Technical Report

VARIATIONS IN ANTIMONY RETENTION

AMONG DIFFERENT ACTIVATED CARBON
GRAIN SIZES
July 23, 2019

CIRCULATION: ENCOURAGED

1.0 BACKGROUND of the STUDY

The decreasing quality of the input materials in smelting leads to a higher content of impurities in the anode
copper which, when electrolytically dissolved, leaves these impurities in the electrolyte. This consequently
requires adaptive electrolyte filtration systems that can cope up with increasing levels of impurities if the
company were to maintain decent copper cathode quality.
Being one of the main impurities imposing pronounced detriment on copper cathode production, utmost
efforts in research and development are being exerted to address the problems emanating from
uncontrolled antimony concentrations in electrolytes. One material that proves prominence in the field as a
feasible agent in Sb removal is activated carbon (AC). Activated carbon is made from wooden and
carbonaceous materials that were subjected to extreme heat in the absence of oxygen. The heat causes
volatile substances to gasify leaving cavities/micropores in the carbon complex which is able to keep most
of its structural integrity given that oxygen is absent for combustion to occur. These micropores give
activated carbon the potential to be used in fluid purification technologies.
Key factors that contribute cumulatively to antimony removal are AC grain size, AC quantity and contact
time. This study will assess these key factors to establish trends relative to Sb removal in hopes of
identifying tractions for improvement.

2.0 OBJECTIVE
The study aims to determine which grain size of activated carbon yields optimum antimony adsorption and
retention. Specifically, it aims to determine, statistically, if antimony adsorption and retention varies
significantly with a) Time & b) AC quantity.

3.0 SIGNIFICANCE
The results of this study will provide additional insights on the workings behind antimony adsorption by
activated carbon. This information will be useful in the improvement of PASAR Corp’s electrolyte filtration
system both in process and design, particularly in Sb removal.
Furthermore, a precise correlation between contact time and AC quantity with Sb removal will establish a
guide regarding the conditions that yield optimal results at the least expense of resources. With this, either
of the scenarios where underspending time and AC causes poor filtration or overallocation of time and AC
expends higher costs at an insignificant performance improvement can be avoided.
4.0 LIMITATIONS
This study is limited to determining the Sb retention of only three AC sizes i.e. 30 x 70 mesh, 12 x 40 mesh
and 6 x 12 mesh. The effective sizes and initial composition of these AC samples were not considered.
Only the effect of AC on antimony concentration at around 50 0C has been taken into account with all the
tests for antimony concentration carried out in the Metallurgical Laboratory. It was also assumed that the
filter paper used to separate AC from electrolyte samples after the contact process did not provide
complementary Sb removal from the samples.

5.0 METHODOLOGY

a. Sampling
The electrolyte sample needed for the experiments was collected from the overflow of block 24, cell 14 on
July 03, 2019. This same sample was used for all the trials and was stirred occasionally before every
decantation into flasks for the contact process. The AC samples were purchased from SBS Philippines
Corporation.
b. Contact Process
Three different AC samples were subjected to experimentations with the electrolyte volume fixed at 200 mL
whilst the mass of AC and contact time were set as independent variables to identify correlations with Sb
adsorption and retention. Magnetic stirrers were used to agitate each setup which were heated using a hot
plate and a bath for uniform temperature distribution and for easier temperature monitoring.
The AC – electrolyte proportions are shown in Table 1. The experimental setup is shown in Figure 1.
Table 1. Experimental Setups

Contact Time 30 mins. 2hrs.

Grain Size AC1 AC2 AC3 AC1 AC2 AC3

Trial 1 5g/200ml 5g/200ml 5g/200ml 5g/200ml 5g/200ml 5g/200ml

Trial 2 10g/200ml 10g/200ml 10g/200ml 10g/200ml 10g/200ml 10g/200ml

Water bath

Electrolyte & AC

Hot plate w/ magnetic

stirring

Figure 1. Visual Description of Setup

 c. Data Analysis
The analysis of the lab results was divided into three sections, for each of which a different statistical tool
and procedure has been employed. The analyses are described as follows:

a) Determining whether difference in Sb removal among AC sizes is significant. To do this, all

twelve values have been divided into three classes based on AC size alone and without regard for
contact time or AC amount. Three sample groups having a sample size of 4 can be derived from
these values and will then be subjected to Single Factor ANOVA to determine whether the groups
belong to the same population or not. If the ANOVA finds that at least one of the groups skews
from the others, a post hoc procedure will be conducted using t-test to determine which one is
different.
Table 2. Data Arrangement for Single Factor ANOVA

AC1 AC2 AC3

0.191 0.150 0.080
0.230 0.226 0.138
0.230 0.204 0.120
0.261 0.249 0.189

b) Determining whether increasing contact time yields significant improvement. In this part of
the analysis, the data will be sorted in terms of contact time alone. Doing this, we get a sample size
of 6 in each class, that is 2 values from every size of activated carbon. The means of each class
will then be analyzed using t-test to determine if the adsorption difference between 30 minutes and
2 hours of contact time is significant.

