Polyaluminum Sulfate with Reduced Chloride Content

Abstract

Methods are described for manufacturing ultra-low chloride, polyaluminum sulfate (PAS) coagulants useful for removing suspended colloidal matter and organic carbon in potable water, industrial process water and wastewater. A method of preparing a PAS solution includes forming a basic solution of sodium carbonate and sodium aluminate, adding an aqueous solution of aluminum sulfate and the basic solution to water to form a mixture having a pH between about 5 to 7, allowing precipitates of aluminum hydroxide to form in the mixture, and adding an additional aqueous solution of aluminum sulfate in an amount sufficient to dissolve the precipitates of the aluminum hydroxide and to form the PAS solution. The PAS solution has reduced corrosivity compared to other aluminum-based coagulants, and is particularly suitable for drinking water applications. The simplified methods used to produce the PAS coagulant provide a high quality product that is less expensive to produce than current methods.

Claims

1. A method of preparing a polyaluminum sulfate (PAS) solution with reduced chloride content, the method comprising: forming a basic solution of sodium carbonate and sodium aluminate; adding an aqueous solution of aluminum sulfate and the basic solution to water to form a mixture having a pH between about 5 and about 7; allowing precipitates of aluminum hydroxide to form in the mixture; and adding an additional aqueous solution of aluminum sulfate to the mixture in an amount sufficient to dissolve the precipitates of the aluminum hydroxide and to form the PAS solution.

2. The method according to claim 1, wherein the aqueous solution of aluminum sulfate and the basic solution of sodium carbonate and sodium aluminate are added to the water as two separate streams that do not contact one another prior to being added to the water.

3. The method according to claim 2, wherein the basic solution has a ratio of the sodium carbonate to the sodium aluminate of 0.1 to 0.3.

4. The method according to claim 2, further comprising agitating the water when the two separate streams are added to the water.

5. The method according to claim 1, further comprising adjusting flow rates of the two separate streams in order to maintain the pH of the mixture.

6. The method according to claim 1, wherein the PAS solution formed has less than 20 ppm chloride.

7. The method according to claim 1, wherein the mixture has a pH between about 6.5 to about 6.8.

8. The method according to claim 1, further comprising adding phosphoric acid to the PAS solution.

9. The method according to claim 8, wherein the phosphoric acid is added at a concentration of about 0.75% to about 1.5% by weight.

10. A polyaluminum sulfate (PAS) solution prepared by the method of claim 1.

11. The PAS solution according to claim 10, having a basicity of between about 40 and about 70, a weight percent sulfate between about 15 and about 22, and a weight percent alumina between about 7.5 and about 12.

12. The PAS solution according to claim 10, having a basicity of between about 48% and about 52%, a weight percent sulfate between about 16.8 and about 17.2, and a weight percent alumina between about 8.0 and about 8.5.

13. The PAS solution according to claim 10, stabilized with between about 0.75% and about 1.125% phosphoric acid by weight.

14. A method for treating water to reduce impurities, the method comprising: adding the PAS solution of claim 10 to the water in order to coagulate the impurities; and separating the coagulated impurities from the water to produce a treated water reduced in the impurities without increasing a chloride to sulfate mass ratio of the treated water.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0009] The foregoing features of embodiments will be more readily understood by reference to the following detailed description, taken with reference to the accompanying drawings, in which:

[0010] FIG. 1 is a diagram of a tank/mixer system suitable for use as a laboratory reactor according to embodiments of the present invention.

[0011] FIG. 2 is a graph showing the settled turbidity (settled NTU) for samples of central Arkansas water treated with increasing concentrations of alum (upper curves) and PAS (lower curve) according to embodiments of the present invention.

[0012] FIG. 3 is a graph showing settled turbidity for the samples of FIG. 2, plotted against the treatment cost in $/Million Gallons (MG). The dashed and the dotted curves are for treatment with alum, whereas the solid curve is for treatment with PAS according to embodiments of the present invention.

[0013] FIG. 4 is a graph showing the percentage of Total Organic Carbon (TOC) for central Arkansas water samples treated with alum (dashed and dotted lines) and with PAS (solid line) according to embodiments of the present invention.

[0014] FIG. 5 is a graph showing settled turbidity plotted against the cost per milligram of alum (dashed curve) and of PAS (solid curve) according to embodiments of the present invention for samples of raw water from Anderson, South Carolina.

[0015] FIG. 6 is a graph showing the percentage of TOC plotted against the cost per milligram of alum (dashed curve) and of PAS (solid curve) according to embodiments of the present invention for samples of raw water from Anderson, South Carolina.

[0016] FIG. 7 shows a stability test for raw water samples for treatments with various concentrations of phosphoric acid stabilizer. The hollow circles show data for untreated samples. The solid diamonds, hollow squares, and solid triangles show data for samples treated with 1%, 1.5%, and 2% phosphoric acid, respectively.

[0017] FIG. 8 shows clarity data obtained, under various experimental conditions, for PAS preparations according to embodiments of the present invention.

DETAILED DESCRIPTION OF SPECIFIC EMBODIMENTS

[0018] Definitions. As used in this description and the accompanying claims, the following terms shall have the meanings indicated, unless the context otherwise requires:

[0019] Expressed as a percentage, the basicity B of polyaluminum complexes, of the type Al.sub.n(OH).sub.mX.sub.p(SO.sub.4).sub.q, where X is a halogen, is given by the formula B=m/3*n*100. Pure polyaluminum sulfate, with the formula Al.sub.4(OH).sub.6(SO.sub.4).sub.3 thus has a basicity of 50%.

[0020] Turbidity corresponds to the cloudiness of a solution. The unit used to measure turbidity is the Nephelometric Turbidity Unit (NTU). As reported here, turbidity is measured by light scattering according to USEPA Method 180.1. ISO 7027. In water testing, turbidity reflects the presence of suspended microscopic particles. Turbidity can be decreased by the use of coagulants, which cause the suspended particles to aggregate and settle.

[0021] % TOC refers to the total percentage of total organic carbon in a water sample. As reported here, TOC is measured according to Standard Methods for the Examination of Water and Wastewater, 18.sup.th Ed. Using the Persulfate-Ultraviolet Oxidation Method 5310 C on a Sievers 900 Portable TOC analyzer utilizing a Sievers Inorganic Carbon Remover (ICR) and a GE autosampler.

[0022] Alum as used herein refers to aluminum sulfate, which has the chemical formula Al.sub.2(SO.sub.4).sub.3.

[0023] Soda ash is a common term for sodium carbonate, which has the chemical formula Na.sub.2CO.sub.3.

[0024] Sodium aluminate has the chemical formula NaAl(OH).sub.4.

[0025] In water purification applications, solutions of polyaluminum sulfate (PAS) function effectively as coagulants, and provide an alternative to other aluminum containing coagulants such as alum, polyaluminum chloride (PAC), sulfated polyaluminum chloride, and polyaluminum chlorosulfate (PACS). PAS solutions can be formulated with ultra-low chloride content. However, current methods of producing PAS are not cost-effective when compared to other aluminum containing coagulants.

[0026] According to embodiments of the present invention, methods are described for manufacturing an ultra-low chloride, PAS coagulant useful for removing suspended colloidal matter and organic carbon in potable water, industrial process water and wastewater. The PAS solution has reduced corrosivity compared to other aluminum based coagulants and is particularly suitable for drinking water applications. The simplified methods used to produce the PAS coagulant provide a high quality product that is less expensive to produce than current methods.

Method Description

[0027] The manufacture of polyaluminum sulfate (PAS) is completed in two steps in embodiments of the present invention. The first two steps involve the mixing of two solutions in a single reaction vessel, followed by an optional third step that stabilizes the resulting PAS solution. The first step involves the precipitation of aluminum hydroxide and the second step involves the digestion of the precipitated aluminum hydroxide. The method begins by forming a basic solution of sodium carbonate and sodium aluminate. Preferably, the basic solution has a sodium carbonate to sodium aluminate ratio of about 0.1 to 0.3. The method further includes simultaneously adding separate streams of an aqueous solution of aluminum sulfate and the basic solution to water to form a mixture having a pH between about 5 and about 7. The two separate streams are added into the reaction vessel such that they do not come into direct contact with one another before being dispersed into the water, under constant agitation, in the reaction vessel. The method further includes allowing precipitates of aluminum hydroxide to form in the mixture. Precipitation occurs as the pH reaches a range of about 5 to about 7 which is the range of minimum solubility for aluminum hydroxide. A key feature of the method is that the addition rates of the two streams into the reaction vessel are adjusted to maintain this pH range so that precipitation continues. The optimal range is a pH of about 6.5 to about 6.8. Sodium sulfate and carbon dioxide are produced as side reaction products. The precipitation step is typically completed in about 1 hour.

[0028] The use of a mixture of sodium aluminate solution with dissolved sodium carbonate is required to form a precipitate that will dissolve to form the final product. If only sodium aluminate solution is used, the resulting precipitate will not dissolve in a reasonable time period. If only sodium carbonate solution is used, the resulting product will be too dilute for commercial use due to its limited solubility in water.

[0029] The second step involves the digestion of the precipitated aluminum hydroxide. The method further includes adding an additional aqueous solution of aluminum sulfate to the mixture in an amount sufficient to dissolve the precipitates of the aluminum hydroxide and to form a liquid PAS solution at the desired basicity. This second step is completed as soon as the first step is finished. The time to digest the precipitated aluminum hydroxide in the additional amount of aluminum sulfate solution ranges from about 6 to about 20 hours when the proper proportion of sodium aluminate solution and sodium carbonate are used during the precipitation step.

[0030] The method may further include adding phosphoric acid to the PAS solution. This optional third and final step to form a stabilized final PAS product may include the addition of about 0.75 to about 1.5% phosphoric acid by weight to the mixture just after the final aluminum sulfate solution is added. The phosphoric acid increases the shelf life from about 2 months to about 6-12 months or more depending on the amount of phosphoric acid added.

[0031] The reactions that occur during the precipitation step and the digestion step are as follows.

Precipitation Step:

[0032] ##STR00001##

Digestion Step:

[0033] ##STR00002##

Overall Reaction:

[0034] ##STR00003##

Product Analysis and Description

[0035] Solutions of the PAS coagulant produced according to embodiments of the present invention, as described in the following working examples, are clear to slightly hazy liquids, colorless to yellow in appearance, having a percentage of alumina within the range of about 7.8% to about 8.7%, ideally within the range of about 8.0% to about 8.5%. The PAS solutions have basicities that are within the range of about 45% to about 55%, ideally within the range of about 48% to about 52%, and a percentage of sulfate within the range of about 16.5% to about 17.4%, ideally within the range of about 16.8% to about 17.2%. Here, the test methods used to determine the percentage of alumina, basicities, and the percentage of sulfate are provided in the Test Method column of Table I.

[0036] Table I further provides a summary of experimental results as described below compared to expected values for solutions of Al.sub.4(OH).sub.6(SO.sub.4).sub.3.

TABLE-US-00001 TABLE 1 Summary of experimental results Expected Attribute Value Range Test Method Appearance Clear Clear to slightly Visual inspection or liquid hazy liquid. turbidity measurement Color Colorless Colorless Visual inspection to yellow % Alumina, 8.2 .sup.8-8.5 ANSI/AWWA B408-18 Al.sub.2O.sub.3 Sec. 5.3 % Basicity 50 48-52 ANSI/AWWA B408-18 Sec. 5.5 % Sulfate, SO.sub.4 17 16.8-17.2 Standard Methods for the Analysis of Water and Wastewater 20th Ed. 4500 - SO42- D. Viscosity, 15 <50 Brookfield @ 23? C. (LV1 spindle at 60 rpm) Specific 1.293 1.285-1.300 Gravity

WORKING EXAMPLES

[0037] The laboratory reactor used for the following working examples is described below and shown in FIG. 1, although other size reactors may be used with embodiments of the present invention. The reactor consists of a 2-liter, thick-walled beaker fitted with three ?-inch 316 stainless steel baffles set equidistantly around the reactor. The beaker is 7? inches tall with a 5-inch inside diameter. The bottom of the beaker is flat. The baffles preferably are 1/10.sup.th the diameter of the beaker as in a full-scale reactor. Agitation was provided using a Caframo model BOC digital vertical shaft overhead mixer fitted with a 7? inch long shaft and a single 3-inch diameter, 45? pitched, four-blade agitator. The agitator is positioned so the blades are just covered by the start-up water and operated at 250 rpm during the process. Two glass serological pipets are clamped in the beaker on opposite sides and away from the baffles. They are set such that the tip of the pipets are close to and level with the middle of the agitator blades just below the surface of the start-up water. Two variable speed Masterflex peristaltic pumps fitted with #13 Masterflex tubing which feeds down into the serological pipets are used to add the components.

Water/Sodium Carbonate/Sodium Aluminate Feed Vessel

[0038] A second beaker of variable size is used to make up and feed the water/sodium carbonate/sodium aluminate mixture. The beaker was placed on a VWR programmable hotplate fitted with an infrared thermocouple for controlling the mixture temperature. Agitation was provided using a second Caframo model BOC digital vertical shaft overhead mixer fitted with a 7? inch long shaft and a single 1? or 2?-inch diameter, 45? pitched, four-blade agitator (depending on the volume of the mixture). The agitator is positioned so the blades are covered by the solution water and operated at 350 rpm initially to dissolve the sodium carbonate and combine the sodium aluminate. The speed is reduced as necessary during process to eliminate splashing. The thermocouple is positioned so that the infrared probe end is near to, but not touching the bottom of the beaker and such that it does not contact the agitator impeller. The hotplate is set to maintain the exotherm temperature of the solution process of the mixture which is usually around 35? C. A glass serological pipet is clamped such that the tip reaches to the bottom of the beaker but on a slight angle so as to not interfere with the flow of the mixture and is positioned so that the piped does not contact the agitator impeller. One end of one of the #13 Masterflex tubing from the precipitator/digestor set up is fed into the serological pipet to feed the reactor with the mixture.

Aluminum Sulfate Feed Vessel

[0039] A plastic Boston Round bottle of appropriate volume was used to feed the aluminum sulfate solution. A hole of the same diameter as the #13 Masterflex tubing was cut into the cap to seal the bottle after the aluminum sulfate solution is added to eliminate evaporating during the process. The end of the other #13 tubing is fitted into the bottle such that the end reaches to the bottom but does not interfere with the flow of the solution.

Laboratory Batch Procedure

[0040] Weigh and record the precipitator/digestor tare weight. Add the required amount of start-up water to the vessel. Place the agitator and serological pipets as described above. Set the agitator to 250 rpm.

[0041] Insert a calibrated pH probe with an automatic temperature compensator and digital pH and temperature readout midway between the serological pipets and downstream of the intended aluminum sulfate feed point. Place the probe such that the tip is covered by the start-up water and will not contact the agitator impeller.

[0042] Weigh and record the tare weigh of the beaker used to make up and feed the water/sodium carbonate/sodium aluminate mixture. Tare the balance with the vessel on it and add a slight excess of the required solution water and record the amount. Place the beaker on the programable hotplate as described above. Set the agitator at 350 rpm.

[0043] In another tared beaker, add a slight excess of the required amount of sodium carbonate and record the amount. Slowly add this to the mixture beaker. Reweigh the addition beaker to confirm all the sodium carbonate has been added. Record any difference. Allow the sodium carbonate to completely dissolve. Once dissolved set the hotplate to match the exotherm temperature of about 35? C.

[0044] In another tared plastic beaker add a 1-2 g excess of the amount of sodium aluminate required. This material is very viscous and careful addition is necessary to add the desired slight excess of material to the mixture. Re-tare the beaker with the sodium aluminate. Slowly added this to the mixture beaker until a slight excess is added. Do this by measuring the weight loss of the beaker containing the sodium aluminate. Record the total amount added by difference. From the recorded weight in steps 3, 4 and 5 the gross weight of mixture beaker can be calculated.

[0045] Tare the plastic Boston Round bottle to be used to feed the aluminum sulfate solution. Add 0.5-1.0 grams excess of the required amount of aluminum sulfate solution. Remove the bottle and tare the balance. Weigh and record the gross weight of the bottle and the aluminum sulfate solution. Insert the Masterflex tubing as described above.

[0046] Start the Masterflex pump feeding the aluminum sulfate solution on its lowest setting. When the solution reaches the reactor, and the pH drops to below 4 turn off the pump and record the temperature and pH using the meter readouts.

[0047] Start the Masterflex pump feeding the mixture on its lowest setting. When the mixture just reaches the bulk solution in the reactor restart the pump feeding the aluminum sulfate solution and start a timer.

[0048] Monitor and record the resulting bulk slurry temperature and pH using the meter readouts at one-minute intervals. Adjust the pump rates as necessary to achieve a bulk solution pH of 6.5-6.8 in as timely a manner as possible. Once the pH has stabilized increase the pump feed rates proportionally so that the water/sodium carbonate/sodium aluminate mixture feed is complete in about one hour. Monitor and record the bulk solution temperature and pH at convenient intervals.

[0049] When the water/sodium carbonate/sodium aluminate mixture feed is complete, record the bulk slurry temperature, pH and time and immediately weigh and record the final gross weight of the mixture beaker and any residual. Flush a small amount of water through the feed tubing.

[0050] Continue feeding the aluminum sulfate solution at the same rate until the bulk slurry drops below pH 5.0. Increase the feed rate to a maximum until all the aluminum sulfate solution is added. Record the bulk slurry temperature, pH and the time and immediately weigh and record the final gross weight of the bottle and residual. If a solid is being added as a stabilizer flush a small amount of water through the tubing. Remove and rinse the serological pipets used to feed the mixture and flush the tubing with water into a waste container.

[0051] In another tared beaker add a slight excess of the amount of stabilizer required. Tare and record the gross weight of the beaker and stabilizer. If a solid is being used add it directly to the top of the bulk slurry. Weigh and record the final gross weight of the beaker and any residual. If a solution is being used add it using the tubing used to feed the aluminum sulfate solution on the lowest pump setting. When all the stabilizer is added record the bulk slurry temperature, pH and the time and immediately weigh and record the final gross weight the beaker and any residual. Flush a small amount of water through the tubing.

[0052] Remove and rinse the serological pipet and flush the tubing with water into a waste container. Allow the slurry to mix until the pH has stabilized and record the final value. Remove the probe and allow as much solution to drain back into the reactor as practical. Rinse and store the probe as required. Allow the slurry to mix until all the solids have dissolved, overnight if necessary.

[0053] Once all the solids have dissolve turn off the agitator and remove the agitator. Allow as much solution to drain back into the reactor as practical. Record the time and weigh and record the final gross weight of the reactor and the final product.

[0054] Filter the solution through a #41 or #541 Whatman filter paper under vacuum. Store the final product in an appropriately sized plastic Boston Round sample bottle. Fill a 40 ml glass TOC vial for stability studies.

[0055] The product analysis and specifications obtained upon application of this procedure are shown above in Table 1.

Performance Testing Results

[0056] The PAS material stabilized with 1% phosphoric acid, prepared according to embodiments of the present invention and described in the Working Examples above, was used to treat raw water samples from central Arkansas and from Anderson, South Carolina. For comparison, water samples from the same batches were treated with alum.

[0057] FIG. 2 shows the results of turbidity measurements following a settling period for a batch of raw water from central Arkansas treated with chlorine dioxide. The batch had an initial alkalinity of 8.8 mg/L, which increased to 17.5 mg/L as ClO.sub.2 was lost. The turbidity of the sample was 4.4 NTU, and the TOC was 3.18 mg/L.

[0058] The lower curve of FIG. 2 shows samples treated with the PAS solution stabilized with 1% phosphoric acid according to embodiments of the present invention, whereas the upper curves show water samples from the same batch treated with alum. For the alum samples, the pH changed due to chlorine dioxide dissipation between the two sets of measurements. As can be seen, the sample treated with phosphoric acid stabilized PAS according to embodiments of the present invention produced settled water turbidities significantly lower than those for samples treated with alum at equivalent alumina dosages.

[0059] Treatment costs in $/MG are shown in FIG. 3 for the treated samples of FIG. 2. The optimum turbidity for the alum sample was about 0.45 NTU, and corresponded to a treatment cost of about $11/MG. If the PAS data are extrapolated back to an equivalent turbidity of 0.45 NTU, the treatment costs would only be about $9/MG. Consequently, to reach an equivalent turbidity, treatment with the PAS solution, prepared according to embodiments of the present invention, is less expensive than treatment with alum.

[0060] As shown in FIG. 4, a comparison of % TOC shows an equal or better performance for samples treated with the PAS solution prepared according to embodiments of the present invention compared to samples treated with alum at equivalent alumina dosages.

[0061] FIGS. 5 and 6 show settled turbidity and % TOC removal for a batch of raw water from Anderson, South Carolina. In FIGS. 5 and 6, the settled turbidity and % TOC numbers are compared versus estimated $/MG. As is evident from FIG. 5, when compared at equivalent costs per MG, phosphoric acid stabilized PAS treatment, according to embodiments of the present invention, produced settled water turbidities generally lower than alum treatment. FIG. 6 demonstrates that TOC removal was likewise better for the PAS treatments, according to embodiments of the present invention, when compared to alum treatment at equivalent costs per MG.

Stability Testing Results

[0062] FIG. 7 shows stability studies performed at ambient temperature for samples with various levels of phosphate stabilizer. For the sample not treated with phosphate stabilizer, a dramatic increase in settled turbidity occurred just beyond 50 days. However, samples treated with 1% by weight of phosphoric acid stabilizer showed no significant increase in turbidity for nearly 100 days, and samples with weight percentages of 1.5% and 2% showed no increase in settled turbidity over the nearly 300 day testing period.

Additional Working Examples of Clarity Tests

[0063] Table 2 shows a summary of results of numerous clarity tests that were conducted with different experimental parameters according to embodiments of the present invention. A more detailed description of the parameters and processes used for each of the clarity tests are shown in Tables 3-37 for Lot numbers MR-105, MS-100, MS-110, MS-170, MU-046, MU-064, MU-162, MU-164, MU-166, MU-168, MU-180, MV-057, MV-061, MV-064, MV-067, MV-070, MV-073, MV-076, MV-080, MV-085, MV-110, MV-115, MV-119, MV-122, MV-125, MV-128, MV-131, MV-142, MV-145, MV-155, MV-158, MV-161, MV-169, MV-173, and MV-176, respectively. FIG. 8 shows graphically the relationship between the basicity and the ratio of sodium carbonate to sodium aluminate for samples that were initially clear (hollow circles) versus samples that were turbid (solid circles). These results support the ranges that are shown in Table 1.

