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Title:
PROCESS FOR RECOVERING VALUE METALS FROM IRON-CONTAINING ALLOYS
Document Type and Number:
WIPO Patent Application WO/2000/065113
Kind Code:
A1
Abstract:
A process for selectively extracting a value metal from a ferrous solid, the value metal being selected from the group consisting of cobalt, nickel and copper, and the ferrous solid being selected from mattes and alloys containing iron and the value metal in metallic form. In a first leach step, an aqueous solution is provided in contact with an oxygen-containing atmosphere, the first aqueous solution having a pH of less than about 2.0 and containing sufficient sulfate ion to form a soluble sulfate with the value metal contained in the ferrous solid. The ferrous solid is added to the first aqueous solution over a period of at least one hour to increase the pH to the range of about 4 to 6, while maintaining the temperature of the first aqueous solution at less than about 100°C during addition of at least the last fifty percent of the solid. At the end of the first leach, a solid/liquid separation is performed to separate a first liquid fraction containing soluble sulfates of the value metal from a solid iron-containing residue. The solid residue is preferably treated in a second leach step to recover copper and unleached cobalt. The second leach step comprises treating the solid residue with an acidic aqueous solution at elevated pressure and a temperature of about 120 to 220°C, to thereby oxidize copper sulfides present in the residue and cause copper to enter the liquid phase as soluble copper salts.

Inventors:
DUNN GRENVIL MARQUIS (ZA)
HOLLIDAY HENRY EDWARD (ZA)
Application Number:
PCT/ZA2000/000074
Publication Date:
November 02, 2000
Filing Date:
April 25, 2000
Export Citation:
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Assignee:
DUNN GRENVIL MARQUIS (ZA)
HOLLIDAY HENRY EDWARD (ZA)
International Classes:
C25C7/02; (IPC1-7): C22B23/00; C22B15/00; C22B7/00
Domestic Patent References:
WO1997007248A11997-02-27
Foreign References:
US4100043A1978-07-11
US4093526A1978-06-06
US5344479A1994-09-06
US4452706A1984-06-05
Attorney, Agent or Firm:
Dunlop, Alan J. S. (Hahn & Hahn Inc. 222 Richard Street Hatfield 0083 Pretoria, ZA)
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Claims:
What is claimed is:
1. A process for selectively extracting a value metal from a ferrous solid, said value metal being selected from the group consisting of cobalt and nickel and said ferrous solid being selected from mattes and alloys containing iron and said value metal in metallic form, wherein said process comprises: (a) providing a first aqueous solution in contact with an oxygencontaining atmosphere, said first aqueous solution having a pH of less than about 2.0 and containing sufficient sulfate ion to form a soluble sulfate with said value metal contained in a predetermined quantity of said ferrous solid ; (b) adding said predetermined quantity of said ferrous solid to said first aqueous solution over a period of at least one hour to increase the pH of the first aqueous solution to the range of from about pH 4 to about pH 6, wherein a temperature of the first aqueous solution during addition of at least a final 50 percent of said ferrous solid is maintained at less than about 1 00°C, (c) conducting a solid/liquid separation to separate a first liquid fraction containing soluble sulfates of said value metal from a first solid residue containing substantially all of the iron in said predetermined quantity of said ferrous solid; and (d) reducing and recovering said value metal from said first liquid fraction.
2. 2 The process of claim 1, wherein the temperature of the first aqueous solution is about 65 to 100°C.
3. The process of claim 1, wherein the temperature of the first aqueous solution is about 75 to 85°C.
4. The process of claim 1, wherein the temperature is maintained at less than about 100°C during addition of substantially all of said ferrous solid.
5. The process of claim 1, wherein the ferrous solid contains about 35 to 70 percent by weight metallic iron and less than about 10 percent metallic cobalt.
6. The process of claim 1, wherein said step (d) comprises an electrowinning process.
7. The process of claim 6, wherein spent electrolyte from said electrowinning process is recycled for use in the first aqueous solution in said step (a).
8. The process of claim 1, wherein said ferrous solid is added over a time of from about I to 6 hours.
9. The process of claim 1, wherein said ferrous solid is added intermittently as a plurality of portions, each of said portions comprising from about 2 to about 50 percent of the predetermined quantity of said ferrous solid.
10. The process of claim 1, wherein a pressure of said oxygencontaining atmosphere is at a pressure ranging from atmospheric pressure to about 1,000 kPa.
11. The process of claim 10, wherein the pressure of said oxygencontaining atmosphere is from about 300 to about 700 kPa.
12. The process of claim 1, wherein said value metals include both nickel and cobalt and said ferrous solid additionally comprises zinc, and wherein said process further comprises a first purification step in which said nickel and zinc are removed from said first liquid fraction prior to said cobalt electrowinning step.
13. The process of claim 1, wherein said ferrous solid additionally contains copper in the form of copper sulfides, said copper comprising up to 30 percent by weight of said ferrous solid and being substantially unleached during said steps (a) and (b), said copper being extracted from the first solid residue by a process comprising : (e) oxidizing said copper sulfides in said first solid residue to produce soluble copper sulfates by contacting said first solid residue with a second aqueous solution containing sulfate ion and having an initial pH of less than about 3.0 in the presence of a pressurized oxygencontaining atmosphere and at a temperature of from about 120 to about 220°C; conducting a liquid/solid separation to produce a second liquid fraction containing said soluble copper sulfates and a second solid residue; (g) reducing and recovering said copper from said second liquid fraction.
14. The process of claim 13, wherein said temperature during said step (e) is maintained at about 130 to about 170°C.
15. The process of claim 13, wherein said pressurized oxygencontaining atmosphere is maintained at a total pressure in the range of from about 400 to about 2,500 kPa during said step (e).
16. The process of claim 13, wherein said pressurized oxygencontaining atmosphere is maintained at a pressure in the range of from about 700 to about 1,200 kPa during said step (e).
Description:
PROCESS FOR RECOVERING VALUE METALS FROM IRON-CONTAINING ALLOYS FIELD OF THE INVENTION The present invention relates to a process for recovering value metals such as cobalt and/or nickel from alloys and mattes containing substantial amounts of iron.

BACKGROUND OF THE INVENTION Substantial reserves are known to exist of ores, both of the oxidic and sulfidic types, as well as slags, which contain relatively small amounts of value metals such as cobalt, copper and/or nickel and relatively large amounts of iron. The first step in recovering value metals from such ores and/or slags is a pyrometallurgical reduction process which converts oxides of metals in the ore or slag to metals having a zero oxidation state. This reduction process is conducted at high temperature in a reduction furnace, and the material produced by the reduction is typically referred to as a"matte"or"alloy".

Alloys typically contain about 35 to 70 percent iron, and less than about 10 to 60 percent of value metals such as cobalt, copper and/or nickel. Mattes are similar in composition to alloys, but have a relatively high sulfur content, typically exceeding about 10 percent. The sulfur is typically associated with copper, which can comprise up to about 30 percent of the matte or alloy.

Metals are recovered from mattes and alloys by a hydrometallurgical process involving an acidic leach process conducted under oxidative conditions, in which all the metals present in the matte or alloy are oxidized and dissolved in the form of soluble metal salts. After separation of the liquid fraction from the solid residue, iron is separated from the remaining metals in the liquid fraction by precipitation.

One disadvantage with conventional processes is that the hydrometallurgical leaching step involves dissolving all the metals to produce a liquid fraction in which the value metals account for only a small fraction of the total dissolved metals. Clearly, it would be desirable from an economic standpoint to reduce the volumes of liquid used in the leaching step and thereby improve its efficiency.

SUMMARY OF THE INVENTION The present invention overcomes the above-mentioned problems of prior art processes for recovering value metals from a matte or alloy by providing a process in which the iron in the matte or alloy remains in a substantially insoluble state during the leaching process, thereby significantly reducing the volume of liquid which is required to dissolve the metals in the matte or alloy.

The process of the present invention is particularly adapted for recovery of value metals such as cobalt, copper and/or nickel from mattes and alloys in which the value metals are entrained with relatively large amounts of iron. The process of the present invention involves a first hydrometallurgical leaching step in which a quantity of matte or alloy is contacted with an aqueous, acidic solution containing sulfate ion to form a soluble sulfate of the value metal contained in the matte or alloy. This first leach is conducted under conditions in which the iron contained in the matte or alloy is oxidized and transiently forms soluble sulfates which are immediately converted to insoluble compounds which precipitate out of the solution. A solid/liquid separation then separates the value-metal containing liquid fraction from the iron- containing solid residue, and the liquid fraction is purified, where necessary, and further processed to recover the value metals therefrom.

Therefore, in one aspect, the present invention provides a process for selectively extracting a value metal from a ferrous solid, said value metal being selected from one or more members of the group consisting of cobalt and nickel and said ferrous solid being selected from mattes and alloys containing iron and said value metal in metallic form, wherein said process comprises: (a) providing a first aqueous solution in contact with an oxygen-containing atmosphere, said first aqueous solution having an initial pH of less than about 2.0 and containing sufficient sulfate ion to form a soluble sulfate with said value metal contained in a predetermined quantity of said ferrous solid ; (b) adding said predetermined quantity of said ferrous solid to said first aqueous solution over a period of at least one hour to increase the pH of the first aqueous solution to the range of from about pH 4 to about pH 6, wherein a temperature of the first aqueous solution during addition of at least a final 50 percent of said ferrous solid is maintained at less than about 100°C; (c) conducting a solid/liquid separation to separate a first liquid fraction containing soluble sulfates of said value metal from a first solid residue containing substantially all of the iron in said predetermined quantity of said ferrous solid; and (d) reducing and recovering said value metal from said first liquid fraction.

In addition to containing large amounts of iron, mattes and alloys may also contain up to about 30 percent copper. Copper is typically contained in a matte or alloy in the form of insoluble sulfides and passes through the first leach substantially unleached, being present in the solid residue recovered from the first leach. In circumstances where it is desired to also recover copper from the matte or alloy, the process of the present invention includes optional steps for treating the solid residue of the first leach under conditions in which the copper sulfides in the solid residue are oxidized to soluble copper sulfates. After a second solid/liquid separation, the liquid fraction containing copper sulfates is purified and treated to recover copper therefrom.

Accordingly, in a second aspect, the present invention provides the process as described above, wherein said ferrous solid additionally contains up to about 10 percent by weight sulfur in the form of copper sulfides, said copper sulfides being substantially unoxidized during said steps (a) and (b) and being contained in said first solid residue, said copper being extracted from the first solid residue by a process comprising: (a) oxidizing said copper sulfides in said first solid residue to produce soluble copper sulfates by contacting said first solid residue with a second aqueous solution containing sulfate ion and having an initial pH of less than about 3.0 in the presence of a pressurized oxygen-containing atmosphere and at a temperature of from about 120 to about 220°C; (b) conducting a liquid/solid separation to produce a second liquid fraction containing said soluble copper sulfates and a second solid residue ; (c) reducing and recovering said copper from said second liquid fraction.

BRIEF DESCRIPTION OF THE DRAWINGS The invention will now be described, by way of example only, with reference to the accompanying drawings, in which: Figure 1 is a flow diagram showing a preferred two-stage leaching process according to the present invention; and Figure 2 is a flow diagram showing an alternate two-stage leaching process according to the present invention.

DETAIL DESCRIPTION OF PREFERRED EMBODIMENTS A preferred process for extracting value metals from a matte or alloy will now be described below with reference to the flow diagrams shown in Figures 1 and 2.

As discussed above, the present invention is useful for extracting value metals from mattes and alloys which are produced by reduction of iron-rich ores. These mattes or alloys typically contain for example about 35 to 70 percent by weight iron, less than about 10 up to about 60 percent cobalt and/or nickel and up to about 30 percent copper. Alloys typically contain little or no sulfur, whereas mattes contain greater than about 10 percent sulfur. The method of the present invention is also useful for extracting value metals from materials having a sulfur content of up to about 10%, which are neither mattes nor alloys. These materials are sometimes referred to as"malloys". However, the terms"matte"and"alloy"as used herein are intended to include materials containing from 0 to 10 percent sulfur.

In a particularly preferred embodiment, the process of the present invention is utilized to recover cobalt and copper from a material which contains about 65 percent iron, 6 to 7 percent cobalt (this amount includes nickel which has similar chemistry), about 13 to 27 percent (average 19 percent) copper, relatively small amounts of zinc, selenium, tellurium, manganese, chromium, cadmium, arsenic and lead, which may or may not be recovered according to the process of the invention. The material also contains about 5 percent sulfur, and therefore, strictly speaking, it can neither be categorized as a matte nor an alloy, but is nevertheless referred to herein as a matte or alloy.

Most of the metals in the matte or alloy, including iron and value metals, are present in their zero oxidation state, having being reduced in the previous ore processing step. However, at least some of the copper in the matte or alloy is present in the form of the copper sulfide Cu2S and, if the sulfur content is relatively high, will also be present as CuS.

The first step in the preferred process of the present invention comprises leaching cobalt from the matte or alloy by an acidic leaching step conducted under oxidative conditions. In a preferred embodiment, the matte or alloy is charged over a period of time into a reactor containing an acidic solution of sulfate ion under an oxygen-containing atmosphere. The amount of sulfate ion contained in the leaching liquid is preferably stoichiometrically matched to the value metal content of the matte or alloy. The adjustment of sulfate content is discussed more fully below.

Under the conditions employed in the preferred leaching step, value metals such as cobalt and nickel are oxidized and form soluble sulfates, namely CoS04 and NiS04. The metallic iron present in the matte or alloy is oxidized and reacts with sulfuric acid in the leaching solution to form the soluble iron sulfates FeSO4 and Fe2 (SO4) 3. However, these iron sulfates immediately undergo disproportionation, primarily forming iron hydroxide FeO (OH) and iron hydroxysulfate Fe (OH) SO4, both of which are insoluble and precipitate from the solution. Sulfuric acid is regenerated in the production of these insoluble iron compounds. Therefore, iron is transiently dissolved during the first leaching step, but is immediately precipitated as insoluble compounds.