Table 3. Data Arrangement for Paired Two-sample t-test

30
2hrs
mins.
0.191 0.230
0.150 0.204
0.080 0.120
0.230 0.261
0.226 0.249
0.138 0.189

c) Determining whether increasing AC quantity yields significant improvement. The statistical

treatment for this section is essentially an iteration of section B, having similar data arrangement
and statistical tool. The only difference is that, instead of contact time, the subject of statistical
treatment is AC quantity.
6.0 RESULTS AND DISCUSSION

I. Laboratory Findings
Table 4. Sb Concentrations in Electrolyte After Treatment

Contact Time 30 mins. 2hrs

Q Average
AC1 AC2 AC3 AC1 AC2 AC3
Grain Size
(30x70) (12x40) (6x12) (30x70) (12x40) (6x12)

5 grams AC 0.154 0.195 0.265 0.115 0.141 0.225 0.1825

10 grams AC 0.115 0.119 0.207 0.084 0.096 0.156 0.1295

T Average 0.1758 0.1362

The results from the laboratory were as displayed in Table 4. One notable observation that is consistent
throughout the table is that, for every specific AC size, Sb concentration in electrolyte is inversely influenced
by an increase in either contact time or AC amount. The decision on whether this influence is significant or
not will be discussed further in the later parts of this section.

Sb Removal in Percentiles
30min 5grams 2hrs 5grams 30min 10grams 2hrs 10grams

80.00

70.00

60.00
Sb in Electrolyte

50.00

40.00

30.00

20.00

10.00

0.00
AC1 AC2 AC3

Figure 2. Percent Sb Removed from 0.345gpl Raw Sample Concentration

AC1 at 30 x 70 mesh, although the highest in terms of percent Sb removed, is generally comparable in
performance as AC2. AC3, however, slacks behind for a discernably higher extent as compared to the
other activated carbon sizes which are both exhibiting near-powder properties. The main reason for this is
that, cavities in the carbon complex of AC, when viewed in a microstructural scale, grow narrower from the
surface. This means that for the same volume of powdered activated carbon (PAC) and granular activated
carbon (GAC), greater adsorption potential is expected of PAC because much more cavities/micropores
are exposed by the individual tiny particles. GAC, on the other hand, has only a portion of its volume utilized
for adsorption, that is for a certain depth from the surface of each granule.

II. Statistical Analyses

Table 5. Values Used in Section A of Statistical Analysis

AC1 AC2 AC3

55.362 43.478 23.188
66.667 65.507 40.000
66.667 59.130 34.783
75.652 72.174 54.783
66.087 60.072 38.188

a) Determining whether difference in Sb removal among AC sizes is significant.

The F-value obtained upon subjecting the data to ANOVA is greater than F critical. This
conveys that among the three sample groups i.e. AC1, AC2 and AC3, at least one is of different
population. Post hoc t-tests are hence necessary to identify which class deviates.

Figure 3. Results of Post hoc t-tests

Upon comparing the obtained t-values to their respective critical values, it can be inferred that
AC1 and AC2 provide essentially similar efficiency in Sb removal as substantiated by the low
t-value of 2.549 compared to a t critical of 3.182. The statistics on AC3, on the other hand,
suggests that the 6x12 mesh AC, with t-values roughly three times the t critical, is largely a
different population and that its effect on Sb removal is significantly apart from those of 30x70
and 12x40 AC mesh sizes.
 Table 6. Values Used in Section B of Statistical Analysis

30
2hrs
mins.
55.36 66.67
43.48 59.13
23.19 34.78
66.67 75.65
65.51 72.17
40.00 54.78

b) Determining whether increasing contact

time yields significant improvement.
Here, the t statistics is greater in magnitude
than the t critical. This means that the null
hypothesis is to be rejected warranting the
assumption that the increase in Sb removal
with time is significant.

Figure 4. t-test for Significance of Effect of Contact Time

Table 7. Values Used in Section C of Statistical Analysis

5grams 10grams
55.36 66.67
43.48 65.51
23.19 40.00
66.67 75.65
59.13 72.17
34.78 54.78
c) Determining whether increasing AC
quantity yields significant improvement.
Similar with contact time, increasing AC
quantity also yields significant increase in Sb
adsorption. It must be noted though that this
only confirms that time and quantity are
affecting factors but does not necessarily
mean increasing them is the best option. For
one, the statistical tools employed don’t
consider the quantitative sense of these
named factors and only considers them as Figure 5. t-test for Significance of Effect of AC Quantity
nominal values.
7.0 CONCLUSION
One of the major noteworthy inferences derived from the results of this study is the negligible difference,
as per the statistics, between AC1 and AC2. This finding suggests that there is a variable choice of AC
sizes for when availability and price come into play. Furthermore, a significant increase in Sb removal has
been observed upon increasing either AC quantity or contact time or both. Again, this only confirms that
the said variables are affecting factors and increasing them don’t amount to a more optimized operation.

8.0 RECOMMENDATIONS

 Given that AC1 and AC2 are at a closely comparable range of Sb adsorption potential, it is
recommended that a thorough analysis considering costs and availability of the two be conducted
to see if any advantages can be gained.
 Due to time and resource restrictions, this study was not able to replicate in laboratory scale the
current Sb column setup. Because of this, the results of the study may be referenced in choices
involving adsorptive materials but cannot be taken as definitive basis when it comes to equipment
design or operations-related decisions. It is, hence, recommended that experimental setups in
further studies on this subject be designed as replicative of the actual as possible for a more valid
and applicable set of results.
 Compare a laboratory scale miniature of the current Sb column with one that has agitation.
 If agitation is a positive factor in Sb adsorption, it will be logical to experiment further on various
characters of flow. It is then recommended that extensive research on the effect of flowrate, flow
turbulence and flow direction (upstream or downstream) be conducted.