Mindanao State University – Iligan Institute of Technology

Department of Materials Resources Engineering and Technology

College of Engineering and Technology
A. Bonifacio Avenue, Tibanga, Iligan City

Leaching of Roasted Copper Ore

Submitted by:
Barcenal, Fabiano Jr. M.
Maca-ayao, Warid S.
Manos, Christian W.
Mariquit, Justin James I.
Sha, Fradzneil M.

Submitted to:
Engr. Monalisa C. Pacaña

In Partial Fulfillment of the Requirements in MET157

Hydrometallurgy Laboratory

June 26, 2023

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 Leaching of Roasted Copper Ore
Barcenal, F. Jr., Maca-ayao, W., Manos, C., Mariquit, J.J., Sha, Fradzneil

SUMMARY

Leaching of copper from roasted copper ore is a hydrometallurgical process used to

extract copper from the roasted ore after the sulfide minerals have been oxidized. This
research report focuses on the extraction of copper from chalcopyrite ore using a
roasting-acid leaching process in a hydrometallurgical setting. Hydrometallurgy, utilizing
sulfuric acid as a lixiviant, offers a more environmentally friendly and efficient approach for
extracting copper from low-grade ores.

The results indicated that the concentration of copper in the leach solution could be
determined by its color. Pale Blue and Blue solutions indicated a higher concentration of
copper ions, while Pale Yellow solutions indicated a lower concentration, likely due to the
presence of iron ions. The temperature of the leaching solution significantly influenced the
rate of leaching reactions, with higher temperatures accelerating mineral dissolution and
metal extraction. The experiments demonstrated that quicker attainment of the desired
leaching temperature through an optimized ramp-up time led to selective copper dissolution
and reduced leaching of impurities.

The color intensity of the leach solution indicated the copper concentration, with
darker colors suggesting higher copper content. The experiments confirmed that longer
leaching times resulted in higher copper concentrations, while shorter times yielded lower
concentrations. The concentration of sulfuric acid used in the leaching process also affected
the copper concentration, with higher acid concentrations indicating higher copper levels in
the leach solution. The findings contribute to the development of efficient and
environmentally sustainable processes for the extraction of copper from sulfide ores using
hydrometallurgical techniques.

Key Terms: Acid-Leaching, Metal Extraction, Copper Ore, Sulfuric acid media

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Barcenal, F. Jr., Maca-ayao, W., Manos, C., Mariquit, J.J., Sha, Fradzneil

INTRODUCTION

According to Padilla et al. (2006), Chalcopyrite (CuFeS2) is the main copper sulfide
mineral used for producing metallic copper. Processing chalcopyrite concentrates using
high-temperature methods like smelting and converting has long been associated with
environmental concerns, including pollution from SO2 gas emissions and toxic compounds
like arsenic and antimony. In order to minimize this, Hydrometallurgy is being utilized to
minimize the environmental impacts and also maximize the extraction in the low-grade
copper ores utilizing Sulfuric acid as its most common lixiviant. This can only be done,
however, on the oxide ores (Ata et al., 2001).

Leaching is a hydrometallurgical process that employs lixiviants to separate valuable

metals from ore gangue. The choice of lixiviant depends on the ore type (Shamsuddin, 2021).
In this study, sulfuric acid was used to leach chalcopyrite ore. Sulfuric acid, also known as
hydrogen sulfate (H2SO4), is a strong mineral acid recognized for its corrosive nature. It is a
colorless, odorless liquid. Its application enables the formation of soluble copper sulfate
compounds when it reacts with copper minerals. The resulting pregnant leach solution (PLS)
is contaminated with other impurities and valuable metal or copper ions. The PLS is typically
processed for additional purification steps, such as solvent extraction or precipitation, after
the leaching process in order to recover pure copper from the solution (Khalid et al., 2019).
According to Bayi et al. (2018), sulfuric acid can dissolve the majority of copper oxide
minerals.

Variables like stirring rate, temperature leaching, and leaching duration may influence
how effective the leaching process is. An increase in stirring speed frequently results in an
increase in the rate at which copper leaches and a decrease in the thickness of the mass
transfer boundary layer on the particle's surface because of the suspended mineral particles
(Tao et al., 2021). Additionally, according to Bayati et al. (2018), the rate at which copper
leaches out gradually increases with temperature.

