical properties due to organic waste applications: a review. Journal of Environmental Quality 25: 133-141. Klocke, N. L., Hergert, G. W. 1996. How Soil Holds Water. NebGuide. Available at: http://ianr.unl.edu/pubs/fieldcrops/q964.htm. 01/23/2003. Klute, A. 1986. Soil Sampling and Methods of Analysis, SSSA, Soil Science Society of. America. Physical and Mineralogical Methods.2nd edition, Chapter 26. Kraske, C. R. 1992. The Influence of Papermill Sludge Application on the Biogeochemistry and Vegetation of Young Red Pine (Pinus resinosa Ait.) Plantations Established in Recent Clearcut Forest Ecosystems. Ph.D. Dissertation. Orono, ME: University of Maine. Kreith, F. 1994. Handbook of Waste Management. McGraw-Hill, Inc. Kunzler, C. 2001. Pulp and paper industry’s diverse organics stream. Biocycle Vol. 42, Issue 5, p. 30-33. JP Press, Inc., Emmaus, May 2001. 81 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Mabee, W.E., 2001. Study of woody fiber in papermill sludge. Graduate Department of Forestry, University of Toronto Publications. 2001. MacDonald, R.G., J.N. Franklin, 1969. Pulp and Paper Manufacture: The Pulping of Wood. Second Edition, Vol.1. McGill, W., 2002. Lab Manual: Biogeochemical Processes in Soil Systems: an environmental perspective, UNBC, Winter 2002, p. 6-8. Macyk, T. M. 1999. Land application of mechanical pulp mill sludges in Alberta: research and operational activities. Pulp & Paper Canada 100 (6): 34-37. Madejon, E.; Burgos, P.; Lopez, R.; Cbrera, F, 2003. Agricultural use of three organic residues: effect on orange production and properties of a soil of the ‘Comarca de Huelva’ (SW Spain). Nutrient Cycling in Agroecosystems. Vol. 65, no. 3, p. 281. Malmstead, M.J.; Bonistall, D.F.; Van Maltby, C. 1999. Closure of a nine-acre industrial landfill using pulp and paper mill residuals. TAPPI Journal vol. 82 (2), February 1999, p. 153-160. Martens, D.A.; Frankenberger, W.T. 1992. Modification of infiltration rates in an organicamended irrigated soil. Agron. J. 84, p. 707-717. McGovern, J.N.;Berbee, J.B.; Bockheim, J.G. 1983. Characteristics of combined effluent treatment sludge from several types of pulp and paper mills. TAPPI Journal 66: 115-118. Merchant, S., Progress R e p o rt# ! UNBC. Spring 2002. Metzger, L., and Yaron, B. 1987. Influence of sludge organic matter on soil physical properties. In Advances in Soil Science, ed. B.A. Stewart., 7: 141-163. New York, NY: Springer Verlag Moo-Young, H. and Zimmie, T. 1996. Geotechnical properties of paper mill sludges for use in landfill covers. Journal of Geotechnical Engineering 9:768-776. Mullen, S. 2002. Co-utilizing paper mill residuals as a sustainable soil amendment on native sandy soils. Royal Roads University. National Council for Air and Stream Improvement (NCASI). 2002. Laboratory Hydraulic Conductivity Testing Protocols for Paper Industry Residuals Used for Hydraulic Barrier Layers. NCASI Technical Bulletin No. 848. Research Triangle Park, N.C.: National Council for Air and Stream Improvement. National Council for Air and Stream Improvement (NCASI). 2000. Utilizing Paper Mill ByProducts as Forest Soil Amendments: Forest Responses, Recommendations, And Industry Case Studies. NCASI Technical Bulletin No. 798. Research Triangle Park, N.C.: National Council for Air and Stream Improvement. 82 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. National Council for Air and Stream Improvement (NCASI). 1999b. Solid Waste Management Practices in the U.S. Paper Industry - 1995. Technical Bulletin No. 793. Research Triangle Park, N.C.: National Council for Air and Stream Improvement. National Council for Air and Stream Improvement (NCASI). 1997. A Field-Scale Study of the Use of Paper Industry Sludges in Landfill Cover Systems: Final Report. Technical Bulletin No. 750. Research Triangle Park, N.C.: National Council for Air and Stream Improvement. National Council for Air and Stream Improvement (NCASI). 1989. Experience with and laboratory studies of the use of pulp and paper mill solid wastes in landfill cover systems. Technical Bulletin No. 559. Research Triangle Park, N.C.: National Council for Air and Stream Improvement. National Council for Air and Stream Improvement (NCASI). 1984a. The land application and related utilization of pulp and papermill sludges. New York, NY: National Council of the Paper Industry for Air and Stream Improvement, Inc., Technical Bulletin No. 439. Nemati, M.R.; Caron, J.; Gallichand, J. 2000. Stability of structural form during infiltration: Laboratory measurements on the effect of de-inking sludge. Journal of Soil Science Society of America 64, p. 543-552. Nyhan, J.W., G.L. DePoorter, D.J. Drennon, J.R. Simanton, and G.R. Foster, 1984. Erosion of earth covers used in shallow land burial at Los Alamos, New Mexico. Journal of Environmental Quality. 13(3): 361-366. Nyhan, J.W. and L.J. Lane, 1986. Erosion control technology: User guide to the use of the Universal Soil Loss Equation at waste burial sites facilities. Los Alamos National Laboratory, Los Alamos, New Mexico. LA-10262-M. O’Brien, T. 2001. Evaluation of paper mill sludge as soil amendment and as a component of topsoil mixtures. University of Massachusetts Amherst. Pais, I. and Jones Jr., J.B., 1997. The handbook of trace elements. St. Lucie Press, Boca Raton, FL, 223 pp. Paul, E. A., Clark, F. E. 1996. Soil Microbiology and Biochemistry. Second Edition. Academic Press, San Diego, California. Pepin, R. 1984. The use of paper mill sludge as a landfill cap. Proc., 1983 National Council of the Pulp and Paper Industry Northeast Regional Meeting, NCASI, New York, N.Y. Pickell, J. and Wunderlich, R. 1995. Sludge disposal: current practices and future options. Pulp & Paper Canada 96(9), p. 41-47. 83 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Richard, L.A. and Weaver, L.R. 1944. Moisture retention by some irrigated soils as related to soil-moisture tension. Washington, D.C. Journal of Agriculture Research, Vol. 69, no. 6, p. 215-235. Roberts, J.C., 1996. The Chemistry of Paper. The Royal Society of Chemistry. Cambridge, UK. 1996. Ross, D.S. Recommended Methods for Determining Soil Cation Exchange Capacity, available at: http://www.analvtika.gr/METHODS/SOIL/cec.htm. 03/26/03. Shields, Jr.; Huddy, M. D., Somers, S. G. 1986. Pulp mill sludge application to cottonwood plantation. In The Forest Alternative For Treatment and Utilization of Municipal and Industrial Wastes, ed. D.W. Cole, C.L. Henry, W.L. Nutter, 553548. Seattle, WA: University of Washington Press. Shoemaker, D.P.; Garland, C.W.; Nibler, J.W. Experiments in physical chemistry. Chapter II. 6th edition, WCB/McGraw-Hill, Inc., 1996. Schuerch, C. 1989. Cellulose and Wood: Chemistry and Technology. John Wiley and Sons. 1989. Siuru, B. "New landfill cover testing may result in reduced costs". World Wastes, Sept.1996, Vol.39 Issue 9, p.12. Soilmoisture Equipment Corp. 2001. Lab 203, Laboratory Setup. Santa Barbara, California; p. 5-7. Sperling, T and Hansen, B. Land Reclamation at Municipal Landfill Sites, available at: http://www.ecowaste.com/swanabc/papers/sper01 .htm. 03/23/00. Stoffel, C., and Ham, R. 1979. Testing of high ash content paper mill sludge for use in sanitary landfill construction. Rep. Prepared for City of Eau Claire, Wis., Ayers and Assoc., Inc. Tchobanoglous, G.; Theisen, H.; Vigil, S.; eds. Integrated Solid Waste Management: Engineering Principles and Management Issues. McGraw-Hill, Inc., 1993. Tester, C.F. 1990. Organic amendment effects on physical and chemical properties of a sandy soil. Soil Science Society of America Journal 54: 827-831. Tisdale, S.L.; Nelson, W.L; Beaton, J.D. 1985. Soil Fertility and Fertilizers. 5th edition, M acm illan P ublishing C o m p a n y , N e w Y o rk. Turner, M.S; Clark, G.A; Stanley, C.D.; Smajestrla, A.G. 1994.Physical characterisitics of a sandy soil amended with municipal solid waste. Pro. Soil Crop Sci. Soc. Fla. 53, p. 24-26. Walker, J.C.F., 1993. Primary Wood Processing: Principles and Practices. Chapman and Hall, 1993. 84 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Webb, L. 2000. Cleaning up after the papermakers. Pulp & Paper International, Aug. 2000, Vol. 42, Iss. 8, p. 24-27. Wei, Q.F.; Lowery, B.; Peterson, A.E. 1985. Effect of sludge application on physical properties of a silty clay loam. J. Environ, Qual. 14, p. 178-180. Whitehead, D.C. 2000. Nutrient elements in grassland. Soil-plant-animal relationship. CABI Publishing, Oxon, UK, 369 pp. Zakis, G.F. 1994. Functional Analysis of Lignins and their Derivatives. Tappi Press, Georgia, USA. 1994. Zibilske, L.M.; Clapham, W.M.; Rourke, R.V. 2000. Multiple applications of paper mill sludge in an agricultural system: Soil effects. J. Environ. Qual. 29: 1975-1981. 85 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix A: Glossary BCTMP: bleached chemi-thermomechanical pulping uses physical forces with some additional heat and/or chemicals to separate wood fibers. Capping system : a combination of several layers of diverse material for the final closure of a landfill. Dioxins: any of a group of chemical compounds that is an undesirable by-product in the manufacture of herbicides, disinfectants, and other agents. In popular terminology, dioxin has become a synonym for one specific dioxin 2,3,7,8-tetrachlorodibenzo-pdioxin (2,3,7,8-TCDD) from Encyclopaedia Britannica. EPA: United States Environmental Protection Agency, responsible for protecting human health and safeguarding the natural environment. ICP-AES: Inductively coupled plasma-atomic emission spectroscopy is a quantitative analytical technique for the determination of trace elements in samples. Kraft pulping: chemical pulping process, also known as alkaline or sulphate process. It is the most common method used in the pulp and paper industry. MoELP: Ministry of Environment, Lands and Parks committed to protecting and enhancing the quality of British Columbia’s environment; now Ministry of Water, Land and Air Pollution and Ministry of Sustainable Resource Management. NCASI: National Council for Air and Stream Improvement; Research Triangle Park in North Carolina serving the forest industry Original sludge: sludge sample as received from the mill without any treatment. SEM: scanning electron microscope 86 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix A: Glossary Sludge: wastewater treatment plant solid residuals are those solid materials collected in the process of treating water used in the mill prior to release into the environment. Typically, these materials consist of solids collected in primary treatment (separation of solids from raw wastewater) and secondary treatment (biological treatment followed by clarification to separate biosolids). Often these primary and secondary residuals are combined to facilitate handling (NCASI, 1999). TAPPI: Technical Association of the Pulp and Paper Industry Turpenes: By-product from the Kraft pulping process; a mixture of turpenes consists of monoterpenes and pinenes. The basic structural unit is isoprene (C5H8). UNBC: University of Northern British Columbia WHC: Water holding capacity or water retention or field capacity or soil wetness characteristics are all expressions for the soils ability to store water. 