SULFUR DETERMINATION USING GRAVIMETRIC METHOD

OXIDATION ROASTING OF COPPER SULPHIDE ORE

Romelyn B. Maandig
METE 159: PYROMETALLURGICAL ENGINEERING LABORATORY

ABSTRACT
Roasting converts the sulfide into the oxide form producing copper oxide. At the same time sulfiding occurs
where copper sulfide is formed. Copper sulfide is insoluble to water and slightly soluble to HCl which makes it
easy for the subsequent recovery processes.
Eight samples of 10g copper ore were weighed and put on crucibles. These samples were roasted at two given
temperatures and four given time which were then cooled and weighed. Two trials of each temperature were
made for this experiment. And the experimental data shows that it is evident that the weight loss increases as the
time of roasting increases and that the weight loss also increases as the temperature increases. Also reactions are
relatively faster as the temperature increases.

INTRODUCTION
Copper-containing rock hosts only a small
percentage of copper. Depending on to what
minerals the copper is bound, the rock is processed
in different ways in order to extract the valuable
copper. There are two main copper ore types of
interest, copper oxide ores and copper sulfide ores.

sulfide with oxides. The sulfur removed goes off as

sulfur dioxide gas. This can be done by giving the
sulphide ore an oxidizing roast. The object of the
roast is to convert a considerable portion of the
copper in the oxide form and a lesser amount is the
form of sulfide, and all of the iron to ferric oxide
which is insoluble in dilute acid.

MATERIALS AND METHODS

The most common source of copper ore is the
sulfide ore which accounts for about 50 percent of
copper produce. Sulfide copper ores are the most
profitable ores because they have high copper
content, and the copper can be more easily
separated from the unwanted minerals. However,
sulfide ores of copper are insoluble in dilute
sulfuric acid leaching solutions, but a very high
extraction can be obtained if the copper ore is in
the oxidized condition. With that, oxidative
roasting is applied for the removal of sulfur.
Another method in determining sulfur content is
by gravimetric method.

OBJECTIVES OF THE STUDY

This experiment aims to study the effects of time
and temperature on the rate of removal of sulfur
using oxidation roasting and the determination of
Sulfur using gravimetric method from a copper
sulfide ore.

A.

SULFUR DETERMINATION USING

GRAVIMETRIC METHOD

The materials that were used were Copper

concentrate, 50 mL graduated cylinder, evaporating
dish, 250 mL beaker, Analytical Balance, hot plate,
stirring rod, filter paper, watch glass, Oven, and
crucible.
1g of copper ore was weighed using 400mL as
container and a 40mL HNO3 was added. It was
then heated until 5mL was left. A pinch of Sodium
Carbonate (NaCO3) was added, evaporated and
cooled. It was then dissolved in 20-30mL HCl and
boiled. After boiling, 50mL of 5% Barium Chloride
solution was added and heated with cover. After
heated just below boiling, it was stirred and stand
for 2 hours. After which, it was then filtered and
transferred to a crucible. Dried in the oven for
about 30 minutes (110C). Cooled and then the
weight was determined.

SIGNIFICANCE OF THE STUDY

Oxidative roasting is used to remove all or part of
the sulfur from sulfide metal compounds replacing

Oxidation Roasting.Submitted to Myra V. Cabatingan, Instructor. Page 1 of 6

B. Oxidation Roasting of Copper Sulphide

Ore
The materials that were used during the activity
were Copper concentrate, Crucible, Tongs, Tube
Furnace and Analytical Balance.
Four samples of 10g copper ore were weighed and
put on crucibles labelled respectively as samples 1,
2, 3 and 4. At 700C, sample 1 was roasted for 15
minutes, sample 2 for 30 minutes, sample 3 for 45
minutes and sample 4 for 60 minutes. Two trials
were made for this temperature. Another set of
four samples having 10g copper ore were weighed
and put on crucibles labelled as samples 1, 2, 3, and
4 were roasted at 500C for 15, 30, 45 and 60
minutes, respectively. Two trials were also made
for this temperature. After roasting and cooling,
the weight of each sample was determined.

Ore Sample

Roasting

Weighing

Table 1 above shows the respective weights

obtained in the experiment.
Sulfur can be determined using the formula below :

%S=

( wt . BaSO 4 ) ( S ) (100)
( wt . sample ) (BaSO 4 )

So,

%S=

( 2.52 g ) ( 32 g ) (100)
( 1.07 g )( 233.33 g )
%S=32.30

B. Oxidation Roasting of Copper Sulfide Ore

TABLE 2A. Weight of the ore after roasting at
700C
TRIAL I
1
(15
minutes)
grams

2
(30
minutes)
grams

3
(45
minutes)
grams

4
(60
minutes)
grams

23.38

27.18

23.38

27.18

10.05

10.08

10.04

10.11

33.43

37.26

33.42

37.29

Crucible
(after
heating)

32.18

35.93

32.04

35.76

Weight
loss

1.25

1.33

1.38

1.53

SAMPLE

Weighing

Cooling
crucible

Figure 1. Process Flow for Oxidation Roasting of a

Copper Sulfide Ore.

RESULTS AND DISCUSSION

A.