The transient dissolution of iron does not need to be accounted for in the design of the leach step, in terms of reactor volume, liquid volume or sulfuric acid concentration, and therefore iron may effectively be regarded as being insoluble during the first leach.

Under the conditions used in the first leaching step, copper which is present in the matte or alloy in the form of copper sulfides, is substantially unleached and remains in the solid phase.

Therefore, the first leach effectively separates value metals such as cobalt and/or nickel from iron and copper. The preferred conditions for the first leach are now discussed below.

The solution which forms the liquid fraction of the first leach is acidic, preferably containing sulfuric acid and copper sulfate and having an initial pH no greater than about 2.0.

More preferably, the leaching solution is a recycled electrolyte from a cobalt and/or copper electrowinning process, discussed in greater detail below. Where the liquid fraction is a recycled electrolyte from copper or cobalt electrowinning, it will contain sulfate ion in the form of sulfuric acid, and in the form of soluble sulfates of metals such as copper. Sulfate ion in these forms is referred to herein as"exchangeable sulfate", since it is available for formation of soluble sulfates of value metals such as cobalt and/or nickel.

In order to provide the oxidative conditions necessary to oxidize the value metals and the iron in the matte or alloy, the acidic leaching solution is preferably in contact with an oxygen- containing atmosphere, such as air (20 percent oxygen) or an atmosphere containing higher amounts of oxygen, for example 93 percent oxygen from a vacuum swing absorption plant or 99.5 percent from a cryogenic plant. The oxidative atmosphere preferably has a pressure at or above atmospheric pressure. More preferably, the oxygen-containing atmosphere is pressurized, thereby increasing the speed of the leaching reaction by increasing the amount of oxygen in solution. Most preferably, the oxygen-containing atmosphere has a pressure of up to about 1,000 kPa, and even more preferably from about 300 to about 700 kPa.

The temperature of the acidic leaching solution is preferably maintained at an average temperature of less than about 1 00°C during the leach in order to avoid oxidizing copper sulfides to soluble copper sulfates. More preferably, the temperature is maintained in a range of from about 65 to about 100°C, and even more preferably from about 75 to 85 °C.

In the process of the present invention, the solid matte or alloy is added to the acidic leaching liquid gradually. The gradual addition of the matte or alloy results in a gradual rise in the pH level of the liquid from an initial pH of less than about 2.0, typically about 1.6, to a pH in the range of from about 4 to 6, and preferably from about 4.5 to about 5.5. This rise in pH reflects the consumption of H2SO4 in the oxidation of value metals such as cobalt and/or nickel to produce soluble metal sulfates.

The addition of the matte or alloy may either be continuous or step-wise in portions. The size and number of portions is variable, with each portion preferably comprising from about 2 to about 50 percent of the total mass of the solid added. In general, continuous addition or addition of a relatively large number of small portions produces better results than the addition of relatively few large portions.

The matte or alloy is preferably added to the leaching liquid over a period of time of from about 1 to about 6 hours, and more preferably from about 2 to about 3 hours. The matte or alloy may be added at either a constant or variable rate over this period of time.

The reaction between the metals in the matte or alloy with the acidic leaching liquid is highly exothermic. In prior art leaching processes, all of the matte or alloy is typically added to the leaching liquid in one portion at the beginning of the leaching process, resulting in a rapid increase in temperature to at least 130°C. Allowing the temperature to increase into this range causes the oxidation of copper sulfides present in the matte or alloy, producing soluble copper sulfates, some of which react further to produce additional sulfuric acid and hydrolyzed copper compounds. This prevents the pH from increasing to the above-mentioned range, resulting in copper contamination of cobalt rich liquors, and a more difficult separation of the liquid and solid fractions. In contrast, the step-wise addition of matte or alloy to the acidic leaching liquid in the process of the present invention removes heat from leach slurry residues and reduces the extent of sulfur oxidation, thereby improving the purity of the cobalt rich liquor.

Preferably, the matte or alloy is added to the liquid such that the temperature is kept below 100°C. However, it is to be noted that some excursions in temperature above 100°C maybe tolerated at the start of the leach. Since the matte or alloy is added gradually, there is typically only a small proportion of the total matte or alloy present in the leaching liquid at the beginning of the leach. The oxidation of the copper sulfides in this portion of the matte or alloy will typically not have a significant detrimental effect on the extraction of the value metals or the purity of the cobalt rich liquor.

For example, the addition of the initial portions of the matte or alloy to the liquid may result in an exotherm to the range of from 100 to I50°C. After this, the temperature may be reduced, for example by flashing off steam, to the preferred range of less than about 100° C.

Preferably, the temperature then remains at less than about 100° C for the remainder of the leach.

In the preferred embodiment of the present invention, the temperature is brought down to the preferred range of less than 1 00°C for the addition of at least the final 50 percent of the matte or alloy. More preferably, the temperature remains at less than 100°C for substantially the entire addition of the matte or alloy to the acidic leaching liquid.

The inventors have found that performing a first leaching step according to the preferred method described above results in substantially all the copper and iron remaining in the solid phase with from about 70 percent to about 95 to 100 percent of the value metals such as cobalt and/or nickel being extracted into the liquid phase. After completion of the leach, a solid/liquid separation is conducted to separate a value metal-containing stream from the solid residue. This separation may preferably be accomplished by filtration or by counter current decantation (CCD).

In leaches conducted with a"malloy"having the composition set out above, the following ratios of cobalt to other metals are typically observed in the value metal stream: Co/Fe > 10,000 Co/Cu > 100 Co/As > 10,000 Co/Pb > 10,000.

Therefore, it can be seen that the first leach in the preferred process of the present invention provides a liquid stream which is predominantly comprised of soluble salts, primarily sulfates, of value metals such as cobalt and/or nickel. As shown in the flow diagram of Figure 1, this value metal stream may preferably be subjected to further purification by conventional means to remove impurities such as nickel or zinc from the solution. After purification, cobalt is recovered from the liquid stream, preferably by electrowinning in which cobalt ions are reduced and precipitated as cobalt metal in its zero oxidation state. The spent electrolyte from the electrowinning step contains sulfuric acid and residual amounts of metal salts. Preferably, at least a portion of this electrolyte is re-circulated for incorporation into the acidic leaching liquid in the first leach, with optional bleeding of a portion of the spent electrolyte or neutralization of the acid in the electrolyte to adjust the amount of sulfate ion contained therein.

Although a specific purification circuit is shown in Figure 1, it is to be appreciated that numerous other methods exist for purifying the value metal-containing stream obtained from the solid/liquid separation conducted at the end of the first leach. In another preferred embodiment of the present invention, illustrated in Figure 2, cobalt is precipitated from the value metal-containing stream in the form of cobalt carbonate by addition of sodium carbonate and sodium hydroxide to the value metal stream The cobalt carbonate then undergoes a series of additional steps by which it is purified, culminating in a cobalt electrowinning step to produce cobalt metal.

Where the matte or alloy contains significant amounts of copper, and where it is desired to recover the copper contained in the matte or alloy, the solid residue obtained from the solid/liquid separation in the first leach is subjected to further processing in a second leaching step. The object of the second leach is to extract copper and the remaining cobalt unextracted in the first leach into the aqueous phase while iron remains in the solid phase. As in the first leach, the solid phase is contacted with an acidic leaching liquid which contains sulfuric acid, the leaching liquid preferably comprising a spent electrolyte from either a cobalt or copper electrowinning step which, as discussed above, may contain residual amounts of soluble metal salts. The initial pH of the leaching liquid is typically less than about 2.0, more typically about 1.4, reflecting the sulfuric acid content of the leaching liquid. After addition of the solid residue to the leaching liquid, the pH may increase to about 2.5 to 5.0, but decreases during the second leach to about 1.4 to 1.6, reflecting the liberation of HzSO4 during the formation of insoluble iron compounds.

The second leaching step is also conducted under oxidative conditions in order to facilitate oxidation of the copper sulfides present in the solid phase. As in the first leach, the oxygen- containing atmosphere may be comprised of air or oxygen in varying states of purity. In the second leach, the oxygen-containing atmosphere is pressurized, preferably to a pressure of from about 400 to about 2,500 kPa, and more preferably from about 700 to about 1,200 kPa. As in the first leach, pressurization of the oxygen-containing atmosphere ensures that sufficient oxygen enters the liquid phase to oxidize any remaining metal compounds, including sulfides, in the matte or alloy.

The temperature in the second leach is preferably higher than that of the first leach in order to provide more vigorous conditions for copper sulfide oxidation. Preferably, the temperature in the second leach is from about 120 to 220°C, and more preferably from about 130 to 170°C. In general, the higher the pressure and temperature in the second leach, the higher will be the degree of copper extracted from the solid phase. However, it will be appreciated that the actual pressure and temperature conditions used in the second step are largely determined by economic considerations, with the increased value of extracted copper being weighed against the costs associated with raising the pressure and/or temperature of the second leach. For example, the use of a temperature of 130 to 170°C and a pressure of from 700 to 1,200 kPa will typically extract about 70 percent of the copper from the solid phase during the second leach. However, the application of more vigorous conditions can increase the level of copper extraction to about 95 to 100 percent.

Under the above conditions, copper is leached into the liquid phase as soluble salts while substantially all the iron remains in the solid phase, primarily in the form of FeO (OH), with some iron (III) oxide (Fe203) being formed, both of these compounds being substantially insoluble in the liquid phase. The relative proportions of the iron compounds formed in the second leach is at least partially dependent on the leach temperature and pressure. For example, higher temperatures and pressures favour the formation of iron m oxide over FeO (OH).

In the second leach, the solid residue from the first leach may preferably be added in one or more portions, the size and number of the portions being relatively unimportant because temperature control is relatively unimportant in the second leach, as long as it is sufficient to oxidize copper sulfides. Preferably, the second leach is continued for a period of from about 1 to 8 hours, most preferably about 3 to 5 hours.

In addition to extraction of copper from the solid phase, the second leach also is useful for removing any residual value metals remaining in the solid residue after the first leach. These value metals may be entrained in the solid residue in the form of soluble sulfates, or in the form of insoluble compounds such as hydroxysulfates or metallics. These compounds are converted in the second leach to soluble sulfates, such as cobalt sulfate, and are extracted into the liquid phase during the second leach. The amounts of value metals extracted during the second leach may be significant, depending on the amounts extracted during the first leach For example, the second leach may extract up to about 30 percent of the cobalt originally contained in the matte or alloy.

A further variation of the preferred process of the present invention involves the exothermic nature of the second leach. In many cases, the unleached sulfur in the form of sulfides present in the solid residue from the first leach is sufficient to provide the exothermic heat required to sustain the leach temperature of the slurry during the second leach. Where an excess of heat is generated, this excess may be recovered as steam in a flash-don process or other cooling method. Where the sulfide content is insufficient to support an autogenous second leach, then a further variation of the preferred process comprises diversion of some of the matte/alloy from the first leach directly to the second leach, thereby producing an energy source for the second leach step.

ARer the completion of the second leach, a solid/liquid separation is conducted in order to separate the copper containing liquid stream, which may also contain some other value metals, from the iron-containing solid residue. As in the first leach, the separation is preferably accomplished by filtration or counter current decantation (CCD) methods. In order to remove soluble copper and cobalt compounds from the solid residue as completely as possible, the solid residue is preferably washed at this point by addition of fresh water, and the wash liquors are added to the copper containing liquid stream. In preferred embodiments of the invention in which spent electrolytes from cobalt and/or copper electrowinning are used as the leaching liquids, this stage is a convenient location for intake of fresh water into the process. After washing the solid residue, the combined liquid phase is subjected to further purification in order to recover copper therefrom.

As a first purification step, shown in Figure 1, the copper containing liquid phase may be subjected to a conventional process in which selenium and/or tellurium are precipitated from the liquid phase. These metals are typically present in the matte or alloy in small amounts. After recovery of selenium and/or tellurium, the purified liquid stream is then preferably subjected to copper electrowinning, during which copper ions are reduced to provide copper metal in its zero oxidation state.

The spent electrolyte from the copper electrowinning step primarily contains sulfuric acid, but typically also contains some amounts of soluble metal sulfates, such as copper sulfate, iron sulfates and cobalt sulfate. The amount of copper in the spent electrolyte can be significant, on the order of about 30 g/L. Similarly, as discussed above the spent electrolyte may contain up to about 30 percent of the cobalt originally present in the matte or alloy. In order to recover these residual metals, the spent electrolyte is preferably recycled for reuse as the leaching liquid in the first and/or second leach, and may optionally be combined with spent electrolyte from the cobalt electrowinning step discussed above. The recycling of spent electrolyte is also preferred because sulfuric acid generated during electrowinning reduces the need to input fresh sulfuric acid into the process.

In the preferred process of the invention in which spent electrolyte is recycled, the sulfur contained in the matte or alloy forms the primary source of sulfate ion in the leaching liquids for the first and second leaches. As discussed above, mattes and alloys contain varying amounts of sulfur. Where the sulfur content is relatively low, the amount of sulfate generated may be insufficient to completely leach value metals from the matte or alloy. Under these circumstances, the sulfate content of the liquid phase is preferably supplemented by addition of sulfuric acid or by recycling cobalt and copper spent electrolytes.

Conversely, in mattes and alloys having a relatively high sulfur content, it may be preferred to reduce the sulfate content of the spent electrolyte in order to balance the exchangeable sulfate demand over the first and second leaches. Sulfate content may preferably be reduced by bleeding some of the spent electrolyte and replacing it with fresh water (preferably during the washing step discussed above) or by neutralizing some of the acid in the spent electrolyte by addition of a base.

An alternate preferred method for reducing sulfate content in the liquid phase is to add a jarosite-forming salt to the second leach in order to form jarosite, a sulfate-containing iron minera, having a formula such as NaFe3 (So,) 2 (OH),, which is insoluble in the leaching liquid, thereby effectively removing some of the sulfate from the liquid phase. Preferred jarosite-forming salts include alkaline metal salts such as sodium or potassium sulfate.