87 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix B: Determination of moisture content in sludge samples TABLE 21: Kraft mill sludge dried at 55 °C (n=8); uncertainty ± 0,0001 # 1 2 3 4 5 6 7 8 w A, W Wt Ww e wd Al dish [g] + sludge wet [g] + sludge dry [g] sludge wet [g] sludge dry [g] 3.1473 9.7137 5.7337 6.5664 2.5864 3.1389 9.9190 6.7801 2.6013 5.7402 3.1339 10.1768 5.7500 7.0429 2.6161 3.1354 9.8010 5.6838 6.6656 2.5484 3.1462 5.7202 6.7610 2.5740 9.9072 3.1463 10.1450 5.7366 6.9987 2.5903 3.1646 10.0738 6.0092 6.9092 2.8446 3.1458 10.0532 5.7814 6.9074 2.6356 moisture content [%] 154 161 169 162 163 170 143 162 160 8.72 + 3.08 average stdev se TABLE 22: Kraft mill sludge dried at 80 °C (n=8); uncertainty ± 0.0001 # 1 2 3 4 5 6 7 8 w A, W W t W ¥VW 3.1541 3.1466 3.1377 3.1554 11.1413 10.5190 10.5869 11.1696 5.9925 5.7488 5.8402 5.9508 7.9872 7.3724 7.4492 8.0142 e wd Al dish [g] + sludge wet [g] + sludge dry [g] sludge wet [g] sludge dry [g] 10.6888 5.8524 7.5656 3.1232 2.7292 10.6486 2.6744 3.1358 5.8102 7.5128 3.1456 10.3413 5.5443 7.1957 2.3987 5.9415 3.1397 11.0038 7.8641 2.8018 moisture content [%] 177 181 200 181 2.8384 2.6022 2.7025 2.7954 181 183 176 187 183 7.58 ±2 .68 average stdev se TABLE 23: Kraft mill sludge dried at 105 °C (n=8); uncertainty ± 0.0001 # 1 2 3 4 5 6 7 8 w A1 W W t W * ¥w wd Al dish [g] + sludge wet [g] + sludge dry [g] sludge wet [g] sludge dry [g] 3.1200 9.9696 5.8332 6.8496 2.7132 3.1300 5.7059 6.4682 2.5759 9.5982 3.1405 10.0065 5.7522 6.8660 2.6117 10.0875 5.6582 2.5228 3.1354 6.9521 3.1497 10.2195 5.7845 7.0698 2.6348 3.1423 10.1312 5.7506 6.9889 2.6083 5.8949 7.6595 2.7632 3.1317 10.7912 3.1524 5.7439 2.5915 9.9102 6.7578 e moisture content [%] 152 151 163 176 168 168 177 161 average stdev se 165 9.65 ±3.41 88 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix B: Determination of moisture content in sludge samples TABLE 24: BCTM P sludge dried at 55 °C (n=8); uncertainty ± 0.0001 # 1 2 3 4 5 6 7 8 wA, W wt W * * W 3.1738 3.1574 3.1677 3.1583 3.1492 3.1516 3.1429 10.1558 10.1315 10.1080 10.4646 10.4175 10.0293 10.0700 5.9669 5.9270 5.8984 6.0204 5.9833 5.8311 5.8303 6.9820 6.9741 6.9403 7.3063 7.2683 6.8777 6.9271 0 wd Al dish [g] + sludge wet [g] + sludge dry [g] sludge wet [g] sludge dry [g] 3.1356 10.0053 5.8749 6.8697 2.7393 moisture content [%] 151 2.7931 2.7696 2.7307 2.8621 2.8341 2.6795 2.6874 150 152 154 155 156 157 158 average stdev se 154 2.93 ± 1.04 TABLE 25: BCTM P sludge dried at 80 °C (n=6); W * =porcelain dish; uncertainty ± 0.0001 # 1 2 3 4 5 6 W* dish [g] 55.5007 55.0895 56.2052 54.9497 55.9984 57.1587 W Wt Ww e wd + sludge wet [g] + sludge dry [g] sludge wet [g] sludge dry [g] 56.9204 5.3120 1.4197 60.8127 56.4515 5.1978 1.3620 60.2873 1.3781 61.4097 57.5833 5.2045 1.3661 60.1029 56.3158 5.1532 61.2109 57.3514 5.2125 1.3530 62.1692 58.4543 5.0105 1.2956 moisture content [%] 274 282 278 277 285 287 280 4.93 ± 2.01 average stdev se TABLE 26: BCTM P sludge dried at 105 °C (n=8); uncertainty ± 0.0001 # 1 2 3 4 5 6 7 8 wA, W wt ww wd Al dish [g] + sludge wet [g] + sludge dry [g] sludge wet [g] sludge dry [g] 5.6825 2 .5480 3.1345 9.8600 6.7255 2.8391 3.1721 10.8150 6.0112 7.6429 2.6408 3.1554 9.9368 5.7962 6.7814 2.6843 3.1645 10.0964 5.8488 6.9319 2.6846 3.1565 10.3138 7.1573 5.8411 5.7983 6.9383 2.6514 3.1469 10.0852 6.0881 2.9385 3.1496 10.9675 7.8179 2.5449 3.1408 10.0391 5.6857 6.8983 e moisture content [%] 164 169 157 158 167 162 average stdev se Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 166 171 164 5.04 ± 1.78 Appendix C: Determination of total C and total N T A B L E 27: T o ta l c a rb o n a n d n itro g e n ra w d a ta ( n = 4 ) sample 'C CM -4— ' Kraft mill sludge (1) Kraft mill sludge (2) Kraft mill sludge (1) Kraft mill sludge (2) total N % total C % 0.00 0.00 0.14 0.12 44.01 44.56 39.66 43.65 sample •f—> CM ■+—> BCTMP sludge (1) BCTMP sludge (2) BCTMP sludge (1) BCTMP sludge (2) total N % total C % 1.18 1.16 1.47 1.32 53.59 53.73 50.06 51.62 a v e ra g e 0.07 4 2.97 a v e ra g e 1.28 52.25 s td e v 0.08 2.24 s td e v 0.14 1.75 ± se 0.04 1.12 ± se 0.07 0.87 90 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix D: Determination of ash content in sludge and soil samples TABLE 28: Ash content of sludge and soil samples (BCTM P and Kraft mill ash samples were weighed with lid. Soil ash samples were weighed without lid.) n=3 sample crucible + lid [g] crucible [g] crucible+sample[g] sample wet [g] dried at 105° C sample dry [g] ash after 4h [g] ash after 6h [g] ash after 8h [g] ash [g] ash content % average % stdev se B C TM P (1) 85.1951 5 4.9472 56.5230 1.5758 55.3414 0.3942 85.2124 85.2109 85.2123 0.0172 4.36 B C TM P (2) 87.3807 55.9816 57.5132 1.5316 56.3607 0.3791 87.3989 87.3969 87.3984 0.0177 4.67 n -3 B C TM P (3) Kraft mill (1) Kraft mill (2) Kraft mill (3) 85.8533 85.8868 90.6643 85.9560 56.1963 55.4978 55.0871 57.1441 57.5989 56.6113 56.5255 5 8.6368 1.4026 1.1135 1.4384 1.4927 56.5761 55.7878 55.4718 57.5114 0.3798 0.2900 0.3847 0.3673 85.9068 85.9670 85.8703 90.6799 85.9036 85.8682 90.6781 85.9657 85.9678 85.8698 85.9052 90.6796 0.0118 0.0165 0.0184 0.0153 4.29 4.84 4.17 4.07 4 .40 0.254 ± 0 .146 4.40 0.400 ± 0.231 n=3 soil (1) 85.9571 55.4977 56.8018 1.3041 56.6137 1.1160 56.5917 56.5932 56.5915 1.0938 98.01 soil (2) 85.8522 55.0868 56.5075 1.4207 56.3030 1.2162 5 6.2796 56.2812 56.1850 1.0982 90.30 soil (3) 85.8868 56.1967 57.5212 1.3245 57.3372 1.1405 57.3151 57.3170 57.3153 1.1186 98.08 95.5 4 .4 7 ± 2 .5 8 91 Appendix E: Energy Dispersive X-ray Analysis TABLE 29: Elemental analysis of Kraft mill sludge; elements are expressed in relative percentage. A:\Kraft Mill.SPC Acquisition Tim e : 08:54:34 Date : 15-Mar- 2 kV:20.00 Tilt: 0.00 Take-off:20.0C Tc:40 Detector Type :SU TW Resolution :151.58 Lsec :183 EDAX ZAF Quantification Element Normalized Standardless Element Wt % At % K-Ratio Z A F C K 0 K NaK SiK S K K K 68.89 26.27 3.69 0.77 75.72 1.008 21.68 2.12 0.3817 0.0395 0.36 0.0056 1.0002 1.0001 1.0001 1.0001 0 0 0 0 0 0 CaK Total 0.38 0.13 0.0037 0.9912 0.928 0.9508 0.9292 0.8981 0.9198 0.5495 0.1518 0.3499 100 100 Element Net Inte. Bkgd Inte. Inte. Error P/B C K 0 K NaK SiK S K K K CaK 7.87 0.64 2.74 12.24 1.28 0.93 0.5 1.99 3.6 2.45 10.43 16.86 25.56 0.64 0.26 0 0 0.22 2.1 1.57 1.3 0 0 0.2 0 0 41.76 0.17 0.012 0.7714 0.9486 1.0462 1.0541 K-Ratio - constant Z, A, F - correction factors: Z= atomic number A= absorption factor F= fluorescence Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 1.0003 1.0014 1 Appendix E: Energy Dispersive X-ray Analysis TABLE 30: Elemental analysis of BCTM P sludge; elemen+s are expressed in relative percentage. A:\BCTMP.spc Acquisition Time : 09:09:03 Date : 15-M ar- 2 kV:20.00 Detector Type :SUTW Tilt: 0.00 Resolution :151.58 EDAX ZAF Quantification Element Normalized Standardless Take-off:20.00 Tc:40 Lsec :37 Element W t% At % K-Ratio Z A F C K 0 K NaK SiK S K KK CaK Total 58.2 38.02 1.42 0.33 0.25 0.55 1.23 65.95 32.34 0.84 0.16 0.3105 0.064 0.0041 0.0023 0.0022 0.19 0.42 0.0052 0.0118 0.5284 0.1696 0.3112 0.7503 0.942 1.0419 1.046 1.0003 0.11 1.0092 0.9925 0.9292 0.952 0.9307 0.8994 0.9212 100 1G8 Element Net Inte. Bkgd Inte. Inte. Error P/B C K 0 K NaK SiK 108.15 35.01 5.38 3.48 2.69 5.54 11.69 2.32 8.39 14.59 20.13 14.8 10.05 9.82 1.58 3.06 13.49 46.58 4.17 0.37 0.17 0.18 0.55 1.19 S K KK CaK K-Ratio - constant Z, A, F - correction factors: 22.66 25.24 11.58 6.44 Z= atomic number A= absorption factor F= fluorescence Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 1 1.0001 1.0005 1.0012 1.0042 1 Appendix F: Cation exchange capacity TABLE 31: Effective cation exchange capacity and exchangable Al, Fe, K, Mg, Mn, and Na for BCTM P and Kraft mill sludge and soil samples. (Analysis was conducted by British Columbia Ministry of Forests Research Laboratory, Analytical Chemistry Section) Sample soil 1 soil 2 soil 3 Exch Al cmol+/kg Exch Ca cmol+/kg Exch Fe Exch K Exch Mg Exch Mn Exch Na CEC (Ba) cmol+/kg cmol+/kg cmol+/kg cmol+/kg cmol+/kg cmol+/kg 5.231 5.142 5.318 0.04 0.04 0.04 0.196 0.195 0.001 0.300 0.294 0.302 0.212 Effective 15.24 15.01 15.51 0.001 0.001 ± 0.0003 0.299 0.004 ± 0.0013 5.230 0.088 ± 0.0293 0.040 0.001 ± 0.0003 0.201 0.010 ± 0.0033 15.25 0.250 ± 0.0833 26.793 27.082 26.585 0.006 0.755 0.761 0.743 3.456 35.23 3.492 3.422 0.06 0.06 0.06 4.124 0.006 0.005 4.163 4.058 35.60 34.91 0.037 0.001 26.820 0.250 0.006 0.001 0.753 0.009 3.457 0.035 0.061 0.001 4.115 0.053 35.25 0.345 ± 0.0003 ± 0.0833 ± 0.0003 ± 0.0030 ± 0 .0 1 1 7 ± 0.0003 ± 0 .0 1 7 7 ± 0 .1 1 5 0 < 0.001 < 0.001 < 0.001 13.015 13.174 12.996 < 0.001 < 0.001 < 0.001 0.474 0.474 0.435 5.428 5.413 5.385 0.07 0.07 0.07 0.686 0.721 0.729 19.66 19.84 19.61 < 0.001 < 0.001 ± 0.0003 13.062 0.098 ± 0.0327 < 0.001 0.461 0.023 ± 0.0077 5.409 0.022 ± 0.0073 0.070 0.001 ± 0.0003 0.712 0.023 ± 0.0077 19.70 0.121 ± 0.0403 0.002 0.009 0.009 9.474 9.328 9.629 < 0.001 0.003 0.007 0.004 ± 0.0013 9.477 0.151 ± 0.0503 BCTMP 1 BCTMP 2 BCTMP 3 0.036 0.037 0.037 average stdev se Kraft mill 1 Kraft mill 2 Kraft mill 3 average stdev se average stdev se < 0.001 ± 0.0003 94 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix G: Elememtal analysis TABLE 32: Elemental analysis of oven-dried BCTM P and Kraft mill sludge by ICP-AES. (Aluminium, Boron, Calcium, Cadmium, Cobalt, Chromium, Copper, Iron, Potassium, Magnesium, Manganese, Molybdenium, Sodium, Nickel, Phosphorus, Lead, Zinc). 1BDL = below detection limit n-4 Element Aluminum Boron Calcium Cadmium Cobalt Chromium Copper Iron Potassium Magnesium Manganese Detection Limit Kraft mill [ppm] [pg/g] stdev n=4 ± se BCTMP stdev ± se [pg/g] 0.068 0.01 0.009 0.008 0.05 0.025 0.006 0.007 0.5 0.003 0.001 702 0.672 5931 0.088 0.582 4.97 14.51 587 72.8 1795 89.0 46.4 0.604 238 0.106 0.416 1.63 3.58 35.0 54.6 36.4 9.99 23.2 0.302 119 0.053 0.208 0.816 1.79 17.5 27.3 18.2 4.99 295 62.0 7936 0.232 1.491 13.52 7.87 312 277 478 28.6 23.7 1.28 86.6 0.241 4.59 1.80 37.4 56.4 21.4 1.06 11.9 0.642 43.3 0.121 0.585 2.30 0.90 18.7 28.3 10.7 0.529 0.062 - - - - 30.7 1.488 54.4 15.36 0.752 27.2 1BDL 904 8.088 932 24.9 6.961 61.4 2.75 10.1 1.38 5.08 1BDL 28.4 49.8 13.75 123 1.84 0.910 Molybdenium Sodium Nickel Phosphorus 0.05 0.019 0.35 1BDL 162 1.819 41.2 Lead Zinc 0.125 0.012 4.09 30.5 1.171 - 95 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric w ater holding capacity P a rt A : Bulk density TABLE 33: Raw data for sludge and soil samples; (n=5) sample Kraft mill sludge 1 Kraft mill sludge 2 Kraft mill sludge 3 Kraft mill sludge 4 Kraft mill sludge 5 BCTMP sludge 1 BCTM P sludge 2 BCTM P sludge 3 BCTM P sludge 4 BCTM P sludge 5 Soil 1 Soil 2 Soil 3 Soil 4 Soil 5 column empty column&sludge mass wet [g] [g] [g] 63.372 63.778 63.170 63.502 63.842 63.504 63.360 63.600 65.150 65.578 63.566 64.194 63.272 63.494 63.850 112.052 114.602 111.812 111.844 112.176 129.685 130.935 132.065 133.835 134.275 220.510 48.680 50.824 48.642 48.342 48.334 66.181 67.575 68.465 68.685 68.697 156.944 213.270 215.632 213.062 214.690 149.076 152.360 149.568 150.840 height [cm] volume [cm3] 4.1 4.0 4.0 3.9 4.0 3.9 3.8 4.0 3.9 3.8 3.8 3.7 3.7 3.7 3.7 153.23 149.50 149.50 145.76 149.50 145.76 142.02 149.50 145.76 142.02 142.02 138.28 138.28 138.28 138.28 height [cm] volume [cm3] 3.7 3.5 3.5 3.7 3.7 3.5 3.9 3.9 3.8 4.0 138.28 130.81 130.81 138.28 138.28 130.81 145.76 145.76 142.02 149.50 145.76 149.50 145.76 149.50 149.50 149.50 149.50 156.97 TABLE 34: Raw data for Kraft mill sludge-soil mixtures; (n=3) sample Kraft mill/so I 10:40; 1 Kraft mill/so I 10:40; 2 Kraft mill/so I 10:40; 3 Kraft mill/so I 20:30; 1 Kraft mill/so I 20:30; 2 Kraft mill/so I 20:30; 3 Kraft mill/so I 25:25: 1 Kraft mill/so I 25:25: 2 Kraft mill/so 125 :2 5:3 Kraft mill/so 130:20; 1 Kraft mill/so I 30:20; 2 Kraft mill/so I 30:20; 3 Kraft mill/so 140:10; 1 Kraft mill/so I 40:10; 2 Kraft mill/so 140:10; 3 Kraft mill orig. blend 1 Kraft mill orig. blend 2 Kraft mill orig. blend 3 column empty column&sludge mass wet [g] [g] [g] 63.918 63.586 63.446 63.282 63.728 63.156 63.392 63.812 63.346 64.342 63.234 63.370 63.798 63.210 63.324 64.918 64.788 63.712 142.585 135.540 138.380 113.336 114.504 113.050 113.322 114.260 113.900 114.702 112.806 113.458 107.488 109.148 107.194 104.416 105.374 105.808 78.667 71.954 74.934 50.054 50.776 49.894 49.930 50.448 50.554 50.360 49.572 50.088 43.690 45.938 43.870 39.498 40.586 42.096 3.9 4.0 3.9 4.0 4.0 4.0 4.0 4.2 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric water holding capacity TABLE 35: Raw data for BCTM P sludge-soil mixtures; (n=3) sample BCTMP/so I 10:40; 1 BCTMP/so I 10:40; 2 BCTMP/so I 10:40; 3 BCTMP/so I 20:30; 1 BCTMP/so I 20:30; 2 BCTMP/so I 20:30; 3 BCTMP/so I 25:25; 1 BCTMP/so I 25:25; 2 BCTMP/so I 25:25; 3 BCTMP/so I 30:20; 1 BCTMP/so I 30:20; 2 BCTMP/so I 30:20; 3 BCTMP/so 140:10; 1 BCTMP/so 140:10; 2 BCTMP/so 140:10; 3 BCTM P orig. blend 1 BCTM P orig. blend 2 BCTM P orig. blend 3 column empty column&sludge mass wet [g] [g] [g] 63.328 63.938 62.900 63.682 63.786 63.854 64.598 65.464 63.556 65.934 64.078 63.802 63.920 63.558 63.398 63.378 63.774 166.365 165.980 163.510 138.655 139.030 138.620 135.750 145.355 133.525 135.920 144.625 139.425 130.700 130.330 131.435 116.058 122.815 127.46 103.037 102.042 100.610 74.973 75.244 74.766 71.152 79.891 69.969 69.986 80.547 75.623 66.780 66.772 63.192 68.037 52.680 59.041 64.268 height [cm] volume [cm3] 3.8 3.5 3.5 3.5 3.5 3.4 3.8 3.9 3.5 4.0 4.1 3.9 3.9 3.9 3.9 3.9 4.0 4.1 142.02 130.81 130.81 130.81 130.81 127.07 142.02 145.76 130.81 149.50 153.23 145.76 145.76 145.76 145.76 145.76 149.50 153.23 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric moisture content TABLE 36: Total dry sample mass and Db for sludge and soil samples (Volume for Db calculation as determined in table 33) sample Kraft mill 1a Kraft mill 1b Kraft mill 2a Kraft mill 2b Kraft mill 3a Kraft mill 3b Kraft mill 4a Kraft mill 4b Kraft mill 5a Kraft mill 5b BCTM P 1a BCTM P 1b BCTM P 2a BCTM P 2b BCTM P 3a BCTM P 3b BCTM P 4a BCTM P 4b BCTM P 5a BCTM P 5b Soil 1a Soil 1b Soil 2a Soil 2b Soil 3a Soil 3b Soil 4a Soil 4b Soil 5a Soil 5b Db average stdev sludge wet sum wet sludge dry sum dry total mass [g/cm3] dry [g] (n=5) [g] [g] [g] [g] 12.231 15.277 15.977 18.522 15.840 19.057 19.384 17.033 20.634 20.293 10.204 9.250 9.501 10.073 12.813 11.749 12.570 12.004 13.339 12.026 28.893 25.484 25.206 27.750 26.399 25.082 31.167 28.342 24.417 25.018 27.508 34.499 34.897 36.417 40.927 19.454 19.574 24.562 24.574 25.365 54.377 52.956 51.481 59.509 49.435 2.122 2.490 2.666 3.087 2.610 3.189 2.999 2.873 3.280 3.207 2.096 1.929 2.046 2.152 2.618 2.390 2.533 2.412 2.525 2.271 21.630 19.219 19.302 21.493 19.876 18.782 23.398 21.023 18.660 19.324 4.612 8.162 0.053 5.753 8.475 0.057 5.799 8.083 0.054 5.872 7.795 0.053 6.487 7.661 0.051 4.025 13.69 0.094 4.198 14.49 0.102 5.008 13.96 0.093 4.945 13.82 0.095 4.796 12.99 0.091 40.849 117.90 0.830 40.795 114.84 0.830 38.658 114.41 0.827 44.421 111.65 0.807 37.984 115.90 0.838 ± se 0.054 0.002 0.001 0.095 0.004 0.002 0.827 0.012 0.005 98 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric moisture content TABLE 37: Total sample mass dry and Db for Kraft mill sludge-soil mixtures (Volume for Db calculation as determined in table 34) sludge wet sum wet sludge dry sum dry total mass Db average stdev [g/cm3] (n=3) dry [g] [g] [g] [g] [g] sample Kraft m ll/soil 10:40 Kraft m ll/soil 10:40 Kraft m ll/soil 10:40 Kraft m ll/soil 10:40 Kraft m ll/soil 10:40 Kraft m ll/soil 10:40 Kraft m ll/soil 20:30 Kraft m ll/soil 20:30 Kraft m ll/soil 20:30 Kraft m ll/soil 20:30 Kraft m ll/soil 20:30 Kraft m ll/soil 20:30 Kraft m ll/soil 25:25 Kraft m ll/soil 25:25 Kraft m ll/soil 25:25 Kraft m ll/soil 25:25 Kraft m ll/soil 25:25 Kraft m ll/soil 25:25 Kraft m ll/soil 30:20 Kraft m ll/soil 30:20 Kraft m ll/soil 30:20 Kraft m ll/soil 30:20 Kraft m ll/soil 30:20 Kraft m ll/soil 30:20 Kraft m ll/soil 40:10 Kraft m ll/soil 40:10 Kraft m ll/soil 40:10 Kraft m ll/soil 40:10 Kraft m ll/soil 40:10 Kraft m ll/soil 40:10 1a 1b 2a 2b 3a 3b 1a 1b 2a 2b 3a 3b 1a 1b 2a 2b 3a 3b 1a 1b 2a 2b 3a 3b 1a 1b 2a 2b 3a 3b 14.646 13.169 11.711 11.748 9.704 10.173 10.303 10.388 9.534 9.287 9.785 12.003 7.882 7.268 10.499 7.744 9.116 8.362 9.119 9.167 11.718 11.099 13.756 10.054 11.513 11.177 13.983 14.085 10.143 9.684 27.815 23.459 19.877 20.691 18.821 21.788 15.150 18.243 17.478 18.286 22.817 23.810 22.690 28.068 19.827 9.024 7.908 7.063 7.152 5.262 6.871 3.735 4 .099 3.900 3.684 4.986 5.643 3.319 2.518 4.972 2.856 3.970 3.561 2.763 2.715 4.067 2.795 3.853 2.523 2.395 1.901 2.427 2.374 2.031 1.778 16.932 47.89 0.346 14.215 43.60 0.333 12.133 45.74 0.350 7.834 18.95 0.137 7.584 20.46 0.148 10.629 24.34 0.186 5.837 19.24 0.132 7.828 21.65 0.149 7.531 21.78 0.153 5.478 15.09 0.101 6.862 14.91 0.102 6.376 13.41 0.090 4.296 8.27 0.057 4.801 7.86 0.053 3.809 8.43 0.056 ± se 0.343 0.009 0.005 0.157 0.026 0.015 0.145 0.011 0.006 0.098 0.007 0.004 0.055 0.002 0.001 99 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric moisture content average stdev Db sludge wet sum wet sludge dry sum dry total mass dry [g] [g/cm3] (n=3) [g] [g] [g] [g] sample Kraft mil orig.blend 1a Kraft mill orig.blend 1 b Kraft mill orig.blend 2a Kraft mill orig.blend 2b Kraft mill orig.blend 3a Kraft mill orig.blend 3b 10.182 12.963 11.025 10.993 13.830 12.810 23.145 22.018 1.262 1.541 1.352 1.324 1.753 1.643 2.803 4.78 0.032 2.676 4.93 0.033 3.396 5.37 0.034 0.001 0.001 average stdev Db sludge wet sum wet sludge dry sum dry total mass [g/cm3] dry [g] (n=3) [g] [g] [g] [g] ± se 26.640 0.033 ± se TABLE 38: Total sample mass dry and Db for BCTM P sludge-soil mixtures (Volume for Db calculation as determined in table 35) sample BCTMP/soil 10:40 BCTMP/soil 10:40 BCTMP/soil 10:40 BCTMP/soil 10:40 BCTMP/soil 10:40 BCTMP/soil 10:40 BCTMP/soil 20:30 BCTMP/soil 20:30 BCTMP/soil 20:30 BCTMP/soil 20:30 BCTMP/soil 20:30 BCTMP/soil 20:30 BCTMP/soil 25:25 BCTMP/soil 25:25 BCTMP/soil 25:25 BCTMP/soil 25:25 BCTMP/soil 25:25 BCTMP/soil 25:25 1a 1b 2a 2b 3a 3b 1a 1b 2a 2b 3a 3b 1a 1b 2a 2b 3a 3b 9.947 10.240 11.705 11.871 11.513 10.754 12.047 11.693 10.084 9.368 12.696 11.169 10.508 8.815 10.658 9.835 9.845 7.904 20.187 23.576 22.267 23.740 19.452 23.865 19.323 20.493 17.749 6.779 6.658 7.620 7.675 7.636 7.082 6.165 5.788 5.512 4.743 7.640 6.191 5.015 4.010 5.212 4.719 5.120 3.762 13.437 68.58 0.483 15.295 66.20 0.506 14.718 66.50 0.508 11.953 37.75 0.289 10.255 39.67 0.303 13.831 43.33 0.341 9.025 33.23 0.234 9.931 38.72 0.266 8.882 35.01 0.268 0.499 0.014 0.008 0.311 0.027 0.016 0.256 0.019 0.011 100 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric moisture content sample BCTMP/soil 30:20; 1a BCTMP/soil 30:20; 1b BCTMP/soil 30:20; 2a BCTMP/soil 30:20; 2b BCTMP/soil 30:20; 3a BCTMP/soil 30:20; 3b BCTMP/soil 40:10; 1a BCTMP/soil 40:10; 1b BCTMP/soil 40:10; 2a BCTMP/soil 40:10; 2b BCTMP/soil 40:10; 3a BCTMP/soil 40:10; 3b B C TM P orig. blend 1a B C TM P orig. blend 1b B C TM P orig. blend 2a B C TM P orig. blend 2b B C TM P orig. blend 3a B C TM P orig. blend 3b average stdev sludge wet sum wet sludge dry sum dry total mass Db [g/cm3] dry [g] (n=3) [g] [g] [g] [g] 12.080 12.124 9.499 9.469 6.927 11.770 7.221 8.829 8.658 7.903 8.435 7.621 7.686 8.224 8.376 7.954 7.322 8.484 24.204 18.968 18.697 16.050 16.561 16.056 15.910 16.330 15.806 4.464 4.300 3.236 3.318 2.754 4.159 1.907 2.284 2.121 1.894 2.290 1.882 1.260 1.353 1.329 1.263 1.167 1.372 8.764 25.34 0.170 6.554 27.83 0.182 6.913 27.96 0.192 4.191 17.44 0.120 4.015 16.19 0.111 4.172 17.68 0.121 2.613 8.65 0.059 2.592 9.37 0.063 2.539 10.32 0.067 ± se 0.181 0.011 0.006 0.117 0.005 0.003 0.063 0.004 0.002 101 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric water holding capacity TABLE 39: Raw data fo r K raft mill sludge-soil layer system s and Db; 1, 2, and 3 layer syste m s (n=3) sample <1) > G) >s _C0 > s— CD >. TO CM d) >. 03 00 sludge (1/1) soil (1/1) sludge (2/1) soil (2/1) sludge (3/1) soil (3/1) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (2/1) soil (2/1) sludge (2/2) soil (2/2) sludge (3/1) soil (3/1) sludge (3/2) soil (3/2) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (1/3) soil (1/3) sludge (2/1) soil (2/1) sludge (2/2) soil (2/2) sludge (2/3) soil (2/3) sludge (3/1) soil (3/1) sludge (3/2) soil (3/2) sludge (3/3) soil (3/3) column empty column&sampie mass wet layer [g] [g] [g] [g] 64.114 64.114 63.998 63.998 63.140 63.140 63.192 63.192 63.192 63.192 63.870 63.870 63.870 63.870 63.122 63.122 63.122 63.122 63.138 63.138 63.138 63.138 63.138 63.138 63.752 63.752 63.752 63.752 63.752 63.752 63.150 63.150 63.150 63.150 63.150 63.150 117.084 242.620 115.350 250.960 112.048 255.955 92.962 147.850 189.470 242.250 93.750 147.685 189.360 252.450 94.596 147.395 182.170 245.495 88.202 134.420 152.660 193.680 220.640 260.345 85.024 132.365 151.545 193.555 220.39 258.470 90.876 133.010 154.745 197.285 224.110 263.690 52.970 178.506 51.352 186.962 48.908 192.815 29.770 84.658 126.278 179.058 29.880 83.815 125.490 188.580 31.474 84.273 119.048 182.373 25.064 71.282 89.522 130.542 157.502 197.207 21.272 68.613 87.793 129.803 156.638 194.718 27.726 69.860 91.595 134.135 160.960 200.540 52.970 125.536 51.352 135.610 48.908 143.907 29.770 54.888 41.620 52.780 29.880 53.935 41.675 63.090 31.474 52.799 34.775 63.325 25.064 46.218 18.240 41.020 26.960 39.705 21.272 47.341 19.180 42.010 26.835 38.080 27.726 42.134 21.735 42.540 26.825 39.580 height volume mass dry Db [g/cm3 ] [cm] [cm3] [g] 3.1 2.7 3.0 2.9 3.0 3.0 1.5 1.5 1.7 1.3 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.1 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.2 1.0 0.9 1.0 1.1 1.0 115.86 100.91 112.12 108.38 112.12 112.12 56.06 56.06 63.54 48.59 56.06 56.06 56.06 56.06 56.06 56.06 56.06 56.06 41.11 37.37 37.37 37.37 37.37 37.37 37.37 37.37 37.37 37.37 37.37 37.37 44.85 37.37 33.64 37.37 41.11 37.37 10.94 88.81 10.78 96.68 10.36 102.92 4.73 38.81 7.60 37.68 5.59 38.43 7.59 45.13 5.95 37.22 6.96 45.07 5.05 32.74 4.00 28.87 5.67 27.76 4.48 33.29 4.10 29.58 4.69 27.22 5.42 29.26 4.92 30.08 5.12 28.18 0.0944 0.8800 0.0961 0.8920 0.0924 0.9180 0.0844 0.6923 0.1197 0.7756 0.0998 0.6855 0.1354 0.8051 0.1061 0.6638 0.1242 0.8039 0.1230 0.8761 0.1071 0.7725 0.1518 0.7429 0.1200 0.8908 0.1096 0.7916 0.1256 0.7282 0.1207 0.7829 0.1463 0.8048 0.1245 0.7540 103 TABLE 41: Db and statistics for Kraft mill sludge-soil layer systems; 1, 2, and 3 layer systems (n=3) sample 1_ D > > eg a) >* J5 CO sludge ( 1 / 1 ) sludge (2/1) sludge (3/1) soil (1/1) soil (2/1) soil (3/1) sludge (1/1) sludge (2/1) sludge (3/1) soil (1/1) soil (2/1) soil (3/1) sludge (1/2) sludge (2/2) sludge (3/2) soil (1/2) soil (2/2) soil (3/2) sludge (1/1) sludge (2/1) sludge (3/1) soil (1/1) soil (2/1) soil (3/1) sludge (1/2) sludge (2/2) sludge (3/2) soil (1/2) soil (2/2) soil (3/2) sludge (1/3) sludge (2/3) sludge (3/3) soil (1/3) soil (2/3) soil (3/3) Db [g/cm3] 0.0741 0.1116 0.0648 0.9287 0.8844 0.9341 0.0591 0.0646 0.0606 0.9371 0.7745 0.8082 0.0655 0.0789 0.0743 1.0289 0.8295 0.9656 0.0700 0.0878 0.0723 0.6582 0.6868 0.6859 0.1386 0.1035 0.1001 0.8256 0.7632 0.8423 0.0995 0.0976 0.0887 1.1793 1.0410 0.8382 average stdev TABLE 42: Db and statistics for BCTMP sludge-soil layer systems; 1, 2, and 3 layer systems (n=3) ± se sample Db [g/cm3] sludge (1/1) sludge (2/1) sludge (3/1) soil (1/1) soil (2/1) soil (3/1) sludge (1/1) sludge (2/1) sludge (3/1) soil (1/1) soil (2/1) soil (3/1) sludge (1/2) sludge (2/2) sludge (3/2) soil (1/2) soil (2/2) soil (3/2) sludge (1/1) sludge (2/1) sludge (3/1) soil (1/1) soil (2/1) soil (3/1) sludge (1/2) sludge (2/2) sludge (3/2) soil (1/2) soil (2/2) soil (3/2) sludge (1/3) sludge (2/3) sludge (3/3) soil (1/3) soil (2/3) soil (3/3) 0.0944 0.0961 0.0924 0.8800 0.8920 0.9180 0.0844 0.0998 0.1061 0.6923 0.6855 0.6638 0.1197 0.1354 0.1242 0.7756 0.8051 0.8039 0.1230 0.1200 0.1207 0.8761 0.8908 0.7829 0.1071 0.1096 0.1463 0.7725 0.7916 0.8048 0.1518 0.1256 0.1245 0.7429 0.7282 0.7540 (n=3) 1_ 0.084 0.025 0.014 CD >* CD 0.916 0.027 0.016 0.061 0.003 0.002 0.840 0.086 0.050 0.073 0.007 0.004 0.941 0.102 0.059 0.077 0.010 0.006 0.677 0.016 0.009 0.114 0.021 0.012 2 layer Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric water holding capacity CD TO CO 0.810 0.042 0.024 0.095 0.006 0.003 1.019 0.172 0.099 average (ii=3) stdev ± se 0.094 0.002 0.001 0.897 0.019 0.011 0.097 0.011 0.006 0.681 0.015 0.009 0.126 0.008 0.005 0.795 0.017 0.010 0.121 0.002 0.001 0.850 0.059 0.034 0.121 0.022 0.013 0.790 0.016 0.009 0.134 0.015 0.009 0.742 0.013 0.007 104 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric water holding capacity P a rt B : Gravimetric moisture content after soaking and draining = WHCg TABLE 43: W HCg of sludge and soil samples; (n = 10) sample Kraft mill 1a Kraft mill 1b Kraft mill 2a Kraft mill 2b Kraft mill 3a Kraft mill 3b Kraft mill 4a Kraft mill 4b Kraft mill 5a Kraft mill 5b BCTMP 1a BCTMP 1b BCTMP 2a BCTMP 2b BCTMP 3a BCTMP 3b BCTMP 4a BCTMP 4b BCTMP 5a BCTMP 5b Soil 1a Soil 1b Soil 2a Soil 2b Soil 3a Soil 3b Soil 4a Soil 4b Soil 5a Soil 5b container cont. & sludge wet sludge wet cont. & sludge dry sludge dry WHCg average stdev ± se [g] [g] [g] [g] [g] 3.142 3.162 3.152 3.128 3.132 3.147 3.130 3.161 3.759 3.148 3.146 3.166 3.154 3.130 3.133 3.148 3.132 3.164 3.761 3.151 3.121 3.152 3.148 3.142 3.170 3.144 3.136 3.132 3.143 3.144 15.373 18.439 19.129 21.650 18.972 22.204 22.514 20.194 24.393 23.441 13.350 12.416 12.655 13.203 15.946 14.897 15.702 15.168 17.100 15.177 32.014 28.636 28.354 30.892 29.569 28.226 34.303 31.474 27.560 28.162 12.231 15.277 15.977 18.522 15.840 19.057 19.384 17.033 20.634 20.293 10.204 9.250 9.501 10.073 12.813 11.749 12.570 12.004 13.339 12.026 28.893 25.484 25.206 27.750 26.399 25.082 31.167 28.342 24.417 25.018 5.264 5.652 5.818 6.215 5.742 6.336 6.129 6.034 7.039 6.355 5.242 5.095 5.200 5.282 5.751 5.538 5.665 5.576 6.286 5.422 24.751 22.371 22.450 24.635 23.046 21.926 26.534 24.155 21.803 22.468 2.122 2.490 2.666 3.087 2.610 3.189 2.999 2.873 3.280 3.207 