TABLE-US-00002 TABLE 2 Clarity tests under various experimental conditions Rxn % Soda Temp. Initial Time Temp. Final Time Lot % Bas. Stablizer Ash % LSA SA/LSA % SO4 (? C.) ppt pH clarity (Hr) (? C.) Clarity (Hr) MR-105 67 None 3.0 11.9 0.25 15.56 49.5 6.34 Heated/ 17-24 Clear MS-100 98 None 5.9 16.7 0.35 12.64 58.5 5.75 Slurry MS-110 95 None 6.3 16.8 0.37 12.45 47.3 5.51 Slurry MS-170 100 None 6.3 16.8 0.37 12.49 49.9 5.90 Slurry MU-046 50 2% Phos 1.4 11.6 0.12 16.65 37.9 6.47 Cloudy 42.1 40 Clear 66.1 MU-064 49 2% Phos 1.8 11.7 0.16 16.57 27.5 6.82 Cloudy 18.6 40 Clear 27.1 MU-162 73 2% Phos 2.2 17.7 0.12 13.70 27.7 6.18 Cloudy 20.25 40 ND ND MU-164 61 2% Phos 1.8 14.7 0.12 14.91 27.7 6.12 Cloudy 20.9 40 Clear 116.9 MU-166 55 2% Phos 3.7 9.8 0.38 16.03 25.6 5.85 Clear 18.5 MU-168 44 2% Phos 3.0 8.1 0.37 16.72 26.1 5.54 Clear 18.4 MU-180 62 2% Phos 3.2 13.3 0.24 15.98 27.4 6.39 Cloudy 22.5 40 Clear 26.5 MV-057 46 0.2% SG 0.0 12.3 0.00 18.54 23.9 6.09 Cloudy 20 35-40 Clear 42 MV-061 45 0.2% SG 1.0 10.5 0.10 18.04 24.4 6.61 Cloudy 20 40 Clear 27 MV-064 48 0.2% SG 2.1 9.0 0.23 17.85 25.5 6.66 Clear 19.5 MV-067 53 0.2% SG 2.1 10.9 0.19 18.05 25.7 6.64 Cloudy 19.5 35 Clear 25 MV-070 52 0.2% SG 2.6 9.7 0.27 17.20 25.8 6.81 Clear 18 MV-073 54 0.2% SG 2.7 10.3 0.26 17.55 25.9 6.45 Cloudy 17.7 35 Clear 21.7 MV-076 58 0.2% SG 3.1 10.3 0.30 16.67 26.2 6.58 Clear 18 MV-080 62 0.2% SG 3.1 11.4 0.28 16.71 27.3 6.63 Cloudy 18.5 35 Clear 21.6 MV-085 65 0.2% SG 3.7 12.0 0.31 16.21 26.8 6.51 Cloudy 22.5 35 Clear 24 MV-110 55 none 2.5 9.4 0.27 16.60 27.2 6.49 Clear 18.2 MV-115 46 2% Phos 2.6 9.5 0.27 16.55 26.6 6.31 Clear 19.5 MV-119 50 2% Phos 2.6 10.6 0.24 16.31 27.0 6.49 Clear 18.1 MV-122 49 0.26% Phos 2.6 9.0 0.29 17.07 25.9 6.42 Clear 20.75 MV-125 49 0.52% Phos 2.6 9.1 0.28 16.96 26.4 6.83 Clear 18.2 MV-128 49 1.0% Phos 2.6 9.6 0.27 16.75 26.9 6.72 Clear 18.25 MV-131 50 1.5% Phos 2.6 10.5 0.24 16.57 26.9 6.60 Clear 18.1 MV-142 59 0.55% Phos 2.6 12.9 0.20 16.43 26.9 6.23 Cloudy 20.5 Clear 45.5 MV-145 60 0.5% Phos 3.0 11.4 0.26 15.54 27.6 6.46 Cloudy 19 30 Clear 24.5 MV-155 49 1.0% Phos 2.6 9.9 0.26 16.90 28. 5.85 Clear 17.33 MV-158 49 0.6% SG 2.6 9.1 0.29 17.19 28.3 6.64 Clear 19.2 MV-161 50 1.0% Phos 2.5 9.7 0.26 16.77 23.4 6.43 Clear 19.75 MV-169 44 1.0% Phos 2.5 7.6 0.33 17.94 26.1 6.13 Clear 18.33 MV-173 47 1.0% Phos 2.5 8.3 0.30 17.63 27.5 6.03 Clear 20.25 MV-176 50 1.0% Phos 2.6 9.3 0.28 17.37 28.5 6.60 Clear 18.42 SG = Sodium gluconate Phos = 75% Phosphoric acid solution

[0064] For Lot numbers MS-100, MS-110, and MS-170, Table 2 shows just the precipitation of aluminum hydroxide step. For Lot number MU-162, the sample initially gelled, but with extra alum became fluid but turbid.

TABLE-US-00003 TABLE 3 Headspace 67% Basic PAS Conversion Gallons Target Initial Actual Working Examples MR-105 MR-105 91.1969 14774.7 11.4 1.0 16.0 8.3 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 60.00 Start Up Water 0 1.000 60.00 3.70 5,470 656 3.70 2,100 23,005 2759 15.56 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 1,869 2,955 354 2.00 252.20 Water (SA) 0 1.000 252.20 15.56 23,000 2,759 15.56 5,518 18,330 2499 12.40 49.20 Soda Ash 0 NA 49.20 3.04 4,485 NA 3.03 5,685 NA 3.85 193.20 43% SAX 23.63 140.1 1.520 193.40 11.93 17,635 1,392 11.93 4,150 10,550 833 7.14 % Na.sub.2O SAX 18.74 1145.40 Alum 8.29 0.74 1.325 1145.50 70.67 104,465 9,457 70.68 26,050 2358 17.62 0.00 UP 290 17.29 41.8 1.370 0.00 0.00 0 0 0.00 63,035 5519 42.65 % Cl UP 290 20.99 0.00 H.sub.3PO.sub.4 (75%) 0 1.570 0.00 0.00 0 0 0.00 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1700.00 UltraPAC 2230 8.68 8.7 1.200 1700.30 104.90 155,060 15,499 104.91 149,610 13,749 101.22 Check 1620.80 100.00% 155,055 148,014 147,806 14,390 100.00% % SA soln 16.3% 1.153 1,350.7 95.32% 147,805 ?7,250 ?208 ?1,804 641 98.79% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.00 0.00% Evap. & CO.sub.2 8.68% 57.2 16.56 0.00 0.00 16.56 2.91 19.47 Actual 79.50 4.90% Just CO.sub.2 8.35% 15.93 0.00 15.93 2.91 18.84 1. Add required amount of start up water to the reactor and start agitation. 1 2. Add the required amount of water into the soda ash mix vessel and start agitator. 1804 1.22% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution Into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum sulfate solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 6 and 7. 9. Increase the feed rate of the aluminum sufate solution when all of the sodium carbonate/sodium aluminate solution has been added. 10. When all of the aluminimc sulfate solution has been added start the phosphoric acid addition. 11. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Calculated Actual Specific Gravity 1.291 % M.sub.2O.sub.3 8.68 8.79 % Al.sub.2O.sub.3 8.68 8.79 % Fe.sub.2O.sub.3 0.00 0.00 % Basicity 57.2 67.1 9.9 170.5 143.6 % Sulfates 16.56 ND Turbidity, NTU 9.4 Viscosity, cps 15.4 Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 48.1 118.6 4.56 19 4 Started both feeds. 4.0 4.3 0.9 1 48.0 118.4 7.01 20 4 4.2 4.3 1.0 2 47.8 118.0 6.67 20 4 4.2 4.3 1.0 3 47.9 118.2 6.81 20 4 4.2 4.3 1.0 4 48.3 118.9 6.83 20 4 4.2 4.3 1.0 5 48.5 119.3 6.83 21 4 4.4 4.3 1.0 18 50.3 122.5 6.21 20 4 4.2 4.3 1.0 30 50.3 122.5 6.34 20 4 4.2 4.3 1.0 40 49.3 120.7 6.34 20 4 4.2 4.3 1.0 50 49.3 120.7 6.36 20 4 4.2 4.3 1.0 60 48.3 118.9 6.36 20 4 4.2 4.3 1.0 70 49.0 120.2 6.13 20 4 Water/soda ash/sodium aluminate mixture feed complete (388/70 = 5.54 ml/min.). Added 492.7 g alum to this point 4.2 4.3 1.0 71 49.3 120.7 6.18 80 0 16.1 0.0 0.0 110 51.3 124.3 3.34 0 0 Alum feed complete ([1145.5 ? 492.7]/1.325/[110 ? 70] = 12.31 ml/min.). 0.0 0.0 0.0 120 53.3 127.9 3.32 0 0 Let solution mix overnight. 0.0 0.0 0.0 1.0 (May 17, 2016) 8:45 am. Solution clear. Turned off heat and let cool. Average 49.5 121.1 6.34

TABLE-US-00004 TABLE 4 Headspace Precipitated Aluminum Hydroxide (PAH) Conversion Gallons Target Initial Actual Working Examples MS-100 MS-100 61.6989 14774.7 11.4 5.2 16.0 10.7 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 233.00 Start Up Water 0 1.000 233.0 9.73 14,375 1,724 9.73 2,100 23,005 2759 15.56 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 1,869 2,955 354 2.00 434.50 Water (SA) 0 1.000 409.0 17.07 25,235 3,027 17.07 6,054 18,330 2294 12.40 149.50 Soda Ash 0 NA 140.7 5.87 8,680 NA 5.87 5,685 NA 3.85 425.00 43% SAX 23.38 140.1 1.520 401.0 16.74 24,740 1,952 16.74 4,979 10,550 833 7.14 % Na.sub.2O SAX 19.57 717.50 Alum 8.35 2.09 1.325 1282.2 53.52 79,110 7,162 53.52 26,050 2358 17.62 0.00 UP 290 16.88 41.8 1.370 0.00 0.00 0 0 0.00 63,035 5519 42.65 % Cl UP 290 20.98 0.00 H.sub.3PO.sub.4 (75%) 0 1.570 0.00 0.00 0 0 0.00 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1900.70 UltraPAC 2230 8.38 8.4 1.200 2465.90 102.93 152,145 15,208 102.93 149,610 13,749 101.22 Check 2395.70 100.00% 152,140 0 147,806 14,185 100.00% % SA soin 25.6% 1.256 1,996.4 97.15% 147,809 ?4,331 147,806 ?1,804 436 98.79% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 58.80 2.44% Evap. & CO.sub.2 8.38% 89.0 12.63 0.00 0.00 12.63 4.87 17.50 Actual 70.20 2.93% Just CO.sub.2 8.29% 12.50 0.00 12.50 4.87 17.36 1. Add required amount of start up water to the reactor and start agitation. 1 2. Add the required amount of water into the soda ash mix vessel and start agitator. 1804 1.22% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution Into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum sulfate solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. Analysis: Calculated Actual Specific Gravity % M.sub.2O.sub.3 8.38 % Al.sub.2O.sub.3 8.38 8.58 0.2 % Fe.sub.2O.sub.3 0.00 % Basicity 89.0 97.2 8.2 157.7 % Sulfates 12.63 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 68.8 155.8 3.23 49 8 Started both feeds @ 10:15 am. 9.9 8.6 1.2 1 66.9 152.4 5.00 49 8 9.9 8.6 1.2 2 64.7 148.5 5.35 49 8 9.9 8.6 1.2 3 62.9 145.2 5.52 49 8 9.9 8.6 1.2 4 61.2 142.2 5.64 50 8 10.1 8.6 1.2 5 59.7 139.5 5.62 50 8 10.1 8.6 1.2 10 55.8 132.4 5.64 50 8 10.1 8.6 1.2 15 59.3 138.7 5.50 50 8 10.1 8.6 1.2 20 58.1 136.6 5.62 100 16 20.0 17.1 1.2 25 56.0 132.8 5.74 100 16 Restarted timer. 20.0 17.1 1.2 35 57.7 135.9 5.90 0 0 Initial alum feed complete. 0.0 0.0 0.0 38 59.6 139.3 5.91 105 16 Began adding additional alum. 21.0 17.1 1.2 55 58.8 137.8 5.73 60 16 12.1 17.1 0.7 577 59.6 139.3 6.08 0 16 Stopped additional alum feed 0.0 17.1 0.0 59 60.8 141.4 6.50 0 0 Stopped water/soda ash/sodium aluminate mixture feed. 0.0 0.0 0.0 65 62.5 144.5 6.32 0 0 Turned off slurry heat. 0.0 0.0 0.0 1.2 225 35.5 95.9 6.61 0 0 0.0 0.0 0.0 Average 58.5 137.4 5.75

TABLE-US-00005 TABLE 5 Headspace Precipitated Aluminum Hydroxide (PAH) Conversion Gallons Target Initial Actual Working Examples MS-110 MS-110 60.8555 14774.7 11.4 3.7 16.0 10.7 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 233.00 Start Up Water 0 1.000 233.0 9.59 14,180 1,701 9.59 2,100 23,005 2759 15.56 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 1,869 2,955 3.54 2.00 456.20 Water (SA) 0 1.000 442.4 18.21 26,920 3,229 18.21 6,458 18,330 2294 12.40 157.00 Soda Ash 0 NA 152.2 6.27 9,260 NA 6.26 5,685 NA 3.85 19.57 421.00 43% SAX 23.38 140.1 1.520 408.3 16.81 24,845 1,961 16.81 5,190 10,550 833 7.14 % Na.sub.2O SAX 1282.20 Alum 8.35 2.09 1.325 1281.8 52.77 78,005 7,061 52.78 26,050 2358 17.62 0.00 UP 290 16.88 41.8 1.370 0.00 0.00 0 0 0.00 63,035 5519 42.65 % Cl UP 290 20.99 0.00 H.sub.3PO.sub.4 (75%) 0 1.570 0.00 0.00 0 0 0.00 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 2472.90 UltraPAC 2230 8.34 8.3 1.200 2517.70 103.65 153,215 15,315 103.66 149,610 13,749 101.22 Check 2428.90 99.99% 153,210 0 147,806 14,185 100.00% % SA soln 25.6% 1.256 2,024.1 96.47% 147,806 ?5,404 147,806 ?1,804 436 98.79% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 76.50 3.13% Evap. & CO.sub.2 8.34% 91.3 12.45 0.00 0.00 12.45 5.04 17.50 Actual 88.80 3.66% Just CO.sub.2 8.20% 12.25 0.00 12.25 5.04 17.29 1. Add required amount of start up water to the reactor and start agitation. 1 2. Add the required amount of water into the soda ash mix vessel and start agitator. 1804 1.22% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum sulfate solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. Analysis: Calculated Actual Specific Gravity % M.sub.2O.sub.3 8.34 % Al.sub.2O.sub.3 8.34 8.23 ?0.1 % Fe.sub.2O.sub.3 0.00 % Basicity 91.3 95.4 4.1 148.9 % Sulfates 12.45 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 48.0 118.4 3.07 50 8 Started both feeds @ 1:45 pm. 10.1 8.6 1.2 1 46.5 115.7 5.00 50 8 10.1 8.6 1.2 2 45.4 113.7 5.26 50 8 10.1 8.6 1.2 3 44.7 112.5 5.22 50 8 10.1 8.6 1.2 4 44.2 111.6 5.39 50 8 10.1 8.6 1.2 6 44.2 111.6 5.44 50 8 10.1 8.6 1.2 10 45.1 113.2 5.55 75 12 15.1 12.8 1.2 15 46.1 115.0 5.60 75 12 15.1 12.8 1.2 20 46.5 115.7 5.27 100 16 Some plugging in the water/soda ash/sodium aluminate mixture feed line. 20.0 17.1 1.2 30 47.9 118.2 5.52 100 16 20.0 17.1 1.2 45 47.0 116.6 5.33 100 16 20.0 17.1 1.2 1.2 60 49.8 121.6 5.83 0 16 Alum feed complete. 0.0 17.1 0.0 66 51.6 124.9 6.97 0 0 Stopped water/soda ash/sodium aluminate mixture feed. 0.0 0.0 0.0 75 51.4 124.5 6.89 0 0 Turned off slurry heat. 0.0 0.0 0.0 Average 47.3 117.1 5.51

TABLE-US-00006 TABLE 6 Headspace 100% Basic PAH Conversion Gallons Target Initial Actual Working Examples MS-170 MS-170 56.9845 14774.7 11.4 3.2 16.0 10.7 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 249.3 Start Up Water 0 1.000 249.3 9.61 14,205 1,704 9.61 2,100 23,005 2759 15.56 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 1,869 2,955 354 2.00 473.2 Water (SA) 1.000 473.2 18.24 26,965 3,234 18.24 6,469 18,330 2294 12.40 162.9 Soda Ash 0 NA 162.9 6.28 9,285 NA 6.28 5,685 NA 3.85 436.9 43% SAX 23.38 140.1 1.520 436.9 16.84 24,895 1,965 16.84 5,199 10,550 833 7.14 % Na.sub.2O SAX 19.57 1372.4 Atum 8.35 2.09 1.325 1372.4 52.91 78,205 7,080 52.91 26,050 2358 17.62 0.00 UP 290 16.88 41.8 1.370 0.00 0.00 0 0 0.00 63,035 5519 42.65 % Cl UP 290 20.99 0.00 H.sub.3PO.sub.4 (75%) 0 1.570 0.00 0.00 0 0 0.00 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 2599.8 UltraPAC 2230 8.36 8.4 1.200 2694.7 103.88 153,555 15,349 103.89 149,610 13,749 101.22 Check 2593.9 99.99% 153,555 0 147,806 14,184 100.00% % SA soin 25.6% 1.256 2,161.6 96.26% 147,811 ?5,744 147,806 ?1,804 436 98.79% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 94.9 3.65% Evap. & CO.sub.2 8.36% 91.2 12.49 0.00 0.00 12.49 5.06 17.54 Actual 100.8 3.89% Just CO.sub.2 8.20% 12.25 0.00 12.25 5.06 17.31 1. Add required amount of start up water to the reactor and start agitation. 1 2. Add the required amount of water into the soda ash mix vessel and start agitator. 1804 1.22% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum sulfate solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 6 and 7. Analysis: Calculated Actual Specific Gravity % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.36 8.45 % Fe.sub.2O.sub.3 0.00 % Basicity 91.2 99.6 8.4 157.9 % Sulfates 12.49 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 50.7 123.3 3.48 50 8 Started both feeds @ 1:35 pm. 10.1 8.6 1.2 1 49.6 121.3 5.70 50 8 Bulk slurry set point @ 50? C. 10.1 8.6 1.2 2 49.3 120.7 5.94 52 8 10.5 8.6 1.2 3 49.1 120.4 6.03 54 8 10.9 8.6 1.3 4 49.0 120.2 5.96 54 8 10.9 8.6 1.3 5 48.9 120.0 5.94 54 8 10.9 8.6 1.3 6 49.0 120.2 5.96 54 8 10.9 8.6 1.3 7 49.0 120.2 5.93 54 8 10.9 8.8 1.3 8 49.1 120,4 5.94 55 8 11.1 8.6 1.3 9 49.2 120.6 5.91 55 8 11.1 8.6 1.3 10 49.4 120.9 5.90 55 8 11.1 8.8 1.3 20 50.6 123.1 5.88 55 8 11.1 8.6 1.3 30 51.2 124.2 5.89 55 8 11.1 8.6 1.3 40 51.1 124.0 5.89 55 8 11.1 8.6 1.3 50 50.6 123.1 5.86 55 8 11.1 8.6 1.3 75 50.1 122.2 5.8 55 8 11.1 8.6 1.3 1.3 90 50.3 122.5 5.83 0 8 Alum feed complete 0.0 8.6 0.0 98 50.0 122.0 7.1 0 0 Water/soda ash/sodium aluminate mixture feed complete. Lowered bulk slurry set point to 40? C. 0.0 0.0 0.0 110 49.4 120.9 7.0 0 0 0.0 0.0 0.0 135 45.5 113.9 6.98 0 0 Let slurry cool to 40? C. Once cooled turned of hotplat and let mix overnight. 0.0 0.0 0.0 7.33 (Nov. 3, 2017) 8:30 am. Solution @ 24? C.ool. Average 49.9 121.7 5.90

TABLE-US-00007 TABLE 7 Headspace 50% Basic PAS + 2% Phos. Acid (75%) soln Conversion Gallons Target Initial Actual Working Examples MU-46 MU-046 230.9346 14774.7 11.4 8.7 16.0 8.4 Digest Temp. (? C.) formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grans % Pounds Gallons % Min. Gallons Pounds Gallons % 60.00 Start to Water 0 1.000 60.00 9.37 13,855 3,662 9.37 2,100 23,005 2759 15.56 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 1,869 2,955 354 2.00 44.45 Water (SA) 0 1.000 44.36 6.93 10,245 1,229 6.93 2,458 18,330 2484 12.40 9.00 Soda Ash 0 NA 9.07 1.42 2,095 NA 1.42 5,685 NA 3.85 73.70 43% SAX 22.71 140.1 1.520 74.19 11.59 17,135 1,352 11.59 2,581 10,550 833 7.14 % Na.sub.2O SAX 18.74 447.30 Alum 8.42 5.2 1.325 447.69 69.95 103,385 9,359 69.94 26,050 2358 17.62 0.00 UP 290 17.29 41.8 1.370 0.00 0.00 0 0 0.00 63,035 5519 42.65 % Cl UP 290 20.99 12.80 H.sub.3PO.sub.4 (75%) 0 1.570 12.97 2.03 2,995 229 2.03 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 640.00 UltraPAC 2230 8.52 8.5 1.200 648.28 101.29 149,710 14,964 99.28 149,610 13,749 101.22 Check 640.06 100.01% 149,710 147,988 147,806 14,374 100.00% % SA soln 17.0% 1.160 533.4 98.73% 147,812 ?1,898 ?162 ?1,804 625 98.79% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 7.25 1.13% Evap. & CO.sub.2 8.52% 49.1 16.65 0.00 0.00 16.65 2.18 18.83 Actual 8.22 1.28% Just CO.sub.2 8.45% 16.51 0.00 16.51 2.18 18.69 1. Add required amount of start up water to the reactor and start agitation. 1 2. Add the required amount of water into the soda ash mix vessel and start agitator. 1804 1.22% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 34.75 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 7.11 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 58.136 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphonic acid (75%) solution addition. 12. When phosphoric acid (75%) solution addition is completet let solution mix until all solids have dissolved. Analysis: Calculated Actual Specific Gravity 1.291 % M.sub.2O.sub.3 8.52 8.47 % Al.sub.2O.sub.3 8.52 8.47 % Fe.sub.2O.sub.3 0.00 0.00 % Basicity 49.1 49.7 0.6 142.0 % Sulfates 16.65 16.46 Turbidity, NTU 3.8 Viscosity, cps 15.6 Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 22.0 71.6 4.04 1.6 6 Agitator @ 400 rpm. Started both feeds @ 2:55 pm. 5.8 1.4 4.1 1 22.4 72.3 5.71 1.6 6 5.8 1.4 4.1 2 22.9 73.2 5.72 1.6 6 5.8 1.4 4.1 3 24.9 76.8 5.73 1.6 6 5.8 1.4 4.3 4 27.6 81.7 5.58 1.5 6 5.4 1.4 3.9 5 31.3 88.3 5.78 1.5 6 5.4 1.3 3.9 6 35.1 95.2 5.91 1.5 6 Hart accidently turned on hotplate for the reactor set at 40? C. Turned it off. 5.4 1.4 3.9 7 39.7 103.5 5.95 1.5 6 5.4 1.4 3.9 8 12.2 108.6 5.94 1.4 6 5.0 1.4 3.6 9 43.5 110.3 6.02 1.4 6 5.0 1.6 3.6 10 44.5 112.1 6.07 1.4 6 5.0 1.4 3.6 11 45.0 113.0 6.10 1.4 6 5.0 1.4 3.6 12 45.1 113.2 6.20 1.4 6 5.0 1.4 3.6 13 45.1 113.2 6.28 1.4 6 5.0 1.4 3.6 14 44.9 112.8 6.33 1.4 6 5.0 1.4 3.6 15 44.7 112.5 6.39 1.4 6 5.0 1.4 3.6 20 42.9 109.2 6.43 2.8 12 16.0 2.6 3.9 25 41.8 107.2 7.34 3.0 11 10.7 2.4 4.5 30 41.0 105.8 7.56 3.0 10 10.7 2.2 4.9 35 39.8 103.6 7.42 3.0 9 10.7 2.0 5.4 40 38.7 101.7 7.06 3.0 9 10.7 2.0 5.4 45 37.7 99.9 6.88 3.0 9 10.7 2.0 5.4 50 36.7 98.1 6.72 3.0 9 10.7 2.0 5.4 4.2 54 36.2 97.2 6.61 3.0 0 Water/soda ash/sodium aluminate mixture feed complete. 10.7 0.0 0.0 70 30.5 86.9 4.16 8.0 0 21.3 0.0 0.0 135 24.3 75.7 3.50 0.0 0 Alum feed complete. 0.0 0.0 0.0 137 24.2 75.6 3.50 3.0 0 Started phosphoric acid feed. 10.7 0.0 0.0 141 27.2 81.0 3.27 0.0 0 Phosphoric acid feed complete 0.0 0.0 0.0 145 27.0 80.6 3.33 0.0 0 Let slurry mix overnight. 1085 (Sep. 4, 2019) 9:00 am. (18 hours 5 minutes) Solution still very cloudy. Let solution mix. 1505 (Sep. 4, 2019) 5:00 pm. (25 hours 5 minutes) Solution still cloudy. Let solution mix overnight. 2529 (Sep. 5, 2019) 9:00 am. (42 hours 5 minutes) Solution still cloudy. Set hotplate to 40? C. Let solution mix 3965 (Sep. 6, 2019) 9:00 am. (66 hours 5 minutes) Solution clear, Turned off agitator. Turbidity 3.8 NTU Average 37.9 100.2 6.47

