Professional Documents
Culture Documents
Steven M. Heilmann †*, Joseph S. Molde †, Jacobe G. Timler †, Brandon M. Wood †, Anthony L. Mikula †,
Georgiy V. Vozhdayev†1, Edward C. Colosky║, Kurt A. Spokas ║,‡ and Kenneth J. Valentas †
† University of Minnesota, Biotechnology Institute, 140 Gortner Laboratory, 1479 Gortner Ave., St. Paul, MN,
55108-1041, USA
║ United States Department of Agriculture, Agricultural Research Service, Soil and Water Management Research
Unit, 1991 Buford Circle, 439 Borlaug Hall, St. Paul, MN, 55108-1041
‡ University of Minnesota, Department of Soil, Water, and Climate, 1991 Buford Circle, 439 Borlaug Hall, St. Paul,
MN, 55108-1041
Digestion of solid starting waste and hydrochar materials was conducted using the following
procedure: Approximately 100 mg of powdered sample was placed in a 30 mL Teflon sleeve also
containing a small magnetic stirring bar. Deionized water (1 mL), concentrated hydrochloric acid (1.5
mL), concentrated hydrofluoric acid (1.5 mL), and concentrated nitric acid (3 mL) were added. The
sleeve was placed in a 30 mL Pyrex tube and capped. The vessel was then microwaved in a CEM
Discover SP-D system available from CEM, Inc. (Matthews, NC) at a temperature of 200o C, with a ramp
and hold time of 8 minutes each. After cooling, a 4% boric acid aqueous solution (13 mL) was
added. This was microwaved at 160o C, with a ramp of 8 minutes and a hold time of 4 minutes. After
cooling, 10 mL of deionized water was added. The resulting solution was diluted 20 fold and an yttrium
internal standard was added before analysis using a Thermo iCAP 6500 ICP-OES available from Thermo
Tables:
S2
a
= From 225º C experiments, standard deviations (σs) were: 0.49 for % Yield, 0.14 for %C, 0.04 for %H, 0.06 for
%N, 0.10 for %P, and 0.60 for System % P in Hydrochar.
b
= Ash content of the hydrochar was 26.89%.
Table S2. Linear regression coefficients for the various outputs from the poultry manure DOE.
Output Intercept Time Temp. Solids Time*Temp Time*Solids Temp*Solids R2
Table S4. Linear regression coefficients for the various outputs from the swine manure DOE.
a
= From 250º C experiments, standard deviations (σs) were: 0.07 for % Yield, 0.32 for %C, 0.20 for %H, 0.07 for
%N, 0.12 for %P, and 2.94 for System % P in Hydrochar.
b
= Ash content of the hydrochar was 22.57%.
Table S6. Linear regression coefficients for the various outputs from the dairy cattle DOE
%P In
Hydro-
Char
Note: The EDS technique measures a variable depth of penetration as a function of the material and is not
confined solely to the surface. These percentages are representative for the interaction volume of the x-
ray beam with the sample, which will be highly variable in these heterogeneous materials and might not
Figures:
Figure S1. SEM and EDS analysis of dairy cattle manure hydrochar.