2.096 1.929 2.046 2.152 2.618 2.390 2.533 2.412 2.525 2.271 21.630 19.219 19.302 21.493 19.876 18.782 23.398 21.023 18.660 19.324 [%] 476 514 499 500 507 498 546 493 529 533 387 380 364 368 389 392 396 398 428 430 34 33 31 29 33 34 33 35 31 29 [%] 509 21.12 6.68 393 21.83 6.90 32 1.92 0.61 105 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric water holding capacity TABLE 44: W H C g of Kraft mill sludge-soil mixtures; (n = 6) sample Kraft mill/so I 10:40 1a Kraft mill/so I 10:40 1b Kraft mill/so I 10:40 2a Kraft mill/so I 10:40 2b Kraft mill/so I 10:40 3a Kraft mill/so I 10:40 3b Kraft mill/so I 20:30 1a Kraft mill/so I 20:30 1b Kraft mill/so I 20:30 2a Kraft mill/so I 20:30 2b Kraft mill/so I 20:30 3a Kraft mill/so I 20:30 3b Kraft mill/so I 25:25 1a Kraft mill/so I 25:25 1b Kraft mill/so I 25:25 2a Kraft mill/so I 25:25 2b Kraft mill/so I 25:25 3a Kraft mill/so I 25:25 3b Kraft mill/so I 30:20 1a Kraft mill/so I 30:20 1b Kraft mill/so I 30:20 2a Kraft mill/so I 30:20 2b Kraft mill/so I 30:20 3a Kraft mill/so I 30:20 3b Kraft mill/so 140:10 1a Kraft mill/so 140:10 1b Kraft mill/so 140:10 2a Kraft mill/so 140:10 2b Kraft mill/so 140:10 3a Kraft mill/so 140:10 3b Kraft mil orig.blend 1a Kraft mill orig.blend 1b Kraft mill orig.blend 2a Kraft mill orig.blend 2b Kraft mill orig.blend 3a Kraft mill orig.blend 3b container cont. & sludge wet sludge wet cont. & sludge dry sludge dry WHCg average stdev ± se [g] [g] [g] [g] [g] 3.130 3.161 3.759 3.147 3.121 3.155 3.142 3.161 3.152 3.127 3.132 3.147 3.141 3.161 3.152 3.128 3.132 3.144 3.169 3.170 3.220 3.171 3.222 3.186 3.133 3.166 3.772 3.156 3.212 3.177 3.133 3.148 3.154 3.160 3.145 3.165 17.776 16.330 15.470 14.895 12.825 13.328 13.445 13.549 12.686 12.414 12.917 15.150 11.023 10.429 13.651 10.872 12.248 11.506 12.288 12.337 14.938 14.270 16.978 13.240 14.646 14.343 17.755 17.241 13.355 12.861 13.315 16.111 14.179 14.153 16.975 15.975 14.646 13.169 11.711 11.748 9.704 10.173 10.303 10.388 9.534 9.287 9.785 12.003 7.882 7.268 10.499 7.744 9.116 8.362 9.119 9.167 11.718 11.099 13.756 10.054 11.513 11.177 13.983 14.085 10.143 9.684 10.182 12.963 11.025 10.993 13.830 12.810 12.154 11.069 10.822 10.299 8.383 10.026 6.877 7.260 7.052 6.811 8.118 8.790 6.460 5.679 8.124 5.984 7.102 6.705 5.932 5.885 7.287 5.966 7.075 5.709 5.528 5.067 6.199 5.530 5.243 4.955 4.395 4.689 4.506 4.484 4.898 4.808 9.024 7.908 7.063 7.152 5.262 6.871 3.735 4.099 3.900 3.684 4.986 5.643 3.319 2.518 4.972 2.856 3.970 3.561 2.763 2.715 4.067 2.795 3.853 2.523 2.395 1.901 2.427 2.374 2.031 1.778 1.262 1.541 1.352 1.324 1.753 1.643 [%] 62 67 66 64 84 48 176 153 144 152 96 113 137 189 111 171 130 135 230 238 188 297 257 298 381 488 476 493 399 445 707 741 715 730 689 680 [%] 65 11.62 4.74 139 29.28 11.95 145 28.74 11.73 251 42.40 17.31 447 47.61 19.44 710 23.61 9.64 106 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric water holding capacity TABLE 45: W H C g of BCTMP sludge-soil mixtures; (n = 6) sample BCTMP/so I 10:40; 1a BCTMP/so I 10:40; 1b BCTMP/so I 10:40; 2a BCTMP/so I 10:40; 2b BCTMP/so I 10:40; 3a BCTMP/so I 10:40; 3b BCTMP/so 120:30; 1a BCTMP/so I 20:30; 1b BCTMP/so I 20:30; 2a BCTMP/so I 20:30; 2b BCTMP/so I 20:30; 3a BCTMP/so I 20:30; 3b BCTMP/so I 25:25; 1a BCTMP/so 125:25; 1b BCTMP/so I 25:25; 2a BCTMP/so I 25:25; 2b BCTMP/so I 25:25; 3a BCTMP/so I 25:25; 3b BCTMP/so I 30:20; 1a BCTMP/so I 30:20; 1b BCTMP/so I 30:20; 2a BCTMP/so I 30:20; 2b BCTMP/so I 30:20; 3a BCTMP/so I 30:20; 3b BCTMP/so 140:10; 1a BCTMP/so 140:10; 1b BCTMP/so I 40:10; 2a BCTMP/so 140:10; 2b BCTMP/so 140:10; 3a BCTMP/so 140:10; 3b BCTMP orig. blend 1a BCTMP orig. blend 1b BCTMP orig. blend 2a BCTMP orig. blend 2b BCTMP orig. blend 3a BCTMP orig. blend 3b container cont. & sludge wet sludge wet cont. & sludge dry sludge dry WHCg average stdev ± se [g] [g] [g] [g] [g] 3.142 3.162 3.151 3.128 3.132 3.144 3.131 3.162 3.757 3.147 3.120 3.154 3.131 3.162 3.757 3.147 3.120 3.153 3.145 3.144 3.171 3.145 3.136 3.131 3.141 3.162 3.757 3.147 3.121 3.154 3.142 3.163 3.152 3.128 3.133 3.144 13.089 13.402 14.856 14.999 14.645 13.898 15.178 14.855 13.841 12.515 15.816 14.323 13.639 11.977 14.415 12.982 12.965 11.057 15.225 15.268 12.670 12.614 10.063 14.901 10.362 11.991 12.415 11.050 11.556 10.775 10.828 11.387 11.528 11.082 10.455 11.628 9.947 10.240 11.705 11.871 11.513 10.754 12.047 11.693 10.084 9.368 12.696 11.169 10.508 8.815 10.658 9.835 9.845 7.904 12.080 12.124 9.499 9.469 6.927 11.770 7.221 8.829 8.658 7.903 8.435 7.621 7.686 8.224 8.376 7.954 7.322 8.484 9.921 9.820 10.771 10.803 10.768 10.226 9.296 8.950 9.269 7.890 10.760 9.345 8.146 7.172 8.969 7.866 8.240 6.915 7.609 7.444 6.407 6.463 5.890 7.290 5.048 5.446 5.878 5.041 5.411 5.036 4.402 4.516 4.481 4.391 4.300 4.516 6.779 6.658 7.620 7.675 7.636 7.082 6.165 5.788 5.512 4.743 7.640 6.191 5.015 4.010 5.212 4.719 5.120 3.762 4.464 4.300 3.236 3.318 2.754 4.159 1.907 2.284 2.121 1.894 2.290 1.882 1.260 1.353 1.329 1.263 1.167 1.372 [%] 47 54 54 55 51 52 95 102 83 98 66 80 110 120 104 108 92 110 171 182 194 185 152 183 279 287 308 317 268 305 510 508 530 530 527 518 [%] 52 2.90 1.19 87 13.41 5.48 107 8.99 3.67 178 14.78 6.03 294 19.04 7.77 521 10.04 4.10 107 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric water holding capacityy TABLE 46: W H C g of Kraft mill sludge-soil layer systems; 1,2, and 3 layer systems (n = 6) sample sludge (1/1/a) sludge (1/1 /b) sludge (2/1/a) L_ sludge (2/1/b) CD 03 sludge (3/1 la) T— sludge (3/1/b) E soil (1/1/a) soil (1/1 lb) CD soil (2/1/a) soil (2/1/b) soil (3/1/a) soil (3/1/b) sludge (1/1/a) sludge (1/1/b) sludge (2/1/a) sludge (2/1/b) sludge (3/1/a) sludge (3/1/b) sludge (1/2/a) sludge (1/2/b) sludge (2/2/a) CO L_ o sludge (2/2/b) JD sludge (3/2/a) CNJ sludge (3/2/b) soil (1/1/a) E soil (1/1/b) CD L_ soil (2/1/a) soil (2/1/b) soil (3/1/a) soil (3/1/b) soil (1/2/a) soil (1/2/b) soil (2/2/a) soil (2/2/b) soil (3/2/a) soil (3/2/b) container cont. & sludge wet sludge wet cont. & sludge dry sludge dry [g] [g] [g] [g] [g] 3.154 3.129 3.132 3.162 3.120 3.153 3.143 3.164 3.132 3.144 3.756 3.146 3.133 3.161 3.759 3.164 3.146 3.134 3.133 3.124 3.140 3.133 3.146 3.145 3.142 3.180 3.155 3.158 3.147 3.155 3.164 3.175 3.146 3.158 3.186 3.153 10.202 10.095 10.977 10.31 10.161 10.17 7.048 6.966 7.845 7.148 7.041 7.017 15.758 16.985 16.066 17.081 17.006 21.281 5.133 4.465 4.320 4.668 4.446 4.701 3.650 3.888 4.550 4.997 5.005 5.078 9.820 10.645 8.249 7.397 9.940 10.697 10.525 10.272 8.908 9.058 10.212 10.315 4.744 4.811 6.285 4.839 4.477 4.456 14.469 15.596 14.571 15.279 15.969 18.364 4.080 3.908 4.533 3.977 3.822 3.924 3.781 3.824 3.871 3.944 3.975 3.99 10.381 10.953 9.082 8.482 10.333 10.999 10.736 10.620 9.532 9.655 10.513 10.562 1.590 1.682 3.153 1.677 1.357 1.303 11.326 12.432 11.439 12.135 12.213 15.218 0.947 0.747 0.774 0.813 0.676 0.700 0.648 0.700 0.731 0.811 0.829 0.845 7.239 7.773 5.927 5.324 7.186 7.844 7.572 7.445 6.386 6.497 7.327 7.409 18.901 20.149 19.198 20.225 20.762 24.427 8.266 7.626 8.079 7.832 7.592 7.835 6.783 7.012 7.69 8.13 8.151 8.223 12.962 13.825 11.404 10.555 13.087 13.852 13.689 13.447 12.054 12.216 13.398 13.468 WHCg [%] 343 314 149 326 419 439 39 37 40 41 39 40 442 498 458 474 558 495 463 455 522 516 504 501 36 37 39 39 38 36 39 38 39 39 39 39 average stdev ± se [%] 332 103 42.0 39 1.48 0.60 487 40.5 16.5 494 27.8 11.4 38 1.45 0.59 39 0.57 0.23 108 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric water holding capacityy sample tn 0 ro n I ro L_ sludge (1/1/a) sludge (1/1/b) sludge (2/1/a) sludge (2/1/b) sludge (3/1/a) sludge (3/1/b) sludge (1/2/a) sludge (1/2/b) sludge (2/2/a) sludge (2/2/b) sludge (3/2/a) sludge (3/2/b) sludge (1/3/a) sludge (1/3/b) sludge (2/3/a) sludge (2/3/b) sludge (3/3/a) sludge (3/3/b) soil (1/1/a) soil (1/1/b) soil (2/1/a) soil (2/1/b) soil (3/1/a) soil (3/1/b) soil (1/2/a) soil (1/2/b) soil (2/2/a) soil (2/2/b) soil (3/2/a) soil (3/2/b) soil (1/3/a) soil (1/3/b) soil (2/3/a) soil (2/3/b) soil (3/3/a) soil (3/3/b) container cont. & sludge wet sludge wet cont. & sludge dry sludge dry [g] [g] [g] [g] [g] 3.133 3.163 3.139 3.133 3.165 3.152 3.129 3.120 3.142 3.130 3.148 3.150 3.757 3.163 3.141 3.142 3.108 3.146 3.132 3.147 3.136 3.150 3.145 3.128 3.151 3.153 3.134 3.142 3.148 3.142 3.141 3.142 3.170 3.144 3.150 3.137 6.452 6.617 8.747 8.566 11.057 10.783 8.558 8.538 9.568 8.998 7.642 7.334 7.433 7.258 8.485 8.483 7.738 8.193 9.768 7.819 11.632 10.567 8.649 9.431 9.436 9.737 13.604 3.319 3.454 5.608 5.433 7.892 7.631 5.429 5.418 6.426 5.868 4.494 4.184 3.676 4.095 5.344 5.341 4.630 5.047 6.636 4.672 8.496 7.417 5.504 6.303 6.285 6.584 10.470 9.588 6.033 6.207 7.306 7.445 8.710 8.896 5.948 6.045 3.730 3.762 4.108 4.053 4.444 4.424 4.406 4.339 4.404 4.269 4.024 4.040 4.324 4.080 4.175 4.150 4.018 4.084 7.945 6.555 9.363 8.669 7.201 7.842 7.790 7.972 10.667 10.041 7.470 7.613 8.448 8.566 9.404 9.549 7.444 7.508 0.597 0.599 0.969 0.920 1.279 1.272 1.277 1.219 1.262 1.139 0.876 0.890 0.567 0.917 1.034 1.008 0.910 0.938 4.813 3.408 6.227 12.730 9.181 9.349 10.447 10.587 11.880 12.040 9.098 9.182 5.519 4.056 4.714 4.639 4.819 7.533 6.899 4.322 4.471 5.307 5.424 6.234 6.405 4.294 4.371 WHCg [%] 456 477 479 491 517 500 325 344 409 415 413 370 548 347 417 430 409 438 38 37 36 34 36 34 35 37 39 39 40 39 38 37 40 39 39 38 average stdev ± se [%] 486 21.1 8.60 380 38.9 15.9 431 65.8 26.9 36 1.60 0.65 38 1.63 0.67 38 0.88 0.36 109 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric water holding capacityy TABLE 47: W H C g of B C TM P sludge-soil layer systems; 1, 2, and 3 layer systems (n = 6) sample sludge (1/1/a) sludge (1/1/b) sludge (2/1 /a) sludge (2/1/b) sludge (3/1/a) sludge (3/1/b) Q. soil (1/1/a) I— soil (1/1/b) o CQ soil (2/1/a) soil (2/1/b) soil (3/1/a) soil (3/1/b) sludge (1/1/a) sludge (1/1/b) sludge (2/1/a) sludge (2/1/b) sludge (3/1/a) sludge (3/1/b) sludge (1/2/a) sludge (1/2/b) sludge (2/2/a) V/J i_ sludge (2/2/b) CD >% ro sludge (3/2/a) CM sludge (3/2/b) CL soil (1/1/a) I— soil (1/1/b) o 00 soil (2/1/a) soil (2/1/b) soil (3/1/a) soil (3/1/b) soil (1/2/a) soil (1/2/b) soil (2/2/a) soil (2/2/b) soil (3/2/a) soil (3/2/b) container cont. & sludge wet sludge wet cont. & sludge dry sludge dry [g] [g] [g] [g] [g] 3.152 3.127 3.129 3.161 3.120 3.153 3.143 3.163 3.131 3.143 3.756 3.146 3.131 3.161 3.758 3.164 3.141 3.131 3.127 3.120 3.139 3.131 3.143 3.144 3.130 3.147 3.142 3.144 10.210 10.111 10.174 10.571 10.068 10.265 18.085 19.77 21.906 19.758 22.243 20.976 7.340 6.976 8.359 8.501 8.240 8.616 10.892 11.821 9.421 10.932 9.814 10.084 9.771 9.83 10.137 9.388 3.135 3.145 3.155 3.153 3.135 3.150 3.170 3.144 10.891 11.256 9.939 9.855 10.178 9.717 10.601 10.299 7.058 6.984 7.045 7.410 6.948 7.112 14.942 16.607 18.775 16.615 18.487 17.830 4.209 3.815 4.601 5.337 5.099 5.485 7.765 8.701 6.282 7.801 6.671 6.940 6.641 6.683 6.995 6.244 7.756 8.111 6.784 6.702 7.043 6.567 7.431 7.155 4.646 4.533 4.603 4.721 4.594 4.658 13.630 14.994 16.449 15.055 16.954 15.922 3.929 3.638 4.615 4.167 4.109 4.164 4.488 4.767 4.216 4.619 4.498 4.515 7.808 7.890 8.147 7.572 8.662 8.802 7.972 7.964 8.177 7.844 8.529 8.166 1.494 1.406 1.474 1.560 1.474 1.505 10.487 11.831 13.318 11.912 13.198 12.776 0.798 0.477 0.857 1.003 0.968 1.033 1.361 1.647 1.077 1.488 1.355 1.371 4.678 4.743 5.005 4.428 5.527 5.657 4.817 4.811 5.042 4.694 5.359 5.022 WHCg [%] 372 397 378 375 371 373 42 40 41 39 40 40 427 700 437 432 427 431 471 428 483 424 392 406 42 41 40 41 40 43 41 39 40 40 39 42 average stdev ± se [%] 378 9.63 3.93 40 1.12 0.46 476 110 44.9 434 35.8 14.6 41 1.29 0.53 40 1.35 0.55 110 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix H: Determination of gravimetric water holding capacityy sample sludge (1/1/a) sludge (1/1/b) sludge (2/1/a) sludge (2/1/b) sludge (3/1/a) sludge (3/1/b) sludge (1/2/a) sludge (1/2/b) sludge (2/2/a) sludge (2/2/b) sludge (3/2/a) sludge (3/2/b) sludge (1/3/a) sludge (1/3/b) sludge (2/3/a) iC/5 _ sludge (2/3/b) CD TO sludge (3/3/a) co sludge (3/3/b) Q . soil (1/1/a) 1 — soil (1/1/b) t \ co soil (2/1/a) soil (2/1/b) soil (3/1/a) soil (3/1/b) soil (1/2/a) soil (1/2/b) soil (2/2/a) soil (2/2/b) soil (3/2/a) soil (3/2/b) soil (1/3/a) soil (1/3/b) soil (2/3/a) soil (2/3/b) soil (3/3/a) soil (3/3/b) container cont. & sludge wet sludge wet cont. & sludge dry sludge dry [g] [g] [g] [g] [g] 3.131 3.161 3.140 3.141 3.169 3.155 3.128 3.119 3.140 3.131 3.153 3.155 3.757 3.164 3.143 3.143 3.115 3.140 3.133 3.148 3.135 3.152 3.151 3.132 3.154 3.154 3.135 3.145 3.155 3.147 3.143 3.144 3.170 3.143 3.154 3.153 7.162 7.346 7.105 7.628 9.678 9.175 7.306 6.861 8.554 9.004 9.746 10.748 8.650 7.057 8.346 8.312 9.184 8.618 7.516 7.250 9.039 9.630 6.614 7.533 6.831 6.494 7.697 8.743 7.608 7.818 7.008 7.306 8.021 7.924 7.416 8.390 4.031 4.185 3.965 4.487 6.509 6.020 4.178 3.742 5.414 5.873 6.593 7.593 4.893 3.893 5.203 5.169 6.069 5.478 4.383 4.102 5.904 6.478 3.463 4.401 3.677 3.340 4.562 5.598 4.453 4.671 3.865 4.162 4.851 4.781 4.262 5.237 3.947 4.002 3.981 4.082 4.422 4.349 4.044 3.941 4.416 4.266 4.619 4.901 4.790 3.980 4.051 4.049 4.281 4.178 6.221 6.071 7.291 7.704 5.577 6.167 5.763 5.484 6.321 7.114 6.281 6.472 5.856 6.044 6.652 6.545 6.186 6.884 0.816 0.841 0.841 0.941 1.253 1.194 0.916 0.822 1.276 1.135 1.466 1.746 1.033 0.816 0.908 0.906 1.166 1.038 3.088 2.923 4.156 4.552 2.426 3.035 2.609 2.330 3.186 3.969 3.126 3.325 2.713 2.900 3.482 3.402 3.032 3.731 WHCg [%] 394 398 371 377 419 404 356 355 324 417 350 335 374 377 473 471 420 428 42 40 42 42 43 45 41 43 43 41 42 40 42 44 39 41 41 40 average stdev ± se [%] 394 17.7 7.23 356 32.5 13.2 424 43.19 17.6 42 1.52 0.62 42 1.24 0.51 41 1.55 0.63 111 Reproduced with permission of the copyright owner. 