SULFUR DETERMINATION USING

GRAVIMETRIC METHOD

TABLE 1. Weight of BaSO4 Precipitate

Weight of Sample (g)

1.07

Weight of crucible (g)

27.41

Weight of filter paper (g)

1.0

Weight after drying (g)

30.93

Weight of BaSO4
precipitate (g)

2.52

ore
Crucible
+ ore

Oxidation Roasting.Submitted to Myra V. Cabatingan, Instructor. Page 2 of 6

TABLE 2B. Weight of the ore after roasting at

700C

TABLE 3B. Weight of the ore after roasting at

500C

TRIAL II
SAMPLE

crucible

5
(15
minutes)
grams

6
(30
minutes)
grams

7
(45
minutes)
grams

8
(60
minutes)
grams

22.71

23.38

22.71

23.38

ore
10.03
Crucible
+ ore

32.74

Crucible
(after
heating)

30.76

Weight
loss

1.98

10.05
33.43
32.03

1.4

10.04
32.75
30.47

2.28

33.41

2
(30
minutes)
grams

3
(45
minutes)
grams

4
(60
minutes)
grams

crucible

25.11

22.90

25.12

22.88

10.04

10.03

10.07

10.01

35.15

32.93

35.19

32.89

Crucible
(after
heating)

34.10

32.03

34.35

32.13

Weight
loss

1.05

0.9

0.84

0.76

ore
Crucible
+ ore

1.51

TRIAL I
10
(30
minutes)
grams

11
(45
minutes)
grams

12
(60
minutes)
grams

23.63

22.61

23.63

22.98

10.03

10.09

10.04

10.05

33.66

32.70

33.67

33.03

Crucible
(after
heating)

32.61

31.97

32.87

32.24

Weight
loss

1.02

0.73

0.8

0.79

ore
Crucible
+ ore

1
(15
minutes)
grams

31.90

9
(15
minutes)
grams

crucible

s
SAMPLE

10.03

TABLE 3A. Weight of the ore after roasting at

500C

SAMPLE

TRIAL II

Table 1A, Table 1B, Table 2A and Table 2B above

shows the respective weights obtained in the
experiment, for the samples roasted at 700C and
500C for 15 minutes, 30 minutes, 45 minutes and
1 hour respectively. It is evident that the weight
loss increases as the time of roasting increases
(Table1A). This is mainly because more time is
allowed for the formation of sulfur dioxide. On the
other hand, weight loss also increases as the
temperature increases. Reactions are relatively
faster as the temperature increases. However, in
roasting, temperatures too high should also be
avoided in order to not melt the valuable metal.
For simplification of calculations, it is assumed that
all the sulfur in the roasted feed is in the form of
copper sulfide (Cu2S).
Calculation of the total sulfur in the ore sample:

wt . Sulfur =g Cu 2 S

1 mol
1 mol Sulfur 32 g
Cu 2 S

159.1 g
1 mol Cu2 S 1 mol

Table below shows the weights of sulfur.

Sample

Weight of

% Sulfur

Sample
1
10.05

2.02137

Oxidation Roasting.Submitted to Myra V. Cabatingan, Instructor. Page 3 of 6

2
3
4
5

10.08
10.04
10.11
10.03

6
7
8

10.05
10.04
10.03

Sample

Weight of

9
10
11
13
14
15
16

Sample
10.03
10.09
10.04
10.05
10.05
10.08
10.04
10.11

2.02740
2.01936
2.03343
2.01735
2.02137
2.01936
2.01735
% Sulfur

2.01735
2.02942
2.01936
2.02137
2.01936
2.01735
2.02539
2.01332

Now, oxidation of ore containing copper sulfide is

according to the following equation:

3
Cu2 S+ O2 Cu2 O+SO 2
2

2.03
2.03
2.03
2.02
% Sulfur 2.02
2.02
2.02
2.02
2.01
10 15 20 25 30 35 40 45 50

Time of Roasting (min)

% Sulfur

Based on the observations made, it is concluded

that the time and temperature of reaction is directly
proportional to the degree of roasting. Increasing
time improves the quality of roast since the amount
of copper sulfide decreases while the amount of
copper sulfate and copper oxide increases.
Uncertainty of the composition of the samples
makes it difficult to understand completely the
effect of roasting on the samples. It is then
recommended to have further examinations on the
samples to determine its composition.

Therefore, the weight loss in the sample are

considered to be the sulfur content in the copper
sulfide ore oxidizing out as SO2 gas. However, the
weight loss obtained in the activity are significantly
less than the calculated sulfur content of the ore
when assumed as pure Cu2S. Also, if all the Cu2S
ore was converted to Cu2O, the maximum weight it
should have is (Sample 1):

10.05 g Cu 2 S

1 mol Cu 2 O 143.1 g
1 mol
Cu 2 S
Cu2 O=9.03931 grams Cu 2 O
R
EFERENCES
159.1 g
1 mol Cu2 S
1 mol

Which means that the maximum weight loss is only

1.01069 grams. Thus, it is assumed that the copper
sulfide ore contains large amounts of impurities.

CONCLUSION AND RECOMMENDATION

Structural and compositional changes in copper

sulfide during leaching and dissolution, Whiteside
L.S, Goble R.J, The Canadian Mineralogist;
(1986);. 24; 2; 247-258
Cu NMR studies of copper sulfide Shin-hachiro
Saito, Hideki Kishi, Kohji Ni, Hisakazu
Nakamaru,
Fumihiko Wagatsuma,
Takeshi
Shinohara, Phys. Rev. B 55, (1997), 21, 14527
W G Davenport, M King, M Schlesinger and A K
Biswas, Extractive Metallurgy of Copper, Fourth
Edition (Elsevier Science Limited: Kidlington,
Oxford, England, 2002

Oxidation Roasting.Submitted to Myra V. Cabatingan, Instructor. Page 4 of 6

http://www.slideshare.net/akshatc/principals-ofroasting-and-its-types
http://digitalcommons.mtech.edu/cgi/viewcontent.c
gi?article=1020&context=bach_theses

Oxidation Roasting.Submitted to Myra V. Cabatingan, Instructor. Page 5 of 6