Weight %
C N O Na Mg Al Si P S Cl K Ca Mn Fe Cu
Cattle_Point1 65.44 0.00 23.65 0.00 2.01 0.00 3.15 0.91 0.97 0.00 0.00 1.94 0.00 1.93 0.00
Cattle_Point2 64.98 0.00 24.19 0.00 0.00 0.00 0.53 0.90 0.13 0.00 1.27 7.99 0.00 0.00 0.00
Cattle_Point3 72.77 0.00 23.62 0.15 0.00 0.00 0.28 0.79 0.42 0.84 0.41 0.70 0.00 0.00 0.00
Cattle_Point4 58.48 3.17 21.45 0.06 2.05 0.23 2.25 3.23 0.53 0.04 0.02 6.16 0.39 1.00 0.93
Weight % Error
C N O Na Mg Al Si P S Cl K Ca Mn Fe Cu
Cattle_Point1 +/-2.97 +/-0.00 +/-2.88 +/-0.00 +/-0.50 +/-0.00 +/-0.73 +/-0.52 +/-0.64 +/-0.00 +/-0.00 +/-0.97 +/-0.00 +/-3.86 +/-0.00
Cattle_Point2 +/-3.05 +/-0.00 +/-4.48 +/-0.00 +/-0.00 +/-0.00 +/-0.53 +/-0.72 +/-0.26 +/-0.00 +/-0.84 +/-1.88 +/-0.00 +/-0.00 +/-0.00
Cattle_Point3 +/-3.17 +/-0.00 +/-3.06 +/-0.45 +/-0.00 +/-0.00 +/-0.37 +/-0.40 +/-0.42 +/-0.42 +/-0.62 +/-0.70 +/-0.00 +/-0.00 +/-0.00
Cattle_Point4 +/-0.52 +/-2.23 +/-0.55 +/-0.06 +/-0.10 +/-0.05 +/-0.07 +/-0.09 +/-0.07 +/-0.06 +/-0.08 +/-0.18 +/-0.35 +/-0.48 +/-3.43
Atom %
C N O Na Mg Al Si P S Cl K Ca Mn Fe Cu
Cattle_Point1 75.00 0.00 20.35 0.00 1.14 0.00 1.55 0.41 0.42 0.00 0.00 0.67 0.00 0.48 0.00
Cattle_Point2 75.08 0.00 20.98 0.00 0.00 0.00 0.26 0.40 0.06 0.00 0.45 2.77 0.00 0.00 0.00
Cattle_Point3 79.28 0.00 19.32 0.09 0.00 0.00 0.13 0.34 0.17 0.31 0.14 0.23 0.00 0.00 0.00
Cattle_Point4 70.28 3.27 19.35 0.04 1.22 0.12 1.16 1.51 0.24 0.01 0.01 2.22 0.10 0.26 0.21
Atom % Error
C N O Na Mg Al Si P S Cl K Ca Mn Fe Cu
Cattle_Point1 +/-3.41 +/-0.00 +/-2.48 +/-0.00 +/-0.29 +/-0.00 +/-0.36 +/-0.23 +/-0.28 +/-0.00 +/-0.00 +/-0.33 +/-0.00 +/-0.95 +/-0.00
Cattle_Point2 +/-3.53 +/-0.00 +/-3.89 +/-0.00 +/-0.00 +/-0.00 +/-0.26 +/-0.32 +/-0.11 +/-0.00 +/-0.30 +/-0.65 +/-0.00 +/-0.00 +/-0.00
Cattle_Point3 +/-3.45 +/-0.00 +/-2.50 +/-0.26 +/-0.00 +/-0.00 +/-0.17 +/-0.17 +/-0.17 +/-0.16 +/-0.21 +/-0.23 +/-0.00 +/-0.00 +/-0.00
Cattle_Point4 +/-0.62 +/-2.30 +/-0.50 +/-0.04 +/-0.06 +/-0.03 +/-0.04 +/-0.04 +/-0.03 +/-0.03 +/-0.03 +/-0.06 +/-0.09 +/-0.13 +/-0.78
S8
Weight %
C N O Na Mg Al Si P S Cl K Ca Ti V Mn Fe Cu Mo