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Appendix I: Pressure Plate Experiment Part A: Moisture retention curves for sludge and soil samples sample height: sample diameter: sample volume: 1.0 cm 6.9 cm 3 7.37 car3 Ah Ad Am 0.02 cm 0.02 cm 0.001 g TABLE 48: Raw data for moisture retention curve of Kraft mill sludge (n=1) cont.&sludge wet sludge wet cont.&sludge dry sludge dry pressure [bar] container [g] [g] [g] [g] [g] 0.1 0.2 0.3 0.4 0.5 0.7 1.0 2.0 5.0 10.0 15.0 3.815 3.816 3.818 3.815 3.815 3.815 3.818 3.818 3.818 3.815 3.816 30.600 24.877 22.025 23.176 20.825 20.616 20.614 19.824 23.734 23.112 23.237 26.785 21.061 18.207 19.361 17.010 16.801 16.796 16.006 19.916 19.297 19.421 8.615 9.060 8.294 8.798 8.314 8.142 8.622 8.468 9.490 9.819 9.739 4.800 5.244 4.476 4.983 4 .499 4.327 4.804 4.650 5.672 6.004 5.923 WHCg [%] 458 302 307 289 278 288 250 244 251 221 228 average stdev se bulk density [g/cmJ] 0.128 0.140 0.120 0.133 0.120 0.116 0.129 0.124 0.152 0.161 0.158 WHCV [%] 58.8 42.3 36.7 38.5 33.5 33.4 32.1 30.4 38.1 35.6 36.1 0 .13 47 0.0159 ± 0.0048 112 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment TABLE 49: Raw data for moisture retention curve of B C TM P sludge (n=1) cont.&sludge wet sludge wet cont.&sludge dry sludge dry pressure [bar] container [g] [g] [g] [g] [g] 0.1 0.2 0.3 0.4 0.5 0.7 1.0 2.0 5.0 10.0 15.0 3.828 3.830 3.826 3.829 3.828 3.828 3.827 3.828 3.830 3.829 3.829 26.992 28.638 29.360 27.433 25.878 25.501 25.467 26.015 27.232 25.041 23.578 23.164 24.808 25.534 23.604 22.050 21.673 21.640 22.187 23.402 21.212 19.749 8.439 8.893 9.293 8.922 8.633 8.494 8.510 8.649 8.969 10.012 9.689 4.611 5.063 [%] 402 390 5.467 5.093 4.805 4.666 4.683 4.821 5.139 367 363 359 364 362 360 355 6.183 5.860 243 237 average stdev se cont.& soil dry soil dry WHCg bulk density [g/cm3] 0.123 0.135 0.146 0.136 0.129 0.125 0.125 0.129 0.138 0.165 0.157 0.1372 0.0138 ± 0.0041 WHCV [%] 49.6 52.8 53.7 49.5 46.1 45.5 45.4 46.5 4 8.9 40.2 37.2 TABLE 50: Raw data for moisture retention curve of soil (n=1) pressure [bar] container cont.& soil wet [g] [g] [g] [g] [g] 0.1 0.2 0.3 0.4 0.5 0.7 1.0 2.0 5 .0 10.0 15.0 3.783 3.807 3.785 3.805 73.136 73.758 65.080 74.858 69.353 69.951 61.295 71.053 53.635 56.920 3.785 3.783 3.785 3.785 3.815 3.812 3.823 58.519 63.518 54.734 59.735 46.652 50.334 70.530 71.218 73.182 71.224 70.398 66.745 67.433 69.367 67.412 66.575 56.315 5 7.660 49.852 53.113 46.657 54.264 42.867 46.551 52.530 53.875 54.299 soil wet 50.442 58.069 58.114 58.126 57.414 54.314 53.591 WHCg [%] 39 32 31 31 28 28 27 25 28 24 24 average stdev se bulk density [g/cm3] 1.334 1.421 1.249 1.452 1.147 1.246 1.406 1.442 1.453 1.453 1.434 1.3670 0.1072 ± 0.0323 WHCV [%] 52.2 45.1 39.2 44.9 31.8 35.3 38.0 36.3 40.3 35.0 34.7 113 Appendix I: Pressure Plate Experiment TABLE 51: Determination of random errors of bulk density, gravimetric (W H C g) and volumetric moisture content (W H C V) for Kraft mill sludge. pressure [bar] 0.1 0.2 0.3 0.4 0.5 0.7 1.0 2.0 5.0 10.0 15.0 m ass w et m ass dry [g] [g] 26.785 21.061 18.207 19.361 17.010 4.800 5.244 WHCg 16.801 16.796 16.006 19.916 19.297 4.476 4.983 4.499 4.327 4.804 4.650 5.672 6.004 [%] 458 302 307 289 278 288 250 244 251 221 19.421 5.923 228 ± AWHCg 0.141 0.090 0.107 0.091 0.098 0.105 0.084 0.086 0.072 0.062 0.064 Db [g/cm 3] 0.128 0.140 0.120 0.133 0.120 0.116 0.129 0.124 0.152 0.161 0.158 ± ADb 0.0026 0.0029 0.0024 0.0027 0.0025 0.0024 0.0026 0.0025 0.0031 0.0033 0.0032 WHCV [%] 58.8 42.3 36.7 38.5 33.5 33.4 32.1 30.4 38.1 35.6 36.1 ± AWHCV 1.201 0.864 0.750 0.786 0.684 0.682 0.655 0.621 0.778 0.726 0.737 TABLE 52: Determination of random errors of bulk density, gravimetric (W H C g) and volumetric moisture content (W H C V) for BCTM P sludge. pressure [bar] 0.1 0.2 0.3 0.4 0.5 0.7 1.0 2.0 5.0 10.0 15.0 m ass w e t m ass dry [g] [g] 23.164 24.808 25.534 23.604 22.050 21.673 21.640 22.187 23.402 4.611 5.063 5.467 5.093 4.805 4.666 4.683 4.821 5.139 6.183 5.860 21.212 19.749 WHCg + AWHCg [%] 402 390 367 363 359 364 362 0.131 0.116 0.102 0.108 0.114 0.118 0.117 360 355 243 237 0.114 0.105 0.064 0.067 Db [g/cm 3] 0.123 0.135 0.146 0.136 0.129 0.125 0.125 0.129 0.138 0.165 0.157 + ADb WHCV + AWHCV 0.0025 0.0028 0.0030 0.0028 0.0026 0.0025 0.0026 [%] 49.6 52.8 53.7 49.5 46.1 45.5 45.4 1.014 1.079 1.096 1.011 0.942 0.929 0.927 0.0026 0.0028 0.0034 0.0032 46.5 48.9 40.2 37.2 0.949 0.998 0.821 0.759 TABLE 53: Determination of random errors of bulk density, gravimetric (W H C g) and volumetric moisture content (W H C V) for soil. pressure [bar] 0.1 0.2 0.3 0.4 0.5 0.7 1.0 2.0 5.0 10.0 15.0 m ass w et m ass dry [g] [g] 69.353 69.951 61.295 71.053 54.734 59.735 66.745 67.433 69.367 67.412 66.575 49.85 53.11 46.66 54.26 42.87 46.55 52.53 53.88 54.30 54.31 53.59 WHCg ± AWHCg Db + ADb WHCV ± AWHCV [%] 39.1 31.7 31.4 30.9 27.7 28.3 27.1 25.2 27.8 24.1 24.2 0.0042 0.0039 0.0044 0.0038 0.0048 0.0044 0.0039 0.0038 0.0038 0.0037 0.0038 [g/cm 3] 1.334 1.421 1.249 1.452 1.147 1.246 1.406 1.442 1.453 1.453 1.434 0.0272 0.0290 0.0255 0.0296 0.0234 0.0254 0.0287 0.0294 0.0297 0.0297 0.0293 [%] 52.2 45.1 39.2 44.9 31.8 35.3 38.0 36.3 40.3 35.0 34.7 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 1.065 0.920 0.800 0.917 0.648 0.720 0.777 0.741 0.823 0.716 0.709 Appendix I: Pressure Plate Experiment Part B: Moisture retention curves for sludge-soil mixtures Table 54: Raw data for moisture retention curve of Kraft mill sludge pressure [bar] 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 trial # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 alu em pty & sam ple w et [g] 3.840 3.840 3.838 3.839 3.651 3.838 3.838 3.650 3.837 3.839 3.650 3.651 3.651 3.651 [g] 27.303 24.055 23.094 23.316 22.122 23.242 21.791 20.380 20.833 22.463 21.673 20.899 20.953 20.686 m ass w e t & sam ple dry [g] 23.463 20.215 19.256 19.477 18.471 19.404 17.953 16.730 16.996 18.624 18.023 17.248 17.302 17.035 [g] 8.591 8.925 8.816 8.756 8.719 9.071 8.881 8.255 8.769 9.146 8.859 8.629 8.880 8.573 m ass dry [g] 4.751 5.085 4.978 4.917 5.068 5.233 5.043 4.605 4.932 5.307 5.209 4.978 5.229 4.922 average stdev ±se Db [g/cm -5] 0.127 0.136 0.133 0.132 0.136 0.140 0.135 0.123 0.132 0.142 0.139 0.133 0.140 0.132 0.134 0.005 0.001 TABLE 55: Raw data for moisture retention curve of blended Kraft mill sludge pressure [bar] 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 trial # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 alu em p ty & sam p le w et [g] 3.818 3.819 3.817 3.818 3.582 3.818 3.819 3.582 3.817 3.817 3.582 3.582 3.583 3.582 [g] 33.607 27.716 27.050 26.848 25.263 29.801 28.311 24.965 23.853 24.024 27.963 24.121 23.302 24.359 m ass w e t & sam ple dry [g] 29.789 23.897 23.233 23.030 21.681 25.983 24.492 21.383 20.036 20.207 24.381 20.539 19.719 20.777 [g] 10.165 9.802 10.293 9.978 9.505 11.124 10.699 9.714 9.611 9.459 11.065 9.971 9.346 9.728 m ass dry [g] 6.347 5.983 6.476 6.160 5.923 7.306 6.880 6.132 5.794 5.642 7.483 6.389 5.763 6.146 average stdev ±se Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Db [g/cm '5] 0.170 0.160 0.173 0.165 0.158 0.196 0.184 0.164 0.155 0.151 0.200 0.171 0.154 0.164 0.169 0.015 0.004 Appendix I: Pressure Plate Experiment Table 56: Raw data for moisture retention curve of Kraft mill sludge-soil mixture 40:10 pressure trial [bar] # 1 1 2 3 1 1 1 2 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 1 1 1 1 2 3 alu em p ty & sam ple w et m ass w et & sam ple dry m ass dry Db [g] [g] [g] [g] [g] 3.699 3.700 3.699 3.701 3.625 3.698 3.700 3.623 3.697 3.701 3.625 3.624 3.625 3.627 34.877 30.793 28.473 29.515 27.321 28.921 28.668 27.561 26.46 28.343 26.025 25.851 26.071 26.107 31.178 27.093 24.774 25.814 23.696 13.435 13.798 12.546 13.731 12.751 9.736 10.098 8.847 10.030 9.126 [g/cm 3] 0.261 0.270 0.237 0.268 0.244 25.223 24.968 23.938 22.763 24.642 22.400 22.227 22.446 22.480 12.639 13.928 12.510 13.023 13.494 13.358 12.872 13.804 13.433 8.941 10.228 8.887 9.326 9.793 9.733 9.248 10.179 9.806 average 0.239 0.274 0.238 0.250 0.262 0.260 0.247 0.272 0.262 0.256 stdev ± se 0.013 0.004 Table 57: Raw data for moisture retention curve of Kraft mill sludge-soil mixture 30:20 pressure trial [bar] 0.1 0.3 0.3 0.3 0.5 0.7 # 1 1 2 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 3 1 1 1 2 1 1 1 1 2 3 alu em p ty & sam ple w et m ass w e t & sam ple d ry m ass dry Db [g] [g] [g] [g] [g] 3.791 3.794 3.795 3.795 3.651 3.794 3.794 3.650 3.794 3.796 3.650 3.649 3.650 3.652 44.371 37.728 36.299 40.580 33.934 32.504 32.989 31.415 33.467 32.685 31.932 30.262 31.218 30.051 29.704 29.512 29.518 19.024 18.455 19.325 19.269 18.691 18.834 20.018 19.906 19.929 21.299 20.650 19.408 19.266 19.420 15.233 14.661 15.530 15.474 15.040 15.040 16.224 16.256 16.135 17.503 17.000 15.759 15.616 15.768 average stdev ± se [g/cm 3] 0.408 0.392 0.416 0.414 0.402 0.402 0.434 0.435 0.432 0.468 0.455 0.422 0.418 0.422 0.423 0.021 0.006 36.784 35.066 37.261 36.479 35.582 34.056 35.014 33.701 33.353 33.162 33.170 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment Table 58: Raw data for moisture retention curve of Kraft mill sludge-soil mixture 25:25 pressure trial [bar] 0.1 0.3 0.3 0.3 0.5 0.7 # 1 1 2 3 1 1 1 2 1 1 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 1 1 2 3 alu em p ty & sam ple w et m ass w e t & sam ple dry m ass dry Db [g/cm 3] 0.529 0.499 0.553 0.506 0.503 0.504 0.506 0.468 0.514 [g] [g] [g] [g] [g] 3.822 3.827 3.826 3.828 3.667 3.827 3.827 3.668 3.825 46.694 40.435 40.975 40.682 39.294 36.435 37.500 36.682 36.565 37.565 36.317 34.720 37.142 36.035 23.586 22.469 24.499 22.749 22.460 22.657 22.726 21.166 23.025 23.471 19.764 18.642 3.828 3.668 3.668 3.669 3.671 42.872 36.608 37.149 36.854 35.627 32.608 33.673 33.014 32.740 33.737 32.649 31.052 33.473 32.364 22.594 21.402 23.272 22.488 20.673 18.921 18.793 18.830 18.899 17.498 19.200 19.643 18.926 17.734 19.603 18.817 0.526 0.506 0.475 0.525 0.504 average stdev ± se 0.508 0.021 0.006 Table 59: Raw data for moisture retention curve of Kraft mill sludge-soil mixture 20:30 pressure trial [bar] 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 alu em pty & sam ple w et m ass w e t & sam ple dry m ass dry Db [g/cm 3] 0.560 0.582 [g] [g] [g] [g] [g] 3.830 3.834 3.835 3.836 3.681 3.835 3.835 3.681 3.834 3.835 3.682 3.682 3.682 3.683 45.428 43.016 41.378 41.698 40.549 40.022 40.115 38.986 38.082 38.705 38.180 36.438 37.211 37.069 41.598 39.182 37.543 37.862 36.868 36.187 36.280 35.305 34.248 34.870 34.498 32.756 33.529 33.386 24.743 25.589 25.898 25.306 25.568 26.667 25.876 23.899 26.270 26.437 25.097 25.072 25.836 24.949 20.913 21.755 22.063 21.470 21.887 22.832 22.041 20.218 22.436 22.602 21.415 21.390 22.154 21.266 average stdev ±se Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 0.590 0.575 0.586 0.611 0.590 0.541 0.600 0.605 0.573 0.572 0.593 0.569 0.582 0.019 0.005 Appendix I: Pressure Plate Experiment Table 60: Raw data for moisture retention curve of Kraft mill sludge-soil mixture 10:40 pressure trial [bar] 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 # 1 1 2 3 1 1 1 2 1 5.0 10.0 15.0 15.0 15.0 1 1 1 2 3 alu em p ty & sam ple w et m ass w e t & sam ple d ry m ass dry Db [g/cm 3] 0.923 0.918 0.933 0.917 0.918 0.941 0.917 0.927 0.940 0.916 0.910 0.914 0.938 0.936 0.925 0.011 0.003 [g] [g] [g] [g] [g] 3.819 3.822 3.821 3.821 3.700 3.819 3.820 3.699 3.819 3.822 3.700 3.701 3.700 3.701 59.523 55.832 56.310 55.869 52.806 53.448 52.823 52.143 52.253 50.887 49.894 51.174 52.313 51.748 55.704 52.010 52.489 52.048 49.106 49.629 49.003 48.444 48.434 47.065 46.194 47.473 48.613 48.047 38.295 38.114 38.685 38.099 38.006 38.994 38.100 38.353 38.953 38.045 37.697 37.863 38.738 38.668 34.476 34.292 34.864 34.278 34.306 35.175 34.280 34.654 35.134 34.223 33.997 34.162 35.038 34.967 average stdev ± se 118 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment TABLE 61: Raw data for moisture retention curve of BCTM P sludge pressure trial [bar] 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 alu em pty & sam ple w et m ass w et & sam ple dry m ass dry Db [g/cm 3] 0.159 0.158 0.159 0.149 0.154 0.156 0.153 0.151 0.153 0.150 0.152 0.151 0.149 0.151 0.153 0.004 0.001 [g] [g] [g] [g] [g] 3.829 3.829 3.830 3.837 3.830 3.830 3.830 3.840 3.841 3.652 3.650 3.651 3.840 3.651 27.017 24.760 26.152 25.179 23.794 24.605 24.184 23.796 23.822 22.823 23.067 22.638 22.700 23.615 23.188 20.931 22.322 21.342 19.964 20.775 20.354 19.956 19.981 19.171 19.417 18.987 18.860 19.964 9.777 9.745 9.774 9.416 9.578 9.658 9.555 9.488 9.572 9.241 9.333 9.276 9.421 9.299 5.948 5.916 5.944 5.579 5.748 5.828 5.725 5.648 5.731 5.589 5.683 5.625 5.581 5.648 average stdev ± se TABLE 62: Raw data for moisture retention curve of blended BCTM P sludge pressure trial [bar] 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 # 1 15.0 15.0 1 2 3 1 1 1 2 1 1 1 1 2 3 alu em p ty & sam ple w et m ass w e t & sam ple dry m ass d ry Db [g] [g] [g] [g] [g] 3.816 3.816 3.817 30.809 25.677 29.486 28.427 27.203 26.684 26.957 26.406 27.354 26.822 27.043 26.645 26.993 21.861 25.669 24.612 23.387 22.866 23.140 22.589 23.536 23.239 23.462 23.065 6.611 6.454 6.870 6.342 6.735 6.529 6.625 6.464 6.606 6.879 6.631 6.783 [g/cm 3] 0.177 0.173 0.184 0.170 0.180 0.175 0.177 0.173 0.177 0.184 0.177 0.182 25.405 26.893 21.588 23.312 10.427 10.270 10.687 10.157 10.551 10.347 10.442 10.281 10.424 10.462 10.212 10.363 10.348 10.134 6.531 6.553 average stdev ±se 0.175 0.175 0 .177 0.004 0.001 3.815 3.816 3.818 3.817 3.817 3.818 3.583 3.581 3.580 3.817 3.581 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment TABLE 63: Raw data for moisture retention curve of BCTMP sludge-soil mixture 40:10 pressure trial [bar] 0.1 0.3 0.3 0.3 # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 alu em pty & sam ple w et m ass w e t & sam ple dry m ass dry Db [g/cm 3] 0.307 0.331 0.308 0.336 0.341 0.337 0.334 0.333 0.324 0.374 0.360 0.348 0.324 0.313 0.334 0.019 0.005 [g] [g] [g] [g] [g] 3.162 3.158 3.158 3.695 3.159 3.157 3.157 3.155 3.704 3.624 36.213 34.812 35.651 36.308 33.499 33.894 34.046 33.479 32.731 36.822 36.060 35.591 32.547 33.429 33.051 31.654 32.493 32.613 30.340 30.737 30.889 30.324 29.027 33.198 32.434 31.967 28.847 29.805 14.629 15.513 14.650 16.261 15.902 15.751 15.635 15.599 15.808 17.596 17.091 16.623 15.807 15.332 11.467 12.355 11.492 12.566 12.743 12.594 12.478 12.444 12.104 13.972 13.465 12.999 12.107 11.708 average stdev ± se 3.626 3.624 3.700 3.624 TABLE 64: Raw data for moisture retention curve of BCTM P sludge-soil mixture 30:20 pressure trial [bar] 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 alu em pty & sam p le w e t m ass w et & sam ple dry m ass dry Db [g/cm 3] 0.433 [g] [g] [g] [g] [g] 3.784 3.797 3.796 3.787 3.794 3.792 3.792 3.792 3.803 3.650 3.652 3.650 3.792 3.651 38.088 36.125 36.530 37.621 36.382 37.351 37.827 37.335 36.717 38.094 37.945 37.436 35.703 35.908 34.304 32.328 32.734 33.834 32.588 33.559 34.035 33.543 32.914 34.444 34.293 33.786 31.911 32.257 19.975 19.873 19.716 19.413 19.904 20.151 21.187 20.888 20.608 21.462 21.255 21.027 20.617 19.312 16.191 16.076 15.920 15.626 16.110 16.359 17.395 17.096 16.805 17.812 17.603 17.377 16.825 15.661 average stdev ±se Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 0.430 0.426 0.418 0.431 0.438 0.465 0.457 0.450 0.477 0.471 0.465 0.450 0.419 0.445 0.020 0.005 Appendix I: Pressure Plate Experiment TABLE 65: Raw data for moisture retention curve of BCTMP sludge-soil mixture 25:25 pressure trial [bar] 0.1 0.3 0.3 0.3 0.5 0.7 # 1 1 2 3 1 1 1.0 1.0 2.0 5.0 10.0 15.0 15.0 1 2 3.821 3.820 1 1 1 1 2 3 3.821 3.668 3.668 3.668 3.823 3.668 15.0 alu em pty & sam ple w et m ass w et & sam p le dry m ass d ry Db [g/cm 3] 0.658 0.569 0.543 0.549 0.467 0.470 0.471 0.470 0.477 0.524 0.536 0.495 0.452 [g] [g] [g] [g] [g] 3.818 3.821 3.822 52.304 42.510 41.830 42.386 34.589 34.772 35.029 35.116 35.219 36.344 36.704 36.224 34.075 48.486 38.689 38.008 38.568 30.761 30.950 31.208 31.296 31.398 32.676 33.036 32.556 30.252 31.352 28.409 25.091 24.130 24.331 21.268 21.392 21.425 21.383 21.652 23.252 23.702 22.153 20.710 21.579 24.591 21.270 20.308 20.513 17.440 17.570 17.604 17.563 17.831 19.584 20.034 18.485 16.887 17.911 average stdev 3.818 3.828 3.822 35.020 0.479 0.511 0.056 + se 0.015 TABLE 66: Raw data for moisture retention curve of BC TM P sludge-soil mixture 20:30 pressure trial [bar] 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 # 1 1 2 15.0 15.0 3 1 1 1 2 1 1 1 1 2 3 alu em p ty & sam ple w e t m ass w e t & sam p le dry m ass dry Db [g/cm 3] 0.504 0.578 0.568 0.559 0.549 0.572 0.558 0.569 0.562 0.620 0.604 0.619 0.542 0.565 0.569 0.031 0.008 [g] [g] [g] [g] [g] 3.827 3.829 3.830 3.826 3.830 3.829 3.828 3.828 3.830 3.679 3.680 3.679 37.420 39.065 42.759 41.559 36.996 37.907 37.563 38.083 37.859 40.949 40.900 39.950 36.795 39.411 33.593 35.236 38.929 22.644 25.425 25.066 24.716 24.360 25.210 24.669 25.092 24.832 26.863 26.250 26.798 24.071 24.804 18.817 21.596 21.236 20.890 20.530 21.381 20.841 21.264 21.002 23.184 22.570 23.119 20.240 21.125 average stdev ± se 3.831 3.679 37.733 33.166 34.078 33.735 34.255 34.029 37.27 37.220 36.271 32.964 35.732 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment TABLE 67: Raw data for moisture retention curve of BCTMP sludge-soil mixture 10:40 pressure trial [bar] 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 alu em p ty & sam ple w e t m ass w e t & sam ple dry m ass dry Db [g/cm 3] 0.982 0.959 0.950 0.954 0.956 0.955 0.965 0.946 0.956 0.960 0.991 0.968 0.986 0.969 0.964 0.014 0.004 [g] [g] [g] [g] [g] 3.786 3.814 3.816 3.816 3.818 3.824 3.824 3.822 3.822 3.699 3.699 3.698 3.821 3.700 60.560 56.166 58.258 58.645 55.981 54.870 56.774 52.352 54.442 54.829 52.163 51.046 40.473 39.666 39.323 39.455 39.559 39.520 36.687 35.852 35.507 55.863 55.167 55.697 55.094 55.879 54.862 56.023 56.148 52.039 51.345 51.875 51.395 52.180 51.164 52.202 52.448 39.868 39.171 39.538 39.569 40.725 39.854 40.666 39.901 35.639 35.741 35.696 36.044 35.349 35.716 35.870 37.026 36.156 36.845 36.201 average stdev ± se 122 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment Part B: Moisture retention curves for sludge-soil mixtures TABLE 68: W HCg, Db, W HCV, and random errors of original Kraft mill sludge. p re s s u re trial [b ar] # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 m a s s w e t m a s s d ry [g] [g] 23.463 20.215 19.256 19.477 18.471 19.404 17.953 16.730 16.996 18.624 18.023 17.248 17.302 17.035 4.751 5.085 4.978 4.917 5.068 5.233 5.043 4.605 4.932 5.307 5.209 4.978 5.229 4.922 WHCg [%] 394 298 287 296 264 271 256 263 245 251 246 246 231 246 ± A WHCg Db ± A Db WHCV ± A WHCV [%] 0.125 0.092 0.091 0.094 0.084 0.083 0.082 0.092 0.081 0.077 0.077 0.081 0.073 0.082 [g /c m 3] [g /c m 3] 0.127 0.136 0.133 0.132 0.136 0.140 0.135 0.123 0.132 0.142 0.139 0.133 0.140 0.132 0.0026 0.0028 0.0027 0.0027 0.0028 0.0029 0.0028 0.0025 0.0027 0.0029 0.0028 0.0027 0.0029 0.0027 [%] 50 40 38 39 36 38 35 32 32 36 34 33 32 32 [%] 1.022 0.827 0.780 0.796 0.732 0.774 0.705 0.663 0.659 0.728 0.700 0.670 0.660 0.662 TABLE 69: WHCg Db, WHCV, and random errors of blended Kraft mill sludge. p re s s u re trial [bar] # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 m a s s w e t m a s s d ry [g] [g] 29.789 23.897 23.233 23.030 21.681 25.983 24.492 21.383 20.036 20.207 24.381 20.539 19.719 20.777 6.347 5.983 6.476 6.160 5.923 7.306 6.880 6.132 5.794 5.642 7.483 6.389 5.763 6.146 WHCg + A WHCg Db ± A Db WHCV ± A WHCV [%] 369 299 259 274 266 256 256 249 246 258 226 221 242 238 [%] 0.088 0.078 0.064 0.071 0.072 0.057 0.060 0.066 0.069 0.074 0.050 0.058 0.069 0.064 [g /c m 3] [g /c m 3] 0.170 0.160 0.173 0.165 0.158 0.196 0.184 0.164 0.155 0.151 0.200 0.171 0.154 0.164 0.0035 0.0033 0.0035 0.0034 0.0032 0.0040 0.0038 0.0034 0.0032 0.0031 0.0041 0.0035 0.0031 0.0034 [%] 63 48 45 45 42 50 47 41 38 39 45 38 37 39 [%] 1.281 0.979 0.916 0.922 0.861 1.020 0.962 0.833 0.778 0.796 0.923 0.773 0.763 0.799 TABLE 70: WHCg , Db, W HCV, and random errors of Kraft mill sludge-soil mixture 40:10. p re s s u re tria l [bar] # 1 1 2 3 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 1 1 1 2 1 1 1 1 2 3 m a s s w e t m a s s d ry [g] [g] 31.178 27.093 24.774 25.814 23.696 25.223 24.968 23.938 22.763 24.642 22.400 22.227 22.446 22.480 9.736 10.098 8.847 10.030 9.126 8.941 10.228 8.887 9.326 9.793 9.733 9.248 10.179 9.806 WHCg [%] 220 168 180 157 160 182 144 169 144 152 130 140 121 129 i A WHCg Db ± A Db WHCV ± A WHCV [%] 0.038 0.031 0.037 0.030 0.033 0.036 0.028 0.035 0.031 0.030 0.028 0.030 0.026 0.028 [g /c m 3] [g /c m 3] 0.261 0.270 0.237 0.268 0.244 0.239 0.274 0.238 0.250 0.262 0.260 0.247 0.272 0.262 0.0053 0.0055 0.0048 0.0055 0.0050 0.0049 0.0056 0.0049 0.0051 0.0053 0.0053 0.0051 0.0056 0.0054 [%] 57 45 43 42 39 44 39 40 36 40 34 35 33 34 [%] 1.171 0.928 0.870 0.862 0.796 0.890 0.805 0.822 0.734 0.811 0.692 0.709 0.670 0.692 123 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment TABLE 71: WHCg, Db, WHCV, and random errors of Kraft mill sludge-soil mixture 30:20. p re s s u re tria l [b ar] # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 m a s s w e t m a s s d ry [g] [g] 40.580 33.934 32.504 32.989 31.415 33.467 32.685 31.932 30.262 31.218 30.051 29.704 29.512 29.518 15.233 14.661 15.530 15.474 15.040 15.040 16.224 16.256 16.135 17.503 17.000 15.759 15.616 15.768 WHC„ ± A W HC„ Db ± A Db WHCV ± A W HCV [%] 166 131 109 113 109 123 101 96 88 78 77 88 89 87 [%] 0.020 0.019 0.016 0.017 0.017 0.018 0.015 0.015 0.015 0.013 0.013 0.015 0.015 0.015 [g /c m 3] [g /c m 3] 0.408 0.392 0.416 0.414 0.402 0.402 0.434 0.435 0.432 0.468 0.455 0.422 0.418 0.422 0.0083 0.0080 0.0085 0.0085 0.0082 0.0082 0.0089 0.0089 0.0088 0.0096 0.0093 0.0086 0.0085 0.0086 [%] 68 52 45 47 44 49 44 42 38 37 35 37 37 37 [%] 1.385 1.053 0.927 0.957 0.895 1.007 0.899 0.856 0.772 0.749 0.713 0.762 0.759 0.751 TABLE 72: W HCg, Db, W HCV, and random errors of Kraft mill sludge-soil mixture 25:25. p re s s u re tria l [b ar] # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 m a s s w e t m a s s d ry [g] [g] 42.872 36.608 37.149 36.854 35.627 32.608 33.673 33.014 32.740 33.737 32.649 31.052 33.473 32.364 19.764 18.642 20.673 18.921 18.793 18.830 18.899 17.498 19.200 19.643 18.926 17.734 19.603 18.817 WHCg [%] 117 96 80 95 90 73 78 89 71 72 73 75 71 72 1 A WHCg Db ± A Db WHCV ± A W HCV [%] 0.013 0.013 0.011 0.013 0.013 0.012 0.012 0.013 0.012 0.011 0.012 0.013 0.011 0.012 [g /c m 3] [g /c m 3] 0.529 0.499 0.553 0.506 0.503 0.504 0.506 0.468 0.514 0.526 0.506 0.475 0.525 0.504 0.0108 0.0102 0.0113 0.0103 0.0103 0.0103 0.0103 0.0096 0.0105 0.0107 0.0103 0.0097 0.0107 0.0103 [%] 62 48 44 48 45 37 40 42 36 38 37 36 37 36 [%] 1.262 0.981 0.900 0.980 0.920 0.753 0.807 0.848 0.740 0.770 0.750 0.728 0.758 0.740 TABLE 73: W HCg, Db, W HCV, and random errors of Kraft mill sludge-soil mixture 20:30. p re s s u re trial [bar] # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 m a s s w e t m a s s d ry [g] [g] 41.598 39.182 37.543 37.862 36.868 36.187 36.280 35.305 34.248 34.870 34.498 32.756 33.529 33.386 20.913 21.755 22.063 21.470 21.887 22.832 22.041 20.218 22.436 22.602 21.415 21.390 22.154 21.266 WHCg [%] 99 80 70 76 68 58 65 75 53 54 61 53 51 57 t AWHCg Db ± A Db WHCV ± A WHCV [%] 0.012 0.011 0.010 0.011 0.010 0.009 0.010 0.011 0.010 0.009 0.010 0.010 0.010 0.010 [g /c m 3] [g /c m 3] 0.560 0.582 0.590 0.575 0.586 0.611 0.590 0.541 0.600 0.605 0.573 0.572 0.593 0.569 0.0114 0.0119 0.0121 0.0117 0.0120 0.0125 0.0120 0.0110 0.0123 0.0123 0.0117 0.0117 0.0121 0.0116 [%] 55 47 41 44 40 36 38 