In this laboratory activity, a hydrometallurgical process is employed to extract copper

from sulfide ore. Additionally, pyrometallurgical roasting is utilized to eliminate the sulfides.
The recovery of copper from a copper sulfide ore using a roasting-acid leaching process
linked to pyrometallurgical and hydrometallurgical processes was the focus of this laboratory
paper. The examined reactions show improved copper recovery from its concentrate into

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Barcenal, F. Jr., Maca-ayao, W., Manos, C., Mariquit, J.J., Sha, Fradzneil

almost iron-free leachate. Following the roasting process, samples of the roasted ore were
mixed with sulfuric acid to perform leaching.

STATEMENT OF OBJECTIVES

Upon completion of this activity, the researchers will achieve the following objectives:
● Proficiency in preparing the acid reagent required for the experiment.
● Competence in conducting leaching experiments at both room temperature and
elevated temperatures.
● Ability to successfully generate a copper-containing solution as an outcome of the
experiment.

SIGNIFICANCE OF THE EXPERIMENT

This laboratory experiment is deemed significant because, at the end of this activity, it
will provide information about copper ore leaching. This experiment was conducted at
Mindanao State University - Iligan Institute of Technology at College of Engineering, Room
117 - Hydrometallurgical Laboratory.

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 Leaching of Roasted Copper Ore
Barcenal, F. Jr., Maca-ayao, W., Manos, C., Mariquit, J.J., Sha, Fradzneil

DESIGN, MATERIALS, AND METHODOLOGY

RESEARCH DESIGN
The study employed an experimental design to conduct research with controlled
variables, ensuring precise and accurate results and drawing valid conclusions based on the
established hypothesis. This laboratory report investigates the impact of manipulating various
parameters on copper extraction yield. The laboratory work took place at Hydrolab 117 in the
College of Engineering and Technology at Mindanao State University- Iligan Institute of
Technology.

MATERIALS
This section lists the materials used in the experiment, along with descriptions and
their corresponding usage. It is organized based on the procedures.

A. Sample Preparation
a. Total of 100g Roasted Copper Ore samples
b. Electronic Weighing Scale

B. Preparation of Lixiviant
a. Distilled Water
b. Sulfuric Acid
c. 10 mL Pipet
d. 50 mL Graduated Cylinder
e. 1 L Volumetric Flask (2 pcs)

C. Copper Ore Leaching

a. 250 mL Beaker
b. Magnetic Stirrer and Hot Plate
c. Mercury Thermometer

D. Filtration
a. Glass Funnel
b. #40 Whatman Filter Paper
c. 50 mL Plastic Vials with cap (8 pcs)
d. 250 mL Erlenmeyer Flask
e. Wash Bottle

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 Leaching of Roasted Copper Ore
Barcenal, F. Jr., Maca-ayao, W., Manos, C., Mariquit, J.J., Sha, Fradzneil

METHODOLOGY

This section shows the different stages of the laboratory procedure, which are divided
into three.

A. Sample Preparation

The initial step of the experiment involves sample preparation. Each crucible containing
roasted copper ore from the furnace weighed 10 grams. Given that four crucibles were
utilized in the preceding process, the contents of each crucible were evenly divided into two,
resulting in a total of 8 samples prepared for leaching.

B. Preparation of Lixiviant

Once the sample has been weighed, the next step involves preparing the leaching solution.
For the preparation of a 6% sulfuric acid solution, measure out precisely 60.3 mL of sulfuric
acid. Then, add an appropriate volume of distilled water to the container, which will act as the
solvent. While slowly pouring the acid, stir the solution using a glass rod to prevent sudden
heat generation or splattering. Thoroughly mix the solution until a homogeneous mixture is
achieved. Gradually add more distilled water to the container until the total volume reaches
1000 mL while continuing to stir to ensure proper mixing of the added water.

For the preparation of a 10% sulfuric acid solution, follow the same process as mentioned
above, with the only difference being the amount of sulfuric acid used. Instead of 60.3 mL,
prepare 90 mL of sulfuric acid before adding water to the container. Once all the samples and
solutions are ready, you can proceed to the next step of the experiment.

