Centro de Tecnologia Mineral Ministrio da Cincia e Tecnologia Coordenao de Processos Metalrgicos e Ambientais

EXTRACCIN DE COBRE A PARTIR DEL PROCESO DE BIOLIXIVIACIN DE CONCENTRADOS DE FLOTACIN DE SULFUROS DE COBRE

CETEM: Luis Gonzaga S. Sobral Renata de Barros Lima Priscila Gonalves Xavier Dbora Monteiro de Oliveira Judith L.S. Lemos Gabriela S.F. Pereira Mariana S. Paula UFRJ Selma G.F. Leite. Caraba Minerao Paulo Medeiros

CT2007-013-00 Contribuio Tcnica elaborada para o HydroCopper IV congreso Internacional de Hidrometalurgia do Cobre realizado no Chile de 16 a 18 de Maio.

MAIO/2007

COPPER EXTRACTION BY BIO-LEACHING OF FLOTATION COPPER SULPHIDE CONCENTRATES

Renata B. Lima, Luis G.S. Sobral, Debora M. Oliveira, Priscila G. Xavier, Judith L.S. Lemos, G.S.F. Pereira and Mariana S. Paula. CETEM Centro de Tecnologia Mineral, BRAZIL. S.G.F. Leite. UFRJ Universidade Federal do Rio de Janeiro, BRAZIL. P. Medeiros. Caraba Minerao, BRAZIL.

ABSTRACT
The bio-assisted leaching of flotation concentrate, produced in a copper mining in Brazil, was initiate with the use of micro-organisms present in the acid mining drainage collected directly in the aforementioned copper mine, besides an strain of Acidithiobacillus ferrooxidans bacteria. That strain came from a primary copper ore of Surubim mine in Bahia state. The concentrate under consideration, after being technologically characterized, was constituted, mainly, of chalcopyrite (CuFeS2) and bornite (Cu5FeS4) at 70 and 30%, respectively. The high chalcopyrite content in this refractory concentrate caused a huge difficulty of extracting copper from such sulphide using only the above-mentioned microorganism, which was verified, once getting the analytical results for copper, ferrous and ferric ions concentrations and monitoring the pH and Eh values, along the bioleaching tests, as being due to no sulphuric acid generation, when such mineral is solubilized, demanding a constant monitoring of those parameters to avoid, mainly, the pH rising, which otherwise would cause the precipitation of iron salts (hydroxides and jarosite). That phenomenon was verified, in some tests, due, certainly, to a sudden pH rising and confirmed, through X-ray diffraction analysis, as being a jarosite precipitate, which contains, in its composition, ferric ions decreasing, in a detrimental way, the oxidizing power of reaction system. Independent of these inconveniences, bearing in mind the operational adjustments, a copper extraction of nearly 67% was reached within 62 days.

EXTRACCIN DE COBRE A PARTIR DEL PROCESO DE BIOLIXIVIACIN DE CONCENTRADOS DE FLOTACIN DE SULFUROS DE COBRE RESUMEN La bio-lixiviacin del concentrado de flotacin producido en las instalaciones de la Empresa Minera Caraba, comenz con la utilizacin de los microorganismos presentes en el agua cida de mina colectada directamente de la mina de cobre de Caraba, junto con una cepa de bacterias de la especie Acidithiobacillus ferrooxidans. Esta cepa se extrajo de un depsito primario de minerales de cobre de la mina Surubim, estado de Baha, perteneciente a la misma empresa. El concentrado en cuestin, despus de ser caracterizado mineralgicamente, estaba compuesto principalmente de calcopirita (CuFeS2) y bornita (Cu5FeS4), en concentraciones de aproximadamente 70 y 30%, respectivamente. El alto contenido de calcopirita en el concentrado provoc, debido a su alta refractariedad, una gran dificultad en la extraccin de cobre, utilizando solamente los microorganismos antes