The present invention is further illustrated by the following examples.

EXAMPLE 1 This Example comprised a two-step process according to the preferred embodiment of the present invention. The conditions for the first leach are shown in Table 1, comprising a batch leach log sheet. In this Example, 1,700 g of an alloy containing 65 percent Fe, 6 to 7 percent Co, 19 percent Cu and 5 percent S was added step-wise in portions to 3,000 ml of a leaching liquid comprising the spent electrolyte from a copper electrowinning process. As shown in Table 1, most of the alloy was added to the leaching liquid during the first hour of the leach, during which time the pH was raised to 4.70. The leach was continued for over five hours, at the end of which time the pH had increased to 5.25. The leach was run at a constant oxygen pressure of 500 kPa and at a temperature of approximately 80°C.

Table 2 shows the extraction data for the first leach of Example 1. As shown in Table 2, the copper content in the liquid phase, initial at 40.7 g/l, was reduced to 0.078 g/ after one hour. This reflects the conversion of soluble copper sulfate in the spent electrolyte to insoluble copper hydroxysulfate, 2 Cu (OH) 2. Cu S04. Also after one hour of leach time, the amount of cobalt in the liquid phase increased from 4.53 g/l to 21.2 g/l, translating to an extraction of 74.4 percent of the cobalt in the solid alloy. Table 2 also shows the content in the liquid phase of a number of other metals. Most notably, iron is present in the liquid phase in an amount of less than 0.45 ppm.

Following filtration of the leach mixture, the solid residue is treated by a second leach under the conditions shown in Table 3. In this leach, the liquid phase comprised spent electrolyte from a copper electrowinning process (Reagent 1), supplemented with additional sulfuric acid (Reagent 2). The composition of the copper spent electrolyte was Cu = 19.7 g/l, Co = 3.31 g/l, H2S04= 28.4 g/1. To this liquid phase was added 2259.8 g of the solid residue obtained from the first leach of Example 1, the residue being added in four portions. This leach was conducted at a total (02 + steam) pressure of 680 kPa and at a temperature of about 1 60°C. The pH of the leach liquid decreased from an initial pH of 4.69 to a final pH of 1.56 after a leach time of eight hours.

As shown in Table 4, most of the copper was removed from the solid residue and into the liquid phase, with the extraction of copper from the solid residue after a leach time of five hours being 92 0 percent. Furthermore, after a leach time of five hours, 97.1 percent of residual cobalt contained in the solid residue was extracted into the liquid phase. In contrast, as shown in Table 4, the content of iron in the liquid phase remains fairly low, being 996 ppm after a leach time of nine hours.

EXAMPLE 4 As shown in Table 5,850 g of the alloy of Example 1 was added into a solution of spent electrolyte from a copper electrowinning process, the alloy being added over a period of one hour at a temperature of about 80°C and an oxygen pressure of 500 kPa. The pH of the liquid phase increased gradually from 2.45 to 5.37 over a period of four hours. The extraction data for the first leach of Example 4 is shown in Table 6, and is generally consistent with that discussed above in Example 1.

The conditions for the second leach of Example 4 are shown in Table 7. In the second leach, 981.76 g of residue was added to a solution containing spent electrolyte and sulfuric acid at a total (ou + steam) pressure of 1,100 to 1,200 kPa and a temperature of 150°C, causing the pH to be reduced to 1.36 after a leach time of eight hours. No fresh sulfuric acid was added, only that recycled in the spent electrolyte (Reagent 1) having the following composition: Cu = 0.55 g/l, Co-20.3 g/l, H2S04= 69.6 g/1. The extraction data for the second leach is shown in Table 8, showing excellent extraction of cobalt and copper during the second leach.

EXAMPLE 5 This Example shows only conditions and extraction data for the first leach in the process.

As shown in Table 9,1,400 g of the alloy of Example 1 was added in small portions to a spent electrolyte solution at a pressure of 50 kPa and a temperature of 85 to 90°C, causing the pH to rise to 5.11 after about ten hours.

As shown in Table 10, the conditions used in the leach of Example 5 resulted in poor extraction of cobalt from the solid phase, whereas most of the copper in the liquid phase was transferred to the solid residue. Significant soluble iron remained in the leach liquor (8.2 g/1).

EXAMPLE 6 As shown in Table 11,1,800 g of the alloy of Example I was added in small portions over a period of five to six hours to a solution containing spent electrolyte at an oxygen pressure of 700 kPa and a temperature of about 70 to 85°C, raising the pH to 5.23 after a leach time of seven hours.

The results of the extraction in the first leach are shown in Table 12, with the cobalt extraction reaching a maximum of 84.7 percent after five hours, and the copper content of the liquid phase being reduced to 0.238 glui at the same time.

The conditions for the second leach of Example 6 are shown in Table 13, in which the solid residue from the first leach was added to a leach liquid at a total (02 + steam) pressure of 1,200 kPa and a temperature of about 160°C, decreasing the pH to 1.66 after eight hours. These conditions resulted in high extraction of both cobalt and copper from the residue, with cobalt extraction reaching a maximum of 97.7 after five hours, and copper extraction reaching a maximum of 95.4 after nine hours.

EXAMPLE 7 As shown in Table 15,1,450 g of the alloy of Example I was added in small portions over a period of six hours to a solution of spent electrolyte at an oxygen pressure of 300 kPa and a temperature of about 80°C, increasing the pH from 1.22 to 5.08 after five hours. As shown in Table 16, the copper content of the liquid phase was reduced to 0.07 g/l after five hours, whereas cobalt was extracted to 74 percent after the same time.

In the second leach of Example 7, the conditions of which are shown in Table 17,2173.33 g of the solid residue from the first leach was added to a solution of spent electrolyte and sulfuric acid at a total (°2 + steam) pressure of 700 kPa and a temperature of about 130°C, decreasing the pH to 1.40. As shown in Table 18, copper extraction reached a maximum of 91.2 percent after seven hours and cobalt extraction reached a maximum of 94.8 percent after seven hours.

EXAMPLE 8 In the first leach of Example 8, the conditions of which are shown in Table g of the alloy of Example 1 was added in small portions over a period of six to seven hours at atmospheric pressure and a temperature of about 85°C, increasing the pH to 4.46 after six and one half hours. As shown in Table 20, cobalt extraction was 92.9 percent after three hours, and the copper content of the liquid phase was reduced to a minimum of 1.2 ppm after five hours.

In the second leach, as shown in Table g of the solid residue from the first leach was added to a solution of sulfuric acid at a pressure of 1,000 kPa and a total (02 + steam) temperature of about 170°C, lowering the pH of the liquid phase to 1.40 after seven hours.

As shown in Table 22, copper extraction from the solid residue reached a maximum of 95.5 percent after eight hours, and cobalt extraction reached a maximum of 95.2 percent, also after eight hours. It is to be noted that since the leach liquid in the second leach comprised a solution of sulfuric acid, and not a spent electrolyte solution, the initial concentration of copper and cobalt in the liquid phase was zero.

EXAMPLE 9 In the first leach of Example 9, shown in Table 23,1,800 g of the alloy of Example 1 was added in small portions over a period of about six hours to a spent electrolyte solution at a total (02+ steam) pressure of 500 kPa, bringing the pH from 1.42 to 5.06 after six hours. It is to be noted that the temperature of the leach was allowed to rise to a high of 150°C over the first hour of the leach, and was subsequently reduced to about 80°C for the remainder of the leach time.

About 28 percent (500 g) of the total mass of the alloy was added during the first hour of the leach.

As shown in Table 24, the copper content of the liquid phase was not reduced during the first hour of the leach, but was subsequently decreased to a minimum of 53 ppm after a leach time of seven hours. The cobalt extraction on the other hand reached a maximum of 94.1 percent after one hour. The leach obtained after five hours, at which time copper was reduced to 0.57 g/1 and zinc was reduced to 0. 29 ppm, while about 75 percent of cobalt was extracted, represents highly preferred reaction conditions to obtain a pure cobalt-containing liquid stream. The lixiviant in the leach had a composition of Cu = 25.3 g/l, Co = 9.73 g/l, H2S04 = 17.6 g/l.

In the second leach of Example 9, shown in Table 25, a total of 2471.93 g of the residue from the first leach was added to a leaching liquid containing spent electrolyte and sulfuric acid at a total (°t + steam) pressure of 1,000 kPa and a temperature of 160*C, the pH being reduced from 2.50 to 1.40 after a leach time of eight hours. It can be seen from Table 26 that copper extraction in the second leach reached a maximum of 92 percent after a leach time of nine hours, and cobalt extraction reached a maximum of 96.8 percent after nine hours. However, it will also be seen that the copper and cobalt extractions were also high after a leach time of only three hours.

EXAMPLE 10 In the first leach of this Example, the conditions of which are shown in Table 27,2,800 g of the alloy of Example 1 was added in small portions over a period of about three hours to a solution of spent electrolyte at a temperature of about 140°C and a total (02 + steam) pressure of 600 kPa. In this Example, the pH rose from 1.03 to 3.84 after 195 minutes, reaching a maximum of 4.45 after 150 minutes.

In this Example, the temperature in the first leach is substantially higher than that in any of the other Examples and, as discussed above, oxidation of copper sulfides present in the alloy occurs, resulting in production of sulfuric acid and therefore the increase in the pH is less than that in the other Examples. The lixiviant in this leach had a composition of Cu = 24.5 g/t, Co = 8.69 gQ, H2SO4 = 16. 7 g/l.

The effect of the increased temperature on the copper and cobalt content of the liquid phase is significant. As shown in Table 28, the copper content of the liquid phase could not be reduced below 0.6 g/l, iron was not completely reduced and cobalt extractions were lower considering the feed alloy to lixiviant ratio. The lixiviant composition was Cu = 24.5 g/l, Co = 8.69 g/l, H2SO4 = 16. 7 g/l.

In the second leach, shown in Table 29, a total of about 120 g of the solid residue from the first leach was extracted with a mixture of spent electrolyte and sulfuric acid at a total (ou + steam) pressure of 1,000 kPa and a temperature of about 160°C, decreasing the pH to 1.41 after a leach time of five hours. However, Table 30 shows that the copper extraction reached a maximum of 94.7 after six hours and cobalt extraction reached a maximum of 88.3 percent after six hours.

EXAMPLE 16 As shown in Table 31,3986 g of alloy was added in portions over a period of 135 minutes to a synthetic solution containing 16.9 g/ ! copper, 10 g/t cobalt and 40 g/l free acid. The leach was conducted over a period of five hours at a temperature of about 85 °C and an oxygen pressure of 500 kPa. The test extraction data for the first leach is shown in Table 32, with the copper being reduced from 16.9 g/1 to 0.35 gÅ after five hours, and cobalt extraction reaching 68.97 percent after the same time frame.

In the second leach, shown in Table 33,1708 g of the solid residue obtained from the first leach was added to a solution of sulfuric acid in portions over a period of ten hours, and a total (02 + steam) pressure of 1,000 to 1,200 kPa and a temperature of about 170°C As shown in Table 34, copper extraction reached a maximum of 93.5 percent after five hours and cobalt extraction reached a maximum of 96.5 percent (also after five hours) of the unleached cobalt fraction.

Although the invention has been described in connection with certain preferred embodiments, it is to be understood that it is not limited thereto. Rather, the invention includes within its scope all embodiments which may fall within the scope of the following claims.