C. Copper Ore Leaching

The 10 g of each sample is placed into beakers with magnetic stirring rods carefully. Then,
100 mL of leaching solution is added to each beaker in an inclined position. Subsequently,
the beakers are placed on a hot plate stirrer at different time frames and temperatures.

For the 50-minute roasted ore, which was divided into four beakers, the first two beakers
were leached with a 6% sulfuric acid solution at room temperature. The first beaker is
leached for 30 minutes and labeled, while the second beaker is leached for 2 hours and
labeled. The remaining two beakers containing the 50-minute roasted ore are also leached
with a 6% sulfuric acid solution but at a temperature of 65 degrees Celsius. The leaching

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duration for the third beaker is 30 minutes, then labeled, and the fourth beaker is leached for
2 hours and labeled.

The same procedure is followed for the 1-hour and 10-minute roasted ore. It is divided into
four beakers and leached with 10% sulfuric acid. The first two beakers are leached at room
temperature, with the third beaker leached for 30 minutes, and the fourth beaker leached for 2
hours. The remaining two beakers containing the 1-hour and 10-minute roasted ore are
leached with a 10% sulfuric acid solution at a temperature of 65 degrees Celsius. The third
beaker is leached for 30 minutes, while the fourth beaker is leached for 2 hours.

D. Filtration
Lastly, after leaching, the researchers prepared an Erlenmeyer flask and funnel and then cut
#40 Whatman Filter paper into a circular shape and folded it into half twice. Placing the filter
paper into the funnel, then placing the funnel in the Erlenmeyer flask. The mixture is
carefully poured into the filter paper till filled up below the brim. This is done in batches,
pouring everything till the mixture is emptied. The beaker where the mixture came from will
be cleaned with distilled water. The liquid solution is then placed in a clean empty vial with a
cap with at least 50 mL and labeled accordingly.

RESEARCH FLOWCHART

Fig. 1 General Procedure for Leaching of Roasted Copper Ore

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 Leaching of Roasted Copper Ore
Barcenal, F. Jr., Maca-ayao, W., Manos, C., Mariquit, J.J., Sha, Fradzneil

RESULTS AND DISCUSSION

To facilitate easy identification of the various experimental trials, the researchers

implemented a systematic coding system. The codes assigned to each trial convey specific
information. To simplify the identification process, a coding system was adopted by the
researchers. The codes assigned to the trials provide essential details. In terms of roasting
time, "A" indicates a roasting duration of 50 minutes, while "B" represents a roasting
duration of 1 hour and 10 minutes. Regarding temperature, "X1" signifies room temperature
or 25°C, and "X2" denotes a heated temperature of 65°C. For the concentration of H2SO4,
"Y1" corresponds to a 6% solution, and "Y2" corresponds to a 10% solution. Finally, the
leaching time is indicated by "Z1" for 30 minutes and "Z2" for 2 hours.

Trial Roasting Amount Leaching

Code Temperature Color
Number Time H2SO4 Time

AX1Y1Z1 PALE
1 50 minutes Room Temp. 6% 30 minutes
YELLOW

AX2Y1Z1 PALE
2 50 minutes 65°C 6% 30 minutes
BLUE

AX1Y1Z2 PALE
3 50 minutes Room Temp. 6% 2 hours
YELLOW

AX2Y1Z2 PALE
4 50 minutes 65°C 6% 2 hours
BLUE

BX1Y2Z1 1 hour and PALE

5 Room Temp. 10 % 30 minutes
10 minutes BLUE

BX2Y2Z1 1 hour and

6 65°C 10 % 30 minutes BLUE
10 minutes

BX1Y2Z2 1 hour and PALE

7 Room Temp. 10 % 2 hours
10 minutes BLUE

BX2Y2Z2 1 hour and

8 65°C 10 % 2 hours BLUE
10 minutes

Table 1 Various parameters per leaching trials in constant 260 RPM stirring

The amount of copper present can be determined by a solution's color. In this

particular instance, Pale Blue and Blue solutions point to the presence of copper ions,

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whereas Pale Yellow solutions point to a lower concentration of copper; this means that the
pregnant leach solution contained more iron ions than the copper ions recovered.

The ramp-up time in the leaching process, which refers to the duration it takes for the
leaching solution to increase in temperature from room temperature to the desired leaching
temperature, i.e., 65°C, was a significant contribution to the leaching process.