mencionados. Esto fue constatado despus de los resultados analticos de las concentraciones de cobre, ferroso y frrico, y de la medicin de los valores de pH y Eh, a lo largo de los ensayos de bio-lixiviacin. No se observ generacin de cido sulfrico durante la solubilizacin del concentrado, lo que exigi un monitoreo constante de los parmetros de proceso antes mencionados, con el objetivo de evitar, principalmente, la elevacin de pH, lo que provocara la precipitacin de sales de hierro (hidrxidos y jarositas). Este fenmeno fue constatado en algunos ensayos, donde se observ una elevacin sbita de pH, junto con la formacin de precipitado de jarosita, lo que fue confirmado por anlisis de difraccin de rayos X. Puesto que la jarosita atrapa iones frrico, la precipitacin de este compuesto reduce el poder oxidante de la solucin. A pesar de los inconvenientes antes mencionados, y efectuando los debidos ajustes operacionales, se logr una extraccin de cobre del orden de 67%, en un periodo de 62 das de operacin. INTRODUCTION
The copper production from flotation concentrate follows conventional technological route as a function of mineralogical species that compose such concentrate. In the case of flotao concentrate, the copper sulphides are converted into blister copper (impure metallic copper) after using previous pirometallurgical unit processes, through flash smelting process and electrolytically refined afterwards. Although the pyrometallurgical process presents the advantage of transforming different copper sulphides of those concentrates into metallic copper, it presents, otherwise, inconveniences of generating sulphur dioxide (SO2) together with heavy metals issues, as cadmium, arsenic, mercury, bismuth, selenium etc. The hydrometallurgical treatment of such concentrate, more precisely the bio-leaching, is being considered as a quite attractive process with respect to the mild process conditions (room temperature) and for obtaining acid liquor containing the metal of interest.

OBJECTIVE
The present work aimed at analysing the technical viability of copper extraction by bio-leaching a flotation concentrate containing chalcopyrite (CuFeS2) and bornite (Cu5FeS4), from the mineral processing unit of Caraba Mining.

LITERATURE SURVEY
The bio-leaching, or bio-assisted leaching, can be defined as a natural dissolution process of sulphide minerals, as a result of the oxidation of those minerals through bacteria releasing the metals of interest in their soluble ionic forms (Rojas, 1998). What turns the bio-leaching technique a very interesting alternative, in replacing the conventional processes, is the capacity of certain bacteria oxidizing iron or sulphur, as the ones of Acidithiobacillus and Leptospirillum kind, growing in highly acids atmospheres and in presence of heavy metals. Besides, if we compare the costs of the bio-leaching process with the costs for operating a conventional plant, it is possible a reduction of up to 50% (Gibbs et al, 1985).

Most of the studies accomplished at lab-scale considered that the metal extraction process was only reached with the use of bacteria of Acidithiobacillus ferrooxidans species. However, those experiences did not correspond to the natural situation and, during the last years, other microorganisms, involved in the leaching process, were discovered and characterized (Leptospirillum ferrooxidans, Acidithiobacillus thiooxidans, thermophilic, anaerobic and heterothrophic bacteria) (Norris, 1990). The bio-leaching, as any other process that uses living microorganisms, is influenced by environmental, biological and physiochemical factors; as such parameters affect the metal extraction (Torma, 1977; Lundgren and Silver, 1980). It is necessary to begin the bio-leaching process in optimal experimental conditions of humidity, pH, temperature, sources of energy and nutrients, as well as the absence of possible inhibitors that can affect the growth of the microorganisms. Besides, it should be taken into account the physiochemical conditions of the system, as for instance: the ore particle size, access of oxygen and humidity for the surface of the ore, acid consumption, and presence of susceptible sulphide to the bacterial oxidation and the possible elimination and precipitation of ferric ions. Examples of metals that can be extracted through bio-leaching are the copper, from chalcopyrite (CuFeS2), bornite (Cu5FeS4) or covellite (CuS), uranium through the uranite (UO2) and gold in an arsenopirite matrix (FeAsS). Chalcopyrite: Covellite: Uranite: Arsenopirite

4CuFeS 2 + 17O2 + 2 H 2 SO4 4CuSO4 + 2 Fe2 (SO4 )3 + 2 H 2 O

(1) (2) (3) (4)