Poultry – Point 1 58.38 5.88 16.70 0.02 0.63 1.36 1.41 4.75 0.79 0.10 0.00 5.26 0.66 1.12 2.34 0.60
Poultry – Point 2 53.05 3.45 19.74 0.40 1.40 2.67 2.71 3.85 0.99 0.12 0.12 4.13 0.77 0.84 3.80 1.95
Poultry – Point 3 44.88 1.76 32.02 0.13 0.76 1.77 11.63 3.58 0.41 0.00 0.09 1.94 0.43 0.59 0.00
Poultry – Point 4 61.50 0.00 16.32 0.29 0.88 2.43 2.38 6.20 1.30 0.18 0.13 5.42 1.43 1.54 0.00
Poultry – Point 5 51.51 2.78 18.91 0.36 1.52 2.67 1.09 7.34 1.01 0.24 0.12 5.80 2.15 4.50 0.00
Poultry – Point 6 53.88 1.68 17.51 0.28 1.38 2.74 1.30 7.48 0.93 0.15 0.07 6.20 1.41 5.00 0.00
Poultry – Point 7 72.18 0.84 20.02 0.05 0.29 0.79 0.57 1.54 0.35 0.00 0.00 1.85 0.24 0.87 0.00 0.41
Weight % Error
C N O Na Mg Al Si P S Cl K Ca Ti V Mn Fe Cu Mo
Poultry – Point 1 +/-0.48 +/-1.92 +/-0.52 +/-0.06 +/-0.05 +/-0.06 +/-0.06 +/-0.10 +/-0.07 +/-0.07 +/-0.00 +/-0.16 +/-0.18 +/-0.38 +/-0.56 +/-3.60
Poultry – Point 2 +/-0.49 +/-1.83 +/-0.50 +/-0.08 +/-0.10 +/-0.07 +/-0.08 +/-0.10 +/-0.08 +/-0.07 +/-0.08 +/-0.15 +/-0.16 +/-0.42 +/-0.62 +/-3.90
Poultry – Point 3 +/-0.44 +/-1.76 +/-0.52 +/-0.06 +/-0.10 +/-0.07 +/-0.22 +/-0.19 +/-0.08 +/-0.00 +/-0.09 +/-0.13 +/-0.41 +/-0.59 +/-0.00
Poultry – Point 4 +/-0.58 +/-0.00 +/-0.99 +/-0.09 +/-0.08 +/-0.09 +/-0.10 +/-0.16 +/-0.12 +/-0.10 +/-0.14 +/-0.43 +/-0.70 +/-1.04 +/-0.00
Poultry – Point 5 +/-0.57 +/-2.08 +/-0.55 +/-0.09 +/-0.12 +/-0.08 +/-0.07 +/-0.21 +/-0.09 +/-0.09 +/-0.10 +/-0.19 +/-0.54 +/-0.87 +/-0.00
Poultry – Point 6 +/-0.50 +/-2.32 +/-0.86 +/-0.09 +/-0.07 +/-0.14 +/-0.08 +/-0.15 +/-0.10 +/-0.09 +/-0.11 +/-0.21 +/-0.57 +/-0.93 +/-0.00
Poultry – Point 7 +/-0.47 +/-2.76 +/-0.61 +/-0.06 +/-0.05 +/-0.09 +/-0.06 +/-0.08 +/-0.24 +/-0.00 +/-0.00 +/-0.14 +/-0.48 +/-0.62 +/-0.00 +/-0.67
Atom %
C N O Na Mg Al Si P S Cl K Ca Ti V Mn Fe Cu Mo
Poultry – Point 1 70.97 6.13 15.24 0.01 0.38 0.73 0.73 2.24 0.36 0.04 0.00 1.92 0.19 0.30 0.61 0.14
Poultry – Point 2 67.31 3.75 18.80 0.27 0.88 1.51 1.47 1.89 0.47 0.05 0.05 1.57 0.24 0.23 1.04 0.47
Poultry – Point 3 56.81 1.91 30.42 0.09 0.47 1.00 6.29 1.76 0.19 0.00 0.03 0.74 0.12 0.16 0.00
Poultry – Point 4 75.28 0.00 15.00 0.18 0.53 1.32 1.25 2.94 0.59 0.08 0.05 1.99 0.38 0.40 0.00
