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CHARACTERISATION OF MANGANESE NODULE

1- Density measurement by pycnometer:


A pycnometer,
also
called pyknometer or specific
gravity
bottle, is a device used to determine the density of a liquid. A
pycnometer is usually made of glass, with a close-fitting ground
glass stopper with a capillary tube through it, so that air bubbles
may escape from the apparatus. This device enables a liquid's
density to be measured accurately by reference to an appropriate
working fluid, such as water or mercury, using an analytical balance.

Fig. 1: Pycnometer

Pycnometer can be also used to determine the density of


homogeneous solid object that does not dissolve in working liquid
(water). First, we need to measure the weight of pycnometer
together with inserted object m0+mS. We add water and determine
the weight H2O m (measured weight minus m0+mS). The volume
of added water H2O V can be obtained as
V

'
H2O

m'H O
=
H O
2

[7]

The volume of measured solid object V S is the difference between


the volume of water that fills the empty pycnometer V and volume
VH2O
V s=V V

'
H2 O

mH Om'H O
=
H O
2

[8]

Density of measured object


s =

ms
Vs

can be then calculated as

[9]

Experimental procedure:
Accuracy of herein described method for density determination of
liquid and/or solid matter relies on precise measurements of weight
and volume. Since it is important to determine weight of empty
pycnometer in its dry state, we do so at the beginning.
1. Determine the weight of empty, dry pycnometer m 0.

2. Fill about 1/3 of pycnometer volume with objects made of


examined material (glass beads or small
metal pieces
as
directed by the teacher) and measure the weight m1.
3. Add water such that pycnometer as well as capillary hole in the
stopper is filled with water. Dry the spare water that leaks through
the capillary hole with a filter paper and measure total weight m2.
4. Empty pycnometer and filled it with distilled water only. Use the
filter paper to dry the spare water again and measure the weight
m3.
5. Empty pycnometer. Rinse it once with a liquid whose density you
are going to determine next. Fill pycnometer with the liquid as
previously and measure the weight
m4.
6. Repeat point 5 for several different liquid materials.
7. Clean pycnometer carefully after finishing the experiment. Rinse it
with distilled water and let dry.
8. Measure the laboratory temperature t, which determines the
temperature of examined liquids and solid objects.
9. Calculate the weight of water mH2O=m3-m0, weight of measured
liquid mL=m4-m0 and determine its density according to equation
[6]. Repeat this calculation for all of the measured liquids.
10. In next, calculate the weight of solid object m s=m1-m0 and
weight of added water
mH2O =m2-m1.
11. Calculate objects volume VS following the equation [8] and its
density s according to equation [9].
Observation Table:
Wt. of empty
Bottle (A) gms.
Wt. of Bottle +
Sample
(B)
gms.
Wt. of Bottle +
Smaple +
Enough water
(C) gms.
Wt. of Bottle +
Water (D) gms.
Particle Density
=

II

III

25.065

27.462

30.037

42.271

46.58

52.281

86.875

91.231

94.651

75.361

78.33

80.015

3.023

3.075

2.998

B A
( DA )(CB)

gm/cc
So, the average density of manganese nodule was found to be 3.032
gm/cc.

2- pH measurement by pH-meter:
pH measurement is done to know the effect of the manganese nodule
sample on the pipelines in which it will be transported. On the basis of it
the pipelines will be designed so that it will remain unaffected.
pH-meter:
pH of 10% solution of manganese nodule with tap water and
measured with pH-meter.

was

Procedure:
1: At first electrode of the pH meter was filled with electrode solution and
then cleaned with distilled water.
2: The pH-meter was then calibrated with three different buffers of pH
4.01, 7.00, 10.01 respectively and its average slope was determined.
3: 10 gm of manganese nodule was taken with 90 mL of tap water in a
beaker to make 10% sample solution.
4: The solution was then placed under the electrode to measure the pH .
5: pH reading was taken up to 5 hrs with 30 min. interval.
6: A plot was made between pH and time to observe the change of pH
with time.
7: The procedure was also repeated for 10 gm of manganese nodule
sample with 90 ml of salt solution (4% salt dissolved in it).
Precautions:
1: Before taking reading each time the solution should be shaked properly
otherwise the sample gets suspended.
2: Reading is to be taken after the reading sign of the instrument stops
beeping.

3: Each time measure


measurements.

button

is

to

be

pressed

before

taking

4: It should be ensured that the instrument calibrated properly before use.

Observation table-1:
1- For tap water and manganese nodule 10% solution
Time
11:15 AM
11:45 AM
12:15 PM
12:45 PM
1:15 PM
1:45 PM
2:15 PM
2:45 PM
3:15 PM
3:45 PM
4:15 PM

Cumulative Hours
0:00
0:30
1:00
1:30
2:00
2:30
3:00
3:30
4:00
4:30
5:00

pH value
8.27
8.36
8.34
8.33
8.33
8.32
8.32
8.31
8.29
8.32
8.34

Plot:

Plot of pH vs. Time of 10% manganese nodule solution in tap water


14
12
10
8.27
8

pH Value

8.36

8.34

8.33

8.33

8.32

8.32

8.31

8.29

8.32

8.34

6
4
2
0
0:00

1:12

2:24

Time in Hrs.

3:36

4:48

6:00

Observation Table-2:
2. For 10% Manganese nodule solution in Salt water (4gm NaCl in
100mL of water)
Time
11:20 AM
11:50 AM
12:20 PM
12:50 PM
1:20 PM
1:50 PM
2:20 PM
2:50 PM
3:20 PM
3:50 PM
4:20 PM

Cumulative Hours
0:00
0:30
1:00
1:30
2:00
2:30
3:00
3:30
4:00
4:30
5:00

pH Value
7.61
7.72
7.71
7.70
7.69
7.68
7.66
7.65
7.69
7.62
7.63

Plot:

Plot of pH vs Time of10% Manganese nodule solution in salt water


10
9
7.61
8

7.72

7.71

7.7

7.69

7.68

7.66

7.65

7.69

7.62

7.63

pH Value

6
5
4
3
2
0:00

1:12

2:24

Time in Hrs

3:36

4:48

6:00

3. Particle size Distribution (PSD) Measurement by Laser beam


particle size analyser:
Laser Beam Particle Size Analyser

BRIEF DESCRIPTION OF EXPERIMENTAL SETUP

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