TABLE1 - BATCH LEACH LOGSHEET FOR FIRST LEACHIN EXAMPLE 1<BR> Cllent<BR> Leach Test Number Allay 1A<BR> Date 25/01/99 Residue Feed (g) Type Unite Detalls Sample Num Residue Dryness (%) Water (ml) Residue Size (u) Liquor (ml) 3000 Alloy1LO (ex Av16@ Sample Number - Reagent 1 Alloy (gms) 1700 Alloy RO Atmosphere Type Gs Oxygen Reagent 2 Water (ml) 600 Operator Carlos Reagent 3 (gms) Vapor Sample Number Time Temp pH EH Pressure Vent Down Reagent 1 Reagent 2 Reagent 3 Residue Mass Remarks/Obse@ Actual Test(min) (°C) (kPaG) (YIN) (g) (ml) (ml) (gms) 9:00 0 79 3.00 286 500 Y 600 50 LO - Purple / blue 9:15 15 82 3.30 278 500 Y 250 50 9:30 30 86 4.16 211 500 Y 400 50 Alloy 1A L1 10:00 60 82 4.70 124 500 Y 100 50 29.25 (L) Murky pink 11:00 120 84 5.07 164 50 Y 50 (R) Dark Red 11:30 150 84 5.05 207 500 Y 50 Alloy 1A L3 12:00 180 82 5.06 205 500 Y 50 31.14 (L) Dark pink 12:30 210 82 5.13 198 500 Y 100 50 (R) Dark Red Alloy 1A L4 13:00 240 87 5.21 168 500 Y 50 45.41 (L) Dark pink 13:30 270 79 5.26 159 500 Y 100 50 (R) Dark Red Alloy 1A L5 14:00 300 83 5.21 167 500 Y 150 50 37.57 (L) Dark pink 14:20 320 81 5.25 158 500 Y 50 (R) Dark Red 1700 600 143.37 Datalls Sample No Colour General Final Filtrate Volume (ml) 2280 Alloy 1A L6 Dark Pink Final Wash Volume (ml) Combined wash and fairale prior lo sampling the final liquor Final Residue Mass-Wet (gms) 3126.19 Alloy 1A R6 Dark Red/Brown Free acld in feed = 4.9 g/L; Cu = ~ 34 g/L Final Residue Mass-Dry (gms) 2406.2 Test 1A TABLE Table 2 - Test Extraction Data for Second Leach in Example 1<BR> Cllent<BR> Leach Test Number Alloy 1A<BR> Date 99/01/26 Start End Residue Weight (g) 2300 2406.2 Volume (ml) 3000 2260 Sample Temp Leach Pressure Conditions In Reactor Cu Co S Number (°C) Time (kPaG) Mass Volume Residue Liquor Extraction Residue Liquor Extraction Residue Liquor Extraction (hours) (g) (ml) (%) g/l (%) (%) g/l (%) (%) g/l (%) AlloyR0/AV16BL5 79 0 500 600 3000 20.5 40.7 0 6.71 4.53 0 Alloy 1A L1 82 1 500 1453 2865 15.6 0.078 -35.00 2.01 21.2 74.4 5.72 Alloy 1A L3 82 3 500 1687 2595 15.6 0.303 -34.8 1.92 15.1 71.6 5.49 Alloy 1A L4 87 4 500 1874 2460 Alloy 1A L5 83 5 500 2219 2325 Alloy 1A L6 6 500 2406 2280 15.9 0.079 -34.6 3.1 13.1 34.6 5.59 Analysis: Mn Zn Nl Fe Cd Pb S= Sample Numbrt ppm ppm ppm ppm (%) ppm ppm (%) Alloy 1A L1 39 Alloy 1A L3 40.2 Alloy 1A L6 45 <4.0 58 <0.45 38.1 <0.32 <7.0 3.12 Basis of extraction: Liquid over solld for Cu<BR> Solid over solid for Co & S Extractions.xlsAV1A Cllent<BR> Leach Test Number Alloy 1B<BR> Date 27/01/99 Residue F*W 9 2252. 1 Retldue0 eft % D WsW mq 7000 ample Numen Heldue Sttv IU neived SAM I@ Numbw Allay I A Rg Liquor mp) a Mumbtf. Atto/lAM <M) tnt) SEttBID (m): 0f) 0 A!) oylBLO OkbMsphom Type GIs oxygen"gtnl I SE loalli Anton Rap ! fItSO) (SD0 pil) (mf 615 Vtpor Vpor lmplv HumCn Tlmv Tmp pH E"Pnmun Vwt Down Rngeot 1 Nogmt Rnyent Ruldue Mas RvmvhdObenaUona Aclual letmln) (G'kPap) IN) mq m ml) (ms) coo oeo . se uvoo tso° seo'rsoa eeo r soo i eu 5: 0o so tet a. ta za 15: 0 680 y eo ao. ao P kene Al t. et an seo v so R petirown ie : aa » oso teZe eeo Y s 1870 30 fA0 1. SI IO2 e ! 0 y je: 30t! 0 tM 1. K <t!)) 0 Y A 18 L3 17: 00 1eD 160 1. 59 SOt eS0 y 17 : 10 210 1B 1. BZ SOS s 17. 19 L Dee e 11:OD 210 1 A t 525 p y R Red Mown tl : 30 270 160 1. 51 52A eep y AI18 L5 19 : 00 300 180 1. 51 521 ee0 y trb trt L3 17 Zo = t62 si 62 _ 2 soet | = Y _ j < _ 17 1 s R j Red bw19 : J030 160 1. 55 101 ea0 y t7.E L le R Rrd biovm 20v00 J80 1D1 1. 61 55 B80 Y 200 : 0 : 303M 160 tK « : 6) 0 Y uhr 1ita u ts : oo _ 300 1eo 1. s4-i 524 _ eoo r _... _ t7. s1e iLs Oorso purPle21 : 00 420 tea 1. 58 501 ago y 21: 00 430 III 1. 34 47$ Alov 18 La lea 1. 56 1435 purple UoyidLit 22 : so so teo 1. 55 j 495 | seo 1 r | | l. _ R) RrcibrowmToldt t000 Red brown Details 5 pie NoColour ciennl Rnd Fplrate Vdume (m 412U AB f8 LO Dtep po k Free AtJd of reepAnll = irigi wash volume (m 1) 2000 A tO Lio PufPL'W93h w3t"not combtn Rh Ina FIW 1 ResIEue Mas. We ms 1 AOl. 50 tB Ri Red bavn M Aot wrler. TAi, m wm A1 18 R10. Fkel Rssldue MasD (pma 1116. 71 t7. 67 0) 20. 06 J110 ml d N uor (L9 Ne h. took out 1 Sa. S of Cu mMal.