Poultry – Point 5 66.72 3.09 18.38 0.24 0.97 1.54 0.61 3.69 0.49 0.10 0.05 2.25 0.61 1.25 0.00
Poultry – Point 6 69.40 1.86 16.93 0.19 0.88 1.57 0.71 3.74 0.45 0.07 0.03 2.39 0.40 1.39 0.00
Poultry – Point 7 79.96 0.79 16.65 0.03 0.16 0.39 0.27 0.66 0.15 0.00 0.00 0.61 0.06 0.21 0.00 0.06
Atom % Error
C N O Na Mg Al Si P S Cl K Ca Ti V Mn Fe Cu Mo
Poultry – Point 1 +/-0.58 +/-2.00 +/-0.47 +/-0.03 +/-0.03 +/-0.03 +/-0.03 +/-0.05 +/-0.03 +/-0.03 +/-0.00 +/-0.06 +/-0.05 +/-0.10 +/-0.15 +/-0.84
Poultry – Point 2 +/-0.62 +/-1.99 +/-0.48 +/-0.05 +/-0.06 +/-0.04 +/-0.04 +/-0.05 +/-0.04 +/-0.03 +/-0.03 +/-0.06 +/-0.05 +/-0.11 +/-0.17 +/-0.94
Poultry – Point 3 +/-0.56 +/-1.91 +/-0.50 +/-0.04 +/-0.06 +/-0.04 +/-0.12 +/-0.09 +/-0.04 +/-0.00 +/-0.03 +/-0.05 +/-0.11 +/-0.16 +/-0.00
Poultry – Point 4 +/-0.72 +/-0.00 +/-0.91 +/-0.05 +/-0.05 +/-0.05 +/-0.05 +/-0.07 +/-0.05 +/-0.05 +/-0.05 +/-0.16 +/-0.19 +/-0.27 +/-0.00
Poultry – Point 5 +/-0.74 +/-2.31 +/-0.54 +/-0.06 +/-0.07 +/-0.05 +/-0.04 +/-0.11 +/-0.05 +/-0.04 +/-0.04 +/-0.08 +/-0.15 +/-0.24 +/-0.00
Poultry – Point 6 +/-0.64 +/-2.57 +/-0.83 +/-0.06 +/-0.05 +/-0.08 +/-0.05 +/-0.07 +/-0.05 +/-0.04 +/-0.05 +/-0.08 +/-0.16 +/-0.26 +/-0.00
Poultry – Point 7 +/-0.52 +/-2.60 +/-0.51 +/-0.04 +/-0.03 +/-0.04 +/-0.03 +/-0.03 +/-0.10 +/-0.00 +/-0.00 +/-0.04 +/-0.12 +/-0.15 +/-0.00 +/-0.10
Weight %
C N O Na Mg Al Si P S Cl K Ca Mn Fe Cu
Swine_pt1 32.33 0.00 29.35 0.00 18.94 0.00 0.00 17.15 0.00 0.39 0.00 0.00 1.23 0.61 0.00
Swine_pt2 46.28 0.00 14.91 0.18 1.76 3.34 1.21 10.15 0.97 0.34 1.34 11.46 0.00 7.91 0.16
Swine_pt3 50.60 2.69 26.04 0.12 4.50 0.00 0.00 12.52 0.03 0.00 1.49 0.70 0.59 0.72 0.00
Swine_pt4 74.61 5.39 14.08 0.15 1.43 0.00 0.13 2.75 0.39 0.09 0.70 0.16 0.09 0.03 0.00
Swine_pt5 67.31 5.60 12.84 0.18 2.89 0.00 0.01 8.95 0.34 0.18 0.84 0.04 0.00 0.81 0.00
Swine_pt6 81.18 3.31 9.53 0.00 0.22 0.00 0.04 2.34 1.08 0.12 1.34 0.60 0.00 0.24 0.00
Weight % Error
C N O Na Mg Al Si P S Cl K Ca Mn Fe Cu
Swine_pt1 +/-0.57 +/-0.00 +/-0.66 +/-0.00 +/-0.42 +/-0.00 +/-0.00 +/-0.68 +/-0.00 +/-0.56 +/-0.00 +/-0.00 +/-2.93 +/-1.27 +/-0.00