TABLE-US-00008 TABLE 8 Headspace 50% Basic PAS + 2% Phos. Acid (75%) soln Conversion Gallons Target Initial Actual Working Examples MU-064 MU-064 236.9466 14774.7 11.4 3.4 16.0 10.1 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 60.00 Start Up Water 0 1.000 60.00 9.62 14,215 1,705 9.62 2,100 23,005 2759 15.56 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 1,869 2,955 354 2.00 38.00 Water (SA) 0 1.000 38.02 6.09 9,010 1,081 6.10 2,161 18,330 2348 12.40 11.35 Soda Ash 0 NA 11.36 1.82 2,690 NA 1.82 5,685 NA 3.85 72.90 43% SAX 22.71 140.1 1.520 72.87 11.68 17,265 1,362 11.68 2,443 10,550 833 7.14 % Na.sub.2O SAX 18.74 452.20 Alum 8.08 2.3 1.325 452.51 72.54 107,220 9,706 72.54 26,050 2358 17.62 % SO.sub.4 Alum 24.16 0.00 UP 290 17.29 41.8 1.370 0.00 0.00 0 0 0.00 63,035 5519 42.65 % Cl UP 290 20.99 12.80 H.sub.3PO.sub.4 (75%) 0 1.570 12.78 2.05 3,030 231 2.05 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 640.00 UltraPAC 2230 8.51 8.9 1.200 647.54 103.80 153,430 15,336 101.75 149,610 13,749 101.22 Check 623.82 100.00% 153,430 148,507 147,806 14,239 100.00% % SA soln 23.0% 1.227 519.9 96.34% 147,810 ?5,620 ?701 ?1,804 490 98.79% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 7.25 1.13% Evap. & CO.sub.2 8.51% 49.0 16.57 0.00 0.00 16.57 2.37 18.93 Actual 23.72 3.80% Just CO.sub.2 8.25% 16.05 0.00 16.05 2.37 18.41 1. Add required amount of start up water to the reactor and start agitation. 1 2. Add the required amount of water into the soda ash mix vessel and start agitator. 1804 1.22% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 31.10 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 9.29 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 59.61 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fail below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Calculated Actual Specific Gravity 1.296 % M.sub.2O.sub.3 8.51 % Al.sub.2O.sub.3 8.51 8.42 % Fe.sub.2O.sub.3 0.00 0.03 % Basicity 49.0 49.1 0.1 140.5 143.6 % Sulfates 16.57 16.81 Turbidity, NTU 2.3 Viscosity, cps 11.8 Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 23.1 73.6 3.77 1.4 6 Agitator @ 400 rpm. Started both feeds @ 2:25 pm. 5.0 1.4 3.6 1 23.6 74.9 5.51 1.4 6 5.0 1.4 3.6 2 24.1 75.4 5.92 1.4 6 5.0 1.4 3.6 3 24.6 76.3 7.63 1.8 6 6.5 1.4 4.6 4 25.1 77.2 6.76 1.5 6 5.4 1.4 3.9 5 25.6 78.1 7.19 1.6 6 5.8 1.4 4.1 6 26.0 78.8 7.00 1.6 6 5.8 1.4 4.1 7 26.3 79.3 6.85 1.6 6 5.8 1.4 4.1 8 26.6 79.9 6.78 1.6 6 5.8 1.4 4.1 9 26.9 80.4 6.81 1.6 6 5.8 1.4 4.1 10 27.2 81.0 6.58 1.6 5 5.8 1.4 4.1 20 29.0 84.2 6.76 1.6 5 5.8 1.4 4.1 60 30.9 87.6 6.70 1.6 6 5.8 1.4 4.1 4.1 71 31.2 88.2 6.71 1.6 0 Water/soda ash/sodium aluminate mixture feed complete. 5.8 0.0 0.0 80 29.0 84.2 4.72 6.0 0 21.3 0.0 0.0 149 24.3 75.7 3.41 6.0 0 Aluminum sulfate feed complete. Started phosphoric acid (75%) solution feed. 21.3 0.0 0.0 153 27.3 81.1 3.19 0.0 0 Phosphoric acid (75%) solution feed complete 0.0 0.0 0.0 160 27.0 80.6 3.28 0.0 0 Let slurry mix overnight. 0.0 0.0 0.0 (Sep. 26, 2019) 9:00 am. (18 hours 35 minutes) Still very cloudy. Turned on hotplate to 40? C. and let mix . (Sep. 26, 2019) 4:30 pm. (27 hours 5 minutes) Solution clear. Turned of hotplate and let cool overnight. Average 27.5 81.5 6.82

TABLE-US-00009 TABLE 9 Headspace 70% Basic PAS + 2% Phos. Acid (75%) soin Conversion Gallons Target Initial Actual Working Examples MU-162 MU-162 98.3931 14774.7 11.4 11.4 16.0 15.6 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 60.00 Start Up Water 0 1.000 120.0 7.99 11,805 1,416 7.99 2,100 11,805 1416 7.99 0.00 Ferric sulfate 17.75 10.5 1.581 0.0 0.00 0 0 0.00 0 0 0 0.00 44.45 Water (SA) 0 1.000 158.8 10.57 15,625 1,874 10.57 3,748 15,625 1946 10.57 9.00 Sada Ash 0 NA 32.5 2.16 3,195 NA 2.1.6 3,195 NA 2.3.6 73.70 43% SAX 24.04 140.1 1.520 265.6 17.68 26,135 2,062 17.68 3,937 26,135 2062 17.68 % Na.sub.2O SAX 18.74 447.30 Alum 8.13 1.8 1.325 895.4 59.60 88,100 7,975 59.60 88,100 7975 59.60 0.00 UP 290 17.29 41.8 1.370 0.0 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 12.80 H.sub.3PO.sub.4 (75%) 0 1.570 30.0 2.00 2.950 225 2.00 2,950 225 2.00 Flush Water 1.000 0.0 0.00 0 0 0.00 0 0 0.00 647.25 UltraPAC 2230 9.10 9.1 1.200 1502.3 100.00 147,810 14,774 98.00 147,810 13,749 100.00 Check 1502.3 100.00% 147,810 0 147,810 13,785 100.00% % SA soln 17.0% 1.160 1,251.9 100.00% 147,810 0 147,810 0 36 100.00% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.00 0.00% Evap. & CO.sub.2 9.10% 71.2 13.70 0.00 0.00 13.70 3.35 17.03 Actual 0.00% Just CO.sub.2 9.16% 13.79 0.00 13.79 3.33 17.12 1. Add required amount of start up water to the reactor and start agitation. 1 2. Add the required amount of water into the soda ash mix vessel and start agitator. 0 0.00% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 3.58 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 34.76 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 7.11 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 58.13 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the alominim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Initial calculations used 22.71% Al2O3 for the 43% sodium aluminate and 8.42% Al2O3 and 5.2% basicity for alum. These were replaced with 24.04% Al2O3 for the 43% sodium aluminate and 8.13% Al2O3 and 1.8% basicity for alum. This made the calculated and actual numbers much more consistant. Analysis: Calculated Actual Specific Gravity % M.sub.2O.sub.3 9.10 9.25 % Al.sub.2O.sub.3 9.10 9.25 0.15 % Fe.sub.2O.sub.3 0.00 0.00 % Basicity 71.2 73.2 2.0 144.4 % Sulfates 13.70 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 22.4 72.3 3.80 0.6 6 Agitator @ 250 rpm. Started both feeds @ 12:45 pm. 2.2 1.4 1.6 1 22.7 72.9 4.75 0.6 6 2.2 1.4 1.6 2 22.9 73.2 4.86 0.6 6 2.2 1.4 1.6 3 23.2 73.8 4.90 0.6 7 2.2 1.6 1.4 4 23.4 74.1 5.28 0.6 7 2.2 1.6 1.4 5 23.7 74.7 5.45 0.6 7 2.2 2.6 1.4 10 24.7 76.5 6.01 0.6 7 2.2 3.6 1.4 15 25.5 77.9 6.17 0.6 7 2.2 2.6 1.4 20 26.1 79.0 6.19 1.2 14 4.3 3.0 1.5 25 27.6 81.7 5.98 1.2 15 4.3 3.2 1.4 30 28.6 83.5 6.34 1.2 15 4.3 3.2 1.4 35 29.4 84.9 6.49 1.2 15 4.3 3.2 1.4 45 30.5 86.9 6.58 1.2 15 4.3 3.2 1.4 65 31.6 88.9 6.59 1.2 15 4.3 3.2 1.4 85 31.7 89.1 6.60 1.2 15 4.3 3.2 1.4 1.4 114 21.9 71.4 6.56 1.2 0 Water/soda ash/sodium aluminate mixture feed complete, 4.3 0.0 0.0 120 30.9 87.6 5.24 1.2 0 4.3 0.0 0.0 180 26.7 80.1 3.91 1.2 0 Aluminum sulfate feed complete. Started phosphoric acid feed. 0.0 0.0 0.0 190 29.7 85.5 3.54 0.0 0 Phosphoric acid feed complete. 0.0 0.0 0.0 240 27.4 81.3 3.84 0.0 0 Solution cloudy. Let mix overnight. 0.0 0.0 0.0 1215 25.0 77.0 (May 5, 2020) 9:00 am. (20 hours 15 minutes} Solution still cloudy. Turned on hotplate to 40? C. 1230 40.0 104.0 Solution has completely gelled. Turned off hotplate. Add 150 g of aluminum sulfate and let mix. Solution still turbid but fluid. Average 27.7 81.9 6.18

TABLE-US-00010 TABLE 10 Headspace 60% Basic PAS + 2% Phos. Acid (75%) soln Conversion Gallons Target Initial Actual Working Examples MU-164 MU-164 98.5413 14774.7 11.4 11.1 16.0 15.6 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 8.00 11,825 1,418 8.00 2,100 11,805 1416 7.99 0.0 Ferric sulfate 17.75 10.5 1.581 0.0 0.00 0 0 0.00 0 0 0 0.00 131.7 Water (SA) 0 1.000 131.6 8.77 12,970 1,556 8.77 3,111 15,625 1946 10.57 26.9 Soda Ash 0 NA 26.9 1.79 2,650 NA 1.79 3,195 NA 2.16 220.3 43% SAX 24.04 140.1 1.520 220.1 14.67 21,690 1,712 14.67 3,267 26,135 2062 17.68 % Na.sub.2O SAX 18.74 971.1 Alum 8.13 1.8 1.325 973.4 64.89 95,920 8,683 64.89 88,100 7975 59.60 0.0 UP 290 17.29 41.8 1.370 0.0 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 30.0 H.sub.3PO.sub.4 (75%) 0 1.570 30.0 2.00 2,955 226 2.00 2,950 225 2.00 0.0 Flush Water 1.000 0.0 0.00 0 0 0.00 0 0 0.00 1500.0 UltraPAC 2230 8.80 8.8 1.200 1502.0 100.12 148,010 14,794 98.13 147,810 13,749 100.00 Check 1500.0 99.99% 148,010 147,810 13,785 100.00% % SA soln 17.0% 1.160 1,250.0 99.87% 147,813 ?197 147,810 0 36 100.00% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.00 0.00% Evap. & CO.sub.2 8.80% 60.8 14.91 0.00 0.00 14.91 2.76 17.68 Actual 2.00 0.13% Just CO.sub.2 8.84% 14.98 0.00 14.98 2.76 17.74 1. Add required amount of start up water to the reactor and start agitation. 1 2. Add the required amount of water into the soda ash mix vessel and start agitator. 0 0.00% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 34.76 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 7.11 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 58.14 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Initial calculations used 22.71% Al2O3 for the 43% sodium aluminate and 8.42% Al2O3 and 5.2% basicity for alum. These were replaced with 24.04% Al2O3 for the 43% sodium aluminate and 8.13% Al2O3 and 1.8% basicity for alum. This made the calculated and actual numbers much more consistant. Analysis: Calculated Actual Specific Gravity % M.sub.2O.sub.3 8.80 9.85 % Al.sub.2O.sub.3 8.80 9.85 Final weight not recorded % Fe.sub.2O.sub.3 0.00 0.3 140.9 % Basicity 60.8 61.1 % Sulfates 14.91 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 22.1 71.8 3.20 1.2 14 Agitator @ 200 rpm. Started both feeds @ 11:55 am. 4.3 3.0 1.5 1 22.1 71.8 4.25 1.2 14 4.3 3.0 1.5 2 22.3 72.1 4.60 1.2 15 4.3 3.2 1.4 3 22.4 72.3 5.24 1.2 15 Agitator @ 250 rpm. 4.3 3.2 1.4 4 23.9 75.0 5.54 1.2 15 4.3 3.2 1.4 5 24.5 76.1 5.75 1.2 15 4.3 3.2 1.4 10 26.2 79.2 6.13 1.2 15 4.3 3.2 1.4 15 27.3 81.1 6.28 1.2 15 4.3 3.2 1.4 40 29.9 85.8 6.31 1.2 16 4.3 3.4 1.3 1.3 105 28.5 83.3 5.07 1.2 0 Water/soda ash/sodium aluminate mixture feed complete. 4.3 0.0 0.0 201 29.6 85.3 3.64 1.2 0 Aluminum sulfate feed complete. Started phosphoric acid feed. 4.3 0.0 0.0 215 27.6 81.7 3.54 0 0 Phosphoric acid feed complete. Let mix overnight. 0.0 0.0 0.0 May 5, 2020 9:00 am (20.9 hrs) solution still cloudy. Turned on hotplate to 40? C. May 11, 2020 9:00 am (116.9 hrs) solution clear. Average 27.7 81.8 6.12

TABLE-US-00011 TABLE 11 Headspace UltraPAC 2286 (55% Basic PAS) + 2% Phos Conversion Gallons Target Initial Actual Working Examples MU-166 MU-166 101.3105 14774.7 11.4 4.9 16.0 11.3 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 8.22 12,155 1,458 8.22 2,100 23,005 2759 15.56 0.0 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 1,869 2,955 354 2.00 139.0 Water (SA) 0 1.000 138.9 9.52 14,070 1,688 9.52 3,375 18,330 2247 12.40 54.0 Soda Ash 0 NA 54.0 3.70 5,470 NA 3.70 5,685 NA 3.85 143.0 43% SAX 24.04 140.1 1.520 142.9 9.79 14,475 1,142 9.79 2,830 10,550 835 7.14 % Na.sub.2O SAX 19.57 1014.0 Alum 8.13 1.8 1.325 1018.1 69.78 103,145 9,337 69.78 26,050 2358 17.62 0.0 UP 290 16.88 41.8 1.370 0.00 0.00 0 0 0.00 63,035 5519 42.65 % Cl UP 290 20.99 30.0 H.sub.3PO.sub.4 (75%) 0 1.570 30.00 2.06 3,040 232 2.06 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1500.0 UltraPAC 2230 8.03 8.0 1.200 1503.9 103.07 152,360 15,229 101.02 149,610 13,749 101.22 Check 1459.0 99.99% 152,355 0 147,806 14,137 100.00% % SA soln 28.0% 1.282 1,215.8 97.01% 147,806 ?4,549 147,806 ?1,804 388 98.79% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.03% $3.8 16.03 0.00 0.00 16.03 2.96 18.99 Actual 44.9 3.08% Just CO.sub.2 7.88% 15.73 0.00 15.73 2.96 18.69 1. Add required amount of start up water to the reactor and start agitation. 1 2. Add the required amount of water into the soda ash mix vessel and start agitator. 1804 1.22% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 41.36 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 16.08 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 42.56 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition, 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Initial calculations used 23.38% Al2O3 and 168.2% effective basicity for the 43% sodium aluminate and 8.35% Al2O3 and 2.09% basicity for alum. These were replaced with 24.04% Al2O3 and 140.1% effective basicity for the 43% sodium aluminate and 8.13% Al2O3 and 1.80% basicity for alum. This made the calculated and actual numbers much more consistant. Analysis: Calculated Actual Specific Gravity % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.03 7.89 ?0.14 % Fe.sub.2O.sub.3 0.00 % Basicity 53.8 54.6 0.8 142.8 % Sulfates 16.03 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 22.4 72.3 3.82 0.6 6 Agitator @ 200 rpm. Started both feeds @ 2:30 pm. 2.2 1.4 1.6 1 22.4 72.3 4.53 0.6 7 2.2 1.6 1.4 2 22.5 72.5 4.90 0.6 7 2.2 1.6 1.4 3 22.7 72.9 5.16 0.6 7 2.2 1.6 1.4 4 22.8 73.0 5.42 0.6 7 2.2 1.6 1.4 5 23.1 73.6 5.56 0.6 7 2.2 1.6 1.4 10 23.9 75.0 5.83 0.6 7 2.2 1.6 1.4 15 24.5 76.1 5.88 1.2 14 4.3 3.0 1.5 20 26.1 79.0 5.64 1.2 15 4.3 3.2 1.4 25 27.1 80.8 5.73 1.2 16 4.3 3.4 1.3 30 28.1 82.6 6.00 1.2 16 4.3 3.4 1.3 35 29.0 84.2 6.09 1.2 16 4.3 3.4 1.3 40 29.7 85.5 6.06 1.2 17 Agitator @ 300 rpm. 4.3 3.6 1.2 60 29.7 85.5 6.18 1.2 17 4.3 3.6 1.2 70 29.7 85.5 6.31 1.2 17 4.3 3.6 1.2 1.3 85 29.9 85.8 5.90 4.2 0 Water/soda ash/sodium aluminate mixture feed complete. 15.0 0.0 0.0 116 24.0 75.2 3.64 0.6 0 Aluminum sulfate feed complete. Started phosphoric acid feed. 2.2 0.0 0.0 130 27.2 81.0 3.56 0 0 Phosphoric acid feed complete. Let mix overnight. 0.0 0.0 0.0 May 12, 2020 9:00 am (18.5 hrs) solution clear. Average 25.6 78.0 5.85

TABLE-US-00012 TABLE 12 Headspace UltraPAC 2361 (50% Basic PAS) Conversion Gallons Target Initial Actual Working Examples MU-168 MU-168 101.3800 14774.7 11.4 5.4 16.0 10.7 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 8.23 12,165 1,459 8.23 2,100 23,005 2759 15.56 0.0 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 1,869 2,955 354 2.00 127.5 Water (SA) 0 1.000 127.4 8.74 12,915 1,549 8.74 3,098 18,330 2297 12.40 43.5 Soda Ash 0 NA 43.5 2.98 4,410 NA 2.98 5,685 NA 3.85 118.0 43% SAX 24.04 140.1 1.520 117.9 8.09 11,955 943 8.09 2,493 10,550 833 7.14 % Na.sub.2O SAX 19.57 1061.0 Alum 8.13 1.8 1.325 1060.8 72.76 107,545 9,736 72.76 26,050 2358 17.62 0.0 UP 290 16.88 41.8 1.370 0.00 0.00 0 0 0.00 63,035 5519 42.65 % Cl UP 290 20.99 30.0 H.sub.3PO.sub.4 (75%) 0 1.570 30.00 2.06 3.040 232 2.06 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1500.0 UltraPAC 2230 7.86 7.9 1.200 1499.6 102.86 152,030 15,196 100.80 149,610 13,749 101.22 Check 1458.0 100.01% 152,030 0 147,806 14,188 100.00% % SA soln 25.5% 1.254 1,215.0 97.23% 147,813 ?4,217 147,806 ?1,804 439 98.79% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 7.86% 44.8 16.72 0.00 0.00 16.72 2.41 19.13 Actual 41.6 2.85% Just CO.sub.2 7.71% 16.40 0.00 16.40 2.41 18.82 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 1804 1.22% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Initial calculations used 23.38% Al2O3 and 168.2% effective basicity for the 43% sodium aluminate and 8.35% Al2O3 and 2.09% basicity for alum. These were replaced with 24.04% Al2O3 and 140.1% effective basicity for the 43% sodium aluminate and 8.13% Al2O3 and 1.80% basicity for alum. This made the calculated and actual numbers much more consistant. Analysis: Calculated Actual Specific Gravity % M.sub.2O.sub.3 % Al.sub.2O.sub.3 7.86 7.67 ?0.19 % Fe.sub.2O.sub.3 0.00 % Basicity 44.8 43.6 ?1.2 135.3 % Sulfates 16.72 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.6 70.9 3.70 1.2 17 Agitator @ 200 rpm. Started both feeds @ 2:37 pm. 4.3 3.6 1.2 1 21.8 71.2 7.72 1.7 17 Stopped Water/soda ash/sodium aluminate mixture feed for a few minutes. 6.1 3.6 1.7 2 22.2 72.0 4.74 1.7 17 6.1 3.6 1.7 3 22.6 72.7 5.24 1.7 17 6.1 3.6 1.7 4 23.0 73.4 5.36 1.7 17 6.1 3.6 1.7 5 23.3 73.9 5.27 1.7 17 6.3 3.6 1.7 7 24.0 75.2 5.24 1.7 18 6.1 3.8 1.6 8 24.4 75.9 5.31 1.7 19 5.1 4.0 1.5 9 24.9 76.8 5.33 1.7 20 Water/soda ash/sodium aluminate mixture feed line clogged. 6.1 4.2 1.5 11 25.6 78.1 5.50 1.7 20 6.1 4.2 1.5 12 26.0 78.8 5.63 1.7 20 6.1 4.2 1.5 13 26.5 79.7 5.73 1.7 20 6.1 4.2 1.5 15 27.3 81.1 5.86 1.7 20 6.1 4.2 1.5 30 29.7 85.9 5.98 1.7 20 6.1 4.2 1.5 45 27.6 81.7 4.42 0 20 Water/soda ash/sodium aluminate mixture feed line pushed against bottom of vessel. 0.1 4.2 0.0 49 28.3 82.9 5.62 1.7 20 6.1 4.2 1.5 50 28.6 83.5 5.75 1.7 20 6.1 4.2 1.5 1.4 53 24.2 75.6 6.09 4.5 0 Water/soda ash/sodium aluminate mixture feed complete. 16.0 0.0 0.0 90 24.7 76.5 3.40 0 3 Aluminum sulfate feed complete. 0.0 0.0 0.0 95 24.7 76.5 3.41 1.7 0 Started phosphoric acid feed. 6.1 0.0 0.0 100 27.4 81.3 3.34 0 0 Phosphoric acid feed complete. Let mix overnight. 0.0 0.0 0.0 May 13, 2020 9:00 am (18.4 hrs) solution clear. Average 26.1 78.9 5.54

