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Universiti Teknologi PETRONAS

CBB 2093

Process Instrumentation

LABORATORY REPORT

EXPERIMENT 3

pH, DISSOLVED OXYGEN AND CONDUCTIVITY MEASUREMENT

KHADIJATUL-AKMAL BINTI AHMAD HAMIZI 0011954

KHUONG MINH CAM TU 0012963

LAILA SAKINAH BINTI JUSOH 0011961

LAURA TIONG SIEW ZIN 0011963

Date of experiment: 14-10-2010

Date of submission: 21-10-2010


Objectives

1. To conduct calibration check on the pH electrode and its amplifier system


2. To conduct calibration check on the conductivity electrode and its amplifier
system
3. Measurement study of the effect of acid-base titration on Ph
4. Measurement study of the effect of acid-base titration on conductivity
5. To conduct calibration check on the dissolved oxygen electrode and its
amplifier system
6. Measurement study of the various gas bubbles on dissolved oxygen

Abstract

In this experiment, the objectives are to investigate the effect of acid-base


titration on pH and conductivity and also the effect of various gas bubbles on
dissolved onxygen (DO) value. For the first part, city water is filled in the tank until
level A and then acid is added in followed by alkali. The readings of pH, DO and
conductivity is taken before and after adding in acid and also after adding in alkali.
Then, the tank is cleaned and the same procedure is repeated but the water is filled
until level A. The readings are taken and compared with readings when water is at
level A.
In the second part, the tank is filled with city water until level C. The initial
readings of pH, DO and conductivity are recorded. Then, air is bubbled in for 10
minutes. The final readings are recorded. The same procedure is repeated but
replacing the air by nitrogen gas. The initial and final readings are onserved and
recorded.
From the data and graphs obtained, we can see the changes of pH, DO and
conductivity of the solution when acid and alkali is added in and also when oxygen
and nitrogen is bubbled in. From the results, we can see that as pH value decreases,
the conductivity increases. As the amount of water increases, the conductivity
decreases. And last but not least, as the amount of dissolved oxygen in the water
incerases, the conductivity will also increase as the oxygen creates an acidic
medium.
Introduction

The starting point for the pH scale is pure water, which is said to be neutral. Water
dissociates into:

H2O ↔ H+ + OH-
Water has equilibrium constant

K w =¿ ¿

pure water divides to give equal number of H+ and OH- ions and consequently the
concentrations of ions are 10-7 so that

pH = pOH = 7

The pH value of pure water is 7. This statement is incomplete since the equilibrium
constant depends on the temperature. The definition should be the pH value of water
is 7 at 25°C. Some examples of common solutions with an acid character are

H2SO4 ↔ SO4- + 2H+

HCl ↔ Cl- + H+

If the concentration of H+ ions in a solution is increased then the solution is said to


have a base character. In this case the pH value of the solution is a number greater
than 7.

pH value of pure water against temperature


Procedure

Experiment 1: Titration of acid HCl and Base NaOH

1. It is ensured that the mixing tank, dosing tank and water tank are clean and do
not have any contamination.

2. A mixing tank is filled with city water to about 80% full. It is ensured that the
manual valve for water tank MV-H2O is fully open.

3. Acid HCl solution and base NaOH solution is put into the dosing tank.

4. Valve MV-EC (manual valve for electrode chamber) is opened to enable


solution to flow back into the mixing tank.

5. MV-EC is shut off and MV-DM is opened (manual valve for demineralizer). The
circulating pump is switched ON. The solution inside the mixing tank would be
drained after going through the demineralizer. The circulating pump is shut
when draining completed.

6. MV-DM is shut off and MV-EC is opened to 45%. Water pump is switched on.
Water will flow into the mixing tank.

7. The circulating pump is switched on when water level is approximately 3 cm


deep.

8. The water pump is switched off when water reaches level A.

9. The dosing volume dial for acid and alkali dosing pumps are checked. It is
made sure that the dial pointer is at 70% of the scale and frequency is at II
position. The reading of pH, conductivity is taken and it is recorded into table
when reading is stabilized.

10. Switch on acid dosing pump and start the stopwatch. Acid HCl solution will be
dosed into the mixing tank. Start recording by pressing REC on recorder. Notice
there should be a light indicator to indicate the start of recording.