Trial Roasting Amount Leaching Ramp-up

Code Temperature
Number Time H2SO4 Time Time

2 AX2Y1Z1 50 minutes 65°C 6% 30 minutes 6:54 min.

4 AX2Y1Z2 50 minutes 65°C 6% 2 hours 6:20 min.

BX2Y2Z1 1 hour and

6 65°C 10 % 30 minutes 6:58 min.
10 minutes

BX2Y2Z2 1 hour and

8 65°C 10 % 2 hours 6:31 min
10 minutes

Table 2 Ramp-up Time of Heated Conditions during Leaching Process

The rate of leaching reactions was influenced by temperature. Increasing the

temperature can accelerate the dissolution of minerals and the subsequent extraction of
valuable metals. By minimizing the ramp-up time and reaching the desired leaching
temperature quickly, the leaching process can commence at the optimal temperature, ensuring
efficient and rapid extraction of copper from the sample. Some leaching processes may
require specific temperature ranges to promote the selective dissolution of target metals while
minimizing the leaching of undesired elements. In this experiment, the ramp-up time ensured
that the leaching solution reached the desired temperature range, allowing for the desired
selectivity in metal extraction and avoiding excessive leaching of impurities.

Upon analyzing the results, it becomes evident that experiments AX2Y1Z1, AX2Y1Z2,
BX1Y2Z1, and BX1Y2Z2, which involved concentrated samples, yielded Pale Blue solutions.
Samples BX2Y2Z1 and BX2Y2Z2 yielded strong Blue solutions, which indicates a higher
copper concentration in the leach solution obtained from the concentrate samples. On the
other hand, experiments AX1Y1Z1 and AX1Y1Z2 yielded Pale Yellow solutions which

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indicated lower copper concentration and higher chances of iron concentration since it was
assumed that the roasted copper ore was chalcopyrite which contains iron.

The color's intensity can be used to gauge how much copper is present in the solution.
A higher copper content may be indicated by darker coloring. The color of the solution when
leaching pure copper ore depends on a number of factors.

● The leaching time emerged as a significant factor in determining the concentration of

leached copper. Comparing the results, it became apparent that a longer leaching time
(2 hours) led to a higher concentration of leached copper, as evidenced by a "Blue"
solution color. Conversely, shorter leaching times (30 minutes) resulted in a lower
concentration of leached copper, manifested through "Pale Blue" solution colors.

● The concentration of sulfuric acid led to a significant effect on the experiment. The
higher concentration of sulfuric acid led to an indication of a higher copper
concentration in the leach solution obtained from the concentrate samples.

● The temperature of the leaching solution led to a much higher concentration of copper
present in the solution. Experiments BX2Y2Z1 and BX2Y2Z2 resulted in having a Blue
solution indicating that the concentration has the possibility of higher copper content.
The preceding experiment supports this claim since most of the preceding
experiments with a leaching temperature of 65°C have a Pale Blue color of solution.

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CONCLUSION AND RECOMMENDATIONS

CONCLUSION

According to the results of the leaching experiment, the pregnant solution's color
development is significantly influenced by temperature, roasting time, and acid
concentrations. A significantly more noticeable blue hue is produced by higher temperatures,
longer roasting periods, and greater acid concentrations. On the other hand, a lighter
(noticeable) hue of blue is produced by roasting at lower temperatures for shorter periods of
time with less acid. The colors of the pregnant solution were also influenced by the presence
of contaminants. These results demonstrate the complex relationship between process factors
and final colors. To optimize the leaching process and create the necessary color variations
and trends, it is crucial to understand these components.

The ramp-up time in the leaching process is also significant as it has influenced
reaction kinetics, energy efficiency, process time, productivity, selectivity, and process
control. By minimizing the time required to reach the desired leaching temperature, the
leaching process can be optimized for efficient metal extraction, reduced energy
consumption, and improved overall process performance.

Even though Atomic Absorption Spectroscopy (AAS) was not used in the experiment,
the solution's color served as a reliable indicator of the amount of copper that had been
leached out of the samples. The Pregnant Leached Solution’s copper content could be
inferred from the difference in color. Additionally, the experiment's outcomes varied
depending on the study's conduct errors.