TABLE-US-00013 TABLE 13 Headspace UltraPAC 2362 (60% Basic PAS} Conversion Gallons Target Initial Actual Working Examples MU-180 MU-180 104.5273 14774.7 11.4 ?1.6 16.0 10.7 Digest Temp. (C) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 8.49 12,545 1,505 8.49 2,100 12,545 1505 8.00 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 135.0 Water (SA) 0 1.000 134.9 9.54 14,100 1,691 9.54 3,383 14,100 1806 8.99 45.0 Sada Ash 0 NA 45.1 3.19 4,715 NA 3.19 4,715 NA 3.01 187.0 43% SAX 23.14 148.2 1.520 187.3 13.25 19,580 1,545 13.25 3,236 19,580 1545 12.48 % Na.sub.2O SAX 16.57 983.0 Alum 8.13 1.8 1.325 983.2 69.53 102,770 9,303 69.53 102,770 9303 65.51 0.00 UP 290 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 30.00 H.sub.3PO.sub.4 (75%) 0 1.570 30.30 2.14 3,165 242 2.14 3,165 242 2.02 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1500.0 UltraPAC 2230 8.72 8.7 1.200 1500.8 106.14 156,875 15,681 103.99 156,875 13,749 100.00 Check 1414.1 100.01% 156,875 0 156,875 14,636 100.00% % SA soln 25.1% 1.250 1,178.4 94.22% 147,812 ?9,063 156,875 0 887 100.00% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.72% 61.8 15.98 0.00 0.00 15.98 3.24 19.21 Actual 86.7 6.13% Just CO.sub.2 8.29% 15.20 0.00 15.20 3.24 18.44 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 1804 1.22% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 6 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Calculated Actual Specific Gravity % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.72 8.68 ?0.04 % Fe.sub.2O.sub.3 0.00 % Basicity 61.8 62.1 0.3 149.0 % Sulfates 15.98 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.5 70.7 3.58 0.6 6 Agitator @ 200 rpm. Started both feeds @ 10:30 am. 2.2 1.4 3.6 1 22.7 71.1 5.23 0.6 6 2.2 1.4 1.6 2 23.9 71.4 5.36 0.6 6 2.2 1.4 1.6 3 22.1 71.8 5.44 0.6 7 2.2 1.6 1.4 4 22.3 72.1 5.62 0.6 7 2.2 1.6 1.4 5 22.5 72.5 5.93 0.6 7 2.2 1.6 1.4 6 22.7 72.9 6.03 0.6 7 2.2 1.6 1.4 7 22.9 73.2 6.21 0.6 7 2.2 1.6 1.4 8 23.1 73.6 6.32 0.6 7 2.2 1.6 1.4 9 23.3 73.9 6.38 0.6 7 2.2 1.6 1.4 10 23.5 74.3 6.43 0.6 7 2.2 1.6 1.4 15 24.4 75.9 6.53 1.2 14 4.3 3.0 1.5 20 26.0 78.8 6.32 2.4 28 Agitator @ 300 rpm. 8.6 5.8 1.5 25 28.7 83.7 6.00 2.4 30 8.6 6.2 1.4 30 30.0 86.0 5.72 2.4 32 Cleared blockage in water/soda ash/sodium aluminate mixture feed line. 8.6 6.5 1.3 35 31.2 88.2 6.40 2.4 32 8.6 6.5 1.3 40 32.4 90.3 6.77 2.4 32 8.6 6.5 1.3 50 33.8 92.8 7.26 2.4 30 8.6 6.2 1.4 1.4 55 34.2 93.6 7.17 2.4 0 Water/soda ash/sodium aluminate mixture feed complete. 8.6 0.0 0.0 60 32.0 89.6 5.13 2.4 0 8.6 0.0 0.0 110 25.7 78.3 3.66 0.6 0 Aluminum sulfate feed complete. Started phosphoric acid feed. 2.2 0.0 0.0 125 28.6 83.5 3.57 0 0 Phosphoric acid feed complete. 0.0 0.0 0.0 155 27.3 81.1 3.59 0 0 Let mix overnight. 0.0 0.0 0.0 Jun. 16, 2020 9:00 am (22.5 hrs) solution still cloudy. Turned hotplate on to 40? C. Jun. 16, 2020 12:00 noon (25.5 hrs) solution mostly clear. Jun. 16, 2020 1:00 pm (26.5 hrs) turned off heat and let cool. Average 27.4 81.2 6.39

TABLE-US-00014 TABLE 14 Headspace UltraPAC 25495GO (45% Basic PAS) Conversion Gallons Target Initial Actual Working Examples MV-057 MV-057 99.1960 14774.7 11.4 9.5 16.0 17.2 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 8.05 11,905 1,428 8.05 2,100 11,905 1428 7.98 3.00 Sodicum Gluconate NA 3.00 0.20 300 36 0.20 300 36 0.20 0.0 Water (SA) 0 1.000 0.0 0.00 0 0 0.00 0 0 0 0.00 0.0 Soda Ash 0 NA 0.0 0.00 0 NA 0.00 0 NA 0.00 181.8 43% SAX 22.99 148.6 1.520 183.6 12.32 18,210 1,437 12.32 1,437 18,210 1437 12.21 % Na.sub.2O SAX 19.41 1195.2 Alum 8.17 0.7 1.325 1196.7 80.31 118,710 10,746 80.31 118,710 10746 79.60 0.00 UP 290 16.91 42.2 1.370 0.0 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.97 0.00 H.sub.3PO.sub.4 (75%) 0 1.570 0.0 0.00 0 0 0.00 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1500.0 UltraPAC 2230 9.39 9.4 1.200 1503.3 100.88 149,120 14,905 100.89 149,120 13,749 100.00 Check 1490.1 99.99% 149,125 150,765 149,125 13,647 100.00% % SA soln 1,241.8 99.12% 147,816 ?1,309 ?1,640 5 ?101 100.00% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 9.39% 45.3 18.54 0.00 0.00 18.54 1.75 20.29 Actual 13.2 0.89% Just CO.sub.2 9.31% 18.38 0.00 18.38 1.75 20.13 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of 43% sodium aluminate solution into the holding vessel, 0 0.00% 3. Add the required amount of aluminum sulfate solution to the alum holding vessel. 4. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 5. Start addition of the sodium aluminate to the reactor. 6. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 7. When all of the sodium aluminate solution has been added increase the aluminum sulfate feed rate. 8. When all of the aluminim sulfate solution addition is complete add the sodium gluconate. 9. Let solution mix until all solids have dissolved. Analysis: Calculated Actual Specific Gravity 1.315 % M.sub.2O.sub.3 % Al.sub.2O.sub.3 9.39 9.33 ?0.06 % Fe.sub.2O.sub.3 0.00 % Basicity 45.3 46.4 1.1 152.3 % Sulfates 18.54 19.1 Turbidity, NTU 3.1 Viscosity, cps 14.4 Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 19.0 66.2 3.80 0.6 6 Agitator @ 200 rpm. Started both feeds @ 11.45 am. 2.2 1.4 1.6 1 19.6 67.3 10.05 1.2 6 4.3 1.4 3.1 2 20.0 68.0 6.08 0.9 6 3.3 1.4 2.3 3 20.4 68.7 5.22 0.8 6 2.9 1.4 2.1 4 21.2 70.2 5.18 0.8 6 Agitator up to 250 rpm. 2.9 1.4 2.1 5 21.5 70.7 5.07 0.7 6 2.6 1.4 1.8 6 21.8 71.2 5.35 0.7 6 2.6 1.4 1.8 7 22.2 72.0 5.67 0.7 6 2.6 1.4 1.8 8 22.6 72.7 5.83 0.7 6 2.6 1.4 1.8 9 22.4 72.3 5.95 0.7 6 2.6 1.4 1.8 10 23.2 73.8 6.04 0.7 6 2.6 1.4 1.8 15 24.3 75.7 6.39 0.7 6 2.6 1.4 1.8 20 25.1 77.2 6.43 0.7 6 2.6 1.4 1.8 30 26.2 79.2 6.58 0.7 6 2.6 1.4 1.8 40 27.0 80.6 6.68 0.7 6 2.6 1.4 1.8 111 28.8 83.8 7.02 0.7 6 Sodium aluminate feed complete. 2.6 1.4 1.8 1.8 120 26.1 79.0 4.32 2.4 0 8.6 0.0 0.0 199 22.5 72.5 3.18 0 0 Aluminum sulfate feed complete. 0.0 0.0 0.0 200 22.5 72.5 3.18 0 0 Added sodium gluconate. 0.0 0.0 0.0 240 22.2 72.0 3.20 0 0 Let solution mix over night. 0.0 0.0 0.0 1200 17.8 64.0 Nov. 24, 2020 (20 hrs) Solution still cloudy. Began heating to 35? C. 1220 17.8 64.0 1340 35.6 96.1 (22 hrs, 20 min) Solution still cloudy. Increased to 40? C. Let mix overnight. 2520 40.2 104.4 Nov. 25, 2020 (42 hrs) Solution clear. Let cool. Average 23.9 75.0 6.09

TABLE-US-00015 TABLE 15 Headspace UltraPAC 2549SG1 (45% Basic PAS) Conversion Gallons Target initial Actual Working Examples MV-061 MV-061 99.5099 14774.7 11.4 9.3 16.0 17.0 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 3.08 11,940 1,432 8.08 2,100 11,825 1418 8.00 3.00 Sodicum Gluconate 3.00 0.20 300 36 0.20 295 35 0.20 45.0 Water (SA) 0 1.000 45.1 8.04 4,490 539 3.04 1,077 4,435 568 3.00 15.0 Soda Ash 0 NA 15.1 1.02 1,505 NA 1.02 1,480 NA 1.00 156.4 43% SAX 22.99 148.6 1.520 156.6 10.54 15,585 1,230 10.54 1,768 15,410 1216 10.43 % Na.sub.2O SAX 19.41 1160.6 Alun 8.17 0.7 1.325 1160.3 78.11 115,460 10,452 78.11 114,365 10353 77.37 0.00 UP 290 16.91 42.2 1.370 0.0 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.97 0.00 H.sub.3PO.sub.4 (75%) 0 1.570 0.0 0.00 0 0 0.00 0 0 0.00 flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1500.0 UltraPAC 2230 8.81 8.8 1.200 1500.1 100.99 149,275 14,921 100.99 147,8.10 13,749 100.00 Check 1485.4 100.00% 149,280 0 147,810 13,664 100.00% % SA soln 25.1% 1.250 1,237.8 99.02% 147,817 ?1,463 147,810 0 ?85 100.00% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.31% 45.11 18.04 0.00 0.00 18.04 1.92 19.96 Actual 14.7 0.99% Just CO.sub.2 8.75% 17.92 0.00 17.92 1.92 19.84 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 0 0.00% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution Into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Stort addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below S increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution addition is complete acid the sodium gluconate. 12. Lat solution mix until all solids have dissolved. Analysis: Calculated Actual Specific Gravity % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.81 ?8.81 % Fe.sub.2O.sub.3 0.00 % Basicity 45.1 ?45.1 ?15.3 % Sulfates 18.04 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 19.1 66.4 3.94 0.6 6 Agitator @ 200 rpm. Started both feeds @ 12.50 pm. 2.2 1.4 1.6 1 19.6 67.3 5.59 0.6 6 Water/soda ash/sodium aluminate mixture at 35? C. 2.2 1.4 1.6 2 20.0 68.0 6.41 0.6 6 2.2 1.4 1.6 3 20.4 63.7 6.97 0.7 6 2.6 1.4 1.8 4 20.8 69.4 6.84 0.7 6 2.6 1.4 1.8 5 21.2 70.2 6.52 0.7 6 2.6 1.4 1.8 6 21.5 70.7 6.30 0.6 6 Agitator up to 250 rpm. 2.2 1.4 1.6 7 21.7 71.1 6.60 0.6 6 2.2 1.4 1.6 8 22.0 71.6 6.89 0.6 6 2.2 1.4 1.6 9 22.3 72.1 7.08 0.7 6 2.6 1.4 1.8 10 22.5 72.5 6.94 0.7 6 2.6 1.4 1.8 11 22.7 72.9 6.68 0.7 6 2.6 1.4 1.8 12 22.5 73.2 6.57 0.7 6 2.6 1.4 1.8 13 23.1 73.6 6.45 0.7 6 2.5 1.4 1.8 14 23.4 74.1 6.34 0.6 6 2.2 1.4 1.6 15 23.5 74.3 6.48 0.6 6 2.2 1.4 1.6 20 24.3 75.7 6.98 0.7 6 Some crystals forming In water/soda ash/sodium aluminate mixture. increased heat to 40? C. 2.6 1.4 1.8 25 24.8 76.6 5.54 0.6 6 2.2 1.4 1.6 30 25.2 77.4 6.84 0.6 6 More crystals forming in water/soda ash/sodium aluminate mixture. 2.2 1.4 1.6 35 25.5 77.9 6.96 0.7 6 Added 5 g water to the water/soda ash/sodium aluminate mixture. 2.5 1.4 1.8 40 25.8 78.4 6.54 0.6 6 2.2 1.4 1.6 45 25.9 78.6 6.45 0.6 6 Water/soda ash/sodium: aluminate mixture feed complete. 2.2 1.4 1.6 50 26.1 79.0 5.45 0.6 6 Flushed several grams of water through water/soda ash/sodium aluminate mixture. Stopped alum feed. 2.2 1.4 1.6 55 26.2 79.2 6.55 0.6 6 Restarted alum feed. Crystals dissolving in water/soda ash/sodium aluminate mixture 2.2 1.4 1.6 60 26.4 79.5 6.57 0.5 6 2.2 1.4 1.6 65 26.5 79.7 6.59 0.6 6 Still some small crystals in the water/soda ash/sodium aluminate mixture. 2.2 1.4 1.6 75 26.7 80.1 6.58 0.6 6 2.2 1.4 1.6 80 26.8 80.2 6.28 0 6 Water/soda ash/sodium aluminate mixture feed line stopped up. Stopped alum feed. 0.0 1.4 0.0 82 26.9 80.4 6.62 0.6 6 Water/soda ash/sodium aluminate mixture feed line cleared. Restarted alum feed. 2.2 1.4 1.6 1.8 125 26.7 80.1 6.33 0.6 0 Water/soda ash/sodium aluminate mixture feed complete. 2.2 0.0 0.0 135 25.7 78.3 4.99 3.5 0 12.8 0.0 0.0 195 22.8 73.0 3.27 0 0 Aluminum sulfate feed complete. Added sodium gluconate. Let slurry mix overnight. 0.0 0.0 0.0 1245 Dec. 1, 2020 (20 hrs) Solution still cloudy. Began heating to 40? C. 1680 Dec. 1, 2020 (27 hrs) Solution clear. Turned off heat and let cool. Dec. 2, 2020 Due to lthe large amount of evaporation during heating added 120.0 g Di water to the reactor. Dec. 7, 2020 A white percipitate has formed on the bottom of the stability study vial at ~5% by volume. Average 24.4 75.9 6.61

TABLE-US-00016 TABLE 16 Headspace UltraPAC 2549SG2 (45% Basic PAS) Conversion Gallons Target Initial Actual Working Examples MV-064 MV-064 101.4844 14774.7 11.4 5.0 16.0 3.8 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 8.24 12,180 1,461 8.24 2,100 12,180 1461 7.77 3.00 Sodicum Gluconate NA 3.00 0.21 305 37 0.21 305 37 0.19 90.0 Water (SA) 0 1.000 90.2 6.19 9,155 1,098 6.19 2,196 9,155 1172 5.84 30.0 Soda Ash 0 NA 30.1 2.07 3,055 NA 2.07 3,055 NA 1.95 130.9 43% SAX 22.99 148.6 1.520 131.2 9.01 13,315 1,051 9.01 2,149 13,315 1051 8.49 % Na.sub.2O SAX 19.41 1126.1 Alum 8.17 0.7 1.325 1126.2 77.32 114,290 10,346 77.32 114,290 10346 72.90 0.00 UP 290 16.91 42.2 1.370 0.0 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.97 0.00 H.sub.3PO.sub.4 (75%) 0 1.570 0.0 0.00 0 0 0.00 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1500.0 UltraPAC 2230 8.39 8.4 1.200 1500.7 103.04 152,300 15,223 103.03 152,300 13,749 97.14 Check 1456.5 100.01% 152,300 148,828 156,786 14,757 100.00% % SA soln 25.0% 1.249 1,213.8 97.05% 147,814 ?4,486 7,958 4,486 1,009 102.95% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.39% 45.1 17.85 0.00 0.00 17.85 2.15 20.00 Actual 44.2 3.03% Just CO.sub.2 8.19% 17.44 0.00 17,44 2.15 19.59 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. ?4486 ?2.86% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution addition is complete add the sodium gluconate. 12. Let solution mix until all solids have dissolved. Analysis: Calculated Actual Specific Gravity 1.2984 % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.39 8.46 0.07 % Fe.sub.2O.sub.3 0.00 % Basicity 45.1 48.0 2.9 160.3 % Sulfates 17.85 Turbidity, NTU 2.4 Viscosity, cps 13.3 Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.5 70.7 3.69 0.6 6 Agitator @ 200 rpm. Started both feeds @ 1:00 pm. 2.2 1.4 1.6 1 21.7 71.1 5.50 0.6 6 2.2 1.4 1.6 2 21.9 71.4 5.69 0.6 6 2.2 1.4 1.6 3 22.2 72.0 5.66 0.6 7 2.2 1.6 1.4 4 22.5 72.5 6.02 0.6 7 2.2 1.6 1.4 5 22.7 72.9 6.24 0.6 7 2.2 1.6 1.4 6 23.0 73.4 6.42 0.6 7 2.2 1.6 1.4 7 23.2 73.8 6.58 0.6 7 2.2 1.6 1.4 8 23.4 74.1 6.68 0.6 7 2.2 1.6 1.4 9 23.6 74.5 6.77 0.6 7 2.2 1.6 1.4 10 23.8 74.8 6.83 0.6 7 2.2 1.6 1.4 15 24.6 76.3 6.99 0.7 7 2.6 1.6 1.6 20 25.3 77.5 6.35 0.7 7 2.6 1.6 1.6 25 25.4 77.7 6.59 0.7 8 2.6 1.8 1.4 30 26.4 79.5 6.65 0.7 8 Sodium aluminate feed complete. 2.6 1.8 1.4 40 27.2 81.0 6.71 0.7 8 2.6 1.8 1.4 60 28.3 82.9 6.76 0.7 8 2.6 1.8 1.4 80 28.8 83.8 6.82 0.7 8 2.6 1.8 1.4 1.4 98 29.0 84.2 6.90 0.7 0 Water/soda ash/sodium aluminate mixture feed complete. 2.6 0.0 0.0 100 29.0 84.2 6.48 0.7 0 2.6 0.0 0.0 115 26.6 79.9 4.78 4.8 0 17.1 0.0 0.0 160 24.0 75.2 3.38 0 0 Aluminum sulfate feed complete. Added sodium gluconate. 0.0 0.0 0.0 320 23.8 74.8 3.41 0 0 Let slurry mix overnight. 0.0 0.0 0.0 Dec. 4, 2020 (19.5 hrs) Solution mostly clear. 0.0 0.0 0.0 Average 25.5 78.0 6.66

TABLE-US-00017 TABLE 17 Headspace UltraPAC 23615G2 (50% Basic PAS) Conversion Gallons Target Initial Actual Working Examples MV-067 MV-067 104.0051 14774.7 11.4 ?1.5 16.0 15.7 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 8.44 12,480 1,497 8.44 2,100 11,825 1418 8.00 3.00 Sodicum Gluconate 1.581 3.00 0.21 310 37 0.21 187 295 35 0.20 90.0 Water (SA) 0 1.000 90.2 6.35 9,380 2,125 6.35 2,250 8,870 1135 6.60 30.0 Soda Ash 0 NA 30.1 2.12 3,130 NA 2.12 2,955 NA 2.00 155.0 13% SAX 22.99 148.6 1.520 155.1 10.91 16,130 3,273 10.91 2,398 15,275 1205 10.33 % Na.sub.2O SAX 19.41 1102.0 Alum 8.18 0.71 1.325 1109.8 78.09 115,425 10,449 78.05 108,595 9831 23.47 0.0 UP 290 16.91 31.8 1.370 0.0 0.00 0 0 0.00 0.00 % Cl UP 290 20.97 0.0 H.sub.3PO.sub.4 (75%) 0 1.570 0.0 0.00 0 0 0.00 0 0 0.00 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 C 0.00 1500.0 UltraPAC 2230 8.90 8.9 1.200 1508.2 106.12 156,860 15,679 106.12 147,815 13,749 100.00 Check 1421.2 100.00% 156,855 149,928 147,815 13,773 100.00% % SA soln 25.0% 1.249 1,184.3 94.23% 147,807 ?9,048 ?2,113 0 2.4 100.00% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.90% 50.1 18.05 0.80 0.00 18.05 2.44 20.49 Actual 87.0 6.12% Just CO.sub.2 8.44% 17.12 0.00 17.12 2.44 19.56 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 0 0.00% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium: aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution addition is complete add the sodium gluconate. 12. Let solution mix until all solids have dissolved. Analysis: Calculated Actual Specific Gravity 1.3080 % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.90 8.84 ?0.06 % Fe.sub.2O.sub.3 0.00 % Basicity 50.1 52.9 2.8 158.7 % Sulfates 18.05 Turbidity, NTU 3.4 Viscosity, cps 12.9 Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.0 69.8 3.73 0.6 6 Agitator @ 200 rpm. Started both feeds @ 1:30 pm. 2.2 1.4 1.6 1 21.3 70.3 5.24 0.6 6 2.2 1.4 1.6 2 21.6 70.9 5.58 0.6 6 2.2 1.4 1.6 3 22.0 71.6 5.75 0.6 6 2.2 1.4 1.8 4 22.3 72.1 5.85 0.6 6 2.2 1.4 1.6 5 22.5 72.5 5.94 0.6 6 2.2 1.4 1.6 6 22.7 72.9 5.98 0.6 6 2.2 1.4 1.6 7 22.9 73.2 5.02 0.6 7 2.2 1.6 1.4 8 23.2 73.8 6.22 0.6 7 2.2 1.6 1.4 9 23.5 74.3 6.47 0.6 7 2.2 1.6 1.4 10 23.1 74.7 5.68 0.6 7 2.2 1.6 1.4 11 23.9 75.0 6.87 0.6 7 2.2 1.6 1.4 12 24.1 75.4 6.96 0.6 6 2.2 1.4 1.6 13 24.2 75.6 6.90 0.6 6 2.2 1.4 1.6 14 24.4 75.9 6.74 0.6 6 2.2 1.4 1.6 15 24.5 76.1 6.65 0.6 6 2.2 1.4 1.6 20 25.0 77.0 6.34 0.6 7 2.2 1.6 1.4 25 25.6 78.1 6.76 0.6 7 2.2 1.6 1.4 30 26.1 79.0 7.01 0.7 7 2.6 1.6 1.6 40 26.9 80.4 6.48 0.7 8 2.6 1.8 1.4 50 27.7 81.9 6.85 0.7 8 2.6 1.8 1.4 60 28.3 82.0 6.98 0.7 7 2.6 1.6 1.6 70 28.5 83.3 6.69 0.7 7 2.6 1.6 1.6 80 28.6 83.5 6.52 0.7 8 2.6 1.8 1.4 90 28.9 84.0 6.74 0.7 8 2.6 1.8 1.4 100 29.1 84.4 6.87 0.7 8 2.6 1.8 1.4 110 29.3 84.7 6.97 0.7 8 2.6 1.8 1.4 1.5 114 29.3 84.7 7.01 0.7 0 Water/soda ash/sodium aluminate mixture feed complete. 2.6 0.0 0.0 135 26.5 79.7 4.69 4.8 0 Aluminum sulfate feed complete. 17.1 0.0 0.0 175 24.2 75.6 3.43 0 0 Added sodium gluconate 0.0 0.0 0.0 185 24.1 75.4 3.49 0 0 0.0 0.0 0.0 190 24.0 75.2 3.44 0 0 Let slurry mix overnight. 0.0 0.0 0.0 1170 22.3 72.1 Dec. 8, 2020 (19.5 hrs) Solution still cloudy. Set heat at 35? C. Reactor gross weight 2273.5 g. 1230 35.7 96.3 Solution clearing. 1500 35.6 96.1 (25 hrs) Solution clear. Turned off heat and let cool. Average 25.7 78.2 6.64

