Froth Flotation of Bicol Ore Sample

Effects of Collector Dosage and pH of Pulp on the Recovery and Grade of Minerals

Gerard Boy A. Regino

Department of Mining, Metallurgical and Materials Engineering
University of the Philippines - Diliman
Quezon City, Philippines
garegino@upd.edu.ph

Abstract— Separation of gangue and valuable minerals can be flotation reagents are used to maintain the right condition of a
done by froth flotation process. The separation of minerals is froth and to control the hydrophobicity of the particles [3][4].
based on the wettability of minerals. In the experiment, ore sample
was mixed with water through an agitator in the flotation cell. The
pulp contains 30% solids and 70% water. An IF6500 frother was
added to the solution. Four set-ups with different parameters such
as collector dosage and pH were performed for comparisons of
recovery of Cu and Fe. Froths were collected in a separate pan for
every minute for 5 minutes and tails were collected after. Both
concentrates and tails were filtered, dried in an oven, weighed and
examined for x-ray fluorescence analysis. Release Analysis Curve
(RAC) of Cu and Fe were plotted for each set-up. Set-up 3 or the
pulp with pH 9 and 5 gpt of sodium isobutyl xanthate (SIBX)
collector yield the highest recovery of Cu of Fe among the four set-
ups. Figure 1. Example of a froth
Index Terms—Froth Flotation, wettability, reagents, Release
The type of reagent used in froth flotation process depends
Analysis Curve, recovery, grade
on the mineral mixture being analyzed. The common reagents
I. INTRODUCTION are collectors, frothers, depressants, activators, modifiers and
pH regulator. Collectors are used for adsoption on the surface of
Froth flotation process is used in separation of gangue and
the mineral resulting the attachment of minerals and bubbles.
valuable minerals. The valuable minerals are to be used in
Frothers improve the froth layer and stabilize the air bubbles for
metallurgical industries by metallurgy means. The separation of
prevention of bursting of bubbles. Modifiers influence the
minerals in this process is based on wettability of the minerals.
attachment between collector and the surface of minerals. Under
Minerals that repel with water are hydrophobic while minerals
modifiers are activators, depressants and pH regulators.
that have affinity for water are hydrophilic [2].
Activators ensure that collectors adsorb onto the surface.
The ore sample with hydrophobic and hydrophilic particles
Depressants are the opposite of activators. The use of these two
are mixed with water. Collectors are surfactants that make the
reagents depends on the wettability of the mineral to be float.
surface hydrophobic. They collect the hydrophobic minerals by
Then pH regulator affects the behavior of attachment between
attaching them to bubbles that are formed by suspension of air
collector and the surface [4].
applied to the solution. The bubbles formed that will rise and
float on the surface carrying the wanted minerals attached to
them are called froths (see Fig. 1). The froth functions as a
buoyant medium in separation of floatable from non-floatable
minerals. Froths are collected which contains concentrates and
the tails which are low in minerals tend to suspend and are
collected as shown in Figure 2 [4].
The bubbles must be strong and big enough to carry the
hydrophobic particles up to the surface especially for denser
particles. At the same time, the bubble and the particle must
remain attached to produce a froth on the surface. Froth must be
stable to prevent it from popping and detachment of particle.
Surface area of the bubbles affects the condition of a froth as
increasing rapid flotation of rate of particles happens during
increasing surface area of bubbles. To prevent these situations,
Figure 2. Illustration of a froth flotation method