RECOMMENDATIONS

Tailings were observed to be present in the roasted copper ore sample. As a result,
tailings samples, which are made up of leftover material from the extraction of valuable
minerals, have a lower copper content, which lowers the copper concentration in the leach
solution. These are the following recommendations to improve the performance while
conducting this experiment:

1. Sample uniformity. To improve the performance of your experiment, it is crucial to

ensure sample uniformity. The origin of the samples used in this activity was not

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determined, and so was the purity. This lack of uniformity can potentially impact the
results of the experiment and introduce additional variability.
2. Explore other lixiviants. To further enhance the extraction of copper ore, it is
important to explore alternative lixiviants. While sulfuric acid (HsSO4) has been
commonly used as the primary lixiviant in this experiment, considering other
extractants can provide valuable insights and potentially improve the extraction
process.
3. Use of more accurate equipment. To enhance the accuracy of copper quantification
in a liquid solution, it is imperative to utilize advanced equipment capable of precisely
determining its elemental composition. This approach ensures a more accurate and
precise measurement of the copper content.

Moreover, additional Pregnant Leached Solution analysis, such as Atomic Absorption

Spectrometry, would yield thorough quantitative results for characterization. Future
researchers might also investigate additional lixiviants to compare the efficacy and efficiency
of various leaching chemicals.

It is necessary to carry out a test created especially for this purpose in order to get a
more precise and quantitative measurement of the copper concentration in the leaching
solution. Although the solution's color can be used to estimate the concentration of copper, it
is not a precise quantitative measurement.

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REFERENCES

Ata, O. N., Çolak, S., Ekinci, Z., & Çopur, M. (2001). Determination of the Optimum
Conditions for Leaching of Malachite Ore in H2SO4 Solutions. Chemical
Engineering & Technology, 24(4), 409–413.
https://doi.org/10.1002/1521-4125(200104)24:4%3C409::aid-ceat409%3E3.0.co;2-0

Azizi, A., Bayati, B., & Karamoozian, M. (2018). A comprehensive study of the leaching
behavior and dissolution kinetics of copper oxide ore in sulfuric acid lixiviant.
Scientia Iranica, 0(0). https://doi.org/10.24200/sci.2018.5226.1154

Padilla, R., Vega, D., & Ruiz, M. C. (2007). Pressure leaching of sulfidized chalcopyrite in
sulfuric acid–oxygen media. Hydrometallurgy, 86(1-2), 80–88.
https://doi.org/10.1016/j.hydromet.2006.10.006

Ríos, G., Ruiz, I., Rius, O., Cruells, M., & Roca, A. (2021). Leaching of Copper from a Flash
Furnace Dust Using Sulfuric Acid. Mineral Processing and Extractive Metallurgy
Review, 1–11. https://doi.org/10.1080/08827508.2020.1861612

Shamsuddin, M. (2021). Hydrometallurgy. Physical Chemistry of Metallurgical Processes,

Second Edition, 429–529. https://doi.org/10.1007/978-3-030-58069-8_11

Tao, L., Wang, L., Yang, K., Wang, X., Chen, L., & Ning, P. (2021). Leaching of iron from
copper tailings by sulfuric acid: behavior, kinetics and mechanism. RSC Advances,
11(10), 5741–5752. https://doi.org/10.1039/d0ra08865j

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APPENDICES
The experimental process for preparing roasted copper ore and carrying out the
leaching activity is briefly summarized in this appendix. It has thorough visual
documentation of the whole experimental procedure. The weighted copper ore that had been
roasted was then exposed to leaching using solutions of different sulfuric acid concentrations.
The leached solution was noticeably colored blue as a result of the leaching process. The
experimental procedures and results are graphically enhanced and explained by the following
photographs.

Appendix A: Leaching Setup with Controlled 65°C Leaching-Temperature

In leaching copper at 65°C temperature, it is important to cover the beaker using a

cling wrap or a foil to refrain the solution from evaporating. Evaporation can lead to a
decrease in the volume of the solution, resulting in an undesirable concentration change. The
cover helps to retain the heat within the beaker, maintaining a stable and consistent
temperature during the leaching process. This is particularly important when operating at a
specific temperature, such as 65°C.

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Appendix B: Filtering of the Solution using a #40 Whatman Filter Paper

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Appendix C: Pregnant Leached Solutions in plastic vials for Electrowinning

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