TABLE-US-00018 TABLE 18 Headspace UltraPAC 2361562.5 (50% Basic PAS)} Conversion Gallons Target Initial Actual Working Examples MV-070 MV-070 101.2688 14774.7 11.4 5.5 16.0 16.2 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 8.22 12,150 1,457 8.22 2,100 12,150 1457 8.22 3.00 Sodicum Gluconate 1.581 3.00 0.21 305 37 0.21 193 305 37 0.21 112.5 Water (SA) 0 1.000 112.5 7.71 11,395 1,367 7.71 2,734 11,395 1459 7.71 37.5 Soda Ash 0 NA 37.5 2.57 3,800 NA 2.57 3,800 NA 2.57 141.0 43% SAX 22.99 148.6 1.520 141.0 9.66 14,280 1,127 9.6 2,494 14,280 1127 9.66 % Na.sub.2O SAX 19.41 1086.0 Alum 8.18 0.71 1.325 1086.0 74.40 109,980 9,956 74.40 109,980 9956 74.40 0.00 UP 290 16.91 41.8 1.370 0.0 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.97 0.00 H.sub.3PO.sub.4 (75%) 0 1.570 0.0 0.00 0 0 0.00 0 0 0.00 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1500.0 UltraPAC 2230 8.31 8.3 1.200 1500.0 102.77 151,905 15,184 102.77 151,910 13,749 102.77 Check 1459.6 100.00% 151,910 147,979 147,819 13,735 100.00% % SA soln 25.0% 1.249 1,216.3 97.31% 147,819 ?4,091 ?160 ?4,091 ?14 97.31% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.31% 50.2 17.20 0.00 0.00 17.20 2.45 19.66 Actual 40.4 2.77% Just CO.sub.2 8.15% 16.87 0.00 16.87 2.45 19.32 1. Add required amount of start tip water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 4091 2.77% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution Into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution addition is complete add the sodium gluconate. 12. Let solution mix until all solids have dissolved. Analysis: Calculated Actual Specific Gravity 1.291 % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.31 8.30 ?0.01 % Fe.sub.2O.sub.3 0.00 % Basicity 50.2 52.4 2.2 157.0 % Sulfates 17.20 Turbidity, NTU 12.6 Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.5 70.7 3.67 0.6 6 Agitator @ 200 rpm. Started both feeds @ 2:00 pm. 2.2 1.4 1.6 1 21.6 70.9 5.07 0.6 7 2.2 1.6 1.4 2 21.8 71.2 5.14 0.6 7 2.2 1.6 1.4 3 22.1 71.8 5.58 0.6 8 2.2 1.8 1.2 4 22.5 72.5 6.23 0.6 8 2.2 1.8 1.2 5 22.8 73.0 6.72 0.6 8 2.2 1.8 1.2 6 23.0 73.4 7.07 0.7 8 2.6 1.8 1.4 7 23.2 73.8 6.86 0.7 8 2.6 1.8 1.4 8 23.5 74.3 6.72 0.7 8 2.6 1.8 1.4 9 23.6 74.5 6.53 0.7 9 2.6 2.0 1.3 10 23.8 74.8 5.70 0.7 9 2.6 2.0 1.3 11 24.0 75.2 6.89 0.7 9 2.6 2.0 1.3 12 24.2 75.6 6.93 0.7 9 2.6 2.0 1.3 13 24.4 75.9 7.05 0.8 9 2.9 2.0 1.5 14 24.5 76.1 6.93 0.8 9 2.9 2.0 1.5 15 24.6 76.3 6.78 1.6 20 5.8 4.2 1.4 16 25.0 77.0 6.46 1.6 20 5.8 4.2 1.4 17 25.5 77.9 6.60 1.6 20 5.8 4.2 1.4 18 26.0 78.8 6.68 1.6 20 5.8 4.2 1.4 19 26.4 79.5 6.80 1.6 20 5.8 4.2 1.4 20 26.8 80.2 6.86 1.6 20 5.8 4.2 1.4 35 30.1 86.2 6.90 1.6 20 5.8 4.2 1.4 50 31.4 88.5 6.96 1.6 20 5.8 4.2 1.4 1.4 56 31.4 88.5 6.96 1.6 0 Water/soda ash/sodium aluminate mixture feed complete. 5.8 0.0 0.0 63 29.1 84.4 5.08 4.2 0 15.0 0.0 0.0 104 29.1 84.4 3.50 0 0 Aluminum sulfate feed complete. Addled sodium gluconate 0.0 0.0 0.0 110 24.6 76.3 3.50 0 0 Let slurry mix overnight. 0.0 0.0 0.0 1065 Dec. 10, 2020 (18 hrs) Solution clear. Filtered solution through #41 Whatman paper. Average 25.8 78.4 6.81

TABLE-US-00019 TABLE 19 Headspace UltraPAC 22865G2.75 (55% Basic PAS) Conversion Gallons Target Initial Actual Working Examples MY-073 MV-073 97.0532 14774.7 11.4 0.6 16.0 5.6 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 7.88 11,645 1,397 7.88 2,100 12,475 1496 8.00 3.00 Sodicum Gluconate 1.582 3.00 0.20 290 35 0.20 196 310 37 0.20 124.0 Water (SA) 0 1.000 124.2 8.15 12,055 1,446 8.1 2,892 12,890 1650 8.27 41.3 Soda Ash 0 NA 41.4 2.72 4,020 NA 2.72 4,295 NA 2.75 156.5 43% SAX 22.99 148.6 1.520 156.6 10.28 15,200 1,199 10.28 2,645 16,270 128 10.43 % Na.sub.2O SAX 19.41 1055.2 Alum 8.18 0.71 1.325 1155.8 75.89 112.175 10,155 75.89 109,685 9929 70.34 0.0 UP 290 16.91 41.8 1.370 0.0 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.97 0.0 H.sub.3PO.sub.4 (75%) 0 1.570 0.0 0.00 0 0 0.00 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1500.0 UltraPAC 2230 8.57 8.6 1.200 1601.0 105.12 155,380 15,531 105.12 155,925 13,749 100.00 Check 1523.0 100.00% 155,385 149,194 155,925 14,611 100.00% % SA soln 23.0% 1.249 1,269.2 95.13% 147,815 ?7,570 6,731 0 863 100.00% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.57% 51.7 17.55 0.00 0.00 17.55 2.60 20.15 Actual 78.0 5.12% Just CO.sub.2 8.22% 16.83 0.00 16.83 2.60 19.43 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 0 0.00% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution addition is complete add the sodium gluconate. 12. Let solution mix until all solids have dissolved. Analysis: Calculated Actual Specific Gravity 1.3016 % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.57 8.56 ?0.01 % Fe.sub.2O.sub.3 0.00 % Basicity 51.7 54.0 2.3 157.1 % Sulfates 17.55 Turbidity, NTU 2.7 Viscosity, cps 12.9 Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 20.9 69.6 3.94 0.6 6 Agitator @ 200 rpm. Started both feeds @ 2:50 pm. 2.2 1.4 1.6 1 21.2 70.2 4.93 0.6 6 2.2 1.4 1.6 4 22.0 71.6 5.39 0.6 6 2.2 1.4 1.6 5 22.2 72.0 5.47 0.6 7 2.2 1.6 1.4 6 22.4 72.3 5.47 0.6 7 2.2 1.5 1.4 7 22.8 73.0 5.65 0.6 7 2.2 1.6 1.4 9 23.4 74.1 5.97 0.6 7 2.2 1.6 1.4 10 23.7 24.7 6.05 0.6 7 2.2 1.5 1.4 12 24.2 75.6 6.18 0.6 7 2.2 1.6 1.4 14 24.5 76.1 6.29 0.6 8 2.2 1.8 1.2 16 24.8 76.6 6.30 0.6 8 2.2 1.8 1.2 18 25.1 77.2 6.59 0.6 8 2.2 1.8 1.2 20 25.2 77.4 6.82 0.6 8 2.2 1.8 1.2 25 25.8 78.4 7.19 0.7 8 2.6 1.8 1.4 30 26.3 79.3 6.87 0.7 8 2.6 1.8 1.4 35 26.6 79.9 6.67 0.7 8 2.6 1.8 1.4 40 26.9 80.4 6.58 0.7 8 2.6 1.8 1.4 45 27.7 81.9 6.50 0.7 8 2.6 1.8 1.4 50 27.7 81.9 6.45 0.7 8 2.6 1.8 1.4 60 27.8 82.0 6.40 0.7 9 2.6 2.0 1.3 70 28.2 82.8 6.70 0.7 9 2.6 2.0 1.3 80 28.5 83.3 6.87 0.7 9 2.6 2.0 1.3 90 28.7 83.7 7.01 0.7 8 2.6 1.8 1.4 100 28.8 83.8 6.85 0.7 8 2.6 1.8 1.4 110 28.8 83.8 6.77 0.7 8 2.6 1.8 1.4 1.4 123 28.8 83.8 6.74 0.7 0 Water/soda ash/sodium aluminate mixture feed complete. 2.6 0.0 0.0 140 26.5 29.7 4.94 4.2 0 15.0 0.0 0.0 182 23.8 74.8 3.53 0 0 Aluminum sulfate feed complete. Added sodium gluconate. 0.0 0.0 0.0 230 23.7 74.7 3.57 0 0 Let slurry mix overnight. 0.0 0.0 0.0 1060 22.5 22.5 Dec. 16, 2020 (17 hrs 40 mins) Solution still cloudy clear. Set heat to 35? C. 1300 35.4 95.7 Dec. 16, 2020 (21 hrs 40 mins) Solution clear. Let cool. Filtered solution through #41 Whatman paper. Average 25.9 78.6 6.45

TABLE-US-00020 TABLE 20 Headspace UltraPAC 2286SG3 (55% Basic PAS) Conversion Gallons Target Initial Actual Working Examples MV-076 MV-076 101.5192 14774.7 11.4 4.7 16.0 14.3 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 8.24 12,180 1,461 8.24 2.100 11,825 1418 8.00 3.00 Sodicum Gluconate 1.581 3.0 0.21 305 37 0.21 187 295 35 0.20 135.0 Water (SA) 0 1.000 135.2 9.29 13,725 1,646 9.29 3,293 13,305 1704 9.00 45.0 Soda Ash 0 NA 45.1 3.10 4,580 NA 3.10 4,435 NA 3.00 149.0 43% SAX 22.99 148.6 1.520 149.4 10.26 15,165 1,197 10.26 2,843 14,685 1159 9.93 % Na.sub.2O SAX 19.41 1048.0 Alum 8.18 0.71 1.325 1049.5 72.09 106,555 9,646 72.09 103,270 9349 69.86 0.0 UP 290 16.91 41.8 1.370 0.0 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.97 0.0 H.sub.3PO.sub.4 (75%) 0 1.570 0.0 0.00 0 0 0.00 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1500.0 UltraPAC 2230 8.26 8.3 1.200 1502.3 103.19 152,510 15,244 103.18 147,815 13,749 1.00.00 Check 1456.0 100.01% 152,510 147,647 147,815 13,886 100.00% % SA soln 25.0% 1.249 1,213.3 96.92% 147,810 ?4,700 168 0 137 100.00% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.26% 55.0 16.67 0.00 0.00 16.67 2.76 19.43 Actual 46.3 3.18% Just CO.sub.2 8.08% 16.31 0.00 16.31 2.76 19.07 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 0 0.00% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution addition is complete add the sodium gluconate. 12. Let solution mix until all solids have dissolved. Analysis: Calculated Actual Specific Gravity 1.2881 % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.26 8.22 ?0.04 % Fe.sub.2O.sub.3 0.00 % Basicity 55.0 58.3 3.3 160.2 % Sulfates 16.67 Turbidity, NTU 4.1 Viscosity, cps 12.5 Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.1 70.0 3.63 0.6 6 Agitator @ 200 rpm. Started both feeds @ 2:50 pm. 2.2 1.4 1.6 1 21.3 70.3 4.87 0.6 6 2.2 1.4 1.6 2 21.5 70.7 4.90 0.6 7 2.2 1.6 1.4 3 21.9 71.4 5.49 0.6 7 2.2 1.6 1.4 4 22.0 71.6 5.65 0.6 8 2.2 1.8 1.2 5 22.3 72.1 6.01 0.6 8 2.2 1.8 1.2 6 22.7 72.9 6.30 0.6 8 2.2 1.8 1.2 7 23.0 73.4 6.47 1.2 16 4.3 3.4 1.3 8 23.6 74.5 6.90 1.2 16 4.3 3.4 1.3 9 24.2 25.6 7.05 1.3 16 4.7 3.4 1.4 10 24.6 76.3 6.97 1.3 24 4.7 5.0 0.9 11 25.0 77.0 6.87 2.0 24 7.2 5.0 1.4 12 25.6 78.1 6.62 2.0 25 7.2 5.2 1.4 13 26.2 79.2 6.43 2.0 25 7.2 5.2 1.4 14 26.7 80.1 6.55 2.0 25 7.2 5.2 1.4 15 27.2 81.0 6.60 2.0 25 7.2 5.2 1.4 20 28.4 33.1 6.58 2.0 25 7.2 5.2 1.4 30 31.0 87.8 6.63 2.0 25 7.2 5.2 1.4 40 32.1 89.8 6.68 2.0 25 7.2 5.2 1.4 14.3 49 32.0 89.6 6.02 2.0 0 Water/soda ash/sodium aluminate mixture feed complete. 7.2 0.0 0.0 55 30.0 86.0 4.90 4.8 0 17.1 0.0 0.0 90 25.1 77.2 3.64 0 0 Aluminum sulfate feed complete. Added sodium gluconate. 0.0 0.0 0.0 95 25.0 77.0 3.64 0 0 Let slurry mix overnight. 0.0 0.0 0.0 1080 22.7 72.9 Dec. 18, 2020 (18 hrs) Solution clear. Filtered solution through #41 Whatman paper. Average 26.2 79.1 6.58

TABLE-US-00021 TABLE 21 Headspace UltraPAC 2362SG3 (60% Basic PAS) Conversion Gallons Target Initial Actual Working Examples MV-080 MV-080 103.2784 14774.7 11.4 1.2 16.0 14.3 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 8.38 12,395 1,487 8.39 2,100 11,825 1418 8.00 3.00 Sodicum Gluconate 1.581 3.00 0.21 310 37 0.21 187 295 35 0.20 135.0 Water (SA) 0 1.000 135.1 9.44 13,955 1,674 9.44 3,348 13,305 1704 9.00 45.0 Soda Ash 0 NA 45.0 3.14 4,650 NA 3.15 4,435 NA 3.00 162.8 43% SAX 22.99 155.6 1.520 163.2 11.40 16,855 1,330 11.40 3,004 14,685 1159 9.93 % Na.sub.2O SAX 19.41 1034.2 Alum 8.18 0.71 1.325 1034.3 72.27 106,820 9,670 72.26 103,270 9349 69.86 0.0 UP 290 16.91 41.8 1.370 0.0 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.97 0.0 H.sub.3PO.sub.4 (75%) 0 1.570 0.0 0.00 0 0 0.00 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1500.0 UltraPAC 2230 8.53 8.5 1.200 1500.6 104.84 154,980 15,491 104.85 147,815 13,749 100.00 Check 1431.2 99.99% 154,985 148,495 147,815 13,886 100.00% % SA soln 25.0% 1.249 1,192.7 95.38% 147,817 ?7,168 ?680 0 137 100.00% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.53% 60.1 16.71 0.00 0.00 16.71 2.94 19.65 Actual 69.4 4.85% Just CO.sub.2 8.22% 16.09 0.00 16.09 2.94 19.03 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 0 0.00% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH fails below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution addition is complete add the sodium gluconate. 12. Let solution mix until all solids have dissolved. Analysis: Calculated Actual Specific Gravity 1.2955 % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.53 8.55 0.02 % Fe.sub.2O.sub.3 0.00 % Basicity 60.1 61.6 % Sulfates 16.71 1.5 160.4 Turbidity, NTU 1.6 Viscosity, cps 12.0 Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.0 69.8 3.96 0.6 6 Agitator @ 200 rpm. Started both feeds @ 3:05 pm. 2.2 1.4 1.6 1 21.2 70.2 4.73 0.6 6 2.2 1.4 1.6 2 21.3 70.3 4.64 0.6 8 2.2 1.8 1.2 3 21.5 70.7 4.49 0.6 8 2.2 1.8 1.2 4 21.7 71.1 4.53 0.6 8 Water/soda ash/sodium aluminate mixture feed line clogged. 2.2 1.8 1.2 6 22.2 72.0 5.80 0.6 8 2.2 1.8 1.2 7 22.5 72.5 6.16 0.6 8 2.2 1.8 1.2 8 22.9 73.2 6.43 0.6 8 2.2 1.8 1.2 23 25.3 77.5 7.79 0.8 8 2.9 1.8 1.6 25 25.5 77.9 7.10 1.6 16 5.8 3.4 1.7 26 25.8 78.4 6.67 1.6 17 5.8 3.6 1.6 27 26.2 79.2 6.44 1.6 18 5.8 3.8 1.5 28 26.7 80.3 6.39 3.2 38 11.4 7.7 1.5 30 27.6 81.7 6.51 3.2 38 11.4 7.7 1.5 35 30.4 86.7 6.70 3.2 38 11.4 7.7 1.5 40 32.0 89.6 6.71 3.2 38 11.4 7.7 1.5 1.5 50 33.9 93.0 6.84 3.2 0 Water/soda ash/sodium aluminate mixture feed complete. 11.4 0.0 0.0 52 33.4 92.1 6.13 3.2 0 11.4 0.0 0.0 67 31.0 87.8 4.87 4.2 0 15.0 0.0 0.0 90 25.9 78.6 3.76 0.0 0 Aluminum sulfate feed complete. Added sodium gluconate. 0.0 0.0 0.0 105 25.7 78.3 3.79 0 0 Let slurry mix overnight. 0.0 0.0 0.0 1110 Jan. 7, 2021 (18.5 hrs) Solution still cloudy clear. Set heat to 35? C. 1300 (21.6 hrs) Solution clear. Filtered solution through #41 Whatman paper. Average 27.3 81.2 6.63

TABLE-US-00022 TABLE 22 Headspace UltraPAC XXXXSG3 (65% Basic PAS) Conversion Gallons Target Initial Actual Working Examples MV-085 MV-085 103.9246 34774.7 11.4 ?0.2 16.0 14.3 Digest Temp. (? C.) Formulation Target Actual Target Overnight (C) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 8.44 12,470 1,496 8.44 2,100 11,825 1418 8.00 3.00 Sodicum Gluconate 1.581 3.00 0.21 310 37 0.21 187 295 35 0.20 157.5 Water (SA) 0 1.000 157.7 11.09 16,390 1,966 11.09 3,932 13,305 1704 9.00 52.5 Sada Ash 0 NA 52.6 3.70 5,465 NA 3.70 4,435 NA 3.00 169.7 43% SAX 22.99 156,4 1.520 169.9 11.95 17,655 1,393 11.94 3,359 14,685 1159 9.93 % Na.sub.2O SAX 19.41 997.3 Alum 8.18 0.71 1.325 997.1 70.10 103,625 9,381 70.11 103,270 9349 69.86 0.0 UP 290 16.91 41.8 1.370 0.0 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.97 0.0 H.sub.3PO.sub.4 (75%) 0 1.570 0.0 0.00 0 0 0.00 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1500.0 UltraPAC 2230 8.48 8.5 1.200 1500.3 105.49 155,920 15,585 105.48 147,815 13,749 100.00 Check 1422.3 100.01% 155,915 148,105 147,815 13,886 100.00% % SA soln 25.0% 1.249 1,185.3 94.80% 147,809 ?8,106 ?290 0 137 100.00% Evaporation % Al.sub.2O.sub.3 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.48% 65.1 16.21 0.00 0.00 16.21 3.25 19.46 Actual 78.0 5.48% Just CO.sub.2 8.13% 15.54 0.00 15.54 3.25 18.79 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 0 0.00% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the phi falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution addition is complete add the sodium gluconate. 12. Let solution mix until all solids have dissolved. Analysis: Calculated Actual Specific Gravity 1.2921 % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.48 8.51 0.03 % Fe.sub.2O.sub.3 0.00 % Basicity 65.1 65.0 ?0.1 156.1 % Sulfates 16.21 Turbidity, NTU 2.8 Viscosity, cps 12.5 Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry UP290 SA/SAX Alum SA/SAX Time Temp. Temp. Bulk pump pump pump rate pump rate Pump (min) (? C.) (? F.) slurry pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.6 70.9 3.70 0.6 6 Agitator @ 200 rpm. Started both feeds @ 10:45 pm. 2.2 1.4 1.6 1 21.6 70.9 5.35 0.6 6 2.2 1.4 1.6 2 21.7 71.1 5.28 0.6 6 2.2 1.4 1.6 3 21.7 71.1 5.26 0.6 7 2.2 1.6 1.4 4 22.2 72.3 5.59 0.6 7 2.2 1.6 1.4 5 22.8 72.7 5.73 0.6 8 2.2 1.8 1.2 6 23.0 73.4 6.02 0.6 8 2.2 1.8 1.2 7 23.3 73.9 6.21 0.6 8 2.2 1.8 1.2 8 23.6 74.5 6.39 1.2 16 4.3 3.4 1.3 9 24.3 75.4 6.68 1.2 16 4.3 3.4 1.3 10 24.6 76.3 6.85 2.4 30 8.6 6.2 1.4 11 25.5 77.9 6.66 2.4 30 8.6 6.2 1.4 17 26.2 79.2 6.80 2.4 29 8.6 6.0 1.4 13 26.9 80.2 6.88 2.4 28 8.6 5.8 1.5 14 27.3 81.1 6.74 2.4 28 8.6 5.8 1.5 15 27.5 82.2 6.65 2.4 28 8.6 5.8 1.5 20 29.6 85.3 6.53 2.4 28 Water/soda ash/sodium aluminate mixture feed complete. 8.6 5.8 1.5 30 31.5 88.1 6.48 2.4 28 8.6 5.8 1.5 40 32.5 90.5 6.48 2.4 28 8.6 5.8 1.5 1.4 50 32.8 91.0 6.51 2.4 0 8.6 0.0 0.0 57 30.5 86.9 5.04 4.8 0 17.1 0.0 0.0 110 25.3 77.5 3.94 0 0 Aluminum sulfate feed complete. Added sodium gluconate. 0.0 0.0 0.0 115 25.2 77.4 3.95 0 0 Let slurry mix overnight. 0.0 0.0 0.0 1350 22.5 72.5 Jan. 13, 2021 (22.5 hrs) Still cloudy. Set heat to 35? C. 1440 35.8 96.4 (24 hrs) Solution clear, filtered through #41 Whatman paper. Average 26.8 80.2 6.51