11. The pH value and conductivity value shall change with the addition of acid HCl.

12. Acid dosing pump is switched off to stop dosing when time is 4 minutes. The
reading is allowed to stabilized for another 4 minutes.

13. At 8.00 minutes alkali dosing pump is switched on to start dosing NaOH.

14. The base is let to be dosed into mixing tank. pH of the system should be getting
higher due to reaction between acid and alkali. You should be able to notice the
change of pH and conductivity values due to the process of naturalization.
15. REC button on the recorder is pressed to stop recording. The button FEED in
the Recorder is pressed for 10 seconds. This will create an extension so that
the chart of that experiment’s data located can be located.

16. The experiment graph is collected on the chart paper.

17. The experiment graph is repeated on the chart paper.

18. Steps 1 to 17 are repeated for water level C.

19. The required data into DATA and RESULTS section are recorded and
calculated.

Experiment 2: Dissolved Oxygen Measurement

1. Water pump is switched on to allow water to be pumped into mixing tank. The
circulating pump is switched on when water reach level A.

2. The water pump is stopped when water fills the mixing tank with city until level
C.

3. It is made sure that there is pneumatic supply at 15 psi. The pneumatic air
regulator is checked to start recording. The stop watch is started.

4. The manual valve MV-AIR is switched on. REC button on the recorder is
pressed to start recording. The stopwatch is started.

5. The pneumatic supply is switched off when time is 10:00.

6. REC button is pressed to stop recording. FEED button is pressed to extant


some length of chart paper so that the chart can be collected from the recorder.

7. The circulating pump is stopped and water from the electrode chamber is
allowed to drain back to the mixing tank.

8. MV-EC is shut off and MV-DM is opened. The circulating pump is started. Water
inside mixing tank to draw into the drain.

9. Circulating pump is turned off when all water inside the mixing tank been drain
out.

10. Steps 1 to 9 are repeated for experiment by using nitrogen air bubbling.
However the manual valve MV-N2 is opened at step 4 and not MV-AIR.
Results:

Experiment 1

Water at Level A

pH DO Conductivity
Initial reading 11.91 7.98 93.0 (mS/cm)
After acid 5.24 7.85 9780 (μS/cm)
After alkali 11.40 7.80 3770 (μS/cm)

Water at Level C

pH DO Conductivity
Initial reading 10.16 7.80 204 (mS/cm)
After acid 4.86 7.89 6260 (μS/cm)
After alkali 9.11 7.88 2130 (μS/cm)

Experiment 2

Air

pH DO Conductivity
(μS/cm)
Initial reading 9.73 7.91 153.8
After air 10.14 8.13 157.7

Nitrogen

pH DO Conductivity
(μS/cm)
Initial reading 10.95 7.88 96.3
After air 11.03 0.20 93.3

Discussion:

The experiment is conducted to study the relationship between pH, dissolved


oxygen and conductivity.
Conductivity is a solution’s ability to transmit and electric charge. It is
established according to the number of ions in the solutionA high concentration of
ions will correspond to high conductivity (assuming there is no reaction between the
ions present). The higher the number of ions is, the higher the conductivity degree
will be. If ions react/bind to form compounds or molecules, conductivity will decrease.
If greater dissociation occurs as a result of the presence of certain ions, conductivity
will increase. For example, two solutions having the same number of ions, the
presence of the hydroxide anion in Solution B decreases the conductivity of the
solution because of its ability to form compounds with other ions. The density and
mobility of the ions, as well as the viscosity of the solution (ability to flow) will also
affect the conductivity. More mobile ions will have higher conductivity, but a highly
viscous solution will make it more difficult for the ions to move (lowering the
conductivity).