CuS + 2O2 CuSO4

2+ UO2 + 2 Fe 3+ UO2 + 2 Fe 2+

2 FeAsS + 7O2 + 2 H 2 O 2 FeAsO4 + 2 H 2 SO4

Characteristics of the Microorganisms Involved in the Bio-leaching

Acidithiobacillus ferrooxidans: The bacteria have been active in the dissolution of copper sulphides in the commercial extraction of that element since 1670. The fundamental role of those bacteria, in the leaching of sulphide minerals, has been demonstrated (Colmer & Hinkle, 1947; Temple & Colmer, 1951) and the A. ferrooxidans strain shows to be the most promising in the dissolution of those sulphides, being those bacteria found, more commonly, in acid mining water. Those species can use as source of energy, besides the ferrous ion, sulphur (sulphur compounds), as can be seen in the following equations (Suzuki, 2001):

2 Fe 2+ + 1 2 O2 + 2 H + 2 Fe 3+ + H 2 O
2 S o + 4 H 2O SO4 + 6e + 8H +

(5) (6)

The bacteria of the A. ferrooxidans species are unicellular organisms, quimiosintetizers, autothrophics, gram-negative and with stick format; some have flagellula, and possess cell size from 0.3 to 0.5 m of diameter and 1.0 to 1.7 m of length (Brewis, 1996; Domic, 2001). The A. ferrooxidans species grows in the pH range of 1.0 to 6.0, being the optimal pH range, to reach the maximum growth speed, of 2.0 to 2.5. In a similar way, it survives in a temperature range of 2 to 40C, but the one from 28 to 35C is more favourable. While the A. ferrooxidans grows in low pH, its internal cytoplasmatic pH is close to the neutrality, and the pH gradient through its cytoplasmatic membrane is one of the largest of all organisms (Brewis, 1996).
Bio-leaching Mechanism It is well known that the temperature, stirring speed, particle size (surface area), acidity, nutrients and addictive affect the dissolution rate of the sulphide minerals through microorganisms. There are two mechanisms involved in the bacterial attack of those sulphides: the direct and indirect attack. In the direct mechanism, the bacterium acts directly in the sulphide mineral. In the indirect mechanism, the bacterium converts, simply, Fe2+ to Fe3+ and elemental sulphur into sulphate, while the Fe3+ ions act directly in the oxidation of the sulphide minerals (Smith & Misra, 1991).

Figure 1 Bio-leaching mechanisms: Direct and indirect ones (Smith & Misra, 1991)

EXPERIMENTAL Flotation Concentrate

The sulphide concentrate used in the experiments is the result of the copper sulphide flotation process from a primary ore (underground mining). The copper sulphide flotation concentrate under study contains about 30% of bornite (Cu5FeS4) and 70% of chalcopyrite (CuFeS2). The particle size analysis was made by wet sieving, using standardized sieves of the Tyler series (0.106 to 0.043 mm).

T & K Culture Medium

For the propagation of the microbial inoculum, the T&K culture medium was used, developed by Tuovinen & Kelly (1973), with small modifications (Monteiro 1998). This medium is specific for

the A. ferrooxidans species cultivation. The aforementioned medium is composed by two solutions (A and B), whose compositions can be seen in the Tables 1 and 2.

Table 1 Nutrients solution composition of T&K medium

Solution A (NH4)2SO4 K2HPO4 MgSO4*7H2O 0.625 g/L 0.625 g/L 0.625 g/L

Table 2 Ferrous Sulphate solution composition of the T&K medium

Solution B FeSO4*7H2O 166.5 g/L

For preparing the T&K culture medium, the A and B solutions were prepared, acidified with H2SO4 10N up to pH 1.8 and sterilized separately. The salts solution (solution A) was sterilized in autoclave, at 120C, for 20 minutes, while the ferrous sulphate solution (solution B) was filtered in Millipore membrane (0.45m). The finalization of the culture medium preparation consisted of the mixture of A and B solutions in a proportion of 4:1, respectively.