Regino, G.B. (2019) Page 1 of 8

 In froth flotation, it is better to determine the best reagent for
an ore with specific minerals. The concentration or dosage of
reagent and pH of the pulp are factors of efficient flotation. The
efficiency of flotation is based the grade and recovery of froth
[2].
Release analysis is used for comparing effectiveness of
flotation of mutiple stage flotation from the single stage
flotation. Froths collected in the first stage are subjected to froth
flotation in a separate flotation cell to collect froths that will have
higher grade than before. This method is repeated until
maximum grade of mineral is achieved (see Figure 3) [2].
Figure 3. Illustration of Release Analysis Method
A Release Analysis Curve (RAC) shows the relationship
betrween % cumulative recovery of the mineral (y axis) versus
the mass of concentrate per 100 units (x axis). The grade of
concentrates and tailings of the mineral are determined by slope
of the RAC curve.
For this experiment, four set-ups with different conditions
are examined in a froth flotation machine. For every set-up, the
froths formed were collected for every minute for 5 minutes. The
concentrates are collected and examined into the x-ray
flourescence to determine minerals present and their grade. RAC
plot is used to determine the best flotation time.
II. METHODOLOGY
A. Sample Preparation
Samples from the bulk ore sample were crushed and grinded
by jaw crusher and then by roll crusher. The samples produced
by the roll crusher were performed particle size analysis by a
RoTap machine. This process was repeated until 4.5 kilograms
of bulk sample with 80% passing -140 mesh size was produced.
B. Reagent Preparation
Reagents were needed in froth flotation to serve as a
collector and as a frother. In this experiment, sodium isobutyl
xanthate (SIBX) was used as a collector and IF6500 was used as
a frother
Regino, G.B. (2019)
C. Flotation
Table 1 shows the parameters for flotation tests. The agitator
for all parameters is at 400 revolutions per minute (rpm).
Setup pH Collector Dosage
1 natural 5 gpt
2 natural 10 gpt
3 9 5 gpt
4 9 10 gpt
Table 1. Flotation Parameters
The ore sample was mixed with water in the flotation cell for
set-ups 1 and 2 while for set-ups 3 and 4, the pH of the pulp was
calibrated by a pH meter and then adjusted to pH 9 by dropping
NaOH and lime concentrations into the pulp. The solution was
conditioned for two minutes and collector was added. Then a
frother was added; for set-ups 1 and 3 (5gpt), for set-ups 2 and
4 (10gpt). Then the solution was conditioned again for two
minutes. Air is released under the flotation cell to produce
bubbles and calibrated it until stable froths on the surface were
formed. The froths were collected in a separate pan for each
minute. Total collection of froths is five minutes.
Once froths are collected and separated from the solution,
releasing of air was stopped. A part of the solution was collected
in a separate pan. Then agitator was stopped and the settled
particles at the bottom of the flotation cell were pressure filtered
and then dried in an oven. The weights of the concentrates were
recorded.
D. XRF Analysis
A representative sample enough to fill the cup was collected
from each concentrates and tails collected from the four set-ups
for XRF analysis. The XRF analysis evaluated the assay of
minerals present in the sample. For this experiment, copper and
iron are the minerals to be considered.
E. Data Treatment
The % recovery of copper and iron were calculated from the
mass concentrate over the total weight. Mass concentrate was
calculated through the weights of the concentrates, tails and their
respective assays
RAC plot was created for each set-up and compared to each
other to see the effect of different parameters to the grade and
recovery of the concentrate.
III. RESULTS AND DISCUSSION
The Release Analysis Curve of Copper and Iron using the
four set-ups are shown in figures 5-8. Looking at the figures
shown, the graphs of copper are almost identical to each other
the same with the graphs of iron. This means that the grade of
concentrates collected per minute were almost equal since
release analysis method was not performed. Release analysis
method shows the improvement of grade of concentrate per
stage of flotation.
Page 2 of 8
 Figure 5. RAC plot of Copper and Iron using Set-up 1
Comparing the % recovery of copper and iron, set-up 3 has
the highest total % recovery of both copper and iron. Reagents
improve the flotation. Reagents make the attachment between
bubble and minerals possible or stronger. Right reagent i.e.
dosage can also affect the level of attachment. The pH regulator
modifies the acidity or alkalinity of the solution. It enhances the
efficiency of flotation.
Figure 6. RAC plot of Copper and Iron using Set-up 2
Regino, G.B. (2019)
Figure 7. RAC plot of Copper and Iron using Set-up 3
Sodium isobutyl xanthate (SIBX) is the collector in the
experiment. This collector is for non-ferrous sulfide ores
resulting to % recovery of iron in all set-ups. For five minutes
with 1-minute intervals, collection of froth was done. The
collection time is not enough to collect concentrates leading to
small % recovery of copper and iron. Increasing the flotation
time and collection time can vary the recovery of concentrate.
Again, release analysis method can be done to distinguish the
difference of grades and recovery of the concentrates.
Figure 8. RAC plot of Copper and Iron using Set-up 4
Page 3 of 8
 IV. CONCLUSION AND RECOMMENDATION V. REFERENCES
In this experiment, release analysis method was not [1] Wills, B. A., & Napier-Munn, T. (2006). Wills mineral
performed. Instead, froths are collected in a separate pan for processing technology: An introduction to the practical
every minute. The concentration of pulp is still the same as aspects of ore treatment and mineral recovery. Amsterdam:
agitator mixed the ore and water the whole time. Release Elsevier.
Analysis method must be used to achieve higher grade of [2] Froth Flotation Fundamental Principles. Accessed May 11,
concentrate and to distinguish the changes of grade and recovery 2019.http://www.chem.mtu.edu/chem_eng/faculty/kawatra/Flot
of concentrate. ation_Fundamentals.pdf
ANOVA analysis was not performed. An ANOVA analysis [3] Froth Flotation. Accessed May 11, 2019.
determines if the results are significant. Good for multiple tests https://nptel.ac.in/courses/103103033/module6/lecture6.pdf.
to see if there are changes between them. This analysis is best to [4] "Flotation Reagents." Accessed May 11, 2019.
identify if there are significant changes in recovery of the https://www.911metallurgist.com/blog/froth-flotation-
concentrate with the effect of pH and collector dosage. An process.
ANOVA Two-Factor analysis is best suited for this experiment.
[5] "Froth Flotation Process." Accessed May 01, 2019.
https://www.911metallurgist.com/blog/froth-flotation-process
[6] Flotation Froth. Accessed May 12, 2019.
https://www.sciencedirect.com/topics/earth-and-planetary-
sciences/flotation-froth
[7] “How Froth Flotation Works”. Accessed May 12, 2019.
http://www.mine-engineer.com/mining//minproc/flotation.htm