Swine_pt2 +/-0.45 +/-0.00 +/-0.41 +/-0.16 +/-0.17 +/-0.31 +/-0.22 +/-0.61 +/-0.37 +/-0.44 +/-0.85 +/-1.91 +/-0.00 +/-1.06 +/-0.43
Swine_pt3 +/-0.61 +/-2.09 +/-0.57 +/-0.06 +/-0.11 +/-0.00 +/-0.00 +/-0.17 +/-0.08 +/-0.00 +/-0.14 +/-0.15 +/-0.59 +/-0.78 +/-0.00
Swine_pt4 +/-0.50 +/-2.06 +/-0.46 +/-0.05 +/-0.05 +/-0.00 +/-0.04 +/-0.07 +/-0.06 +/-0.05 +/-0.07 +/-0.07 +/-0.17 +/-0.11 +/-0.00
Swine_pt5 +/-0.84 +/-3.32 +/-0.74 +/-0.10 +/-0.14 +/-0.00 +/-0.08 +/-0.29 +/-0.13 +/-0.14 +/-0.22 +/-0.24 +/-0.00 +/-0.49 +/-0.00
Swine_pt6 +/-0.55 +/-2.51 +/-0.56 +/-0.00 +/-0.05 +/-0.00 +/-0.06 +/-0.09 +/-0.09 +/-0.10 +/-0.13 +/-0.15 +/-0.00 +/-0.78 +/-0.00
Atom %
C N O Na Mg Al Si P S Cl K Ca Mn Fe Cu
Swine_pt1 45.60 0.00 31.07 0.00 13.20 0.00 0.00 9.38 0.00 0.19 0.00 0.00 0.38 0.18 0.00
Swine_pt2 65.71 0.00 15.89 0.13 1.23 2.11 0.73 5.59 0.51 0.16 0.59 4.87 0.00 2.42 0.04
Swine_pt3 62.81 2.87 24.26 0.07 2.76 0.00 0.00 6.03 0.01 0.00 0.57 0.26 0.16 0.19 0.00
Swine_pt4 80.94 5.01 11.47 0.09 0.77 0.00 0.06 1.16 0.16 0.03 0.23 0.05 0.02 0.01 0.00
Swine_pt5 77.02 5.49 11.03 0.11 1.63 0.00 0.01 3.97 0.15 0.07 0.29 0.01 0.00 0.20 0.00
Swine_pt6 87.01 3.04 7.67 0.00 0.12 0.00 0.02 0.97 0.43 0.04 0.44 0.19 0.00 0.05 0.00
Atom % Error
C N O Na Mg Al Si P S Cl K Ca Mn Fe Cu
Swine_pt1 +/-0.81 +/-0.00 +/-0.70 +/-0.00 +/-0.29 +/-0.00 +/-0.00 +/-0.37 +/-0.00 +/-0.27 +/-0.00 +/-0.00 +/-0.90 +/-0.39 +/-0.00
Swine_pt2 +/-0.64 +/-0.00 +/-0.44 +/-0.12 +/-0.12 +/-0.20 +/-0.13 +/-0.33 +/-0.20 +/-0.21 +/-0.37 +/-0.81 +/-0.00 +/-0.32 +/-0.11
Swine_pt3 +/-0.76 +/-2.23 +/-0.53 +/-0.04 +/-0.07 +/-0.00 +/-0.00 +/-0.08 +/-0.04 +/-0.00 +/-0.05 +/-0.06 +/-0.16 +/-0.21 +/-0.00
Swine_pt4 +/-0.55 +/-1.91 +/-0.37 +/-0.03 +/-0.03 +/-0.00 +/-0.02 +/-0.03 +/-0.02 +/-0.02 +/-0.02 +/-0.02 +/-0.04 +/-0.03 +/-0.00
Swine_pt5 +/-0.97 +/-3.26 +/-0.64 +/-0.06 +/-0.08 +/-0.00 +/-0.04 +/-0.13 +/-0.06 +/-0.05 +/-0.08 +/-0.08 +/-0.00 +/-0.12 +/-0.00
Swine_pt6 +/-0.59 +/-2.30 +/-0.45 +/-0.00 +/-0.03 +/-0.00 +/-0.03 +/-0.04 +/-0.04 +/-0.04 +/-0.04 +/-0.05 +/-0.00 +/-0.18 +/-0.00