Test 1B(1)table3.xls.es@ Table 4 - Test Extraction Data for Second Leach of Example 1<BR> Cllent<BR> Leach Test Number Alloy 1B<BR> Date 99/01/27 Start End Residue Weight (g) 2259.8 1416.73 Volume (ml) 2000 4420 Sample Temp Leach Pressure Conditions in Resctor Cu Co S Number (°C) Time (kPaG) Mass Volume Residue Liquor Extraction Realdue Liquor Extraction Residue Liquor (hours) (g) (ml) (%) g/l (%) (%) g/l (%) (%) g/l Alloy 1B L0 160 0 680 2260 3500 15.9 NA 0 3.1 NA 0 Alloy 1B L3 160 3 680 1944 4610 4.9 63.6 73.5 0.6827 16.5 81.1 3.38 Alloy 1B L5 160 5 680 1733 4615 1.66 85.2 92.0 0.1183 16.2 97.1 1.44 Alloy 1B L9 160 9 680 1417 4420 2.32 64.3 90.9 0.2245 12.6 95.5 1.76 Analysis: Mn Zn Nl Fe S= Sample Number ppm ppm ppm ppm [%] Alloy 1B L9 68 105 301 996 0.46 Basis of extraction: Solid over solid for Cu, Co & S<BR> Extraction TABLE 5 - BATCH LEACH LOGSHEET FOR FIRST LEACH OFEXAMPLE 4<BR> Cllent<BR> Leach Test Number Alloy 4A<BR> Date 01/02/99 Residue Feed (g) Type Units Details Sample @ Residue Dryness (%) Liquor Alloy 2BL10 (ml) 2000 Combined 10 gi@ Residue Size (µ) Liquor Alloy 2BL9 (ml) 1000 Sample Number - Reagert 1 Alloy (gms) 850 Alloy Almosphere Type Gas Oxygen Reagert 2 Water (ml) 800 Operator Carlos Reagert 3 (gms) Vapor Sample Number Time Temp pH EH Pressure Vent Down Reagent 1 Reagent 2 Reagent 3 Residue Mass Remarks/O@ Actual Test (min) (°C) (kPaG) (Y/N) (g) (ml) (ml) (gms) 8:15 0 79 2.45 386 500 Y 400 100 8:30 15 83 4.51 70 500 Y 130 100 8:45 30 83 4.58 58 500 Y 250 100 Alloy 4A L1 9:15 60 86 5.15 50 500 Y 100 100 R1 10.79 (L) Dark pink 9:45 90 79 5.34 83 500 Y 100 (R) Dark red/brow@ 10:15 120 78 5.36 128 500 Y 100 Alloy 4A L3 11:15 180 82 5.33 152 500 Y 100 R3 13.19 (L) Dark pink Alloy 4A L4 12:15 240 81 5.37 174 500 Y 100 (R) Dark red/brow@ R4 19.83 (L) Dark pink (R) Dark red/brow@ R5 10.61 (L) Dark pink (R) Dark red/brow@ Totals 850 800 (D) = 54.42 Detalls Sampte No Colour General Final Filtrate Volume (ml) 2660 Alloy 4A L5 Dark pink Final Wash Volume (ml) 400 Final filtrate mined with wash water prior to sampling. Final Residue Mass-Wet (gms) 1291.79 Alloy 4A R5 Dark red/brown Final Residue Mass-Dry (gms) 981.75+54.42 = 1036.18 Test Table 6 - Test Textraction Datafor First Leach of Example 4<BR> Cllent<BR> Leach Test Number Alloy 4A<BR> Date 99/02/01 Start End Residue Weight (g) 850 1036.18 Volume (ml) 3000 3060 Sample Temp Leach Pressure Conditin in Reacher Cu Co S Number (°C) Time (kPaG) Mass Volume Residue Liquor Extraction Residue Liquor Extraction Residue Liquor Extra (hours) (g) (ml) (%) g/l (%) (%) g/l (%) (%) g/l (@ Alloy 4A L0 79 0 500 850 3000 20.5 22.4 0 6.71 7.81 0 5.37 Alloy 4A L1 86 1 500 912 2830 12.2 0.367 -37.90 1.48 15.6 76.3 4.51 9. Alloy 4A L3 82 3 500 974 2660 14.6 0.275 -38.0 2.23 13.5 61.9 5.06 -8 Alloy 4A L5 81 5 500 1036 3060 12.9 0.295 -38.7 2.26 13 58.9 4.64 -9 Analysis: Mn Zn Nl Fe Cd Pb S= Sample Number ppm ppm ppm ppm ppm ppm (%) Alloy 4A L5 35 <4.0 82 <0.45 <0.32 <7.0 2.72 Basis of Extraction : Solid over Solid for Co & S.<BR> <P>Liquid over Solid for Cu.<BR> <P>Extractions.@ TABLE 7 - BATCH LEACH LOGSHEET FOR SECOND LEACH OF EXAMPLE 4<BR> Cllent<BR> Leach Test Number Alloy 4B<BR> Date 08/02/99 Residue Feed (g) 981.76 Type Units Details Sam Residue Dryness (%) DRY Walter (ml) Residue Size (µ) As required Liquer Alloy 3BL9 (ml) 2000 Al Sample Number - Alloy 4A R5 Reagent 1 Alloy 3BL9 (ml) 1100 Free Atmosphere Type Gas O2 Reagent 2 500 g/l H2SO4 (ml) Operator Reagent 3 H2O (ml) 850 Vapor Sample Number Time Temp pH EH Pressure Vent Down Reagent 1 Reagent 2 Reagent 3 Resldue Mass Remark Actual Test (min) (°C) (kPaG) (Y/N) (ml) (ml) (ml) (gms) 9:15 0 100 2.76 298 1100 Y 9:45 30 150 1.80 455 1200 Y 900 250 Alloy 4BL1 10:15 60 151 1.67 455 1200 Y 200 100 (VV)33.62(O)23.30 (L) Yellow/Bro 10:45 90 150 1.58 469 1200 Y 11:15 120 149 1.44 460 1200 Y 11:45 150 150 1.56 434 1200 Y Alloy 4BL3 12:15 160 150 1.50 477 1200 Y 100 (VV)34.84(D)23.67 (L) Purple (R) 12:45 210 150 1.48 45 1200 Y 13:15 240 151 1.53 462 1200 Y 13:45 270 150 1.54 455 1200 Y 100 Alloy 4BL5 14:15 300 150 1.45 465 1200 Y 100 (VV)34.19(D)23.32 (L) Purple (R) 14:45 330 151 1.40 450 1200 Y 15:15 360 150 1.39 467 1200 Y 15:45 390 150 1.36 467 1200 Y 100 16:15 420 150 1.34 460 1200 Y 16:45 450 150 1.34 475 1200 Y 100 Alloy 4BL8 17:15 480 150 1.36 476 1200 Y (VV)35.85 (D)24.07 (L) Purple (R) Detalls Sample No Colour General Final Fillrale Volume (ml) 4600 Alloy 4BL9 Purple Opened O2 at 100@ start adjusting pH Final Wash Volume (ml) 2000 Alloy 4BL10 Light Purple Repulped caks & filtered twice with 1@ H2O al a time then wash with 1@ insitu Final Residue Mass-Wet (gms) 844.29 Alloy 4BR9 Red Brown Final Residue Mass-Dry (gms) 591.56 + 110.30 TABLE7-Filtration- Table 8 - Test Extraction Data for second Leach of Example 4<BR> Client<BR> Leach Test Number Alloy 4B<BR> Date 99/02/08 Start End Residue Weight (g) 981.76 685.92 Volume (ml) 3100 6600 Sample Temp Leach Pressure Conditions in Reactor Co Cu S Number (°C) Time (kPaG) Mass Volume Residue Liquor Extraction Residue Liquor Extraction Residue Liquor Extractio@ (hours) (g) (ml) (%) g/l (%) (%) g/l (%) (%) g/l (%) Alloy 4BL0 151 0 1200 981.76 3100 6.67 20.30 20.8 0.6 5.37 Alloy 4BL3 150 3 1200 883.12 3850 0.18 22.40 9760 0.5 34.1 97.8 2.60 56.40 Alloy 4BL5 150 5 1200 784.5 4600 0.25 22.30 97.00 0.8 33.8 96.9 1.94 71.20 Alloy 4BL9 150 8 1200 685.92 6600 0.32 15.90 96.60 0.9 23.8 96.9 1.56 79.40 Alloy 4BL10 2.79 4.7 Analysis: Mn Zn Nl Fe S@ Se Te Sample Number ppm ppm ppm g/l (%) ppm ppm Alloy 4BL0 130 26 342 0.99 <0.2 <0.2 Alloy 4BL9 236 34 230 2.7 0.48 <0.2 <0.2 Basis of Extraction : Solid over Solid for Co, Cu & S.<BR> <P>Extraction TABLE9 - BATCH LEACH LOGSHEET FOR FIRST LEACH OF EXAMPLE 5<BR> Client<BR> Leach Test Number Alloy 5A<BR> Date 03/02/99 Residue Feed (g) Type Units Details Sample Residue Dryness (%) Liquor (Wash) Alloy 3BL10 (ml) 2000 Combined to give @ Residue Size (µ) Liquor (SE) Alloy 4BL0 (ml) 1000 Free Acid=19.6 g Sample Number - Reagent 1 Alloy (gms) 1400 Alloy RO Atmosphere Type Gas Oxygen Reagent 2 Waler (ml) 1400 Operator GMD Reagent 3 (gms) Vapor Sample Number Time Temp pH EH Pressure Vent Down Reagent 1 Reagent 2 Reagent 3 Residue Mass Remarks/O Actual Test (min) (°C) (kPaG) (Y/N) (g) (ml) (ml) (gms) 12:20 0 50 Y 400 100 12:35 15 88 3.93 50 Y 100 Vent gas -s weet @ Alloy 5AL1 12:50 30 88 4.32 50 Y 200 100 (D) 10.32 13:20 60 88 4.88 50 Y 200 100 Alloy 5AL2 13:50 90 90 4.53 50 Y 200 100 (D) 16.69 Alloy 5AL3 14:20 120 86 5.59 50 Y 200 100 (D) 20.22 Colour light pink Alloy 5AL4 15:20 180 87 5.35 -26 50 Y 100 (D) 56.29 Colour light pink 17:15 295 91 3.08 < 10 Y 100 Alloy is still unreac 18:35 375 86 4.99 50 Y 100 400 Oxidation proceed 20:00 460 85 5.5 50 Y 100 100 Reaction autothen 21:00 520 85 5.41 50 Y 100 Alloy 5AL10 22:00 580 84 5.11 50 Y (D) 22.38 Residue in slurry Hes a high pH > 5 Liquor pH = 4.8 Combined blend p Totals 1400 1400 Total dry = 126.1 Detalls Sample No Colour General Final Filtrate Volume (ml) 2600 Alloy 5AL10 Red Wash Blended with the final filtrate (Free acid of SE Alloy 4BLO = 43.8 g/l) Final Wash Volume (ml) 360 Red Final Residue Mass-Wet (gms) 2011.35 Alloy 5AR10 Black Final Residue Mass-Dry (gms) 1568.85+126.1=1694.95 Batch#Filtration 1A-5A TABLES.xls..x Table 10 - Test Extraction Data for First Leach of Example 5<BR> Client<BR> Leach Test Number Alloy 5A<BR> Date 99/02/03 Start End Residue Weight (g) 1400 1694.95 Volume (ml) 3000 2960 Sample Temp Leach Pressure Conditions in Reactor Cu Co S Number (°C) Time (kPaG) Mass Volume Residue Liquor Entraction Residue Liquor Extraction Residue Liquor Extracti@ (hours) (g) (ml) (%) g/l (%) (%) g/l (%) (%) g/l (%) Alloy 5AL0 0 0 50 1400 3000 20.5 12.7 0 6.71 11.5 0 5.37 Alloy 5AL1 86 1 50 1498 2800 10.3 0.087 -13.20 4.22 14.4 32 3.2 36.3 Alloy 5AL3 86 3 50 1596 2600 10.3 0.0014 -13.3 4.26 1.34 29.3 3.34 29.1 Alloy 5AL10 64 10 50 1695 2960 16.1 0.023 -13.3 4 10.2 27.8 4.52 -1.9 Analysis: Mn Zn Nl Fe Cd Pb S= Sample Number ppm ppm ppm g/l ppm ppm (%) Alloy 5AL1 2.72 Alloy 5AL3 2.87 Alloy %AL10 35 <4.0 134 8.23 <0.32 <7.0 4.22 Basis of Extraction : Solid over Solid for Co & S.<BR> <P>Liquid over Solid for Cu.<BR> <P>Extractions.xisA TABLE 11 - BATCH LEACH LOGSHEET FOR FIRST LEACH OF EXAMPLE 6 Client Leaeh Tast Numbet Alloy 6A Date99/OM9 Type Un) Details Sample Number Reeldue Feed (g Waier lmO Rnldw Drynen (1y llQtror AAoy 1B L9 (m 7500 Alloy 6A l0 RaaWu Sle Rea nl 1 ALLOY mt 1EOD Sample Number Reagontl HIO (mo 900 Abnosphere Type Gas a Reaoenl 3 Igms 0 lor Sample Number Time Tvmp pH E"Prntun Vnt Down Rnpent 1 Rapent 7 Rnynt RmukWOhsmtlans Actual Te timlnl rcl {XPaGI ItlN) (gmtl (ma (ma Igms} UQ 14 : 00 0 65 1. 22 7Gd 700 Y Hi h saWhemic 1d : 15 15 1. l7 751 700 Y 100 so A"BA Ll 14 : 30 30 74 2. 49 348 700 Y 100 so ID) 8. 15 (L) Lighl Purple (R) Light Mustard 15 00 S0 7J 2 40 345 70D Y 100 so AII Ell L2 13 : 30 9D N I. EE 71I 700 Y 100 50 U l. ES L Bmwn R L hf MuslaN 16: 00 120 72 3. 04 147 700 Y 100 so 16:0 150 ! 9 7. 00 lE5 700 Y 100 50 17*00 ISO 72 3. 40 228 700 y-200 ioa 1730 210 77 371 1t2 700 Y Do 100 AUoy M L4 tt 00 240 71 4 ot 131 700 Y 2w loo (D) 1g 17 (L) Dalk Plnk IR) LbhlBrowntOnnge 18: 30 270 79 45 36 700 Y : M 100 AA EA LS 19vD0 300 A2 4. lE 15 700 Y 200 100 D 20. 29 L OarkPlnk R Oon vlNed A"« y t6 19 zo 330 tS S N 25 700 y-200 100 15 tL) Dark Pink (R) Orange Aloy 6A L7 20 00 3v0 24 S 23 50 700 y (D) 3 (L) Dark Pink (R) Red RI D 70. 10 RS D 30. 10 teoo ioo Tata 0 u. oa Dwbll4 SomDI No Colour Finsl Flltrate Vdume (mf) 710 Alloy 6A l. ! DARK PINK FNn WaA Vduma (mh 100 ComDined MdIlnb md wnh prior M famplinp Fnalwashvdume (mr) g 400Final Raildus Mass-wfgt 3494. 79 Alloy BA Ri DARK RED Feed Uo FIn71 Reaidue MassD ms) 27E0. 16 174. 01 2es1. 91 TABLES AvAlloy 6A 10B xIzAvdoy IA Table 12 - Test Extraction Data for First Leach of Example 6<BR> Client<BR> Leach Test Number Alloy 6A<BR> Date 99/02/09 Start End Residue Weight (g) 1800 2894.91 Volume (ml) 3500 2540 Sample Temp Leach Pressure Conditions in Reactor Co Cu S Number (°C) Time (kPaG) Mass Volume Residue Liquor Extraction Residus Liquor Extraction Residue Liquor Extrac (hours) (g) (ml) (%) g/l (%) (%) g/l (%) (%) g/l (% Alloy 6AL0 0 0 700 1800 3500 6.67 17.2 20.5 6.05 5.37 Alloy 6AL1 74 0.5 700 1956.4 3273 2.35 23 45.50 6.62 14.5 11.2 10.6 -11 Alloy 6AL2 74 1.5 700 2112.8 3047.4 2.91 21.6 48.8 13.7 3.57 1.31 9.6 -109 Alloy 6AL4 78 4 700 2269.2 2821.4 1.37 33.8 74.1 11.3 0.814 -1.02 6.3 -47 Alloy 6AL5 82 5 700 2425.6 2595.4 0.8 28.2 84.7 13 0.238 -1.47 5.6 -40 Alloh 6AL6 85 5.5 700 2582 2369.4 2.63 27.2 43.5 12 0.061 -1.6 5.7 -52 Alloy 6AL7 84 6 700 2738.4 2140 2.97 26.6 32.3 11.5 0.109 -1.57 5.3 -50 Alloy 6AL8 2894.9 2540 2.66 22.7 35.8 13.4 0.146 -1.53 6.6 -6.4 Analysis: Mn Zn Ni Fe Cd Pb S= Sample Number ppm ppm ppm ppm (%) ppm ppm (%) Alloy 6AL1 27.5 Alloy 6AL2 27.9 Alloy 6AL4 36.9 Alloy 6AL5 41.2 Alloy 6AL6 39.3 Alloy 6AL7 39 Alloy 6AL8 250 1.8 84.0 <0.45 40.1 <0.32 <70 3.06 BAsis of Extraction: Solid over Solid for Co & S.<BR> <P>Liquid over Solid for Cu.<BR> <P>Extractions.@ TABLE 13 - BATCHLEACH LOGSHEET FOR SECOND LEACH OF EXAMPLE 6 CHent Leath Test Number Alloy 6B Date 99/02/13 Type Unlta Detalla Sample Nu@ Residue Feed (g) 2725.84 Wsier DIW (m#) 1500 Combined to make Residue Dryness (%) 0.78 Liquor (wash) Alloy 4B L10 (m#) 2000 Residue Size (µ) Reagent 1 H2SO4 (500 g/l) (m#) 650 Sample Number Reagent 2 H@O (m#) 1200 Almosphare Type Gas O2 Reagent 3 Liq sample (m#) 250 Operator Anton Sample Number Time Tamp pH EN Pressure Vent Down Reagent 1 Reagent 2 Sample Vol. Residue Mass Ra@arks/Obs@ Actual Test (min) (°C) (kPaG) (YIN) (m#) (m#) (m#) (gms) LIQ 11:30 0 181 3.81 229 1200 Y 200 100 12:00 30 159 3.41 259 1200 Y 150 100 Alloy 8B L1 12:30 60 162 3.02 286 1200 Y 100 100 50 (W)14.00 (L) Light Pink 13:00 90 158 2.65 302 1200 Y 100 100 (D)8.28 (R) Red 13:30 120 182 2.41 334 1200 Y 100 100 14:00 150 159 1.55 351 1200 Y 100 Alloy 6B L3 14:30 180 153 1.65 371 1200 Y 100 50 (W)44.43 (L) Purple 15:00 210 159 1.63 365 1200 Y 100 (D)24.80 (R) Red 15:30 240 180 1.56 365 1200 Y 100 Alloy 5B L5 18:00 270 159 1.83 365 1200 Y 100 50 (W)46.20 (L) Dark Purple 16:30 300 150 1.62 364 1200 Y 100 (D) 27.28 (R) Red 17:00 330 159 1.84 367 1200 Y 100 17:30 360 162 1.83 365 1200 Y 18:00 390 159 1.64 367 1200 Y 18:30 420 160 1.65 368 1200 Y 19:00 450 162 1.65 365 1200 Y Alloy 8B L8 19:30 480 160 1.68 385 1200 Y 50 (D) 3@:10 (L) Dark Purple L9= 50 R@= (D)23.02 850 1200 250 122.48 Detalls Sample No Colour General Final Filtrate Volume (m#) 3375 Alloy 8B L@ Repulped cake in 1@ water = wash 1 Repuiped cake in 1 (water = wash 2 Final Wash Volume (m#) 2000 Alloy 8B L10 Wash 1 & 2 = Alloy 6B L10. Kepl separsts Final Residue Mass-Wet (gms) 2160.68 Alloy 6B R@ Put @@ insitue wash through cake @@ Institue wash + @@@ate to electrowinning. Lost ~ 100 ml @g in electro Final Residue Mass-Dry (gms) 1447.66 + 122.48 = 157.14 Volume of liquor after eleckowinning 3890 ml - FA =35.28 g/@ TABLES Alloy-6A-108 xi@ Table 14 - Test Extraction Data for Second Leach of Example 6<BR> Client<BR> Leach Test Number Alloy 6B<BR> Date 99/02/13 Start End Residue Weight (g) 2725.94 1570.14 Volume (m#) 3500 3375 Sample Temp Leach Pressure Conditions in Reactor Ca Cu S Number (°C) Time (kPaG) Mass Volume Residue Liquor Extraction Residue Liquor Extraction Residue Liquor Extract@ (hours) (g) (m#) (%) g/# (%) (%) g/# (%) (%) g/# (%) Alloy 6B L0 0 0 1200 2726 3500 6.67 17.1 20.8 25.5 5.37 Alloy 6B L1 159 1 1200 2494.9 3475 0.37 16.9 94.90 2.1 55.3 90.7 1.72 70.7 Alloy 6B L3 163 3 1200 2263.7 3450 0.23 14.4 97.10 1.6 48.4 93.6 1.44 77.7 Alloy 6B L5 159 5 1200 2032.5 3425 0.2 12.3 97.7 1.44 41 94.6 1.35 81.3 Alloy 6B L6 160 8 1200 1801.3 3400 0.97 13.7 90.4 4.17 44.9 86.3 3.21 60.5 Alloy 6B L9 9 1200 1570.1 3375 0.29 14.6 97.5 1.65 48.9 95.4 1.61 82.7 Alloy 6B L10(2L Wash) 10 1200 4.87 16.6 Analysis: Mn Zn Nl Fe S= Se Te Sample Number ppm ppm ppm g/# (%) (%) ppm ppm Alloy 6B L1 57.4 Alloy 6B L3 59 Alloy 6B L5 59.1 Alloy 6B L8 52.2 Alloy 6B L9 93 8.6 170 2.05 58.8 0.31 <0.2 <0.2 Basis of Extraction : Solid over Solid for Co,Cu & S.<BR> <P>Extractions.xis TABLE 15-BATCH LEACM LUGSHEET FOR FIRST LEACH OF EXAMPLE 7<BR> Cliant<BR> Leach Test Number Alloy 7A<BR> Date @9/02/13 Unlh W bll Wcriif Dryness 2000 Combined 10 make Afty 7A La Liquor Riklus Site lpuor Alloy BB l9 (mq 1500 Svmpla Number. Rea nt I AAO 1150 RtgeMI H0 (m () B50 Atmosphere Type G 3ptfMorAnton Banlon Smple Number llmv Temp pH E". Precun Venl Down Rnpent 1 Regent 7 Smpte Vol Reddu Mme RvmmksrOMenationa AetuaiTect/mln//'C/kPO)YIN) gmy (mlmQ (gms) LIO AN: 15: Di 1. 21 117 J00 Y 1D0 50 LO-Murk Pu k 13: 15 J Dt I. t !pe00 Y 50 Sp AA 7A L1 11 : 15 60 e. 01 21700 Y SO 50 SO 10. 5o L P Ie t : 15 AO e1. 17 2100 Y 100 50 S.o R l htTan 1C15 10 EO D. 1G 2J200 Y 30 15ssO 2 326 237 Joo Y i0 so 17 : 15 142 300 y ISO so 270 83 82 300 y iso so Y 150 50 Dt5.7 R DetkTan Aliay 7A LS 17 : 45 300 82 4. 74 n : 1s mo e so etoo rso so A7AL5 17 : 15 J00 E 1. 71 ! 0 700 Y 200 SO 50 21. 62 L DaAcPinkIRed 8715 330 @3 4 92 30 300 Y 2W so D) l ? ; 79 IRl Dlrk Red M 7A Le 1A : 15 76D E7 5. 0 ! ! 7 700 Y 150 SG SO SO. A2 Ouk PinWRed . __ _. _ _ |. j _ (D) 39. 21 [R} ûark Reo_ Flire pH 5 5 21 _ j L7-50 _ _R7- ? l esD9. 11 R Dark Red .H = S. t1 l7 50 R7-N31. 55 (D) 24. 37 50 250 Total D Oefalls Sampb No Colour Gmral Aloy ? A L7 Dark Pink Final Rftrate combined with wash prior to sampling Final Wash Volume ImNi 400 Feed tiquwhet uHe. es yf Finel RssiCue Maef-Wel m :l2. 51tl 7A R7 Dar Red FinalResdusMass-Dry (9m1t171.1, ta2.7ansed TABLES AvAlloy-5A-10B.xis Table 16-Test Extraction Data for First Leach of Example 7<BR> Clie<BR> L@aest Number Alloy 7A<BR> Dat@ 99/02/13 Start End Res:Weight (g) 1450 2275.8 Volt (m#) 3500 3960 Sample Temp Leach Pressure Conditions in Reactor Cu Co S Number (°C) Time (kPaG) Mass Volume Residue Liquor Extraction Residue Liquor Extraction Residue Liquor Extraction (hours) (g) (m#) (%) g/# (%) (%) g/# (%) (%) g/# (%) AlloL0 0 0 300 1450 3500 20.5 22.40 6.7 9.2 5.37 AlloL1 83 1 300 1615.2 3515 14.4 22.60 0.40 0.2 9.3 96.7 6.38 -11.40 AlloL3 81 3 300 1780.4 3530 14.8 11.10 -0.13 0.7 14.0 87.2 6.66 -28.10 AlloL5 82 5 300 1945.5 3545 11.2 0.07 -26.30 1.3 13.9 74 4.51 5.18 AlloL6 83 6 300 2110.7 3560 12.6 0.02 -26.40 2.5 11.2 45.7 5.32 -21.30 AlloL7 7 300 2275.8 3960 12.8 0.15 -26.20 2.8 10.9 34.5 5.47 -34.60 Ana: Mn Zn Nl Fe Cd Pb S= Sa@@umber ppm ppm ppm ppm (%) ppm ppm (%) AlloL1 37.6 AlloL3 37 AlloL5 42.9 AlloL6 40.6 AlloL7 66 ND 27 20 39.8 <0.32 <7.0 3.3 BasExtraction: Solid over Solid for Co & S.<BR> <P>Liquid over Solid for Cu.<BR> <P>ND@ctected.