Regino, G.B. (2019) Page 4 of 8

 VI. APPENDIX

For Copper:

Table 2. Weights of concentrates and tails of set-up 1

Test Data (natural pH, 5 gpt)

Product Flot. Time (min) Weight Conc (g) Assay (ppm Cu) Assay (% Cu) Mass Cu (g)
Conc 1 1 8.77 397 0.0397 0.0035
Conc 2 2 7.87 247 0.0247 0.0019
Conc 3 3 5.41 258 0.0258 0.0014
Conc 4 4 8.12 271 0.0271 0.0022
Conc 5 5 7.06 201 0.0201 0.0014
Tails - 962.77 140 0.014 0.1348
total 1000 0.0251 0.251

Table 2. Weights of concentrates and tails of set-up 2

Test Data (natural pH, 10 gpt)

Product Flot. Time (min) Weight Conc (g) Assay (ppm Cu) Assay (% Cu) Mass Cu (g)
Conc 1 1 4.208 315 0.0315 0.0013
Conc 2 2 6.0498 246 0.0246 0.0015
Conc 3 3 11.1325 220 0.022 0.0024
Conc 4 4 10.8769 269 0.0269 0.0029
Conc 5 5 14.5656 240 0.024 0.0035
Tails - 953.1672 83.2 0.00832 0.0793
total 1000 0.0251 0.251

Table 3. Weights of concentrates and tails of set-up 3

Test Data (pH 9, 5 gpt)

Product Flot. Time (min) Weight Conc (g) Assay (ppm Cu) Assay (% Cu) Mass Cu (g)
Conc 1 1 29.88 374 0.0374 0.0112
Conc 2 2 23.38 290 0.029 0.0068
Conc 3 3 31.08 378 0.0378 0.0117
Conc 4 4 29.51 440 0.044 0.0130
Conc 5 5 14.5656 321 0.0321 0.0047
Tails - 871.5844 132 0.0132 0.1150
total 1000 0.0251 0.251