Leaching Experiments
For all those tests it was used as inoculum the pure culture of Acidithiobacillus ferrooxidans from the growth in T&K culture medium (10% v/v of microbial inoculum), for 48 hours at 30C and 150 rpm. Bio-leaching Tests Monitoring the Process Parameters Four tests were accomplished monitoring at this stage the process parameters, such as pH, being constantly adjusted for the range of 1.8 to 2.2, redox potential, Fe2+ and Fe3+ ionic species concentrations and copper extraction. The tests were kept under stirring at 150 rpm, at 30C for 62 days. Test 1 Test in T&K Culture medium without Fe2+ This test consisted of leaching the sulphide concentrate using T&K culture medium, without using Fe2+ salt (ferrous sulphate), in two different tests: one inoculated, where 10% v/v of microbial inoculum was used and, simultaneously, a control test, without microbial inoculum. The tests were carried out in agreement with the following parameters: Flotation concentrate: 50 g/L Solution A (nutrients) of T&K culture medium: 90 cm3 Microbial inoculum: 10% v/v Stirring speed: 150 rpm

In the control tests, the microbial inoculum was not added, being maintained the solid-liquid ratio (50 g/L), in other words, 90 cm3 of the A of the T&K culture medium, 10 cm3 of distilled water and 5g of flotation concentrate.

Test 2: Test with Completed T&K Culture Medium In that test, the flotation concentrate was leached with the completed T&K culture medium, in other words, containing the solutions A and B. It was accomplished an inoculated series and other without inoculum. The experimental conditions of that test are described as follows: Flotation concentrate: 50 g/L T&K culture medium: 90 cm3 Microbial inoculum: 10% v/v Stirring speed: 150 rpm

In the control tests, the microbial inoculum was not added, being maintained the same solid-liquid ratio (50 g/L), in other words, 90 cm3 of T&K culture medium, 10cm3 of distilled water and 5g of flotation concentrate. Test 3: Test with T&K Culture medium previously Oxidized These tests were carried out with the T&K medium, previously oxidized; in other words, the medium was inoculated (10% v/v), being this system stirred at 150 rpm for 2 days in incubator at 30C. Flotation concentrate: 50 g/L Oxidized T&K culture medium (as described before): 90 cm3 Microbial inoculum: 10 %v/v Stirring speed: 150 rpm

Test 4: Test in T&K culture medium previously oxidized without biomass For accomplishing this test, the oxidized culture medium was used, as previously described (item 4.4.1.3), followed by its filtration in a 0.22 m membrane, aiming at separating the bacterial cells of the system, as well as to use only Fe3+ as leaching agent supposing it has been generated biologically. The tests were carried out in agreement with the following experimental conditions: Flotation concentrate: 50 g/L Oxidized and filtrated T&K culture medium (as described before): 90 cm3 Stirring speed: 150 rpm

Analytical Determinations of Control Parameters

pH Maintenance For the maintenance of pH, in the range of 1.8 to 2.2, a sterile 10N H2SO4 solution was used. For measuring the pH, the electrode was previously sterilized (30 minutes of immersion in 5% v/v formaldehyde solution) and to avoid contamination of the samples, the measurements were always initiated by the "control" samples, as they didn't contain the microbial inoculum.

Redox Potential Eh measurement The redox potential measurement was carried out using a platinum electrode with Ag/AgCl electrode as reference; however, with the same precautions of the previous item as the sterilization of the electrode and the non contamination of the samples. The reaction between the sulphides and the ferric ions, in a sulphuric acid solution, was followed by monitoring the redox potential of the sulphide suspension in the mentioned acid solution. The cell representing the redox potential measurement is shown as followed: Pt | Fe3+ , Fe2+ || Cl- , AgCl | Ag Evaporation Control The flasks used in the bio-leaching tests were weighed every 3 days, for controlling the evaporation. Whenever necessary, the volume was readjusted using deionised sterile water. Analysis of Ferrous and Copper Ions Concentration (Fe2+ and Cu2+ ) The analysis of Fe2+ ions was accomplished immediately, still in the laboratory where the bioleaching tests were accomplished, so as to avoid any interference. On the other hand, the copper and total iron analyses were accomplished by Atomic Absorption spectrometry.