<BR> <P>Extractions.sixAV TABLE 17-BATCH LEACH LOGSHEET FOR SECOND LEACH OF EXAMPLE 7 C@ient Leach Test Number Alloy 7B Date 99/02/16 Type Units Details Sample Numb@ Residue Feed (g) 2173.33 Water (wash) Alloy @B L9 (m#) 2190 Combined to make All Residue Dryness (%) DRY Liquor H2O (m#) 1310 Residue Size (µ) Reagent 1 H2SO4 (500 g/#) (m#) 520 Sample Number - Alloy 7A R7 Reagent 2 H2O (m#) 1300 A@mosphere Type Gas O2 Reagent 3 Operator Car@os Sample Number Time T@mp pH E@ Pressure Vent Down Reagent 1 Reagent 2 Sample Vol. Residue Mass Remarks/Observ@ Actual Test (min) (°C) (kPaG) (Y/N) (m#) (m#) (m#) (gms) LIQ 10:30 0 132 2.89 225 700 Y 100 100 L@= Dirty Purple 11:00 30 134 2.54 253 700 Y 50 50 Alloy 7B L1 11.30 80 133 2.42 273 700 Y 150 150 50 (VV)23.20 (L) Purple 12:00 90 129 2.35 294 700 V 100 100 (D)15.45 (R) Dark Red 12:30 120 128 1.56 354 700 Y 100 100 13:00 150 128 1.56 356 700 Y 100 Alloy 7B L3 13:30 180 126 1.58 358 700 Y 100 50 (VV)21.43 (L) Dark Purple 14:00 210 127 1.57 355 700 Y 100 (D)19.62 (R) Dark Red 14:30 240 12@ 1.52 364 700 Y 20 100 Alloy 7B L5 15:00 270 129 1.46 380 700 Y 100 15:30 300 131 1.44 374 700 Y 100 50 (VV)28.40 (L) Dark Purple 16:00 330 130 1.42 374 700 Y 100 (D) 14.28 (R) Dark Red 16:30 360 130 1.40 376 700 Y 100 50 (VV)32.70 (L) Dark Purple (D)20.16 (R) Dark Red L7= 50 (VV)17.66 (L) Dark Purple (D)12.48 (R) Dark Red 520 1300 250 Total Dry = @1.99 gms Detalls Sample No Colour General Final Filtrate Volume (m#) 3760 Alloy 7B L7 Dark Blue Repuiped cake in 1 (water = wash 1, repuiped cake in 1 (water = wash 2 Final Wash Volume (m#) 1900 Alloy 7B L5 Wash 1+2 = Alloy 7B L8 Kept separa@@ 1900 ml Final Residue Mass-Wet (gms) 1892.39 Alloy 7B R7 Red 1@ Insitue wash through cake, 1@ Insitue wash + filtrate to electrowinning Final Residue Mass-Dry (gms) 1343.60 + 81.99 = 1425.59 Feed Uquor free scid = 20.58 g/# TABLES AvAlloy-6A-108.@ Table 18-Test Extraction Data for Second Leach of Example 7<BR> Client Leach Test Number Alloy 7B<BR> Date 99/02/09 Start End Residue Weight (g) 2173.3 1425.59 Volume (m#) 3500 3760 Sample Temp Leach Pressure Conditions in Reactor Cu Co S Number (°C) Time (kPaG) Mass Volume Residue Liquor Extraction Residue Liquor Extraction Residue Liquor Extraction (hours) (g) (m#) (%) g/# (%) (%) g/# (%) (%) g/# (%) Alloy 7B L0 132 0 700 2173 3500 12.8 19.5 2.8 8.69 5.47 Alloy 7B L1 133 1 700 1986.2 3565 6.19 62.2 55.80 0.42 19.7 56.3 2.5 58.2 Alloy 7B L3 126 3 700 1799.4 3630 2.48 81 83.9 0.4 20.5 86.2 2.41 63.5 Alloy 7B L5 129 5 700 1612.6 3695 2.11 56.2 87.8 0.26 14.7 92.6 2.13 71.1 Alloy 7B L7 130 7 700 1425.6 3760 1.72 60.4 91.2 0.22 15.5 94.@ 2 76 Alloy 7B L@(2LWash) 8 700 2.12 23.8 0.3 5.97 2.34 Analysis: Mn Zn Nl Fe S= Se Te Sample Number ppm ppm ppm g/# (%) (%) Alloy 7B L1 49.2 Alloy 7B L3 53.3 Alloy 7B L5 54.6 Alloy 7B L7 58 ND 136 1.14 55.8 0.25 <0.2 <0.2 Alloy 7B L8 54.6 ND=Not Detected.<BR> <P>Basis of Extraction : Solid over Solid for Co,Cu & S.<BR> <P>Extractions.xis.AV@ TABLE 19-BATCH LEACH LOGSHEET FOR FIRST LEACH OF EXAMPLE 8 Chent Leach Test Number Alloy BA Date 99/02/17 Type Units Detalls Sample Numt Residue Feed (g) Water H2O (mt) 1500 Combined lo make Al Residue Dryness (%) Liquor Synthetic liq (mt) 2000 Residue Size (µ) Resgent 1 Alloy (gms) 1900 Alloy RD Sample Number Reagent 2 H2O (mt) 1250 Atmesphere Type Gas O2 Reagent 3 Sample Vol. (mt) 250 Operator Carios Sample Nomber Time Temp pH E" Pressure Vent Down Reagent 1 Reagent 2 Reagent 3 Residue Masz Remacks/obssrv Actual Test(min) (°C) (kPaG) (YIN) (gms) (me) (me) (gms) LIQ 08:30 0 84 1.06 188 ATM 150 50 Colours of Liquors 08:45 15 85 1.02 137 ATM 150 100 09:00 30 83 3.02 147 ATM 100 L0 = Light Blue Alloy BAL1 09:30 60 87 2.60 228 ATM 100 100 50 (W)11.38 (L)Purple 10:00 90 86 2.80 69 ATM 100 100 (0)6.42 (R)Red 10:30 120 86 3.09 120 ATM 100 100 11:00 150 83 3.31 128 ATM 50 50 Alloy BAL@ 11:30 180 84 3.28 132 ATM 200 50 50 (W)28.55 (L)Pink 12:00 210 83 3.64 135 ATM 150 50 (D)21.82 (R)Dark Brown 12:30 240 83 4.00 27 ATM 100 100 13:00 270 83 4.19 8 ATM 200 50 Allay BAL5 13:30 300 85 4.56 -506 ATM 200 50 50 (W)40.44 (L) Dark Pink 14:00 330 86 4.30 -36 ATM 100 100 (D)33.74 (R)Dark Red/Brown Allay BAL6 14:30 360 83 4.54 -23 ATM 150 150 50 (W)51.50 (L)Dark Pink Alloy BAL7 15:00 390 85 4.46 -38 ATM 150 100 50 (D)42.51 (R)Drak Red (L) Dark Pink (W)38.85 (R)Dark Red (D)31.40 (L)Dark Pink (R)Dark Red 1900 1250 250 Detalls Sample No Colour General Final Fitrate Volume (mt) 3220 Alloy SALS Dark Pink Combined finsi fitrale and wash prolor to Sampling Final wash Volume (mt) 400 0.01% Dryness on finel cake going to "B" Leach Final Residue Mass-Wel (gms) 3082.37 Aloy SARS Dark Red feed Liquor free acid = 18.6 g/l Final Residue Mass-Dry (gms) 2408.52 + 137.89 = 2618.41 TABLES AvAlloy - SA.10B.k Table 20 - Test Extraction Data for First Leach of Example 8<BR> Client<BR> Leach Test Number Alloy 8A<BR> Date 99/02/09 Start End. Residue Weight (g) 1900 2618.41 Volume (me) 3500 3620 Sample Temp Leach Pressure Conditions In Reactor Cu Co S Number (°C) Time (kPaG) Mass Volume Residue Liquer Estraction Residue Liquor Extraction Resldue Liquor Extractio (hours) (g) (me) (%) g/l (%) (%) g/l (%) (%) g/e (%) Alloy BALD 84 0 ATM 1900 3500 20.5 16.8 6.71 4.9ppm 5.37 Alloy BAL1 87 1 ATM 2019.6 3520 12 14.1 -2.36 0.24 4.88 96.2 5.52 -9.3 Alloy BAL3 84 3 ATM 2139.2 3540 12.8 1.61 -1.6 0.42 10.4 92.9 4.54 4.8 Alloy BAL5 55 5 ATM 2258.8 3560 14.9 1.2ppm -15.1 2.21 9.77 60.9 4.24 6.08 Alloy BAL6 83 6 ATM 2378.4 3580 14.5 62ppm -15 2.68 10.6 50 4.45 -3.73 Alloy BAL7 85 7 aTM 2498 3600 14.4 4.8ppm -15.1 2.71 9.29 46.9 4.14 -1.37 Allay BAL8 85 8 ATM 2618 3620 14.9 5.5ppm -15.1 2.65 8.07 41.5 4.78 -22.6 Analysis: Mn Zn NI Fe Cd Pb S= Sample Number ppm ppm ppm ppm (%) ppm ppm (%) Allay BAL1 42 Alloy BAL3 41.4 Alloy BAL5 44 Alloy BAL6 43.5 Alloy BAL7 44.1 Alloy BAL8 9.1 ND <1.3 20 42.6 <0.32 <7.0 3.69 Basis of Extraction : Solid over Solid for Co & S.<BR> <P>Liquid over Solid for Cu.<BR> <P>ND=Not Detected<BR> Extractions.xisA TABLE 21-BATCHLEACH LOGSHEET FOR sECOND LEACH nOF EXAMPLE 8<BR> Cllent<BR> Leach Test Number Alloy 8B<BR> Date 99/02/18 Type Units Detaits Semple Numt Residue Feed (g) 2480.52 Waler H2O (mt) 3500 Residue Dryness (%) Dry Liquor (mt) Residue Size (µ) As Received Reagent 1 H2SO4(500 g/@) (mt) 670 Sample Number - Alloy BAR@ Reagent 2 H2O (mt) 500 Atmasphere Type Gas O2 Reagent3 Liq Sample (mt) 250 Operator Cartos Sample Number Time Temp pH E14 Presswre Vent Down Reagent 1 Reagent 2 Reagent 3 Residue Mase Remarks/Observ Actual Test(min) (°C) (kPaG) (Y/N) (me) (me) (me) (gms) LIQ 10:00 0 171 292 133 1000 Y 570 Colours of Liquors 10:30 30 168 2.09 382 1000 Y Alloy SBL1 11:00 60 167 1.39 398 1000 Y 50 (W)46.85 (L)Purple 11:30 90 158 141 397 1000 Y 100 (D)33.75 (S)Red 12:00 120 174 1.40 305 1000 Y 12:30 150 173 1.41 298 1000 Y 100 Alloy SBL3 13:00 180 173 1.43 263 1000 Y 5D (W)52.56 (L) Purple 13:30 210 174 1.44 322 1000 Y 100 (D)37.21 (S)Red 14:00 240 172 1.43 324 1000 Y 14:30 270 171 1.42 318 1000 Y 100 Alloy SBL5 15:00 300 172 1.40 389 1000 Y 50 (W)47.47 (L)Purpie 15:30 330 173 1.40 368 1000 Y 100 (D)32.83 (S)Red Alloy SBL5 16:00 360 172 1.40 303 1000 Y 50 (W)42.50 (L)Purpie 16:30 390 171 1.42 324 1000 Y 100 (D)29.68 (S)Red Allay SBL7 17:00 420 170 1.40 348 1000 Y 50 (W)41.45 (L)Purple (D)29.09 (S)Red Total Dry = 670 600 250 135.54 Detalis Sample No Colour General Final Fitrale Voluem (mt) 4085 Alloy SBL@ Purple @ H2O Sluried with cake and @Mered = Wash 1 @H2O Slumed with cake and fatered = Wash 2 Final Wash Volume (mt) 2000 Alloy SBL@ Light Purple Wash 1 + Wash 2 combined and kept 2000 mt. @Institue wash put through cake and kept separate. Final Residue Mase-Wel (gms) 1728.44 Alloy 8SBR@ Red Final Residue Mass-Dryt (gms) +135.54= TABLES AvAlloy-6A-108.xl@ Table 22 - Test Extraction Data for Second Leach of Example 8<BR> Client<BR> Leach Test Number Alloy 8B<BR> date 99/02/18 Start End Residue Weight (g) 2480.52 1420.83 Voluem (mt) 3500 4065 Sample Temp Leach Pressure Conditions in Reactor Cu Co S Number (°C) Time (kPaG) Mass Volume Residue Liquor Extraction Residue Liquor Extraction Residue Liquor Extraction (hours) (g) (mt) (%) gl/ (%) g/l g/l (%) (%) g/l (%) Alloy SBL0 171 0 1000 2480.5 3500 14.9 2.85 4.78 Alloy SBL1 167 1 1000 2303.9 3594.2 1.54 66.5 90.40 0.57 11.9 81.4 1.42 72.4 Alloy SBL3 173 3 1000 2127.3 3688.4 1.33 61.5 92.3 0.43 11.8 87.1 1.22 78.1 Alloy SBL5 172 5 1000 1950.7 3782 1.62 55.6 91.5 0.4 11 89 1.42 76.6 Alloy SBL6 172 6 1000 1774.1 3876.8 62.8 11.9 Alloy SBL7 170 7 1000 1597.5 3971 60 11.9 Alloy SBL8 8 1000 1420.6 4065 1.18 58.9 95.5 02.4 11.6 95.2 1.23 85.2 Alloy SBL9(2LWash) 9.52 1.85 Analysis: Mn Zn Ni Fe Sm Se Te Sample Number ppm ppm ppm g/l (%) (%) Alloy SBL1 57.3 Alloy SBL3 58.6 alloy SBL5 58.9 Alloy SBL8 19 17 88 1.13 60.4 0.52 <0.2 <0.2 Basis of Extraction: Solid over Solid for Co,Cu& S.<BR> <P>Extractions.xisAV TABLE 23 - BATCHLEACH LOGSHEET FOR FIRST LEACH OF EXAMPLE 9<BR> Cllent<BR> Leach Test Number Alloy 9A<BR> Date 99/02/17 Type Units Detalle Sample Numb Resldue Fead (g) Waler (wash) Alloy 7BL8 (mt) 1900 Combined la make Ar Residue Dryness (%) Liquor Alloy 7BL7 (mt) 1600 Free Aeid = 17.@ Residue Size (µ) Reagent 1 Alloy (gms) 1800 Alloy Ro Sample Number - Reagent 2 H2O (mt) 800 Atmosphere Type Gas O2 Reagent 3 Sample Vol. (mt) 200 Opetator Anton Sample Number Time Temp pH E" Preseure Vent Down Reagent 1 Reagent 2 Resgent 3 Residue Mass Remarks/Observ@ Actual Test(min) (°C) (kPaG) (Y/N) (gms) (mt) (mt) (gms) LIQ 14:20 0 115 1.42 511 500 N 50 50 14.35 15 146 1.78 423 500 Y 50 50 14:50 30 147 2.16 339 500 Y 200 50 Alloy DAL1 15:20 60 150 2.94 296 500 Y 200 50 50 (W)13.68 (L)Dsep Purple 15:50 90 80 3.14 283 500 Y 50 50 (D)8.45 (R)Dark Red 16:20 120 81 0.43 327 500 Y 50 50 16:50 150 82 3.44 328 500 Y 50 50 Alloy BAL3 17:20 180 83 3.69 286 500 Y 150 50 50 (W)28.98 (L)Light Purple 17:40 200 81 3.79 248 500 Y 100 50 (D)19.10 (R)Dark Red 18:00 220 83 3.91 148 500 Y 100 50 18:20 240 82 4.34 180 500 Y 200 50 18:40 260 81 4.48 181 500 Y 100 50 Alloy SAL5 19:00 260 83 4.87 166 500 Y 200 50 50 (w)31.62 (L)Dark Pink 19:20 300 82 4.81 158 600 Y 100 50 (D)23.62 (R)Dark Red 19:40 320 63 4.77 119 500 Y 100 50 20:00 340 81 4.82 109 500 Y 100 50 Alloy 9Al6 20:20 360 82 5.08 89 500 Y 50 (W)32.70 (L) Dark Pink (D)23.68 (R)Dark Red 1600 400 200 Total Dry=76.1 Details Sample No Colour General Final Fitraie Voluem (mt) 3230 Allay 9 A17 Dark Pink Combined final fitrale and wash prior to sampling Finel wash Volume (mt) 400 At 15:25 cool down cleve to 80°C Final Residue Mass-Wet (gms) 3320.11 Alloy 9AR7 Dark Red 74% Drynesss on final cacke going to B Leach Final Residue Mass Dry (gms) 2470.93 + 78.18 = 2547.06 Feed Liquor free acid = 17.64 g/t TABLES Alloy-6A-10B.xl@ Table 24 - Test Extraction Data for First Leach of Example 9<BR> Cllent<BR> Leach Test Number Alloy 9A<BR> Date 99/02/17 Start End. Residue Weight (g) 180 2547.06 Volume (ml) 3500 3630 Sample Temp Leach Pressure Conditions in Reactor Cu Co S Number (°C) Time (kPsG) mass Volume Residue Liquor Extrsction Residue Liquor Extrateion Residue Liquor Extraction (hours) (g) (ml) (%) g/l (%) (%) g/l (%) (%) g/l (%) Alloy 9A LO 115 0 500 1800 3500 20.5 25.3 6.67 9.73 5.37 Alloy 9A L1 150 1 500 1849.4 3526 13.3 24.2 -0.89 0.38 16.8 94.1 4.42 15.5 Alloy 9A L3 83 3 500 1998.6 3552 16 8.07 -16.2 0.44 17.1 92.7 5.07 -4.65 Alloy 9A L5 83 5 500 2146.2 3578 16.2 0.57 -23.5 1.4 19.1 74.96 4.5 0 Alloy 9A L6 82 6 500 2297.6 3604 15.2 90ppm -23.9 2.29 16.4 56.2 4.51 -7.1 Alloy 9A L7 7 500 2547.1 3630 14.1 53ppm -24 2.43 16.7 46.4 4.54 -19.5 Analysis: Mn Zn NI Fe Cd Pb S= Sample Number ppm ppm ppm ppm (%) ppm ppm (%) Alloy 9A L1 9.1 47.5 Alloy 9A L3 8.1 40.8 Alloy 9A L5 0.29 43.6 Alloy 9A L6 ND 42.9 Alloy 9A L7 277 ND 31 25 42.8 <0.32 <7.0 2.46 Basis of Extraction : Solid over Solid for Co & S.<BR> <P>Liquid over Soild for Cu.<BR> <P>ND=Not Delected.<BR> <P>Extractions.xisAV9A TABLE 25- BATCH LEACH LOGSHEET FOR SECOND LEACH OF EXAMPLE 9 Cllemt Lesch Test Number Alloy 98 Date 99/02/18 Typs Units Detalls Semple Number Resldue Faed (g) 2471.93 Water H2O (mt) 700 Cambined le make Alloy S Residue Drynese (%) Dry Liqueor Alloy 78 LT (mt) 2800 F/A=33.32 g/l Residue Site (µ) As Recalved Resgant 1 h2SO4 (Sog g/l) (m/t) 490 Sampie Number - Alloy 9A Reagent2 H2O (mt) 400 Atmosphenre Type Gas O2 Reagent3 Liq Sample (mt) 300 Sample Number Time Temp Ptf EM Pressurs Vsnt Dewn Resgents 1 Reaent 2 Rsegent 3 Residue Mawse Remsrks/Observatfae Actual Test (min) (°C) (kPaG) (Y/N) (mt) (mt) (mt) (gma) LI@ 09:10 0 181 2.50 251 1000 Y 50 09:40 30 160 2.05 265 1000 Y 200 100 Alloy 9B L1 10:10 60 161 1.49 400 1000 Y 230 50 (w)31.38 (L)Green/Black 10:40 90 161 1.44 446 1000 Y (D)22.94 (R) red Brown 11:10 120 160 1.41 423 1000 Y 11:40 150 160 1.46 446 1000 Y 5 100 Alloy 9B L3 12:10 180 180 1.42 442 1000 Y 50 50 (w)41.33 (L) Drak Purle 12:40 210 161 1.41 457 1000 Y 50 (D)29.18 (R) Red Brown 13:10 240 160 1.44 451 1000 Y 5 13:40 270 161 1.42 449 1000 Y Alloy 9B L5 14:10 300 180 1.41 392 1000 Y 50 (w)36.52 (L) Dark Purpla 14:40 330 160 1.41 387 1000 Y (D) 25.83 (R) Red Brown Alloy 9B L6 15:10 360 161 140 410 1000 Y 50 (w)31.41 (L) Dark Purple 15:40 390 160 1.41 417 1000 Y 100 (D)22.44 (R) Red Brown Alloy 9B L7 16:10 420 181 1.41 438 1000 Y 50 (w)36.56 (L) Dark Purple Alloy SB L8 17:10 480 160 1.40 441 1000 Y 50 (W) 55.93 (L) Dark Purple (D)24.40 (R) Red Brown 490 400 300 Dotalle Sempla Ne Colour General Finel Firale Volume (mt) 4500 Alloy 8B L9 Dark Purple Repufped caken In it water = Wash 2. Final Wash Volume (mt) 2000 Alloy 9B L10 Red Brown Wash 1 + 2 = Alloy 9B L/O. Kept separata 2000 ml. Final Residue Maess-Wet (gms) 176.447 Alloy 9B R9 Light Purple if Intue was Shorugh cake. it inskus was + Finket be slceirwinging. Final Residus Mass-Dry (gms) 1362.10 + 192.80 + 1488.70 (W) 16.06 (D) 12.07 Voluem of Lique of EV-4306 mt F/A -40.18 g/l 0.75% Drynas em Wet Cake<BR> TABLES AvAlloy-#A-108.xis Table 26 - Test Extraction Data for Second Leach of Example 9<BR> Client<BR> Leach Test Number Alloy 9B<BR> Date 99/02/18 Start End Residue Weight (g) 2471.93 1468.7 Voluem (mt) 3500 4500 Sample Temp Leach Pressure Canditions in Resctor Cu Co S Number (°C) Time (kPaG) Mass Volume Residue Liquor Extraction Residue Liquor Extraction Residue Liquor Extrac (hours) (g) (mt) (%) g/l (%) (%) g/l (%) (%) g/l (%) Alloy 9B L0 161 0 1000 2471.9 3500 14.1 21.3 2.43 11.1 4.54 Alloy 9B L3 160 3 1000 2144.1 3833.3 1.95 89.2 88.3 0.13 20.5 95.4 1.46 72. Alloy 9B L5 160 5 1000 1816.4 4166.6 1.95 87.7 90.1 0.18 20.7 96.4 1.58 74. Alloy 9B L9 9 1000 1488.7 4500 1.9 76.1 92 0.13 17.9 96.8 1.61 78. Alloy 9B L 10 (2LWash) 10 1000 17.5 4.07 Analysls: Mn Zn NI Fe Se Se Te Sample Number ppm ppm ppm ppm (%) (%) Alloy 9B L0 7.8 895 Alloy 9A L3 13 58.6 Alloy 9A L5 13 59.3 Alloy 9A L9 235 3.3 131.0 602.0 58.5 0.29 <0.2 <0.2 Basis of Extraction: Solld over Solid for Co. Cu & S.<BR> <P>Extractions. xis TABLE 27-BATCH LEACH LOGSHEET FOR FIRST LEACH Or EXAMPLE 10 Cllemt Lesch Test Number Alloy 10A Date 99/02/19 Typs Units Detalls Semple Number Resldue Faed (g) Water(Wash) Alloy 9B L10 (mt) 2000 Combined to maks Allay 10B L0 Residue Drynese (%) Free ACid = 18.7 g/l Residue Site (µ) Liquor (SE) Alloy 9BL9 (mt) 1500 Alloy RO Sampie Number - Rasgent 1 Alloy (gms) 2800 Atmosphenre Type Gas O2 Reagent2 Water (mt) 750 Oparator Anton Sample Number Time Tsmp pH EM Pressure Vent Dawn Resgent 1 Resgent2 Sample Vel. Residue Mases Remarha/Observatlo Actual Test (min) (°C) (kPaG) (Y/N) (mt) (mt) (mt) Dry(gms) LI@ 12H45 0 134 1.03 341 600 Y 100 13H00 15 140 2.12 293 600 Y 200 100 13H15 30 141.0 2.82 200 600 Y 400 100 13H30 45 141.0 3.08 55 800 Y 300 50 Alloy 10AL1 13H45 60 141.0 5.38 96 600 Y 200 40 dj 30.97 (L)DARK PINK 14H00 75 140.0 3.6 57 600 Y 200 50 (R)DARK BROWN 14H50 105 140 4.18 48 600 Y 200 50 Alloy 10AL2 14H45 120 141 4.14 57 600 Y 200 60 25 d) 38.47 (L)DARK PINK 15H00 135 140 4.36 82 600 Y 200 50 (R)DARK BROWN/RED. 15H15 150 141 4.45 71 600 Y 200 50 15H30 165 140 4.38 75 600 Y 100 Alloy 1DAL3 15H45 180 140 4.01 100 600 Y 200 50 40 d) 82.76 (L)DARK PINK 16H00 195 141 3.84 82 600 Y 200 50 (R)DARK BROWN/RED. PH of Fit/ats=4.43 2800 750 105 132.2 Dotalle Sempla Ne Colour General Finel Firale Volume (mt) 2680 Alloy 10AL4 OARKPINK COMBINED FINAL FIL TRATE+WASH PRIOR TO SAMPLNG. Final Wash Volume (mt) 400 FA In SE Llq=40.18 g/l Final Residue Maess-Wet (g) 4982.51 Alloy 10AR4 DARK BROWN/REO. Cate=20% Meisture. Final Residus Mass-Dry (g) 3986+151.78= 4137.78 TABLES Beteh - Filtrshon - 5. A108. sisA Table 28 - Test Extraction Data forFirst Leach of Example 10<BR> Client<BR> Leach Test Number Alloy 10A<BR> Date 99/02/19 Start End Residue Weight (g) 2800 4137.78 Voluem (mt) 3500 3080 Sample Temp Leach Pressure Canditions in Resctor Cu Co S Number (°C) Time (kPaG) Mass Volume Residue Liquor Extraction Residue Liquor Extraction Residue Liquor Extraction (hours) (g) (mt) (%) g/l (%) (%) g/l (%) (%) g/l (%) Alloy 10A L0 134 0 600 2800 3500 20.5 24.5 6.67 6.69 Alloy 10A L1 141 1 600 3135.1 3395 15.6 1.41 -6.68 1.26 66.9 94.91 5.11 -6.5 Alloy 10A L2 141 2 600 3469.3 3290 13.6 0.69 -8.2 2.59 12.2 81.42 4.91 -13.3 Alloy 10A L3 140 3 600 3803.55 3185 13.1 0.6 -8.4 2.74 13.1 44.2 4.6 -16.4 Alloy 10A L4 4 600 4137.8 3080 14.3 1.15 -7.4 2.99 13.6 33.7 4.56 -25.5 Analysls: Mn Zn NI Fe Cd Pb S= Sample Number ppm ppm ppm ppm (%) ppm ppm (%) Alloy 10A L1 42.2 Alloy 10A L2 41.5 Alloy 10A L3 41.6 Alloy 10A L4 59 1.1 51 18 41 <0.32 1.98 Basis of Extraction: Solld over Solid for Co. Cu & S.<BR> <P>Liquid over Solid for Cu<BR> Extractions.