Table 4. Weights of concentrates and tails of set-up 4

Test Data (pH 9, 10 gpt)

Product Flot. Time (min) Weight Conc (g) Assay (ppm Cu) Assay (% Cu) Mass Cu (g)
Conc 1 1 7.7223 1100 0.11 0.0085
Conc 2 2 18.7288 382 0.0382 0.0072
Conc 3 3 10.6985 819 0.0819 0.0088
Conc 4 4 10.1185 524 0.0524 0.0053
Conc 5 5 10.6925 545 0.0545 0.0058
Tails - 942.0394 166 0.0166 0.1564
total 1000 0.0251 0.251

Regino, G.B. (2019) Page 5 of 8

Table 5. RAC plot for set up 1

Calculated Data
Recovery of Cu Mass Concentrate per 100 units of Cu
% Cum % % Cum % Cum. Grade
1.3871 1.3871 3494.0239 3494.0239 0.0397
0.7745 2.1616 3135.4582 6629.4821 0.0326
0.5561 2.7177 2155.3785 8784.8606 0.0309
0.8767 3.5944 3235.0598 12019.9203 0.0299
0.5654 4.1597 2812.7490 14832.6693 0.0280
53.7003 57.8601 383573.7052 398406.3745 0.0145

Table 6. RAC plot for set up 1

Calculated Data
Recovery of Cu Mass Concentrate per 100 units of Cu
% Cum % % Cum % Cum. Grade
0.5281 0.5281 1676.4940 1676.4940 0.0315
0.5929 1.1210 2410.2789 4086.7729 0.0274
0.9758 2.0968 4435.2590 8522.0319 0.0246
1.1657 3.2625 4333.4263 12855.4582 0.0254
1.3927 4.6552 5803.0279 18658.4861 0.0249
31.5950 36.2502 379747.8884 398406.3745 0.0091

Table 7. RAC plot for set up 1

Calculated Data
Recovery Mass Concentrate per 100 units of Cu
% Cum % % Cum % Cum. Grade
4.4522 4.4522 11904.3825 11904.3825 0.0374
2.7013 7.1535 9314.7410 21219.1235 0.0337
4.6806 11.8341 12382.4701 33601.5936 0.0352
5.1731 17.0072 11756.9721 45358.5657 0.0375
1.8628 18.8699 5803.0279 51161.5936 0.0369
45.8363 64.7062 347244.7809 398406.3745 0.0162

Table 8. RAC plot for set up 1

Calculated Data
Recovery Mass Concentrate per 100 units of Cu
% Cum % % Cum % Cum. Grade
3.3843 3.3843 3076.6135 3076.6135 0.1100
2.8504 6.2346 7461.6733 10538.2869 0.0592
3.4909 9.7255 4262.3506 14800.6375 0.0657
2.1124 11.8379 4031.2749 18831.9124 0.0629
2.3217 14.1596 4259.9602 23091.8725 0.0613
62.3022 76.4618 375314.5020 398406.3745 0.0192

Regino, G.B. (2019) Page 6 of 8

For Iron (Fe)

Table 9. Weights of concentrates and tails of set-up 1

Test Data (natural pH, 5 gpt)

Product Flot. Time (min) Weight Conc (g) Assay (ppm Fe) Assay (% Fe) Mass Fe (g)
Conc 1 1 8.77 51618 5.1618 0.4527
Conc 2 2 7.87 54804 5.4804 0.4313
Conc 3 3 5.41 54314 5.4314 0.2938
Conc 4 4 8.12 53941 5.3941 0.4380
Conc 5 5 7.06 52104 5.2104 0.3679
Tails - 962.77 51852 5.1852 49.9216
total 1000 5.0668 50.668

Table 10. Weights of concentrates and tails of set-up 1

Test Data (natural pH, 10 gpt)