TABLE-US-00023 TABLE 23 Headspace 50% Basic PAS Conversion Gallons Target Initial Actual Working Examples MV-110 MV-110 105.9717 14774.7 11.4 9.2 16.0 2.9 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 120.0 Start Up Water 0 1.000 120.0 8.00 12,715 1,525 8.00 2,100 12,715 1525 8.00 0.00 Sodicum Gluconate 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 112.3 Water (SA) 0 1.000 112.7 7.53 11,945 1,433 2.51 2,866 11,945 1530 7.51 37.5 Soda Ash 0 NA 37.6 2.51 3,985 NA 2.51 3,985 NA 2.51 126.3 43% SAX 22.96 149.0 1.520 141.4 9.42 14,985 1,183 9.42 2,615 14,985 1183 9.42 % Na.sub.2O SAX 19.35 1103.9 Alum 7.98 3.8 1.325 1104.4 73.60 117,035 10,595 73.60 117,035 10595 73.60 0.0 UP 290 16.91 41.8 1.370 0.0 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.97 0.0 H.sub.3PO.sub.4 (75%) 0 1.570 0.0 0.00 0 0 0.00 0 0 0.00 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 1500.0 50% Basic PAS 8.04 8.0 1.291 1516.1 101.04 160,665 14,927 101.03 160,665 13,749 101.03 Check 1500.6 100.01% 160,665 0 159,022 14,834 100.00% % SA soln 25.0% 1.249 1,162.4 98.98% 159,022 ?1,643 159,022 ?1,643 1,085 98.98% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.04% 52.9 16.60 0.00 0.00 16.60 2.39 18.99 Actual 15.5 1.03% Just CO.sub.2 8.02% 16.56 0.00 16.56 2.39 18.95 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 1,643 1.03% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between: 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution addition is complete add the sodium gluconate. 12. Let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.04 8.13 0.09 (final weight prior to digestion) % Fe.sub.2O.sub.3 0.00 % Basicity 52.6 54.6 1.7 155.4 (average % Basicity of 5 fractions) % Sulfates 16.60 Turbidity, NTU 2.6 Viscosity, cps 14.2 Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.1 70.0 3.89 0.6 6 Agitator @ 200 rpm. Started both feeds @ 3:20 pm. 2.2 1.4 1.6 1 21.3 70.3 4.89 0.6 6 2.2 1.4 1.6 2 21.5 70.7 5.07 0.6 7 2.2 1.6 1.4 3 21.9 71.4 5.65 0.6 7 2.2 1.6 1.4 6 22.2 72.0 5.83 0.6 7 2.2 1.6 1.4 10 22.7 72.9 6.11 1.8 21 6.5 4.4 1.5 12 23.8 74.8 5.79 1.8 24 Agitator up to 250 rpm. 6.5 5.0 1.3 15 25.7 78.3 6.72 3.6 48 12.8 9.7 1.3 17 27.5 81.5 6.90 3.6 48 12.8 9.7 1.3 18 28.2 82.8 7.06 3.6 46 12.8 9.3 1.4 19 28.9 84.0 7.05 3.6 44 12.8 8.9 1.4 20 29.5 85.1 6.97 3.6 44 12.8 8.9 1.4 25 21.4 70.5 6.82 3.6 44 12.8 8.9 1.4 30 32.6 90.7 6.80 3.6 44 12.8 8.9 1.4 32 32.9 91.2 6.74 3.7 44 13.2 8.9 1.5 1.4 36 30.5 86.9 5.09 4.8 0 Water/soda ash/sodium aluminate mixture feed complete. 17.1 0.0 0.0 110 25.0 77.0 3.99 0 0 Aluminum sulfate feed complete. 0.0 0.0 0.0 Split samples into six fractions and added required amount of sodium gluconate to each. Sample MV-110 - 0.0% sodium gluconate. Sample MV-111A - 0.2% sodium: gluconate. Sample MV-111B - 0.4% sodium gluconate. Sample MV-113C - 0.6% sodium gluconate. Sample MV-111D - 0.8% sodium gluconate. Sample MV-111E - 1.0% sodium gluconate, Let slurries mix overnight. Sep. 22, 2021 9:00 am (18.2 hrs) - all samples clear. Filtered all through # 541 Whatman paper. Samples used for accelerated stability studies. Average 27.2 80.9 6.49

TABLE-US-00024 TABLE 24 UltraPAC 2361 Headspace (50% Basic PAS) Conversion Gallons Target Initial Actual Working Examples MV-115 MV-115 305.8833 14774.7 11.4 3.8 16.0 17.1 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 40.00 Start Up Water 0 1.000 40.00 8.28 12,235 1,468 8.28 2,100 12,235 1468 8.28 0.00 Ferric sulfate 17.75 10.5 1.583 0.00 0.00 0 0 0.00 0 0 0 0.00 37.41 Water (SA) 0 1.000 37.49 7.76 11,470 1,376 7.76 2,752 11,470 1469 7.76 12.50 Soda Ash 0 NA 12.53 2.59 3,835 NA 2.59 3,835 NA 2.59 45.60 43% SAX 22.96 149.0 1.520 45.69 9.46 13,975 1,103 9.45 2,479 13,975 1103 9.45 % Na.sub.2O SAX 19.35 354.50 Alum 7.98 3.8 1.325 354.57 73.37 108,455 9,818 73.37 108,455 9818 73.37 0.00 UP 290 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 10.00 H.sub.3PO.sub.4 (75%) 0 1.570 10.26 2.12 3,140 240 2.12 3,140 240 2.12 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 500.0 UltraPAC 2230 8.03 8.0 1.200 500.5 103.58 153,105 15,304 101.46 153,110 13,749 103.58 Check 483.2 100.00% 153,110 0 147,820 13,654 100.00% % SA soln 25.0% 1.249 402.7 96.54% 147,815 ?5,295 147,820 ?5,290 ?95 96.55% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.03% 46.6 16.55 0.00 0.00 16.55 2.43 18.98 Actual 17.3 3.58% Just CO.sub.2 7.81% 16.10 0.00 16.10 2.43 18.53 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 5,290 3.58% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate reed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all sulids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.03 7.98 ?0.05 % Fe.sub.2O.sub.3 0.00 % Basicity 46.6 46.2 ?0.4 147.7 % Sulfates 16.55 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 20.4 68.7 3.53 0.6 6 Agitator at 175 rpm. Started both feeds at 4:30 pm. 2.2 1.4 1.6 1 21.0 69.8 4.50 0.6 6 2.2 1.4 1.6 2 21.4 70.5 4.66 0.6 6 2.2 1.4 1.6 3 21.7 71.3 4.79 0.6 7 2.2 1.6 1.4 4 22.3 72.1 5.08 0.6 7 2.2 1.6 1.4 5 22.6 72.7 5.16 0.6 7 2.2 1.6 1.4 6 23.2 73.8 5.32 0.6 7 2.2 1.6 1.4 7 23.8 74.8 5.77 0.6 7 2.2 1.6 1.4 8 24.3 75.7 5.63 0.6 8 2.2 1.8 1.2 9 24.8 76.6 5.75 0.6 8 2.2 1.8 1.2 10 25.3 77.5 5.89 0.6 8 2.2 1.8 1.2 12 26.1 79.0 6.10 0.6 8 2.2 1.8 1.2 14 26.7 80.3 6.27 0.6 8 2.2 1.8 1.2 16 27.1 80.8 6.40 0.6 8 2.2 1.8 1.2 18 27.5 81.5 6.27 0.6 9 Agitator at 200 rpm. 2.2 2.0 1.1 20 27.9 82.2 7.12 0.6 8 2.2 1.8 1.2 22 28.1 82.6 7.19 0.6 6 2.2 1.4 1.6 24 28.1 82.6 6.82 0.6 6 2.2 1.4 1.6 26 28.1 82.6 6.49 0.6 6 2.2 1.4 1.6 28 28.1 82.6 6.51 0.6 7 2.2 1.6 1.4 30 28.3 82.9 6.36 0.6 8 2.2 1.8 1.2 32 28.5 83.3 6.49 0.6 8 2.2 1.8 1.2 34 28.6 83.5 6.62 0.6 8 2.2 1.8 1.2 36 28.7 83.7 6.70 0.6 8 2.2 1.8 1.2 40 29.0 84.2 6.91 0.6 8 2.2 1.8 1.2 1.3 41 29.0 84.2 6.84 0.6 0 Water/soda ash/sodium aluminate mixture feed complete. 2.2 0.0 0.0 50 26.3 79.3 5.01 4.8 0 17.1 0.0 0.0 60 23.2 73.8 3.98 0.6 0 Aluminum sulfate feed complete. Started Phosphoric acid (75%) solution feed. 2.2 0.0 0.0 66 26.1 79.0 3.91 0.0 0 Phosphoric acid (75%) solution feed complete. Let mix overnight. 0.0 0.0 0.0 Sep. 24, 2021 - 9:00 am (19.5 hrs) Solution clear, Filtered through # 541 Whatman paper. Average 26.6 80.0 6.31

TABLE-US-00025 TABLE 25 UltraPAC 2361 (50% Basic PAS) Headspace 2.0% Phosphoric acid (75%) solution Conversion Gallons Target Initial Actual Working Examples MV-119 MV-119 305.9720 14774.7 11.4 3.8 16.0 17.4 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 40.00 Start Up Water 0 1.000 40.00 8.28 12,240 1,468 8.28 2,100 12,240 1468 8.28 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 37.41 Solution Water 0 1.000 37.44 7.75 11,455 1,374 7.75 2,748 11,455 1467 7.75 12.50 Sodium carbonate 0 NA 12.52 2.59 3,830 NA 2.59 3,830 NA 2.59 50.58 43% Sodium aluminate 22.96 149.0 1.520 51.09 10.58 15,630 1,233 10.57 2,607 15,630 1235 10.57 % Na.sub.2O SAX 19.35 349.52 Alumium sulfate 7.98 3.8 1.325 349.28 72.30 106,870 9,675 72.30 106,870 9675 72.30 0.00 Pressure PAC (UP 290) 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 10.00 Phosphoric acid (75%) 0 1.570 10.11 2.09 3,095 236 2.09 3,095 236 2.09 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 500.0 Final product 8.20 8.20 1.200 500.4 1.03.59 153,120 15,305 101.50 153,120 13,749 103.59 Check 483.1 100.00% 153,120 0 147,811 13,634 100.00% % SA soln 25.1% 1.250 402.6 96.53% 147,811 ?5,309 147,811 ?5,309 ?115 96.53% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.20% 50.3 16.31 0.00 0.00 16.31 2.59 18.89 Actual 17.4 3.59% Just CO.sub.2 7.98% 15.87 0.00 15.87 2.59 18.45 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 5,309 3.59% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.21 8.10 ?0.10 % Fe.sub.2O.sub.3 0.00 % Basicity 50.3 49.9 ?0.4 147.6 % Sulfates 16.31 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 22.2 72.0 3.66 0.6 6 Agitator at 200 rpm. Started both feeds at 2:55 pm. 2.2 1.4 1.6 1 22.5 72.5 8.77 0.6 6 2.2 1.4 1.6 2 22.9 73.2 4.48 0.6 6 2.2 1.4 1.6 3 23.1 73.6 4.69 0.6 8 2.2 1.8 1.2 4 23.7 74.7 4.94 0.6 8 2.2 1.8 1.2 5 24.3 75.7 5.77 0.6 8 2.2 1.8 1.2 6 24.9 76.8 6.02 0.6 8 2.2 1.8 1.2 7 25.6 78.1 5.84 0.6 8 Agitator at 250 rpm. 2.2 1.8 1.2 8 25.9 78.8 6.11 0.6 8 2.2 1.8 1.2 9 26.3 79.3 6.28 0.6 8 2.2 1.8 1.2 10 26.6 79.9 6.42 0.6 8 2.2 1.8 1.2 14 27.8 82.0 7.22 0.6 7 2.2 1.6 1.4 15 28.0 82.4 7.05 0.6 7 2.2 1.6 1.4 20 28.5 83.3 6.69 0.6 7 2.2 1.6 1.4 25 29.0 84.2 6.69 0.6 7 2.2 1.6 1.4 30 29.3 84.7 6.74 0.6 7 2.2 1.6 1.4 35 29.5 85.1 6.70 0.6 7 2.2 1.6 1.4 40 29.0 85.3 6.69 0.6 7 2.2 1.6 1.4 1.3 45 29.7 85.5 6.67 0.6 0 Water/soda ash/sodium aluminate mixture feed complete. 2.2 0.0 0.0 55 26.8 80.2 4.99 4.8 0 17.1 0.0 0.0 63 24.3 75.7 4.05 0.6 0 Aluminum sulfate feed complete. 2.2 0.0 0.0 65 24.3 75.7 4.06 0.6 0 Started Phosphoric acid (75%) solution feed. 2.2 0.0 0.0 71 27.1 80.8 3.96 0.6 0 Phosphoric acid (75%) solution feed complete. 2.2 0.0 0.0 105 25.5 77.5 4.14 0 0 Let mix overnight. 0.0 0.0 0.0 Sep. 29, 2021 - 9:00 am (18.1 hrs) Solution clear. Filtered through # 541 Whatman paper. Average 27.0 80.6 6.49

TABLE-US-00026 TABLE 26 UltraPAC 2361 (50% Basic PAS) Headspace 0.25% Phosphoric acid (75%) solution Conversion Gallons Target Initial Actual Working Examples MV-122 MV-122 306.0417 14774.7 11.6 3.9 16.0 16.6 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 40.00 Start Up Water 0 1.000 40.00 8.28 12,240 1,468 8.28 2,100 12,240 1468 8.28 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 37.41 Solution Water 0 1.000 37.44 7.75 11,460 1,375 7.75 2,745 11,460 1468 7.75 12.50 Sodium carbonate 0 NA 12.52 2.59 3,830 NA 2.59 3,830 NA 2.59 43.10 43% Sodium aluminate 22.96 149.0 1.520 43.31 8.97 13,255 1,046 8.97 2,421 13,255 1046 8.97 % Na.sub.2O SAX 19.35 365.70 Alumium sulfate 7.98 3.8 1.325 365.62 75.70 111,895 10,129 75.70 111,895 10129 75.70 0.00 Pressure PAC (UP 290) 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 1.25 Phosphoric acid (75%) 0 1.570 1.25 0.26 385 29 0.26 385 29 0.26 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 500.0 Final product 8.10 8.10 1.200 500.1 103.55 153,065 15,300 105.29 153,065 13,749 103.55 Check 483.0 100.00% 153,065 147,813 13,702 100.00% % SA soln 25.1% 1.250 402.5 96.57% 147,813 ?5,252 147,813 ?5,252 ?47 96.57% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.10% 50.1 17.07 0.00 0.00 17.07 2.36 19.43 Actual 17.2 3.55% Just CO.sub.2 7.82% 16.49 0.00 16.49 2.36 18.85 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 5,252 3.55% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.10 8.07 ?0.03 % Fe.sub.2O.sub.3 0.00 % Basicity 50.1 48.6 ?1.5 142.9 % Sulfates 17.07 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.2 70.2 3.79 0.6 7 Agitator at 200 rpm. Started both feeds at 12:45 pm. 2.2 1.6 1.4 1 21.8 71.2 5.46 0.6 7 2.2 1.6 1.4 2 22.4 72.3 5.93 0.6 7 2.2 1.6 1.4 3 22.9 73.2 4.87 0.6 7 2.2 1.6 1.4 4 23.4 74.1 5.80 0.6 7 Agitator at 250 rpm. 2.2 1.6 1.4 5 23.8 74.8 5.80 0.6 7 2.2 1.6 1.4 6 24.1 75.4 5.85 0.6 7 2.2 1.6 1.4 7 24.4 75.5 5.90 0.6 7 2.2 1.6 1.4 8 24.7 76.5 5.91 0.6 8 2.2 1.8 1.2 9 25.1 77.2 6.09 0.6 8 2.2 1.8 1.2 10 25.5 77.9 6.16 0.6 8 2.2 1.8 1.2 11 25.8 78.4 6.36 0.6 8 2.2 1.8 1.2 12 26. 79.0 6.44 0.6 8 2.2 1.8 1.2 13 26.4 79.5 6.55 0.6 8 2.2 1.8 1.2 14 26.6 79.9 6.70 0.6 8 2.2 1.8 1.2 15 26.9 80.4 6.67 0.6 8 2.2 1.8 1.2 20 27.7 81.9 6.82 0.6 8 2.2 1.8 1.2 25 28.3 82.9 6.73 0.6 8 2.2 1.8 1.2 30 28.7 83.7 6.71 0.6 8 2.2 1.8 1.2 35 28.9 84.0 6.98 0.6 8 2.2 1.8 1.2 1.3 39 29.1 84.4 6.98 0.6 0 Water/soda ash/sodium aluminate mixture feed complete. 2.2 0.0 0.0 49 25.1 77.2 4.98 4.8 0 17.1 0.0 0.0 59 23.5 74.3 3.94 0.6 0 Aluminum sulfate feed complete. Started Phosphoric acid (75%) solution feed. 2.2 0.0 0.0 65 23.8 74.8 3.95 0 0 Phosphoric acid (75%) solution feed complete. 0.0 0.0 0.0 150 22.6 72.7 4.10 0 0 Let mix overnight. 0.0 0.0 0.0 Sep. 30, 2021 - 9:00 am (20.75 hrs) Solution clear. Filtered through # 541 Whatman paper. Average 25.9 78.5 6.42

TABLE-US-00027 TABLE 27 UltraPAC 2361 (50% Basic PAS) Headspace 0.50% Phosphoric acid (75%) solution Conversion Gallons Target Initial Actual Working Examples MV-125 MV-125 305.8201 14774.7 11.4 4.1 16.0 16.6 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 40.00 Start Up Water 0 1.000 40.00 8.28 12,235 1,468 8.28 2,100 12,235 1468 8.28 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 37.41 Solution Water 0 1.000 37.41 7.74 11,440 1,372 7.74 2,744 11,440 1465 7.74 12.50 Sodium carbonate 0 NA 12.50 2.59 3,825 NA 2.59 3,825 NA 2.59 44.20 43% Sodium aluminate 22.96 149.0 1.520 44.13 9.13 13,495 1,065 9.15 2,437 13,495 1065 9.13 % Na.sub.2O SAX 19.35 363.40 Alumium sulfate 7.98 3.8 1.375 363.49 75.21 111,165 10,063 75.20 111,165 10063 75.20 0.00 Pressure PAC (UP 290) 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 2.50 H3PO4 (75%) solution 0 1.570 2.50 0.52 765 58 0.52 765 58 0.52 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 500.0 Final product 8.10 8.10 1.200 500.0 103.47 152,920 15,285 102.94 152,925 13,749 1.03.45 Check 483.3 100.01% 152,925 0 147,823 13,698 100.00% % SA soln 25.0% 1.249 402.8 96.66% 147,818 ?5,107 147,823 ?5,102 ?50 96.66% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.10% 50.0 16.96 0.00 0.00 16.96 2.38 19.34 Actual 16.7 3.46% Just CO.sub.2 7.83% 16.40 0.00 16.40 2.38 18.78 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 5,102 3.45% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below S. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.10 8.05 ?0.05 % Fe.sub.2O.sub.3 0.00 % Basicity 50.0 49.0 ?1.0 145.3 % Sulfates 16.96 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.6 70.9 3.37 0.6 8 Agitator at 250 rpm. Started both feeds at 2:50 pm. 2.2 1.8 1.2 1 22.3 72.1 5.97 0.6 8 2.2 1.8 1.2 2 23.0 73.4 6.69 0.6 8 2.2 1.8 1.2 3 23.7 74.7 6.73 0.6 8 2.2 1.8 1.2 4 24.4 75.9 6.93 0.6 8 2.2 1.8 1.2 5 24.8 76.6 6.92 0.6 8 2.2 1.8 1.2 6 25.2 77.4 6.86 0.6 8 2.2 1.8 1.2 7 25.6 78.1 6.67 0.6 8 2.2 1.8 1.2 8 25.9 78.6 6.61 0.6 8 2.2 1.8 1.2 9 26.2 79.2 6.80 0.6 8 2.2 1.8 1.2 10 26.4 79.5 6.80 0.6 8 2.2 1.8 1.2 15 27.4 81.3 6.70 0.6 8 2.2 1.8 1.2 20 28.2 82.8 6.94 0.6 8 2.2 1.8 1.2 22 28.4 83.1 7.01 0.6 7 2.2 1.6 1.4 25 28.6 83.5 6.81 0.6 7 2.2 1.6 1.4 30 28.9 84.0 6.68 0.6 8 2.2 1.8 1.2 35 23.1 73.6 6.93 0.6 8 2.2 1.8 1.2 1.3 39 29.2 84.6 7.01 0.6 0 Water/soda ash/sodium aluminate mixture feed complete. 2.2 0.0 0.0 40 29.0 84.3 5.59 0.6 0 2.2 0.0 0.0 49 26.2 79.2 5.00 4.8 0 17.1 0.0 0.0 59 26.3 79.3 3.90 0.6 0 Aluminum sulfate feed complete. 2.2 0.0 0.0 60 23.5 74.3 3.90 0.6 0 Started Phosphoric acid (75%) solution feed. 2.2 0.0 0.0 66 24.1 75.4 3.90 0.6 0 Phosphoric acid (75%) solution feed complete. 2.2 0.0 0.0 72 24.0 75.2 3.91 0.0 0 Let mix overnight. 0.0 0.0 0.0 Oct. 1, 2021 - 9:00 am (18.2 hrs) Solution clear. Filtered through # 541 Whatman paper. Average 26.4 79.5 5.83