TABLE 29-BATCH LEACH LOGSHEET FOR SECOND LEACH OF EXAMPLE 10 Cilent Lesch Test Number Alloy 10B Date 99/02/22 Type Unlls Delzlls Sample Number Resldus Food (g) Water DIW (ml) 3200 Combined to make Aloy I Resldue Dryness (%) Dry Llquor Aloy 98 L@ (ml) 2800 Rasldus Size (µ) As Recelved $esgenl 1 H2SO4 (SOO g/l) (ml) 1320 Sample Number - Alloy 100 R4 Resgenl 2 H2O (ml) 1100 Atmosphare Type Gas O1 Reagenl 3 (ml) Operstor Anion Sample Number Time Temp pH EN Pressure Vont Down Reagenl 1 Resgenl 2 Sample Vol. Residue Mass Remarks/Observation Actual Test (min) (°C) (kPaG) (Y/N) (ml) (ml) (ml) (gms) LIQ 10:10 0 159 2.93 249 1000 Y Colours of Lig & Solld 10:40 30 160 1.67 360 1000 Y 1100 200 Alloy 10B L1 11:10 60 161 1.52 402 1000 Y 120 200 100 (W)33.27 (L) Darh Purple 11:40 90 160 1.44 420 1000 Y 40 200 (D)27.30 (S)Dark Red/Brown 12:10 120 160 1.43 425 1000 Y 60 200 12:40 150 160 1.40 394 1000 Y 100 Alloy 10B L3 13:10 180 161 1.41 417 1000 Y 100 (W)39.20 (L) Dark Purple 13:40 210 160 1.41 413 1000 Y 100 (D)28.88 (S) Dark Red/Brown 14:10 240 160 1.42 431 1000 Y 14:40 270 161 1.42 444 1000 Y 100 Alloy 10B L5 15:10 300 160 1.41 441 1000 Y 100 (W)42 52 (L) Dark Purpls (D)36.95 (S) Dark Red/Brown R6= (W)32.60 (D)28.72 1320 1100 300 Tolal Dry Weight 119.85 Delalis Sample No Colour Gensral Final Flinate Volume (ml) 8050 Alloy 10B L6 Dark Purple Took 2f and repuped both cakes in two @@ars = Wash 1. look 21 repulped both cakes in two filters - Wash 2. Final Wash Volume (ml) 3520 Alloy 10B L7 Purple Wash 1 & Wash 2 combined and kepl 3520 ml. Put it through each cake and kept as Insitus wash. Final Residue Mass-Wei (gms) 2799.78 Alloy 10B R6 Dark Brown/Rad Volume of in sihus = 1990 ml. Final Residue Mass-Dry 2295.82 + 2415.87 (W)16.06 (D) 12.07 0.82% Dryne@@ in Final Cak@<BR> TABLES AvAlloy#6A-10B.xlsA.