RESULTS DISCUSSION
According to the chemical analysis, the copper content of the flotation concentrate was of 37.3%, and the particle size analysis of that concentrate presented the following result: Table 3 Particle size analysis of the flotation concentrate.
Diameter Interval (# - mesh) 150 200 325 > 325 Particle Size (mm) 0.106 0.074 0.043 < 0.043 Ponderal Fraction kept (%) 10.7 23.0 27.6 38.7

Analysing the Table 3, one can observe that nearly 60% of the concentrate particles is equal or less than 325 mesh, what turns that concentrate more reactive, since as smaller the particle, the higher will be the reaction area, favouring the bio-leaching process. Bio-leaching Tests Using Pure Strains of A. ferrooxidans

The initial pH of the process was 1.8, as this is the pH value of the used culture medium. However, the Table below shows the pH values verified before adjusting it.

Table 4 Average of the initial solution pH on each sample before adjusting it in the range of 1.8 to 2.0.
Test
Test 1 Test 2 Test 3 Test 4 Sol. A + Ino + Conc Sol. A + Conc T&K + Ino + Conc T&K + Conc T&K Ino + Conc T&K Oxid. + Conc

Days
1 4.01 4.22 3.27 3.33 2.73 2.84 3 3.71 4.54 2.56 2.57 2.51 2.56 4 3.45 3.32 2.84 2.85 2.73 2.65 7 3.31 3.21 2.85 2.93 2.66 2.69 9 2.06 2.27 2.25 2.41 2.42 2.42 16 2.22 2.15 2.28 2.26 2.56 2.35 18 2.08 2.24 2.17 2.20 2.46 2.34 21 2.27 1.47 2.43 2.33 2.51 2.41 24 2.89 1.31 2,33 2.13 2.11 2.22 35 3.19 2.13 2.67 2.54 2.32 2.65 39 2.69 1.84 2.59 2.41 2.15 2.39 47 2.56 1.90 2.57 2.69 2.18 2.44 62 2.20 2.29 2.49 2.60 2.2 2.51

It is possible to evaluate that, in the first days of test; the pH of tests 1 and 2 suffered a significant increment, evidencing the importance of closely adjusting it in the first hours of test. However, as from the 9th day of leaching it can be verified that there was pH stabilization, preferentially in test 1, as it is nearly 2.2. This happened due to the acid consumption (according to equation 1), which is not that evident as in the beginning of the leaching process. In the results of test 1 (control), it was, still, observed that the pH drops down as from the 21st day, what can be related to a possible contamination of the system or, still, a decrease in the reaction speed. Such statement can be evaluated observing the potential values and other parameters that will be presented later on. The redox potential was monitored and its evolution can be observed in the Figure 2, below, where it is possible to verify that in the test 3, where the T&K medium is inoculated and completely oxidized, a larger Eh increase takes place in a shorter while, reaching values between 770mV and 800mV vs SHE, being the test 3 the more beneficiary with the cellular addition.
900

Sol. A + Ino + Conc

Sol. A + Conc
800

Eh (mv vs SHE)

T&K + Ino + Conc

T&K + Conc

700

T&K Oxid. + Conc

T&K Inoculado + Conc

600

500 1 9 21

Time (days)

35

39

47

62

Figure 2 Redox potential reading in mV vs. SHE. It is observed that as from the 24th day of leaching process, a significant increase in the redox potential in the test 3 takes place, evidencing a considerable increase in the oxidative process. It can be concluded that, from that period onward, the oxidative process is happening in a more intense way, probably, due to the microorganisms acclimatization. It is possible also to find out the redox potential difference in the inoculated systems and in their respective controls.

Evaluating the Figure 3 it is possible to observe that in the test 2 (inoculated) and in the test 3, the ferrous ion concentration drops down. This result was already expected, as the bacteria present in the system are acting on the flotation concentrate and aiding in the oxidation of ferrous to ferric ions. However, the Fe2+ concentration drop was not expected regarding the results of the test 1 (control), when, as from the 25th day, a significant increment of this concentration takes place, followed by a drop in the upper concentration in comparison with the same inoculated test, which configure a possible contamination of the system during the leaching process. It can be also observed that in the control tests, the Fe2+ did not change a great deal; however, in the control of test 2 and 4, both without microbial inoculum and with the complete T&K culture medium (with Fe2+), the Fe2+ concentration was the largest one obtained at the end of the bioleaching process, about 3 and 4 g/L, respectively.
6