TABLE-US-00028 TABLE 28 UltraPAC 2361 (50% Basic PAS) Headspace 1.0% Phosphoric acid (75%) solution Conversion Gallons Target Initial Actual Working Examples MV-128 MV-128 305.4409 14774.7 11.4 3.9 16.0 16.9 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 40.00 Start Up Water 0 1.000 40.00 8.27 12,220 1,466 8.27 2,100 12,220 1466 8.27 0.00 Ferric sulfate 17.75 10.9 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 37.41 Solution Water 0 1.000 37.43 7.73 11,435 1,372 7.74 2,743 11,435 1464 7.74 12.50 Sodium carbonate 0 NA 12.51 2.59 3,820 NA 2.58 3,820 NA 2.58 46.30 43% Sodium aluminate 22.96 149.0 1.520 46.46 9.60 14,190 1,120 9.60 2,491 14,190 1120 9.60 % Na.sub.2O SAX 19.35 358.80 Alumium sulfate 7.98 3.8 1.325 359.38 74.26 109,770 9,937 74.26 109,770 9937 74.26 0.00 Pressure PAC (UP 290) 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 5.00 H3PO4 (75%) solution 0 1.570 5.28 1.09 1,615 123 1.09 1,615 123 1.09 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 500.0 Final product 8.13 8.13 1.200 501.3 103.54 153,045 15,298 102.45 153,050 13,749 103.54 Check 483.9 100.00% 153,050 0 147,823 13,674 100.00% % SA soln 25.1% 1.249 403.3 96.58% 147,818 ?5,232 147,823 ?5,227 ?75 96.58% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.13% 49.9 16.75 0.00 0.00 16.75 2.45 19.20 Actual 17.1 3.54% Just CO.sub.2 7.85% 16.18 0.00 16.18 2.45 18.62 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 5,227 3.54% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alumni holding vessel. 6. Start addition of the aluminum solution and the sodium carbonate/sodium aluminate mixture to the reactor. 7. Adjust feed rates to add the solutions over desired time period maintaining the ph between 5.5 and 7. 8. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 9. When the pH falls below 5 increase the aluminum sulfate feed rate. 10. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 11. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.13 8.09 ?0.04 % Fe.sub.2O.sub.3 0.00 % Basicity 49.9 48.8 ?1.1 145.1 % Sulfates 1.6.75 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 22.1 71.8 5.14 0.6 8 Agitator at 250 rpm. Started both feeds at 2:15 pm. No initial alum. 2.2 1.8 1.2 1 22.9 73.2 5.49 0.6 8 2.2 1.8 1.2 2 23.7 74.7 6.36 0.6 8 2.2 1.8 1.2 3 24.4 75.9 6.09 0.6 8 2.2 1.8 1.2 4 24.9 76.8 6.67 0.6 8 2.2 1.8 1.2 5 25.3 77.5 6.31 0.6 8 2.2 1.8 1.2 6 25.7 78.3 6.51 0.6 8 2.2 1.8 1.2 7 26.0 78.8 6.91 0.6 8 2.2 1.8 1.2 8 26.3 79.3 7.13 0.6 7 2.2 1.6 1.4 9 26.5 79.7 6.93 0.6 7 2.2 1.6 1.4 10 26.7 80.1 6.85 0.6 7 2.2 1.6 1.4 11 26.9 80.4 6.56 0.6 7 2.2 1.6 1.4 12 27.1 80.8 6.41 0.6 8 2.2 1.8 1.2 13 27.3 81.1 6.57 0.6 8 2.2 1.8 1.2 14 27.5 81.5 6.53 0.6 8 2.2 1.8 1.2 15 27.7 81.9 6.54 0.6 8 2.2 1.8 1.2 20 28.5 83.3 7.00 0.6 7 2.2 1.6 1.4 25 28.9 84.0 6.75 0.6 7 2.2 1.6 1.4 30 29.1 84.4 6.59 0.6 8 2.2 1.8 1.2 35 29.5 85.1 6.79 0.6 8 2.2 1.8 1.2 40 29.7 85.5 6.94 0.6 8 2.2 1.8 1.2 1.3 41 29.7 85.5 6.99 0.6 0 Water/soda ash/sodium aluminate mixture feed complete. 2.2 0.0 0.0 51 26.6 79.9 4.98 4.8 0 17.1 0.0 0.0 63 24.0 75.2 3.98 0.0 0 Aluminum sulfate feed complete. 0.0 0.0 0.0 65 24.0 75.2 3.99 0.6 0 Started Phosphoric acid (75%) solution feed. 2.2 0.0 0.0 68 25.3 77.5 3.97 0.0 0 Phosphoric acid (75%) solution feed complete. 0.0 0.0 0.0 95 24.5 76.1 4.08 0.0 0 Let mix overnight. 0.0 0.0 0.0 Oct. 5, 2021 - 8:30 am (18.25 hrs) Solution clear. Filtered through # 541 Whatman paper. Average 26.9 80.5 6.72

TABLE-US-00029 TABLE 29 UltraPAC 2361 (50% Basic PAS) Headspace 1.5% Phosphoric acid (75%) solution Conversion Gallons Target Initial Actual Working Examples MV-131 MV-131 305.4220 14774.7 11.4 4.4 16.0 17.1 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 40.00 Start Up Water 0 1.000 40.00 8.27 12,215 1,465 8.26 2,100 12,215 1465 8.26 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 37.41 Solution Water 0 1.000 37.42 7.73 11,430 1,371 7.73 2,742 11,430 1464 7.73 12.50 Sodium carbonate 0 NA 12.50 2.58 3,820 NA 2.58 3,820 NA 2.58 50.10 43% Sodium aluminate 22.96 149.0 1.520 50.99 10.54 15,575 1,229 10.54 2,600 15,575 1229 10.54 % Na.sub.2O SAX 19.35 352.50 Alumium sulfate 8.07 2.7 1.325 351.56 72.64 107,375 9,720 72.64 107,375 9720 72.64 0.00 Pressure PAC (UP 290) 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 7.50 H3PO4 (7%) solution 0 1.570 7.60 1.57 2,320 177 1.57 2,320 177 1.57 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 500.0 Final product 8.28 8.28 1.200 500.07 103.33 152,730 15,266 101.76 152,755 13,749 103.33 Check 483.96 100.00% 152,735 0 147,820 13,657 100.00% % SA soln 25.0% 1.249 403.30 96.78% 147,815 ?4,920 147,820 ?4,915 ?92 96.78% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.28% 50.5 16.57 0.00 0.00 16.57 2.58 19.15 Actual 16.11 3.33% Just CO.sub.2 8.01% 16.04 0.00 16.04 2.58 18.61 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 4,915 3.33% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution and the sodium carbonate/sodium aluminate mixture to the reactor. 7. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 8. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 9. When the pH falls below 5 increase the aluminum sulfate feed rate. 10. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 11. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.28 8.20 ?0.08 % Fe.sub.2O.sub.3 0.00 % Basicity 50.5 50.3 ?0.2 148.3 % Sulfates 16.57 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.5 70.7 5.72 0.6 8 Agitator at 2.50 rom. Started both feeds at 2:55 pm. No initial alum. 7.2 1.8 1.2 1 22.3 72.1 6.16 0.6 8 2.2 1.8 1.2 2 23.1 73.6 6.91 0.6 7 2.2 1.6 1.4 3 23.6 74.5 5.65 0.6 8 2.2 1.8 1.2 4 24.2 75.6 5.88 0.6 8 2.2 1.8 1.2 5 24.6 76.3 6.13 0.6 8 2.2 1.8 1.2 6 25.1 77.2 6.27 0.6 8 2.2 1.8 1.2 7 25.9 77.9 6.45 0.6 8 2.2 1.8 1.2 8 25.8 78.4 6.79 0.6 8 2.2 1.8 1.2 9 26.1 79.0 7.05 0.7 8 2.6 1.8 1.4 10 26.5 79.7 7.00 0.7 8 2.6 1.8 1.4 11 26.7 80.1 6.79 0.7 8 2.6 1.8 1.4 12 26.9 80.4 6.62 0.7 8 2.6 1.8 1.4 13 27.2 81.0 6.61 0.7 8 2.6 1.8 1.4 14 27.4 81.3 6.43 0.7 8 2.6 1.8 1.4 15 27.6 81.7 6.50 0.7 8 2.6 1.8 1.4 20 28.4 83.1 6.26 0.6 8 2.2 1.8 1.2 25 29.0 84.2 6.71 0.6 8 2.2 1.8 1.2 30 29.2 84.6 6.92 0.7 8 2.6 1.8 1.4 35 29.6 84.9 6.56 0.7 8 2.6 1.8 1.4 41 29.7 85.5 6.56 0.7 0 Water/soda ash/sodium aluminate mixture feed complete. 2.6 0.2 12.1 2.0 53 26.0 78.8 4.71 4.8 0 17.1 0.0 0.0 66 24.0 75.2 4.03 0.6 0 Aluminum sulfate feed complete. Started Phosphoric acid (75%) solution feed. 2.2 0.0 0.0 71 26.1 79.0 3.97 0.0 0 Phosphoric acid (75%) solution feed complete 0.0 0.0 0.0 80 25.8 78.4 4.03 0 0 Let mix overnight. 0.1 0.0 0.0 Oct. 7, 2021 - 9:00 am (18.1 hrs) Solution clear. Filtered through # 541 Whatman paper. 0.0 0.0 0.0 Average 26.5 80.3 5.60

TABLE-US-00030 TABLE 30 60% Basic PAS Headspace 0.50% Phosphoric acid (75%) solution Conversion Gallons Target Initial Actual Working Examples MV-142 MV-142 307.8647 14774.7 11. 2.5 16.0 17.8 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 40.00 Start Up Water 0 1.000 40.00 8.33 12,315 1,477 8.33 2,100 12,315 1477 8.33 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 37.41 Solution Water 0 1.000 37.42 7.79 11,520 1,382 7.79 2,764 11,520 1476 7.79 12.50 Sodium carbonate 0 NA 12.50 2.60 3,850 NA 2.60 3,850 NA 2.60 61.80 43% Sodium aluminate 22.96 149.0 1.520 61.87 12.89 19,050 1,503 12.89 2,885 19,050 1503 12.89 % Na.sub.2O SAX 19.35 345.80 Alumium sulfate 8.07 2.7 1.325 345.87 72.04 106,480 9,639 72.04 106,480 9639 72.04 0.00 Pressure PAC (UP 290) 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 2.50 H3PO4 (75%) solution 0 1.570 2.65 0.55 815 62 0.55 815 62 0.55 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 500.0 Final product 8.77 8.77 1.200 500.3 104.20 154,030 15,396 103.65 154,030 13,749 104.21 Check 480.1 99.99% 154,030 0 147,814 13,604 100.00% % SA soln 25.0% 1.249 400.1 95.96% 147,814 ?6,216 147,814 ?6,216 ?145 95.96% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.77% 59.9 16.45 0.00 0.00 16.43 2.92 19.35 Actual 20.2 4.21% Just CO.sub.2 8.42% 15.77 0.00 15.77 2.9 18.69 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 6,216 4.21% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution and the sodium carbonate/sodium aluminate mixture to the reactor. 7. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 8. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 9. When the pH falls below 5 increase the aluminum sulfate feed rate. 10. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 11. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.77 8.78 0.01 % Fe.sub.2O.sub.3 0.00 % Basicity 59.9 59.3 ?0.6 147.1 % Sulfates 16.43 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 20.3 68.5 6.64 0.6 6 Agitator at 200 rpm. Started both feeds at 11:59 pm. No initial alum. 2.2 1.4 1.6 1 20.9 69.6 3.84 0.6 6 2.2 1.4 1.6 2 21.5 70.7 4.01 0.6 7 2.2 1.6 1.4 3 22.2 72.0 4.11 0.6 8 2.2 1.8 1.2 4 22.7 72.9 4.46 0.6 8 2.2 1.8 1.2 5 23.0 73.4 4.82 0.6 8 2.2 1.8 1.2 6 23.8 74.8 5.24 0.6 8 2.2 1.8 1.2 7 24.4 75.9 5.34 0.6 8 2.2 1.8 1.2 8 25.0 77.0 5.50 0.6 8 2.2 1.8 1.2 9 25.7 78.3 6.10 0.6 8 2.2 1.8 1.2 10 26.1 79.0 6.14 0.6 8 2.2 1.8 1.2 11 26.5 79.7 6.41 0.6 8 2.2 1.8 1.2 12 26.8 80.2 6.57 0.6 7 2.2 1.6 1.4 13 27.3 80.8 6.53 0.6 7 2.2 1.6 1.4 14 27.3 81.1 6.53 0.6 7 2.2 1.6 1.4 15 27.5 81.5 6.56 0.6 7 2.2 1.6 1.4 20 28.2 82.8 6.77 0.6 6 2.2 1.4 1.6 25 28.4 83.1 6.32 0.6 7 2.2 1.6 1.4 30 28.9 84.0 6.41 0.6 7 2.2 1.6 1.4 35 29.2 84.6 6.35 0.6 8 2.2 1.8 1.2 37 29.4 84.9 6.64 0.6 7 2.2 1.6 1.4 40 29.6 85.3 6.62 0.6 7 2.2 1.6 1.4 45 29.8 85.6 6.43 0.6 7 2.2 1.6 1.4 50 29.9 85.8 6.64 0.6 7 2.2 1.6 1.4 1.3 51 29.9 85.8 6.64 0.6 0 Water/soda ash/sodium aluminate mixture feed complete. 2.2 0.0 0.0 62 27.2 81.0 4.96 4.8 0 17.1 0.0 0.0 70 24.5 76.1 4.07 0.6 0 Aluminum sulfate feed complete. 2.2 0.0 0.0 71 24.4 75.9 4.09 0.6 0 Started Phosphoric acid (75%) solution feed 2.2 0.0 0.0 74 25.0 77.0 4.10 0 0 Phosphoric acid (75%) solution feed complete. 0.0 0.0 0.0 82 24.9 76.8 4.12 0 0 Let mix overnight. 0.0 0.0 0.0 Oct. 20, 2021 - 8:30 am (20.5 hrs) Solution still cloudy. Let mix overnight. Oct. 21, 2021 - 9:30 am (45.5 hrs) Solution dear. Filtered through # 541 Whatman paper. Average 26.9 80.4 6.23

TABLE-US-00031 TABLE 31 60% Basic PAS Headspace 0.50% Phosphoric acid (75%) solution Conversion Gallons Target Initial Actual Working Examples MV-145 MV-145 295.6772 14774.7 11.4 11.4 16.0 14.9 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 40.00 Start Up Water 0 1.000 40.00 8.00 11,825 1,418 8.00 2,100 11,825 1418 8.00 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 45.00 Solution Water 0 1.000 45.00 9.00 13,305 1,596 9.00 3,192 13,305 1704 9.00 15.00 Sodium carbonate 0 NA 15.00 3.00 4,435 NA 3.00 4,435 NA 3.00 56.80 43% Sodium aluminate 22.96 149.0 1.520 56.80 11.36 16,795 1,325 11.36 2,921 16,795 1325 11.36 % Na.sub.2O SAX 19.35 340.61 Alumium sulfate 8.07 2.7 1.325 340.61 68.13 100,710 9,117 68.13 100,710 9117 68.13 0.00 Pressure PAC (UP 290) 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 2.50 H3PO4 (75%) solution 0 1.570 2.50 0.50 740 57 0.50 740 57 0.50 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 499.9 Final product 8.11 8.11 1.200 499.9 99.99 147,810 14,774 99.50 147,810 13,749 100.00 Check 499.9 99.99% 147,810 0 147,810 13,842 100.00% % SA soln 25.0% 1.249 416.6 100.00% 147,810 0 147,810 0 93 100.00% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.11% 60.0 15.54 0.00 0.00 15.54 2.87 18.41 Actual 0.0 0.00% Just CO.sub.2 8.11% 15.54 0.00 15.54 2.87 18.41 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 0 0.00% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alumni holding vessel. 6. Start addition of the aluminum solution and the sodium carbonate/sodium aluminate mixture to the reactor. 7. Adjust feed rates to add the solutions over desired time period maintaining the phi between 5.5 and 7. 8. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 9. When the pH falls below 5 increase the aluminum sulfate feed rate. 10. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 11. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.11 8.58 0.47 % Fe.sub.2O.sub.3 0.00 % Basicity 60.0 60.0 0.0 148.9 % Sulfates 15.54 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.8 71.2 6.31 0.6 6 Agitator at 200 rpm. Started both feeds at 2:30 pm. No initial alum. 2.2 1.4 1.6 1 22.5 72.5 4.84 0.6 6 2.2 1.4 1.6 2 23.1 73.6 4.95 0.6 7 2.2 1.6 1.4 3 23.6 74.5 5.16 0.6 8 2.2 1.8 1.2 4 24.7 76.5 6.70 0.6 7 2.2 1.6 1.4 5 25.1 77.2 5.86 0.6 7 2.2 1.6 1.4 6 25.6 78.1 5.99 0.6 8 2.2 1.8 1.2 7 26.1 79.0 6.16 0.6 8 2.2 1.8 1.2 8 26.6 79.9 6.30 0.6 8 2.2 1.8 1.2 9 27.0 80.6 6.44 0.6 8 2.2 1.8 1.2 10 27.4 81.3 6.56 0.6 8 2.2 1.8 1.2 11 27.7 81.9 6.67 0.6 7 2.2 1.6 1.4 12 27.9 82.2 6.63 0.6 7 2.2 1.6 1.4 13 28.0 82.4 6.59 0.6 7 2.2 1.6 1.4 14 28.2 82.8 6.54 0.6 7 2.2 1.6 1.4 15 28.3 82.9 6.47 0.6 7 2.2 1.6 1.4 20 29.0 84.2 6.53 0.6 7 2.2 1.6 1.4 25 29.4 84.5 6.35 0.5 8 2.2 1.8 1.2 30 29.9 85.8 6.60 0.6 8 2.2 1.8 1.2 40 30.6 87.1 6.91 0.6 7 2.2 1.6 1.4 45 30.6 87.1 6.72 0.6 7 2.2 1.6 1.4 52 30.7 87.3 6.56 0.6 7 Water/soda ash/sodium aluminate mixture feed complete. 2.2 1.6 1.4 1.3 64 27.3 81.3 4.97 4.8 0 17.1 0.0 0.0 71 25.2 77.6 4.22 0.6 0 2.2 0.0 0.0 77 25.0 77.0 4.25 0.6 0 Aluminum sulfate feed complete. Started Phosphoric acid (75%) solution feed. 2.2 0.0 0.0 80 25.5 77.9 4.26 0.0 0 Phosphoric acid (75%) solution feed complete. 0.0 0.0 0.0 90 25.5 77.9 4.29 0.0 0 Let mix overnight. 0.0 0.0 0.0 Oct. 21, 2021 9:30 am (19 hrs) Solution still cloudy clear. Set heat to 30? C. 3:00 pm (24.5 hrs) Solution clear. Filtered solution through #41 Whatman paper. Average 27.6 81.6 6.46

TABLE-US-00032 TABLE 32 UltraPAC 2361 (50% Basic PAS) Headspace 1.0% Phosphoric acid (75%) solution Conversion Gallons Target Initial Actual Working Examples MV-155 MV-155 306.8804 14774.7 11.4 3.5 16.0 17.0 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 40.00 Start Up Water 0 1.000 40.00 8.30 12,275 1,472 8.30 2,100 12,275 1472 8.30 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 37.41 Solution Water 0 1.000 37.37 7.76 11,470 1,376 7.76 2,752 11,470 1469 7.76 12.50 Sodium carbonate 0 NA 12.49 2.59 3,835 NA 2.59 3,835 NA 2.59 48.00 43% Sodium aluminate 22.96 149.0 1.520 47.87 9.94 14,690 1,359 9.94 2,535 14,690 1,159 9.94 % Na.sub.2O SAX 19.35 357.10 Alumium sulfate 8.07 2.7 1.325 356.92 74.10 109,530 9,915 74.10 109,530 9915 74.10 0.00 Pressure PAC (UP 290) 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 5.00 H3PO4 (75%) solution 0 1.570 5.03 1.04 1,545 118 1.05 1,545 118 1.05 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 500.0 Final product 8.28 8.26 1.200 499.68 103.73 153,340 15,327 102.70 153,345 13,749 103.74 Check 481.66 99.99% 153,345 0 147,820 13,663 100.00% % SA soln 25.1% 1.249 401.4 96.39% 147,815 ?5,530 147,820 ?5,525 ?86 96.40% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.26% 49.9 16.90 0.00 0.00 16.90 2.50 19.40 Actual 18.0 3.74% Just CO.sub.2 7.96% 16.29 0.00 16.29 2.50 18.79 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 5,525 3.74% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower PH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.26 8.22 ?0.04 % Fe.sub.2O.sub.3 0.00 % Basicity 49.9 48.9 ?1.0 145.4 % Sulfates 16.90 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.9 71.4 3.62 0.6 6 Agitator at 200 rpm. Started both feeds at 3:10 pm. 2.2 1.4 1.6 1 22.6 72.7 4.62 0.6 5 2.2 1.4 1.6 2 22.9 73.2 4.66 0.6 8 2.2 1.8 1.2 3 23.2 73.8 5.10 0.6 8 2.2 2.8 1.2 4 23.8 74.8 5.61 0.6 8 Agitator increased to 250 rpm. 2.2 1.8 1.2 5 24.1 75.4 5.58 1.2 16 4.3 3.4 1.3 6 25.2 77.4 5.42 1.2 17 4.3 3.6 1.2 7 25.7 78.3 5.34 1.2 18 4.3 3.8 1.1 8 26.8 80.2 5.53 1.2 19 4.3 4.0 1.1 9 27.7 81.9 5.53 1.2 20 4.3 4.2 1.0 10 28.4 83.1 5.59 1.2 21 4.3 4.4 1.0 11 29.2 84.0 5.82 1.2 22 4.3 4.6 1.0 12 30.0 86.0 5.83 1.2 23 4.3 4.8 0.9 13 30.5 86.9 5.95 1.2 24 4.3 5.0 0.9 14 31.0 87.8 6.01 1.2 24 4.3 5.0 0.9 15 31.5 88.7 6.06 1.2 24 4.3 5.0 0.9 17 32.3 90.1 6.76 1.2 24 4.3 5.0 0.9 1.0 19 33.1 91.6 6.68 1.2 0 Water/soda ash/sodium aluminate mixture feed complete. 4.3 0.0 0.0 21 31.4 88.5 5.35 1.2 0 4.3 0.0 0.0 23 29.8 85.6 4.87 4.8 0 17.1 0.0 0.0 30 26.4 79.5 4.01 4.8 0 17.1 0.0 0.0 33 26.1 79.0 3.95 0.6 0 Aluminum sulfate feed complete. 2.2 0.0 0.0 35 26.1 79.0 3.96 0.6 0 Started Phosphoric acid (75%) solution feed. 2.2 0.0 0.0 37 27.5 81.5 3.95 0 0 Phosphoric acid (75%) solution feed complete. 0.0 0.0 0.0 40 27.4 81.3 3.95 0 0 Let mix overnight. 0.0 0.0 0.0 Dec. 15, 2021 8:30 am (17.33 hrs) Solution clear. Filtered solution through #4 Whatman paper. Average 28.5 83.3 5.85