Product Flot. Time (min) Weight Conc (g) Assay (ppm Fe) Assay (% Fe) Mass Fe (g)
Conc 1 1 4.208 52833 5.2833 0.2223
Conc 2 2 6.0498 53477 5.3477 0.3235
Conc 3 3 11.1325 51898 5.1898 0.5778
Conc 4 4 10.8769 51365 5.1365 0.5587
Conc 5 5 14.5656 51858 5.1858 0.7553
Tails - 953.1672 53372 5.3372 50.8724
total 1000 5.0668 50.668

Table 11. Weights of concentrates and tails of set-up 1

Test Data (pH 9, 5 gpt)

Product Flot. Time (min) Weight Conc (g) Assay (ppm Fe) Assay (% Fe) Mass Fe (g)
Conc 1 1 29.88 58404 5.8404 1.7451
Conc 2 2 23.38 57633 5.7633 1.3475
Conc 3 3 31.08 56073 5.6073 1.7427
Conc 4 4 29.51 53193 5.3193 1.5697
Conc 5 5 14.5656 56284 5.6284 0.8198
Tails - 871.5844 50738 5.0738 44.2224
total 1000 5.0668 50.668

Table 12. Weights of concentrates and tails of set-up 1

Test Data (pH 9, 10 gpt)

Product Flot. Time (min) Weight Conc (g) Assay (ppm Fe) Assay (% Fe) Mass Fe (g)
Conc 1 1 7.7223 58224 5.8224 0.4496
Conc 2 2 18.7288 56097 5.6097 1.0506
Conc 3 3 10.6985 57493 5.7493 0.6151
Conc 4 4 10.1185 57784 5.7784 0.5847
Conc 5 5 10.6925 60173 6.0173 0.6434
Tails - 942.0394 52350 5.235 49.3158
total 1000 5.0668 50.668

Regino, G.B. (2019) Page 7 of 8

Table 13. RAC plot for set up 1

Calculated Data
Recovery of Fe Mass Concentrate per 100 units of Fe
% Cum % % Cum % Cum. Grade
0.8934 0.8934 17.3088 17.3088 5.1618
0.8512 1.7447 15.5325 32.8412 5.3125
0.5799 2.3246 10.6774 43.5186 5.3417
0.8645 3.1891 16.0259 59.5445 5.3558
0.7260 3.9151 13.9338 73.4783 5.3282
98.5268 102.4419 1900.1539 1973.6323 5.1905

Table 14. RAC plot for set up 1

Calculated Data
Recovery of Fe Mass Concentrate per 100 units of Fe
% Cum % % Cum % Cum. Grade
0.4388 0.4388 8.3050 8.3050 5.2833
0.6385 1.0773 11.9401 20.2451 5.3213
1.1403 2.2176 21.9715 42.2166 5.2529
1.1027 3.3202 21.4670 63.6836 5.2136
1.4908 4.8110 28.7471 92.4307 5.2050
100.4035 105.2145 1881.2015 1973.6323 5.3310

Table 15. RAC plot for set up 1

Calculated Data
Recovery Mass Concentrate per 100 units of Fe
% Cum % % Cum % Cum. Grade
3.4442 3.4442 58.9721 58.9721 5.8404
2.6594 6.1036 46.1435 105.1157 5.8066
3.4395 9.5431 61.3405 166.4561 5.7331
3.0981 12.6412 58.2419 224.6980 5.6259
1.6180 14.2592 28.7471 253.4452 5.6262
87.2789 101.5381 1720.1871 1973.6323 5.1447

Table 16.RAC plot for set up 1

Calculated Data
Recovery Mass Concentrate per 100 units of Fe
% Cum % % Cum % Cum. Grade
0.8874 0.8874 15.2410 15.2410 5.8224
2.0736 2.9609 36.9638 52.2047 5.6718
1.2140 4.1749 21.1149 73.3196 5.6941
1.1540 5.3289 19.9702 93.2898 5.7122
1.2698 6.5987 21.1031 114.3929 5.7685
97.3312 103.9299 1859.2394 1973.6323 5.2659

Regino, G.B. (2019) Page 8 of 8