40 32 33 35 30 30 32 [%] 1.130 0.952 0.846 0.896 0.818 0.730 0.778 0.824 0.645 0.670 0.715 0.621 0.621 0.662 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment TABLE 74: WHCg, Db, WHCV, and random errors of Kraft mill sludge-soil mixture 10:40. p re s s u re tria l [b ar] # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 m a s s w e t m a s s d ry [g] 55.704 52.010 52.489 52.048 49.106 49.629 49.003 48.444 48.434 47.065 46.194 47.473 48.613 48.047 [g] 34.476 34.292 34.864 34.278 34.306 35.175 34.280 34.654 35.134 34.223 33.997 34.162 35.038 34.967 WHC„ ± A WHCg Db ± A Db W HCV ± A WHCV [%] 62 52 51 52 43 41 43 40 38 38 36 39 39 37 [%] 0.006 0.006 0.006 0.006 0.006 0.006 0.006 0.006 0.006 0.006 0.006 0.006 0.006 0.006 [g /c m 3] [g /c m 3] 0.923 0.918 0.933 0.917 0.918 0.941 0.917 0.927 0.940 0.916 0.910 0.914 0.938 0.936 0.0188 0.0187 0.0190 0.0187 0.0187 0.0192 0.0187 0.0189 0.0192 0.0187 0.0186 0.0187 0.0191 0.0191 [%] 57 47 47 48 40 39 39 37 36 34 33 36 36 35 [%] 1.160 0.968 0.963 0.971 0.809 0.790 0.804 0.753 0.727 0.702 0.666 0.727 0.742 0.715 125 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment TABLE 75: W H C g, Db, W HCV, and random errors of original BCTMP sludge. p re s s u re tria l [b ar] # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 m a s s w e t m a s s d ry [g] [g] 23.188 20.931 22.322 21.342 19.964 20.775 20.354 19.956 19.981 19.171 19.417 18.987 18.860 19.964 5.948 5.916 5.944 5.579 5.748 5.828 5.725 5.648 5.731 5.589 5.683 5.625 5.581 5.648 WHCg [%] 290 254 276 283 247 256 256 253 249 243 242 238 238 253 + A WHCg Db ± A Db WHCV ± A WHCV [%] 0.077 0.069 0.074 0.080 0.070 0.071 0.072 0.073 0.071 0.071 0.070 0.070 0.070 0.073 [g /c m 3] [g /c m 3] 0.159 0.158 0.159 0.149 0.154 0.156 0.153 0.151 0.153 0.150 0.152 0.151 0.149 0.151 0.0032 0.0032 0.0032 0.0030 0.0031 0.0032 0.0031 0.0031 0.0031 0.0031 0.0031 0.0031 0.0030 0.0031 [%] 46 40 44 42 38 40 39 38 38 36 37 36 36 38 [%] 0.942 0.820 0.895 0.861 0.777 0.817 0.799 0.782 0.779 0.742 0.750 0.730 0.726 0.782 TABLE 76: WHCg Db, W HCV, and random errors of blended BCTMP sludge. p re s s u re tria l [bar] # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 m a s s w e t m a s s d ry [g] [g] 26.993 21.861 25.669 24.612 23.387 22.866 23.140 22.589 23.536 23.239 23.462 23.065 21.588 23.312 6.611 6.454 6.870 6.342 6.735 6.529 6.625 6.464 6.606 6.879 6.631 6.783 6.531 6.553 WHCg + A WHCg Db ± ADb WHCV ± A WHCV [%] 308 239 274 288 247 250 249 249 256 238 254 240 231 256 [%] 0.073 0.061 0.063 0.072 0.060 0.062 0.061 0.063 0.063 0.057 0.062 0.058 0.059 0.063 [g /c m 3] [g /c m 3] 0.177 0.173 0.184 0.170 0.180 0.175 0.177 0.173 0.177 0.184 0.177 0.182 0.175 0.175 0.0036 0.0035 0.0038 0.0035 0.0037 0.0036 0.0036 0.0035 0.0036 0.0038 0.0036 0.0037 0.0036 0.0036 [%] 55 41 50 49 45 44 44 43 45 44 45 44 40 45 [%] 1.114 0.842 1.027 0.998 0.910 0.893 0.902 0.881 0.925 0.894 0.920 0.890 0.823 0.916 TABLE 77: W HCg, Db, WHCV, and random errors of BCTMP sludge-soil mixture 40:10. p re s s u re trial [b ar] # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 m a s s w e t m a s s d ry [g] [g] 33.051 31.654 32.493 32.613 30.340 30.737 30.889 30.324 29.027 33.198 32.434 31.967 28.847 29.805 11.467 12.355 11.492 12.566 12.743 12.594 12.478 12.444 12.104 13.972 13.465 12.999 12.107 11.708 WHCg + A WHCg Db ± A Db WHCV ± A WHCV [%] 188 156 183 160 138 144 148 144 140 138 141 146 138 155 [%] 0.029 0.024 0.028 0.024 0.022 0.023 0.023 0.023 0.023 0.020 0.021 0.022 0.023 0.025 [g /c m 3] [g /c m 3] 0.307 0.331 0.308 0.336 0.341 0.337 0.334 0.333 0.324 0.374 0.360 0.348 0.324 0.313 0.0063 0.0067 0.0063 0.0069 0.0070 0.0069 0.0068 0.0068 0.0066 0.0076 0.0074 0.0071 0.0066 0.0064 [%] 58 52 56 54 47 49 49 48 45 51 51 51 45 48 [%] 1.179 1.054 1.147 1.095 0.961 0.991 1.006 0.977 0.925 1.050 1.036 1.036 0.915 0.989 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment TABLE 78: WHCg, Db, WHCV, and random errors of BCTMP sludge-soil mixture 30:20. p re s s u re trial [bar] # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 m a s s w e t m a s s d ry [g] [g] 34.304 32.328 32.734 33.834 32.588 33.559 34.035 33.543 32.914 34.444 34.293 33.786 31.911 32.257 16.191 16.076 15.920 15.626 16.110 16.359 17.395 17.096 16.805 17.812 17.603 17.377 16.825 15.661 WHCg + A WHCg Db ± A Db WHCV + A WHCV [%] 112 101 106 117 102 105 96 96 96 93 95 94 90 106 [%] 0.016 0.015 0.016 0.017 0.015 0.015 0.014 0.014 0.014 0.013 0.014 0.014 0.014 0.016 [g /c m 3] [g /c m 3] 0.433 0.430 0.426 0.418 0.431 0.438 0.465 0.457 0.450 0.477 0.471 0.465 0.450 0.419 0.0088 0.0088 0.0087 0.0085 0.0088 0.0089 0.0095 0.0093 0.0092 0.0097 0.0096 0.0095 0.0092 0.0086 [%] 48 43 45 49 44 46 45 44 43 45 45 44 40 44 [%] 0.990 0.888 0.919 0.995 0.900 0.940 0.909 0.899 0.880 0.909 0.912 0.896 0.824 0.907 TABLE 79: WHCg Db, W HCV, and random errors of BCTMP sludge-soil mixture 25:25. p re s s u re trial [bar] # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 m a s s w e t m a s s d ry [g] [g] 48.486 38.689 38.008 38.568 30.761 30.950 31.208 31.296 31.398 32.676 33.036 32.556 30.252 31.352 24.591 21.270 20.308 20.513 17.440 17.570 17.604 17.563 17.831 19.584 20.034 18.485 16.887 17.911 WHCg [%] 97 82 87 88 76 76 77 78 76 67 65 76 79 75 ± A WHCg Db ± A Db WHCV ± A WHCV [%] 0.010 0.011 0.012 0.011 0.013 0.013 0.013 0.013 0.013 0.011 0.011 0.012 0.014 0.013 [g /c m 3] [g /c m 3] 0.658 0.569 0.543 0.549 0.467 0.470 0.471 0.470 0.477 0.524 0.536 0.495 0.452 0.479 0.0134 0.0116 0.0111 0.0112 0.0095 0.0096 0.0096 0.0096 0.0097 0.0107 0.0109 0.0101 0.0092 0.0098 [%] 64 47 47 48 36 36 36 37 36 35 35 38 36 36 [%] 1.305 0.952 0.967 0.986 0.728 0.731 0.743 0.750 0.741 0.715 0.710 0.769 0.730 0.734 TABLE 80: W H C g, Db, W HCV, and random errors of BCTMP sludge-soil mixture 20:30. p re s s u re tria l [bar] # 1 1 2 3 1 1 1 2 1 1 1 1 2 3 0.1 0.3 0.3 0.3 0.5 0.7 1.0 1.0 2.0 5.0 10.0 15.0 15.0 15.0 m a s s w e t m a s s d ry [g] [g] 33.593 35.236 38.929 37.733 33.166 34.078 33.735 34.255 34.029 37.270 37.220 36.271 32.964 35.732 18.817 21.596 21.236 20.890 20.530 21.381 20.841 21.264 21.002 23.184 22.570 23.119 20.240 21.125 WHCg [%] 79 63 83 81 62 59 62 61 62 61 65 57 63 69 ± A WHCg Db ± A Db WHCV ± A WHCV [%] 0.012 0.010 0.011 0.011 0.011 0.010 0.010 0.010 0.010 0.009 0.010 0.009 0.011 0.011 [g /c m 3] [g /c m 3] 0.504 0.578 0.568 0.559 0.549 0.572 0.558 0.569 0.562 0.620 0.604 0.619 0.542 0.565 0.0103 0.0118 0.0116 0.0114 0.0112 0.0117 0.0114 0.0116 0.0115 0.0127 0.0123 0.0126 0.0111 0.0115 [%] 40 36 47 45 34 34 35 35 35 38 39 35 34 39 [%] 0.807 0.745 0.967 0.920 0.690 0.694 0.704 0.710 0.712 0.770 0.800 0.719 0.695 0.798 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment TABLE 81: WHCg, Db, WHCV, and random errors of BCTMP sludge-soil mixture 10:40. p re s s u re trial [bar] # m a s s w e t m a s s d ry [g] [g] 0.1 1 5 6 .7 7 4 3 6 .6 8 7 W HCn ±A W H C „ Db ± A Db W HCV ± A W HCV [%] 55 [%] 0 .0 0 6 [g /c m 3] [g /c m 3] 0 .9 8 2 0 .0 2 0 0 [% ] 54 [%] 1.097 0.901 0.3 1 5 2 .3 5 2 3 5 .8 5 2 46 0 .0 0 6 0 .9 5 9 0 .0 1 9 6 44 0.3 2 5 4 .4 4 2 3 5 .5 0 7 53 0 .0 0 6 0 .9 5 0 0 .0 1 9 4 51 1.034 0.3 3 5 4 .8 2 9 3 5 .6 3 9 54 0 .0 0 6 0 .9 5 4 0 .0 1 9 5 51 1.048 0.5 1 5 2 .1 6 3 35.741 46 0 .0 0 6 0 .9 5 6 0 .0 1 9 5 44 0.8 9 7 0 .7 1 5 1 .0 4 6 3 5 .6 9 6 43 0 .0 0 6 0 .9 5 5 0 .0 1 9 5 41 0.8 3 9 1.0 1 5 2 .0 3 9 3 6 .0 4 4 44 0 .0 0 6 0 .9 6 5 0 .0 1 9 7 43 0.8 7 4 1.0 2 5 1 .3 4 5 3 5 .3 4 9 45 0 .0 0 6 0 .9 4 6 0 .0 1 9 3 43 0.8 7 4 2.0 1 5 1 .8 7 5 3 5 .7 1 6 45 0.0 0 6 0 .9 5 6 0 .0 1 9 5 43 0.8 8 3 5.0 1 5 1 .3 9 5 3 5 .8 7 0 43 0.0 0 6 0 .9 6 0 0 .0 1 9 6 42 0.8 4 8 10.0 1 5 2 .1 8 0 3 7 .0 2 6 41 0.0 0 6 0.991 0 .0 2 0 2 41 0.8 2 8 15.0 1 5 1 .1 6 4 3 6 .1 5 6 42 0.0 0 6 0 .9 6 8 0 .0 1 9 8 40 0 .8 2 0 15.0 2 5 2 .2 0 2 3 6 .8 4 5 42 0.0 0 6 0 .9 8 6 0.0201 41 0.8 3 9 15.0 3 5 2 .4 4 8 36.201 45 0.0 0 6 0 .9 6 9 0 .0 1 9 8 43 0.8 8 8 128 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment Moisture retention curves for Kraft mill sludge-soil mixtures —♦ — original - X - 40:10 30:20 □ 10:40 £ 50 40 0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 p r e s s u r e [b a r ] x (-1 ) FIGURE 15: Moisture retention curves for Kraft mill sludge, Kraft mill sludge-soil mixtures 40:10, 30:20 and 10:40 from 0.1 to 15 bar x (-1). 129 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment 80 -□— blend X - 25:25 • -2 0 :3 0 70 60 2 50 40 30 20 0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 p r e s s u r e [b a r ] x (-1 ) FIGURE 16: Moisture retention curves for blended Kraft mill sludge, Kraft mill sludge-soil mixtures 25:25 and 20:30 from 0.1 to 15 bar x (-1). 130 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment ■♦ original —X— 40:10 A 30:20 SI 10:40 40 0.0 2.0 0.5 2.5 pressure [bar] x (-1) FIGURE 17: Moisture retention curves for Kraft mill sludge, Kraft mill sludge-soil mixtures 40:10, 30:20 and 10:40 from 0.1 to 2.5 bar x (-1). 131 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix i: Pressure Plate Experiment -□— blend - X - - 25:25 ♦ — 20:30 '""X -X 40 X 0.0 2.0 0.5 2.5 pressure [bar] x (-1) FIGURE 18 : Moisture retention curves for blended Kraft mill sludge, Kraft mill sludge-soil mixtures 25:25 and 20:30 from 0.1 to 2.5 bar x (-1). 132 Appendix I: Pressure Plate Experiment Moisture retention curves for Kraft mill sludge-soil mixtures with random errors 80 ♦ original —x — 40:10 70 A 30:20 □ 10:40 60 50 40 30 20 0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 pressure [bar] x (-1) F IG U R E 19: Moisture retention curves for original Kraft mill sludge, Kraft mill sludge-soil mixtures 40:10, 30:20 and 10:40 with random errors from 0.1 to 15 b a rx (-1). — □ — blend -- X- 25:25 — • — 20:30 40 □-------- X ^ — 30 0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 pressure [bar] x (-1) F IG U R E 20: Moisture retention curves for blended Kraft mill sludge, Kraft mill sludge-soil mixtures 25:25 and 20:30 with random errors from 0.1 to 15 bar x (-1). 133 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment —♦ — o rig in a l - x - 4 0 :1 0 A 3 0 :2 0 H 10:40 40 0.0 2.0 0.5 2 .5 pressure [bar] x (-1) F IG U R E 2 1 : M o is tu re re te n tio n c u rv e s fo r o rig in a l K ra ft m ill s lu d g e , K ra ft m ill s lu d g e -s o il m ix tu re s 4 0 :1 0 , 3 0 :2 0 a n d 10:4 0 w ith ra n d o m e rro rs fro m 0.1 to 2 .5 b a r x (-1 ). — □ — ble n d - X- 2 5 :2 5 — • — 2 0 :3 0 0.0 2.0 0.5 2 .5 pressure [bar] x (-1) F IG U R E 22 : M o is tu re re te n tio n c u rv e s fo r b le n d e d K ra ft m ill s lu d g e , K ra ft m ill s lu d g e -s o il m ix tu re s 2 5 :2 5 a n d 2 0 :3 0 w ith ra n d o m e rro rs fro m 0.1 to 2 .5 b a r x (-1). 134 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment Moisture retention curves for BCTMP sludge-soil mixtures original - - -X - - 25:25 13 10:40 3r 40 >©< 20 0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 pressure [bar] x (-1) FIGURE 23 : Moisture retention curves for BCTMP sludge, BCTMP sludge-soil mixtures 40:10, 25:25 and 10:40 from 0.1 to 15 bar x (-1). 135 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment blend 30:20 20:30 0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 pressure [bar] x (-1) FIGURE 2 4 : Moisture retention curves fo r blended BCTMP sludge, BCTMP sludge-soil mixtures 20:30 and 30:20 from 0.1 to 15 bar x (-1). 136 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment ♦ — original X 25:25 ■ 10:40 E 50 0.0 2.0 0.5 2.5 pressure [bar] x (-1) FIGURE 2 5 : Moisture retention curves for BCTMP sludge, BCTMP sludge-soil mixtures 40:10, 25:25 and 10:40 from 0.1 to 2.5 b a rx (-1). 137 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment 80 70 60 40 30 20 0.0 0.5 1.0 1.5 2.0 2.5 pressure [bar] x (-1) FIGURE 26 : Moisture retention curves for blended BCTMP sludge, BCTMP sludge-soil mixtures 20:30 and 30:20 from 0.1 to 2.5 bar x (-1). 138 Appendix I: Pressure Plate Experiment Moisture retention curves for BCTMP sludge-soil mixtures with random errors original 40:10 25:25 10:40 ^ 60 E 40 0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 pressure [bar] x (-1) F IG U R E 2 7 : Moisture retention curves for BCTM P sludge, BCTM P sludge-soil mixtures 40:10, 25:25 and 10:40 with random errors from 0.1 to 15 b a rx (-1). 30 0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 pressure [bar] x (-1) F IG U R E 28 : Moisture retention curves for blended BCTM P sludge, BCTM P sludge-soil mixtures 30:20 and 20:30 with random errors from 0.1 to 15 bar x (-1). 