Fe(II) g/L

So l. A + Ino + Co nc
3

So l. A + Co nc
T&K + Ino + Co nc
T&K + Co nc
T&K Oxid. + Co nc
T&K Ino culado + Co nc

0 1 9 17 25 39 46 62

Tim e (days )

Figure 3 Fe (II) concentration, in g/L, obtained as from the flotation concentrate leaching process. Bearing in mind the comparison between the ferrous and ferric ions concentrations, as shown in Figure 4, it is possible to conclude, that the Fe2+concentration decreases, while the Fe3+ one increases, (tests 2 and 3), evidencing the biological activity with respect to the oxidation of the flotation concentrate. At the end of the experiments, the Fe3+ concentration is decreasing and it is expected that the Fe2+ concentration increases; however, such behaviour is not observed. Evaluating the redox potential, it is noticed that it keeps on growing, which imply that the ferric ion is precipitating and not reducing, as expected. This precipitation of the ferric ion can takes place due to jarosite formation (K+, Na+, NH4+, H3O+) Fe3(SO4)2 (OH)6. (Mascarin, 1999).

6.00 5.00

4.00

g/L

3.00 2.00

Teste 2 Ino Fe3+

Teste 4 Fe3+

Teste 2 Ino Fe2+

1.00 0.00 1

Teste 4 Fe 2+

17

Time (days)

25

35

39

Figure 4 Monitoring of Fe2+ and Fe3+ concentrations, in g/L, in the leaching liquor from the bioleaching process. It is observed that in the 38th day all the inoculated tests presented a copper extraction higher than 60%. On the other hand, evaluating the non-inoculated tests one can observe the extraction difference, as these present results of extraction lower than 25%, evidencing the presence of a biological process, taking into consideration that in the inoculated samples a higher copper extraction was obtained. Except for the control of the test 1, where there was possibly a contamination of the reaction system, it is evidenced that a biological process is taking place. Therefore, the presence of a biological process is evidenced in the inoculated tests.
80 70

Sol. A + Ino + Conc

Sol. A + Conc

60

T&K + Ino + Conc

50

Cu (%)

40 30 20 10 0 1

T&K + Conc
T&K Oxid. + Conc

17

25

38

45

62

Time (days)

Figure 5 Copper extraction during the bio-leaching process. The Figure 5 shows the evolution of the copper extraction, where in the test 2, a maximum extraction was reached, with about 67% in the inoculated test and 25% for its control test. The copper extraction reached is close to the results obtained by Agate & Khinvasara (1986), where a flotation concentrate was used containing 25.2% of copper. Such a concentrate was leached using 9K culture medium and A. ferrooxidans microbial inoculum. Those authors reached a copper extraction of 68.2%; however, it is worth to stand out that the concentrate they used contained

25.2% of copper, while the one used in this technical contribution contains 37.7% of copper, which comes mainly from chalcopyrite, the main component of the concentrate used in this study. They concluded that the copper extraction, in their tests, was not higher due to jarosita formation, which is deposited in the chalcopyrite surface, blocking the action of the bacteria.

CONCLUSIONS
When the A. ferrooxidans strains were used as microbial inoculum it is observed, until the 35th day, that the control parameters present differences between the results of the inoculated tests and their respective controls, evidencing the performance of the used strain. Due to the refractory nature of chalcopyrite (major component of the flotation concentrate), its biological oxidation is more intense after a period of approximately 24 days, reaching 784 mV vs. SHE, when a copper extraction of approximately 32% took place. It is possible to observe that with the use of the Acidithiobacillus ferrooxidans microorganism copper extractions of 67% were reached (12.4 g/L), and 64% (12 g/L) for the tests 2 and 3, respectively. According to the results reached in terms of copper extraction, considering, in particular, the high chalcopyrite content and the A. ferrooxidans, the only mesophile microorganism acting in the bioleaching process, one can assure that such leaching process is quite promising for extracting copper from the aforementioned flotation concentrate. In addition, this project is still in progress and, for sure, some other microorganisms will join the one in use so as to improve the copper extraction figures.

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