Table 30-Test Extraction Data for Second Leach of Example 10<BR> Client<BR> Leach Test Number Alloy 10B<BR> Date 99/02/22 Start End Resldue Weight (g) 3986 2415.67 Volume (ml) 6000 8050 Sample Temp Leach Pressure Conditions in Reactor Cu Co S Number (°C) Time (kPaG) Mass Volume Resldue Liquor Extraction Residue Liquor Extraction Residue Liquor Extraction (hours) (g) (ml) (%) g/l (%) (%) g/l (%) (%) g/l (%) Alloy 10B L0 159 0 1000 3986 6000 14.3 15.7 2.99 7.2 Alloy 10B L1 161 1 1000 3593 6513 1.64 85.5 89.60 0.79 22.3 76.2 1.75 65.4 Alloy 10B L3 161 3 1000 3200.8 7025 1.39 80.6 92.3 0.67 20.7 82 1.6 71.8 Alloy 10B L5 160 5 1000 2808.2 7537.5 1.28 77.2 93.7 0.58 20.6 86.3 1.46 77.4 Alloy 10B L6 6 1000 2415.7 8050 1.25 70.1 94.7 0.58 18.4 88.3 1.58 78.9 Alloy 10B L7(21 wash) 7 1000 10.3 2.82 Analysis: Mn Zn Ni Fe S@ Se Te Sampel Number ppm ppm ppm g/l (%) (%) Alloy 10B L1 56.4 Alloy 10B L3 57.4 Alloy 10B L5 58.4 Alloy 10B L6 102 12 120 2.22 58.4 0.4 <0.2 <0.2 Basis of Extraction: Soild over Solld for Co.Cu&S.<BR> <P>Exiractions.xlsAV1 TABLE 31-BATHCLEACH LOGSHEET FOR FIRST LEACH FO EXAMPLE 16<BR> Cilent<BR> Losch Test Number Alloy 16A<BR> Date 99/01/13 Residue Feed (g) 2400 Type Units Detalis Sample Mr Residus Dryness (%) DRY Water (ml) Residue Size (µ) as recalved Liquor SYNTHETIC (ml) 3500 16 LO Sample Number # Reagent 1 ALLOY (gms) 2400 Atmosphere Type Gas O2 Reagent 2 WATER (ml) 500 Operator A.BOTHA Reagent 3 (gms) Sampls Number Time Temp pH EM Pressure Vent Down Reagent 1 H2O Filtrate Vol. Reslude Mass Remaris/Obs Actuzl Test (min) (°C) (kPsG) (Y/N) (ml) (ml) (gms) 07:00 0 79 1.01 443 500 Y 400 Cooling to Pot 15 88 2.60 301 500 Y 500 50 (D)9.84 Extemal 16 L1 07:30 30 85 3.10 330 500 Y 500 100 (D)16.11 16 L2 08:00 60 87 3.95 279 500 Y 500 200 50 (D)31.91 Valve dogged 16 L3 09:45 105 80 3.84 250 500 Y 200 50 (D)29.8 ~ 200 ml soid lost 16 L4 10:15 135 79 4.48 219 500 Y 300 100 50 (D)35.5 16 L5 10:50 170 85 4.93 159 500 Y 100 50 F@trate 20 5.20 247 Filtrate pH = 5.2 Red in coulour Total Dry 200 gms of feed lost ( 2200 500 250 123.22 Detalis Sample Number Colour General Final Filbaie Volume (ml) 2200 16 FINAL Raspberry Red Final Wash Volume (ml) 3040 18 FINAL Respberry Red Synthetic Liquor@Cu=16.8 g/l Co=10 g/l. Free Acld=40 g/l Final Residue Mass-Wet (gms) 3796.78 16 FINAL Dark Red Final Residue Mass-Dry (gms) 2834.45 16 FINAL Dark Red Table 32-Test Extraction Data for First Leach of Example 16<BR> Cllent<BR> Leach Test Number 16A<BR> Date 99/01/13 Start End Residue Weight (g) 2200 2834.45 Volume (ml) 3500 2200 Sample Leach Time Temperature Pressure Conditions in Reactor Cu Co Number (hours) (°C) (kPaG) Mass (g) Volume (mL) Residue Liquor Extraction Residue Liquor Extractic (5) (g/l) (%) (%) (g/l) (%) 16 L0 0 79 500 2200 3500 21.6 16.9 0.0 7.1 10.2 0.0 15 86 500 2562 3403 16 L1 30 85 500 2935 3405 15.9 6.7 -7.6 2.96 22.2 44.4 16 L2 30 87 500 3435 3605 15.8 4.98 -8.7 2.68 27.4 41.1 16 L3 135 80 500 2708 2923 16.8 3.33 -10.4 0.94 28.0 83.7 16 L4 165 79 500 2743 2828 16.7 0.81 -12.0 1.32 31.9 76.8 16 L5 200 85 500 2834 2700 15.8 0.35 -12.2 1.71 27.0 68.97 Basis of Extraction: Liquid over Solid for CU Head Cu 21.80% Sample 16LO Lixiviant g/l Cu 16.9 g/l<BR> Solid over Solid for CO Co 7.10% Co 10.2 g/l<BR> Fe 73 ppm<BR> TABLE 16A.xlsE TABLE 33-BATCH LEACH LOGSHEET FOR SECOND LEACH OF EXAMPLE 16<BR> Client<BR> Leach Test No 16B<BR> Date 99/01/15 Residus Feed (g) 1708 Type Units Detslis Sample Number Residue Dryness (%) Dry Water (ml) 3000 Residue Size (µ) As received Liquor (ml) Sample Number @ AV 18 RS ex lest AV 18A Reagant 1 500 g/l H2SO4 (ml) 160 Atmosphere Type Gas Reagent 2 (ml) Operator Reagent 3 (gms) Sample Number Time Tamp pH EM Pressure Vant Down Reagent 1 H2O Filtrate Vol. Residue Mass Remarks/Observstions Actual Test (min) (°C) (KPaG) (Y/N) (ml) (ml) (ml) (gms) 10:00 0 173 2.68 253 1000 Y 100 16B L0 15 165 2.68 247 1000 Y 50 (D) 12.78 H2S SMELL COMING OFF THE 30 159 1.64 348 1100 Y 16B L1 11:00 60 172 1.40 350 1100 Y 90 160 1.35 356 1100 Y (D) 13.35 HIGHLY EXOTHERMIC 12:00 12 170 1.45 382 1100 Y 12:30 150 150 0.15 372 1100 Y 16B L2 13:00 180 170 1.51 375 1100 Y (D) 22.26 13:30 210 171 1.52 268 1100 Y 14:00 240 172 1.51 362 1100 Y 14:30 270 172 1.48 359 1100 Y 15:00 300 172 1.47 375 1100 Y 15:30 330 172 1.50 382 1100 Y 16B L3 16:00 360 171 1.48 358 1100 Y (D) 19.6 EH DROP 16:30 390 172 1.58 358 1100 Y 17:30 450 172 1.61 355 1200 Y 1200 AIR PRESSURE 16B L4 18:00 480 172 1.64 1200 Y (D) 14.11 19:00 540 177 1.55 352 1200 Y 19:30 570 172 1.64 343 1200 Y 20:00 600 1.60 348 (D)9.5 150 TOTAL 91.62 Dry Sample Details Sample No Colour General Final Filtrate Volume (ml) 4400 16B L5 BLUE ComBINED WASH + FILTRATE PRIOR TO SAMPLING Final Wash Volume (ml) 400 16B L5 BLUE USED 60% OF TEST 16A RESIOUE AS FEED TO TEST 16B Final Residue Mass-Wet (gms) 1484.70 16B R5 Final Residue Mass-Dry 1043.2 16B R5 FINAL SOLID SAMPLE WEIGHT 0.50 TABLES @@@ @@@@.

Table 34-Test Extraction Data for Second Leach of Example 16<BR> Client<BR> Leach Test Number 16 B<BR> Date 99/01/15 Start End Residue Weight (g) 1708 1125.32 Volume (ml) 3000 4400 Sample Leach Time Temperature Pressure Conditions in Reactor Cu Co Number (hours) (°C) (kPaG) Mass (g) Volume (mL) Residue Liquor Extraction Residue Liquor (%) (g/l) (%) (%) (g/l) 16 L0 0 165 1000 1708 3000 15.8 0 0.0 1.71 0 16 L1 60 172 1100 1650 3140 2.33 71.4 85.8 0.26 7.2 16 L2 180 170 1100 1533 3420 4.51 70.8 74.4 0.41 7.6 16 L3 360 171 1100 1358 3840 4.36 71.3 78.1 0.37 7.6 16 L4 480 172 1200 1242 4120 3.84 62.7 82.3 0.31 6.8 16 L5 600 170 1200 1125 4400 1.55 47.8 93.5 0.09 5.2 Basis for Extraction: Solid over Solid for Cu and Co<BR> table 16BExtraction.xlsEx