139 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment 80 —♦ — original - * — 40:10 0.0 X 25:25 a 10:40 2.0 0.5 2.5 pressure [bar] x (-1) F IG U R E 29 : Moisture retention curves for BCTM P sludge, B C TM P sludge-soil mixtures 40:10, 25:25 and 10:40 with random errors from 0.1 to 2.5 bar x (-1). hh— blend A 30:20 •--2 0 :3 0 0.0 2.0 0.5 2.5 pressure [bar] x (-1) F IG U R E 30 : Moisture retention curves for blended BCTM P sludge, BCTM P sludge-soil mixtures 30:20 and 20:30 with random errors from 0.1 to 2.5 bar x (-1). Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment Part C : Moisture retention curves for sludge-soil layer systems TABLE 82: Raw data for bulk density, W H C g and W H C V determination of each sludge and soil layer for Kraft mill sludge. pressure [bar] 0.5 sample [g] 1 layer 2 layer 3 layer 1.0 column empty column&sample mass wet 1 layer 2 layer 3 layer sludge (1/1) soil (1/1) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (1/3) soil (1/3) sludge (1/1) soil (1/1) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (1/3) soil (1/3) 63.636 63.636 63.184 63.184 63.184 63.184 63.956 63.956 63.956 63.956 63.956 63.956 63.670 63.670 63.112 63.112 63.112 63.112 63.760 63.760 63.760 63.760 63.760 63.760 [g] [g] 105.876 233.100 90.656 138.430 163.370 221.905 80.854 121.990 139.910 179.120 191.845 234.665 106.402 240.765 90.836 145.445 170.240 235.855 81.566 122.045 142.875 182.695 198.170 239.965 42.240 127.224 27.472 47.774 24.940 58.535 16.898 41.136 17.920 39.210 12.725 42.820 42.732 134.363 27.724 54.609 24.795 65.615 17.806 40.479 20.830 39.820 15.475 4 1.795 height [cm] volume [cm3] mass dry 2.5 3.2 1.5 1.5 1.5 1.5 1.0 1.0 1.0 1.0 1.0 1.0 3.0 3.0 1.5 1.5 1.5 1.5 1.0 1.0 1.0 1.0 93.435 119.596 56.061 56.061 56.061 56.061 37.374 37.374 37.374 37.374 37.374 37.374 112.122 112.122 56.061 56.061 56.061 56.061 37.374 37.374 9.281 93.857 6.028 35.819 5.741 43.036 3.871 30.95998 4.347611 29.17028 3.34202 31.72521 12.39111 101.0059 8.21771 41.82798 7.562232 1.0 1.0 37.374 37.374 37.374 37.374 [g] 49.3774 5.499461 30.79523 6.488033 28.56459 4.805622 31.65859 Db [g/cm3] 0.099 0.785 0.108 0.639 0.102 0.768 0.104 0.828 0.116 0.780 0.089 0.849 0.111 0.901 0.147 0.746 0.135 0.881 0.147 0.824 0.174 0.764 0.129 0.847 WHCg WHCV [%] 355 36 356 33 334 36 337 33 312 34 281 35 245 33 237 31 228 33 224 31 221 40 222 32 [%] 35 28 38 21 34 28 35 27 36 27 25 30 27 30 35 23 31 29 33 26 38 31 29 27 141 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment pressure [bar] sample 5.0 sludge (1/1) soil (1/1) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (1/3) soil (1/3) 1 layer 2 layer 3 layer column empty column&sample mass [g] [g] [g] height [cm] 63.504 63.504 63.958 63.958 63.958 63.958 63.934 63.934 63.934 63.934 63.934 63.934 106.128 233.500 91.160 146.480 167.945 236.305 81.026 122.190 140.660 180.260 193.210 235.190 42.624 127.372 27.202 55.320 21.465 68.360 17.092 41.164 18.470 39.600 12.950 41.980 2.9 3.0 1.6 1.5 1.5 1.5 1.0 1.0 1.1 1.0 0.9 1.0 volume [cm3] mass dry [g] Db [g/cm3] 108.384 112.122 59.798 56.061 56.061 56.061 37.374 37.374 41.111 37.374 33.636 37.374 14.5458 96.47162 8.942058 41.85136 6.860678 51.64439 6.731907 31.59084 6.914675 30.29019 4.810314 32.34456 0.134 0.860 0.150 0.747 0.122 0.921 0.180 0.845 0.168 0.810 0.143 0.865 WHCg W HCV [%] 193 32 204 32 213 32 154 30 167 30 169 30 [%] 26 28 31 24 26 29 28 25 28 24 24 26 142 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment TABLE 83: Raw data for bulk density, W H C g and W H C V determination of each sludge and soil layer for B C TM P sludge. pressure [bar] sample 0.5 sludge (1/1) soil (1/1) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (1/3) soil (1/3) sludge (1/1) soil (1/1) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (1/3) soil (1/3) 1 layer 2 layer 3 layer 1.0 1 layer 2 layer 3 layer column empty column&sample mass wet [g] [g] [g] 61.758 61.758 62.266 62.266 62.266 62.266 61.862 61.862 61.862 61.862 61.862 61.862 61.670 61.670 62.184 62.184 62.184 62.184 133.890 260.180 100.600 153.630 194.095 258.420 83.036 123.930 143.200 193.535 215.145 258.200 139.925 245.480 99.570 152.285 188.010 239.860 89.590 130.210 152.750 199.990 220.950 258.185 72.132 126.290 38.334 53.030 40.465 64.325 21.174 40.894 19.270 50.335 21.610 43.055 78.255 105.555 37.386 52.715 35.725 51.850 61.832 61.832 61.832 61.832 61.832 61.832 27.758 40.620 22.540 47.240 20.960 37.235 height [cm] volume [cm3] mass dry 3.0 3.0 1.5 1.5 1.7 1.5 1.0 1.0 1.0 1.0 1.1 1.0 3.0 3.0 1.5 1.5 1.5 1.5 1.0 1.0 1.0 1.0 1.0 1.0 112.122 112.122 56.061 56.061 63.536 56.061 37.374 37.374 37.374 37.374 41.111 37.374 112.122 112.122 56.061 56.061 56.061 56.061 37.374 37.374 37.374 37.374 37.374 37.374 18.257 92.116 9.951 38.920 10.389 45.888 5.592 29.689 5.277 36.948 5.918 31.228 21.634 78.350 10.607 39.037 10.207 38.540 8.031 29.971 6.560 34.766 6.097 [g] 27.713 Db [g/cm3] 0.163 0.822 0.178 0.694 0.164 0.819 0.150 0.794 0.141 0.989 0.144 0.836 0.193 0.699 0.189 0.696 0.182 0.687 0.215 0.802 0.176 0.930 0.163 0.742 WHCg WHCV [%] 295 37 285 36 289 40 279 38 277 36 266 38 262 35 253 35 250 35 246 36 244 36 244 34 [%] 48 30 51 25 47 33 42 30 39 36 38 32 51 24 48 24 46 24 53 29 43 33 40 25 143 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment pressure [bar] sample 5.0 sludge (1/1) soil (1/1) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (1/1) soil (1/1) sludge (1/2) soil (1/2) sludge (1/3) soil (1/3) 1 layer 2 layer 3 layer column empty column&sample mass wet [g] [g] [g] height [cm] 64.270 64.270 63.998 63.998 63.998 63.998 64.812 64.812 64.812 64.812 64.812 64.812 136.550 260.810 101.120 154.380 195.040 259.625 86.754 126.575 146.305 196.490 218.715 261.520 72.280 124.260 37.122 53.260 40.660 64.585 21.942 39.821 19.730 50.185 22.225 42.805 3.0 3.0 1.5 1.5 1.5 1.5 1.0 1.0 1.0 1.0 1.0 1.0 volume [cm3] mass dry [g] Db [g/cm3] 112.122 112.122 56.061 56.061 56.061 56.061 37.374 37.374 37.374 37.374 37.374 37.374 21.204 92.100 11.542 39.823 11.999 48.718 6.973 29.960 6.272 37.705 6.698 32.323 0.189 0.821 0.206 0.710 0.214 0.869 0.187 0.802 0.168 1.009 0.179 0.865 WHCg W HCV [%] 241 35 222 34 239 33 215 33 215 33 221 32 [%] 46 29 46 24 51 29 40 26 36 33 40 28 144 Appendix I: Pressure Plate Experiment TABLE 84: Determination of bulk density, gravimetric and volumetric moisture content with random errors of each layer and the total W H C V of the sludge-soil layers for Kraft mill sludge. pressure sam ple [bar] 0.5 sludge (1/1) 1.0 5.0 soil (1/1) sludge (1/1) sludge (1/2) soil (1/1) soil (1/2) sludge (1/1) sludge (1/2) sludge (1/3) soil (1/1) soil (1/2) soil (1/3) sludge (1/1) soil (1/1) sludge (1/1) sludge (1/2) soil (1/1) soil (1/2) sludge (1/1) sludge (1/2) sludge (1/3) soil (1/1) soil (1/2) soil (1/3) sludge (1/1) soil (1/1) sludge (1/1) sludge (1/2) soil (1/1) soil (1/2) sludge (1/1) sludge (1/2) sludge (1/3) soil (1/1) soil (1/2) soil (1/3) WHCg ± A WHCg Db ± A Db W HCV [%] 355 36 356 334 33 36 337 312 281 33 34 35 245 33 237 228 31 33 224 221 222 31 40 32 193 32 204 213 32 32 154 167 169 30 31 30 [%] 0.058 0.002 0.090 0.089 0.006 0.005 0.134 0.111 0.133 0.007 0.007 0.006 0.032 0.002 0.047 0.050 0.005 0.004 0.068 0.057 0.077 0.007 0.007 0.006 0.023 0.002 0.039 0.053 0.005 0.004 0.044 [g/cm 3] 0.099 0.785 0.108 0.102 0.639 0.768 0.104 0.116 0.089 0.828 0.780 0.849 0.111 0.901 0.147 0.135 0.746 0.881 0.147 0.174 0.129 0.824 [g/cm 3] [%] 35 28 38 34 21 28 35 36 25 27 27 30 27 30 35 31 23 29 33 38 29 26 31 27 26 28 31 26 24 29 28 28 24 0.045 0.065 0.006 0.007 0.006 0.764 0.847 0.134 0.860 0.150 0.122 0.747 0.921 0.180 0.168 0.143 0.845 0.810 0.865 0.0008 0.0049 0.0014 0.0014 0.0085 0.0102 0.0021 0.0023 0.0018 0.0166 0.0156 0.0170 0.0007 0.0060 0.0020 0.0018 0.0100 0.0118 0.0029 0.0035 0.0026 0.0165 0.0153 0.0170 0.0009 0.0058 0.0019 0.0016 0.0100 0.0123 0.0036 0.0031 0.0032 0.0169 0.0162 0.0173 25 24 26 ± A W H C V total WHCV ± A W H C V [%] 0.283 0.177 0.511 0.466 0.281 0.369 [%] [%] 31.76 0.167 30.30 0.208 30.05 0.248 28.40 0.134 29.42 0.199 30.58 0.252 26.72 0.128 26.79 0.181 25.99 0.213 0.699 0.727 0.512 0.547 0.531 0.595 0.181 0.199 0.464 0.414 0.309 0.388 0.660 0.768 0.574 0.511 0.612 0.543 0.179 0.184 0.382 0.351 0.319 0.394 0.555 0.511 0.540 0.508 0.487 0.520 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment TABLE 85: Determination of bulk density, gravimetric and volumetric moisture content with random errors of each layer and the total W H C V of the sludge-soil layers for B C TM P sludge. pressure [bar] sample 0.5 sludge (1/1) soil (1/1) sludge (1/1) sludge (1/2) soil (1/1) soil (1/2) sludge (1/1) sludge (1/2) sludge (1/3) soil (1/1) soil (1/2) soil (1/3) sludge (1/1) soil (1/1) sludge (1/1) sludge (1/2) soil (1/1) 1.0 5.0 soil (1/2) sludge (1/1) sludge (1/2) sludge (1/3) soil (1/1) soil (1/2) soil (1/3) sludge (1/1) soil (1/1) sludge (1/1) sludge (1/2) soil (1/1) soil (1/2) sludge (1/1) sludge (1/2) sludge (1/3) soil (1/1) soil (1/2) soil (1/3) WHCg ± A WHCg [%] 295 37 285 289 36 40 279 277 266 38 36 38 262 35 253 250 35 35 246 244 244 36 36 34 241 35 222 239 34 33 215 215 221 33 33 32 [%] 0.025 0.002 0.045 0.044 0.005 0.005 0.079 0.084 0.072 0.007 0.006 0.007 0.019 0.003 0.039 0.040 0.005 0.005 0.050 0.061 0.065 0.007 0.006 0.007 0.019 0.002 0.032 0.033 0.005 0.004 0.052 0.058 0.082 0.007 0.005 0.006 Db [g/cm3] ± A Db [g/cm3] 0.163 0.822 0.178 0.164 0.0011 0.0055 0.0024 0.0019 0.694 0.819 0.150 0.141 0.144 0.794 0.989 0.836 0.193 0.699 0.189 0.182 0.696 0.687 0.215 0.176 0.163 0.802 0.930 0.742 0.189 0.821 0.206 0.214 0.0093 0.0109 0.0030 0.0028 0.0026 0.0159 0.0198 0.0167 0.0013 0.0047 0.0025 0.0024 0.0093 0.0092 0.0043 0.0035 0.0033 0.0161 0.0186 0.0148 0.0013 0.0055 0.0027 0.0029 0.710 0.869 0.187 0.168 0.179 0.802 0.0095 0.0116 0.0037 0.0034 0.0036 0.0160 0.0202 0.0173 1.009 0.865 WHCV ± A WHCV total WHCV ± A WHCV [%] 48 30 51 47 [%] 0.321 0.203 0.675 0.560 25 33 42 39 38 30 36 32 51 24 48 46 24 24 53 43 40 29 33 25 46 29 0.334 0.437 0.836 0.783 0.712 0.604 0.701 0.636 0.338 0.163 0.639 0.610 0.325 0.321 1.058 0.857 0.800 0.578 0.670 0.505 0.305 0.192 46 51 24 29 40 36 40 26 33 28 0.610 0.685 0.322 0.383 0.803 0.722 0.792 0.530 0.666 0.554 [%] [%] 39.22 0.190 38.90 0.259 36.18 0.292 37.51 0.188 35.45 0.249 37.25 0.313 37.16 0.180 37.42 0.261 34.00 0.280 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Appendix I: Pressure Plate Experiment Summary: Volumetric moisture content determination for Kraft mill sludge-soil layers TABLE 86: Total volumetric moisture content of 1, 2, and 3 Kraft mill sludge-soil layer systems at 0.5, 1.0, and 5.0 bar pressure with random errors. 5.0 bar 1.0 bar 0.5 bar WHCV ± A WHCV total WHCV ± A WHCV WHCV ± A WHCV total WHCV ± A WHCV WHCV ± A WHCV total WHCV ± A WHCV [%] [%] [%] [%] [%] [%] [%] [%] [%] [%] [%] [%] pressure Kraft mill 1 layer Kraft mill 2 layers Kraft mill 3 layers sludge soil sludge 1 sludge 2 soil 1 soil 2 sludge 1 sludge 2 sludge 3 soil 1 soil 2 soil 3 35 28 38 34 21 28 35 36 25 27 27 30 0.283 0.177 0.511 0.466 0.281 0.369 0.699 0.727 0.512 0.547 0.531 0.595 31.8 0.167 30.3 0.208 30.1 0.248 27 30 35 31 23 29 33 38 29 26 31 27 0.181 0.199 0.464 0.414 0.309 0.388 0.660 0.768 0.574 0.511 0.612 0.543 28.4 0.134 29.4 0.199 30.6 0.252 26 28 31 26 24 29 28 28 24 25 24 26 0.179 0.184 0.382 0.351 0.319 0.394 0.555 0.511 0.540 0.508 0.487 0.520 26.7 0.128 26.8 0.181 26.0 0.213 Summary: Volumetric moisture content determination for BCTMP sludge-soil layers TABLE 87: Total volumetric moisture content of 1, 2, and 3 BCTMP sludge-soil layer systems at 0.5, 1.0, and 5.0 bar pressure with random errors. 5.0 bar 0.5 bar 1.0 bar WHCV ± A WHCV total WHCV ± A WHCV WHCV ± A WHCV total WHCV ± A WHCV WHCV ± A WHCV total WHCV ± A WHCV pressure BCTMP 1 layer BCTMP 2 layers BCTMP 3 layers sludge soil sludge 1 sludge 2 soil 1 soil 2 sludge 1 sludge 2 sludge 3 soil 1 soil 2 soil 3 [%] 48 30 51 47 25 33 42 39 38 30 36 32 [%] 0.321 0.203 0.675 0.560 0.334 0.437 0.836 0.783 0.712 0.604 0.701 0.636 [%] [%] 39.2 0.190 38.9 0.259 36.2 0.292 [%] 51 24 48 46 24 24 53 43 40 29 33 25 [%] 0.338 0.163 0.639 0.610 0.325 0.321 1.058 0.857 0.800 0.578 0.670 0.505 [%] [%] 37.5 0.188 35.5 0.249 37.3 0.313 [%] 46 29 46 51 24 29 40 36 40 26 33 28 [%] 0.305 0.192 0.610 0.685 0.322 0.383 0.803 0.722 0.792 0.530 0.666 0.554 [%] [%] 37.2 0.180 37.4 0.261 34.0 0.282 147