TABLE-US-00033 TABLE 33 UitraPAC 2361 (50% Basic PAS) Headspace 0.6% sodium gluconate Conversion Gallons Target Initial Actual Working Examples MV-158 MV-158 306.2065 14774.7 11.4 3.6 16.0 16.3 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 40.00 Start Up Water 0 1.000 40.00 8.29 12,250 1,469 8.29 2,100 12,250 1469 8.29 3.00 Sodium gluconate 1.581 3.11 0.64 950 114 0.64 601 950 114 0.64 37.41 Solution Water 0 1.000 37.40 7.75 11,450 1,373 7.75 2,747 11,450 1467 7.75 12.50 Sodium carbonate 0 NA 12.52 2.59 3,835 NA 2.59 3,835 NA 2.59 43.50 43% Sodium aluminate 22.96 149.0 1.520 43.70 9.05 13,380 1,056 9.05 2,429 13,380 1056 9.05 % Na.sub.2O SAX 19.35 363.60 Alumium sulfate 8.07 2.7 1.325 363.73 75.35 111,375 10,082 75.35 111,375 10082 75.35 0.00 Pressure PAC (UP 290) 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 0.00 H3PO4 (75%) solution 0 1.570 0.00 0.00 0 0 0.00 0 0 0.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 500.0 Final product 8.16 8.16 1.200 500.5 103.67 153,245 15,318 103.68 153,240 13,749 103.68 Check 482.7 99.99% 153,240 0 147,803 13,727 100.00% % SA soln 25.1% 1.250 402.3 96.46% 147,808 ?5,432 147,803 ?5,437 ?21 96.45% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 0.0 0.00% Evap. & CO.sub.2 8.16% 50.2 17.19 0.00 0.00 17.19 2.37 19.56 Actual 17.7 3.68% Just CO.sub.2 7.87% 16.58 0.00 16.58 2.37 18.95 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 5,437 3.68% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added , add the sodium gluconate. 12. When the sodium gluconate has been added let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.16 8.18 0.02 % Fe.sub.2O.sub.3 0.00 % Basicity 50.2 49.3 ?1.1 144.8 % Sulfates 17.19 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 22.5 72.5 3.55 0.6 6 Agitator at 250 rpm. Started both feeds at 12:40 pm. 2.2 1.4 1.6 1 23.6 74.5 4.70 0.6 6 2.2 1.4 1.6 2 24.0 75.2 4.82 0.6 8 2.2 1.8 1.2 3 24.4 75.9 5.44 0.6 8 2.2 1.8 1.2 4 25.2 77.4 5.74 0.6 8 2.2 1.8 1.2 5 26.0 78.8 5.92 0.6 9 2.2 2.0 1.1 6 26.7 80.1 6.20 0.6 9 2.2 2.0 1.1 7 27.2 81.0 6.71 0.6 8 2.2 1.8 1.2 8 27.7 81.9 6.67 0.6 8 2.2 1.8 1.2 9 28.0 82.4 6.71 0.6 8 2.2 1.8 1.2 10 28.3 82.9 6.72 0.6 8 2.2 1.8 1.2 15 29.4 84.9 6.73 0.6 8 2.2 1.8 1.2 20 30.0 86.0 6.72 0.6 8 2.2 1.8 1.2 25 30.4 86.7 6.79 0.6 8 2.2 1.8 1.2 30 30.8 87.4 6.81 0.6 8 2.2 1.8 1.2 35 31.0 87.8 6.84 0.6 8 2.2 1.8 1.2 1.2 40 31.1 88.0 6.84 0.6 0 Water/soda ash/sodium aluminate mixture feed complete. 2.2 0.0 0.0 45 29.4 84.9 5.48 0.6 0 2.2 0.0 0.0 50 27.9 82.2 4.98 4.2 0 15.0 0.0 0.0 60 25.7 78.3 4.06 4.2 0 15.0 0.0 0.0 62 25.6 78.1 4.03 0.0 0 Aluminum sulfate feed complete. Added sodium gluconate. 0.0 0.0 0.0 70 25.3 77.5 4.06 0.0 0 Let mix overnight. 0.0 0.0 0.0 Dec. 16, 2021 8:30 am (19.2 hrs) Solution clear. Filtered solution through #4 Whatman paper. Average 28.3 82.9 6.64

TABLE-US-00034 TABLE 34 UitraPAC 2361 (50% Basic PAS) Headspace 1.0% Phosphoric acid (75%) solution Conversion Gallons Target Initial Actual Working Examples MV-161 MV-161 65.6957 14774.7 11.4 3.9 16.0 16.9 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 185.96 Start Up Water 0 1.000 185.96 8.27 12,215 1,465 8.26 2,100 12,215 1465 8.26 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 174.02 Solution Water 0 1.000 174.02 7.73 11,430 1,371 7.73 2.742 11,430 1460 7.73 56.25 Sodium carbonate 0 NA 56.25 2.50 3,695 NA 2.50 3,695 NA 2.50 218.10 43% Sodiun; aluminate 22.96 149.0 1.520 218.10 9.69 14,330 1,131 9.69 2,502 14,330 1131 9.69 % Na.sub.2O SAX 19.35 1672.77 Alumium sulfate 7.98 3.8 1.325 1672.77 74.35 109,895 9,948 74.35 109,895 9948 74.35 0.00 Pressure PAC (UP 290) 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 22.50 H3PO4 (75%) solution 0 1.570 22.50 1.00 1,480 113 1.00 1,480 113 1.00 First: Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 2250.0 Final product 8.18 8.16 1.200 2329.6 103.54 153,045 15,298 102.54 153,045 13,749 103.54 Check 2250.0 100.00% 153,045 0 147,812 13,674 100.00% % SA soln 24.4% 1.243 1,875.0 96.38% 147,812 ?5,233 147,812 ?5,233 ?75 96.58% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 79.65 3.54% Evap. & CO.sub.2 8.16% 50.0 16.77 0.00 0.00 16.77 2.42 19.19 Actual 79.65 3.54% Just CO.sub.2 7.88% 16.20 0.00 16.20 2.42 18.62 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 5,233 3.54% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculateci Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.16 8.10 ?0.06 % Fe.sub.2O.sub.3 0.00 0.0 148.8 % Basicity 50.0 50.0 % Sulfates 16.77 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 18.2 64.8 3.81 0.6 6 Agitator at 200 rpm. Starter both feeds at 12:45 pm. 2.2 1.4 1.6 1 18.4 65.1 4.50 0.6 6 2.2 1.4 1.6 2 18.5 65.3 4.70 0.6 8 2.2 1.8 1.2 3 18.7 65.1 5.29 0.6 8 2.2 1.8 1.2 4 19.0 66.2 5.69 0.6 8 2.2 1.8 1.2 5 19.2 66.6 5.91 0.6 9 2.2 2.0 1.1 6 19.4 66.9 6.14 0.6 9 2.2 2.0 1.1 7 19.7 67.5 6.29 0.6 8 2.2 1.8 1.2 8 19.9 67.8 6.39 0.6 8 2.2 1.8 1.2 9 20.1 68.2 6.48 0.6 8 2.2 1.8 1.2 10 20.3 68.5 6.54 1.2 16 4.3 3.4 1.3 11 20.8 69.1 6.48 1.2 15 4.3 3.4 1.3 12 21.0 69.8 6.46 2.4 32 8.6 6.5 1.3 13 21.5 70.7 6.23 2.4 32 8.6 6.5 1.3 14 22.2 72.0 6.27 2.4 32 Increased agitator to 250 rpm. 8.6 6.5 1.3 15 22.7 72.9 6.23 2.4 34 8.6 6.9 1.2 16 23.2 73.8 6.35 2.4 34 8.6 6.9 1.2 17 23.5 74.3 6.45 2.4 34 8.6 6.9 1.2 18 24.1 75.4 6.60 2.4 34 8.6 6.9 1.2 19 24.4 75.9 6.66 2.5 34 8.9 6.9 1.3 20 24.8 76.6 6.64 2.5 34 8.9 6.9 1.3 21 25.2 77.4 6.63 2.5 34 8.9 6.9 1.3 25 26.2 79.2 6.60 2.6 34 9.3 6.9 1.3 30 27.3 81.1 6.45 2.5 34 8.9 6.9 1.3 40 28.6 83.5 6.54 2.5 34 8.9 6.9 1.3 50 29.3 84.7 6.57 2.5 34 8.9 6.9 1.3 1.3 60 29.0 84.2 5.85 2.5 0 Water/soda ash/sodium aluminate mixture feed complete. 8.9 0.0 0.0 70 26.2 79.2 4.85 5.0 0 17.8 0.0 0.0 115 22.7 72.9 4.13 0.6 0 Aluminum sulfate feed complete. Started phosphoric acid (75%) solution feed. 2.2 0.0 0.0 120 23.5 74.3 4.19 0.0 0 Phosphoric acid (75%) solution feed complete 0.0 0.0 0.0 170 23.5 74.3 4.19 0.0 0 Let mix overnight. 0.0 0.0 0.0 Jan. 28, 2022 8:30 am (19.75 hrs) Solution clear. filtered solution through #41 Whatman paper. Average 23.4 74.3 6.43

TABLE-US-00035 TABLE 35 UltraPAC 2361 (50% Basic PAS) Headspace 1.0% Phosphoric acid (75%) solution Conversion Gallons Target Initial Actual Working Examples MV-169 MV-169 65.3448 14774.7 11.4 5.2 16.0 16.9 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 185.96 Start Up Water 0 1.000 185.96 8.22 12,150 1,457 8.22 2.100 12,150 1457 8.22 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 174.02 Solution Water 0 1.000 173.92 7.69 11,365 1,363 7.69 2,726 11,365 1452 7.69 56.25 Sodium carbonate 0 NA 56.28 2.49 3,680 NA 2.49 3,680 NA 2.49 172.00 43% Sodium aluminate 23.87 149.0 1.520 171.93 7.60 11,235 887 7.60 2,250 11,235 887 7.60 % Na.sub.2O SAX 19.35 1718.90 Alumium sulfate 8.36 6.7 1.325 1717.36 75.92 112,220 10,159 75.92 112,220 10159 75.92 0.00 Pressure PAC (UP 290) 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 22.50 H3PO4 (75%) solution 0 1.570 22.67 1.00 1,480 113 1.00 1,480 113 1.00 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 2250.0 Final product 8.16 8.16 1.200 2328.1 102.92 152,130 15,206 101.92 152,130 13,749 102.92 Check 2262.0 100.00% 152,130 0 147,811 13,733 100.00% % SA soln 24.4% 1.243 1,885.0 97.16% 147,811 ?4,319 147,811 ?4,319 ?15 97.16% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 79.65 3.54% Evap. & CO.sub.2 8.16% 44.9 17.94 0.00 0.00 17.94 2.18 20.11 Actual 66.09 2.92% Just CO.sub.2 7.93% 17.43 0.00 17.43 2.18 19.60 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 4,319 2.92% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH falls below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.16 8.19 0.03 % Fe.sub.2O.sub.3 0.00 % Basicity 44.9 44.4 ?0.5 146.7 % Sulfates 17.94 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.4 70.5 3.86 0.6 6 Agitator at 200 rpm. Started both feeds at 2:40 pm. 2.2 1.4 1.6 1 21.5 70.7 4.41 0.6 6 2.2 1.4 1.6 2 21.6 70.9 4.58 0.6 8 2.2 1.8 1.2 3 21.7 71.1 5.08 0.6 8 2.2 1.8 1.2 4 21.5 71.4 5.31 0.6 8 2.2 1.8 1.2 5 22.1 71.8 5.57 0.6 9 2.2 2.0 1.1 6 22.3 72.1 5.71 0.6 9 2.2 2.0 1.1 7 22.5 72.5 5.81 0.6 8 2.2 1.8 1.2 8 22.7 72.9 5.92 0.6 8 2.2 1.8 1.2 9 22.9 73.2 6.01 0.6 8 2.2 1.8 1.2 10 23.1 73.6 6.06 1.2 16 4.3 3.4 1.3 12 23.7 74.7 6.12 2.4 32 8.6 6.5 1.3 14 24.9 75.8 6.10 2.4 34 8.6 6.9 1.2 16 26.2 79.2 6.22 2.4 34 8.6 6.9 1.2 18 27.1 80.8 6.31 2.4 34 8.6 6.9 1.2 20 28.0 82.4 6.35 2.4 34 8.6 6.9 1.2 25 29.4 84.9 6.39 2.4 34 8.6 6.9 1.2 30 30.3 86.5 6.40 2.4 34 8.6 6.9 1.2 40 31.4 88.5 6.40 2.4 34 8.6 6.9 1.2 1.2 51 31.9 89.4 6.55 2.5 0 Water/soda ash/sodium aluminate mixture feed complete. 8.9 0.0 0.0 60 29.4 84.9 4.93 4.8 0 17.1 0.0 0.0 115 24.8 76.6 5.51 0.6 0 Aluminum sulfate feed complete. Started phosphoric acid (75%) solution feed. 2.2 0.0 0.0 122 26.3 79.3 3.47 0.00 0 Phosphoric acid (75%) solution feed complete. 0.0 0.0 0.0 135 26.1 79.0 3.49 0.0 0 Let mix overnight. 0.0 0.0 0.0 Apr. 19, 2022 9:00 am (18.33 hrs) Solution clear. Filtered solution through #41 Whatman paper. Average 26.1 78.9 5.13

TABLE-US-00036 TABLE 36 UltraPAC 2361 (50% Basic PAS) Headspace 1.0% Phosphoric acid (75%) solution Conversion Gallons Target Initial Actual Working Examples MV-173 MV-173 64.8222 14774.7 11.4 6.9 16.0 16.0 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 185.96 Start Up Water 0 1.000 185.96 8.16 12,055 1,446 8.16 2,100 12,055 1446 8.16 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 174.02 Solution Water 0 1.000 173.97 7.63 11,275 1,352 7.63 2,705 11,275 1441 7.63 56.25 Sodium carbonate 0 NA 56.27 2.47 3,650 NA 2.47 3,650 NA 2.47 188.50 43% Sodium aluminate 23.87 149.0 1.520 188.43 8.26 12,215 964 8.26 2,316 12,215 964 8.26 % Na.sub.2O SAX 20.27 1701.50 Alumium sulfate 8.36 6.7 1.325 1701.31 74.61 110,285 9,984 74.61 110,285 9984 74.61 0.00 Pressure PAC (UP 290) 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 22.50 H3PO4 (75%) solution 0 1.570 22.66 0.99 1,470 112 0.99 1,470 112 0.99 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 2250.0 Final product 8.21 8.21 1.200 2328.6 102.12 150,945 15,088 101.12 150,950 13,749 102.12 Check 2280.3 100.00% 150,950 0 147,822 13,753 100.00% % SA soln 24.4% 1.243 1,900.2 97.92% 147,817 ?3,133 147,822 ?3,128 4 97.93% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 78.70 3.50% Evap. & CO.sub.2 8.21% 47.4 17.63 0.00 0.00 17.63 2.26 19.89 Actual 48.33 2.12% Just CO.sub.2 8.04% 17.26 0.00 17.26 2.26 19.53 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 3,128 2.12% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel, 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH fails below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.21 8.22 0.01 % Fe.sub.2O.sub.3 0.00 % Basicity 47.4 46.8 ?0.6 146.6 % Sulfates 17.63 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 21.9 71.4 3.75 0.6 6 Agitator at 200 rpm. Started both feeds at 12:15 pm. 2.2 1.4 1.6 1 21.9 71.4 4.33 0.6 6 2.2 1.4 1.6 2 22.0 71.6 4.32 1.2 12 4.3 2.6 1.7 3 22.2 72.0 4.66 2.4 28 8.6 5.8 1.5 4 22.8 73.0 5.06 2.4 28 8.6 5.8 1.5 5 23.3 73.9 5.19 2.4 32 8.6 6.5 1.3 6 23.6 74.5 5.18 2.4 32 8.6 6.5 1.3 7 24.5 76.1 5.33 2.4 32 8.6 6.5 1.3 8 25.1 77.2 5.70 2.4 32 8.6 6.5 1.3 9 25.6 78.1 5.86 2.4 32 8.6 6.5 1.3 10 26.2 79.2 5.91 2.4 32 8.6 6.5 1.3 11 26.6 79.9 6.01 2.4 32 8.6 6.5 1.3 15 28.1 82.6 6.18 2.4 34 8.6 6.9 1.2 20 29.7 85.5 6.47 2.4 34 8.6 6.9 1.2 25 30.5 86.9 6.60 2.4 34 8.6 6.9 1.2 30 31.1 88.0 6.67 2.4 33 8.6 6.7 1.3 35 31.5 88.7 6.64 2.4 33 8.6 6.7 1.3 40 31.8 89.2 6.62 2.4 33 8.6 6.7 1.3 50 31.7 89.1 6.10 2.4 0 Water/soda ash/sodium aluminate mixture feed complete. 8.6 0.2 40.5 4.1 55 30.0 86.0 5.27 4.8 0 17.1 0.0 0.0 142 25.1 77.2 4.13 0.6 0 Aluminum sulfate feed complete. Started phosphoric acid (75%) solution feed. 2.2 0.0 0.0 150 26.6 79.9 4.09 0.0 0 Phosphoric acid (75%) solution feed complete. 0.1 0.0 0.0 290 24.3 75.7 4.19 0.0 0 Let mix overnight. 0.0 0.0 0.0 Apr. 21, 2022 8:30 am (20.25 hrs) Solution clear. Filtered solution through #41 Whatman paper. 0.0 0.0 0.0 Average 27.5 81.5 6.03

TABLE-US-00037 TABLE 37 UltraPAC 2361 (50% Basic PAS) Headspace 1.0% Phosphoric acid (75%) solution Conversion Gallons Target Initial Actual Working Examples MV-176 MV-176 66.6691 14774.7 11.4 8.2 16.0 15.6 Digest Temp. (? C.) Formulation Target Actual Target Overnight (? C.) % M.sub.2O.sub.3 % Basicity Sp. Gr. grams % Pounds Gallons % Min. Gallons Pounds Gallons % 185.96 Start Up Water 0 1.000 185.96 8.39 12,400 1,487 8.39 2,100 12,400 1487 8.39 0.00 Ferric sulfate 17.75 10.5 1.581 0.00 0.00 0 0 0.00 0 0 0 0.00 174.02 Solution Water 0 1.000 174.10 7.85 11,605 1,392 7.85 2,784 11,605 1482 7.85 56.25 Sodium carbonate 0 NA 56.21 2.54 3,745 NA 2.53 3,745 NA 2.53 203.50 43% Sodium aluminate 23.87 135.5 1.520 203.59 9.18 13,575 1,071 9.18 2,463 13,575 1071 9.18 % Na.sub.2O SAX 20.27 1607.80 Alumium sulfate 8.36 6.7 1.325 1608.08 72.53 107,210 9,705 72.53 107,210 9705 72.53 0.00 Pressure PAC (UP 290) 16.88 41.8 1.370 0.00 0.00 0 0 0.00 0 0 0.00 % Cl UP 290 20.99 22.50 H3PO4 (75%) solution 0 1.570 22.59 1.02 1,505 115 1.02 1,505 115 1.02 Flush Water 1.000 0.00 0.00 0 0 0.00 0 0 0.00 2187.5 Final product 8.26 8.26 1.200 2250.5 101.51 150,040 14,997 100.49 150,040 13,749 101.51 Check 2217.1 100.00% 150,040 0 147,811 13,780 100.00% % SA soln 24.4% 1.242 1,847.6 98.51% 147,811 ?2,229 147,811 ?2,229 31 98.51% Evaporation % Al.sub.2O.sub.2 % Basicity % SO.sub.4 % Cl Cl/SO.sub.4 ratio Cl + SO.sub.4 Na Cl + SO.sub.4 + Na Expected 62.50 2.86% Evap. & CO.sub.2 8.26% 47.5 17.14 0.00 0.00 17.14 2.43 19.57 Actual 33.43 1.51% Just CO.sub.2 8.13% 16.88 0.00 16.88 2.43 19.31 1. Add required amount of start up water to the reactor and start agitation. 0.9541 2. Add the required amount of water into the soda ash mix vessel and start agitator. 2,229 1.51% 3. Add required amount of sodium carbonate (soda ash) to the soda ash mix vessel and agitate until dissolved. 4. Add the required amount of 43% sodium aluminate solution into the soda ash mix vessel. 5. Add the required amount of aluminum sulfate solution to the alum holding vessel. 6. Start addition of the aluminum solution to the reactor to lower pH to less than 4. 7. Start addition of the sodium carbonate/sodium aluminate mixture to the reactor. 8. Adjust feed rates to add the solutions over desired time period maintaining the pH between 5.5 and 7. 9. When all of the sodium carbonate/sodium aluminate solution has been added let the pH fall below 5. 10. When the pH fails below 5 increase the aluminum sulfate feed rate. 11. When all of the aluminim sulfate solution has been added start the phosphoric acid addition. 12. When phosphoric acid addition is completet let solution mix until all solids have dissolved. Analysis: Specific Gravity Calculated Actual % M.sub.2O.sub.3 % Al.sub.2O.sub.3 8.26 8.31 0.05 % Fe.sub.2O.sub.3 0.00 % Basicity 47.5 49.8 2.3 144.0 % Sulfates 17.14 Turbidity, NTU Viscosity, cps Precipitation observations and data Bulk Bulk Alum/ H.sub.2O/ H.sub.2O/ slurry slurry Bulk UP290 SA/SAX Alum SA/SAX Time Temp. Temp. slurry pump pump pump rate pump rate Pump (min) (? C.) (? F.) pH setting setting Comments (ml/min.) (ml/min.) Ratio 0 22.2 72.0 3.82 0.6 6 Agitator at 200 rpm. Started both feeds at 1:35 pm. 2.2 1.4 1.6 1 22.4 72.3 4.15 0.6 6 2.2 1.4 1.6 2 22.5 72.5 4.23 2.4 34 8.6 6.9 1.2 3 23.0 73.4 4.50 2.4 34 8.6 6.9 1.2 4 23.0 73.4 4.57 2.4 38 8.6 7.7 1.1 5 24.8 76.6 6.20 2.4 38 8.6 7.7 1.1 6 25.7 78.3 6.34 2.4 38 Increased agitator to 250 rpm. 8.6 7.7 1.1 7 26.5 79.7 6.65 2.4 34 8.6 6.9 1.2 8 27.1 80.8 6.85 2.4 34 8.6 6.9 1.2 9 27.7 81.9 6.86 2.4 32 8.6 6.5 1.3 10 28.1 82.6 6.85 2.4 32 8.6 6.5 1.3 15 29.5 85.1 6.70 2.4 32 8.6 6.5 1.3 20 30.6 87.1 6.65 2.4 32 8.6 6.5 1.3 30 31.8 89.2 6.57 2.4 32 8.6 6.5 1.3 40 32.5 90.5 6.49 2.4 32 8.6 6.5 1.3 1.3 50 32.9 91.2 6.49 2.4 0 Water/soda ash/sodium aluminate mixture feed complete. 8.6 0.0 0.0 60 29.8 85.6 5.01 4.8 0 17.1 0.0 0.0 123 26.0 78.8 4.17 0.6 0 Aluminum sulfate feed complete. Started phosphoric acid (75%) solution feed. 2.2 0.0 0.0 130 27.4 81.3 4.13 0.0 0 Phosphoric acid (75%) solution feed complete. 0.0 0.0 0.0 147 27.3 81.1 4.16 0.0 0 Let mix overnight. 0.0 0.0 0.0 Apr. 25, 2022 8:00 am (18.42 hrs) Solution clear. Filtered solution through #41 Whatman paper. Average 28.5 83.3 6.60

[0065] The embodiments of the invention described above are intended to be merely exemplary; numerous variations and modifications will be apparent to those skilled in the art. All such variations and modifications are intended to be within the scope of the present invention as defined in any appended claims.