Ph value is the measurement of amount of H+ ions present in the solution. The


pH scale ranges from 0-14. These are standardized values used to measure the
acidity or alkalinity (how basic) a particular substances is. A pH of seven indicates
that the substance/solution is neutral. Any pH reading below 7 denotes the solution is
acidic, while readings above 7 denote the solution is basic. Essentially, pH is a
measurement of the concentration of hydronium ions (H+) present and is given by
the equation:
pH = -log [H+]

For this experiment, the objective is to conduct calibration check on the pH


electrode, conductivity electrode and its amplifier system and to study of the effect of
acid-base titration on pH and conductivity. For both parts, we insert water, following
by acid and alkali both with interval of 4 minutes. For part 1(a), we inserted water
until level A whereas for part 1(b), we inserted water until level C which is higher than
level A. The volume of water in part b is larger than that of part a. The amount of
alkali and acid added is same for both experiments. Thus, the result is collected from
the graph obtained from the experiment. The value of dissolved oxygen remains
almost constant in both parts of the experiment. Thus, the major concern of this
experiment is the relationship between concentration of acid-base in the solution and
its conductivity.
The pH scale corresponds to the concentration of (H 3O+) hydronium ions in a
solution. In fact, if we take the exponent of the H 3O+ concentration and remove the
negative sign, you have the pH of a solution.  For example, in pure water the
concentration of hydronium ions is 1 x 10 -7 M.  Thus, the pH of a solution of pure
water is 7. The solution becomes acidic because it contains more H 3O+ ions but when
pH value increase, it means that it contains less H 3O+ ions.

From the result, we can see that there is significant change in conductivity
when the acid and alkali are added. When we add in acid, the pH value will
decrease but conductivity will increase. From this, it can be explain that acid medium
favour the transmission of electric charge. This is because when a medium is more
acid, that means there are more hydronium ions present in the medium. Hydronium
ions are good conductor of electric charge. However, after the alkali has been added
in, the conductivity of the solution decreases because most of the electric charge
transmit agent are being neutralize by the alkali. There is less hydronium ion in more
alkali solution. Thus, the conductivity of solution is higher when acid is added as
compared to alkali.

Next, we will look at the effect of water volume to the conductivity of the
solution with condition the amount of acid and alkali added are same in both
experiment. The water volume added in part 1b is more than that of part 1a. From
the result, we can see that the conductivity of the part 1a solution is higher than that
of part 1b. The amount of water and the concentration of acid-base affect the pH
value and their conductivity. When the water volume is increased, the solution tends
to become more diluted as the amount of acid alkali added is the same. This means
that the distance between ions are increased and it will take longer time for the
electric charges to be transmitted in larger medium which has same hydronium ions
as in the smaller medium. Thus, when the amount of acid alkali added is made
constant, the conductivity of the solution will decreases, when the water volume
added is increased.

For the second part of the experiment, the objective is to study the effect of
dissolved oxygen in the composition of water when two different gases are inserted
into the water. For part 2(a), we inserted air which contained 78% nitrogen gases,
21% oxygen gases and1 % of inert gases whereas for part 2(b), we inserted a pure
nitrogen gas into the dosing tank containing water. Thus, the result is collected from
the graph obtained from the experiment. The major concern is the amount of
dissolved oxygen in the solution.
From part 2b, we can see that there is significant change in the amount of
dissolved oxygen, from 7.88 to 0.2, this lead us to the conclusion that N 2 dissolves in
water much more than O2, and N2 took place of O2 in the solution and decreased the
amount of O2 in the solution. This is suitable with the fact is that the solubility of N 2
and O2 in the water are 0.0138 and 0.0089 g/kg, respectively.

However, in part 2a, although the amount of N 2 in air is quite high (79%) but
the amount of dissolved O2 was increased (from 7.91 to 8.13) but not decreased as in
part 2b. This may be due to the “affinity phenomena”. Oxygen existed in the solution
attracted more oxygen from air but not nitrogen, leading the amount of oxygen
dissolved increased.

The conductivity of the water in part 2a is higher as compared in part 2b. This
is because the dissolved oxygen contained in part 2a is higher. More dissolved
oxygen will lead to more acidic condition as there is more H+ ion presented in the
water. Acidic medium favours conductivity.

Error Analysis:

During the experiment, there are errors which occur and influence the accuracy of
the result obtained.
1) Parallax error may occur when water is added into the tank to a certain
desired level. As the tank is located quite high from the reach of student,
chances of parallax error is very high when student could not read the level of
the water directly proportional to the point made on the surface of the tank.
Proper scale is not given too.
 It is suggested to provide ladder for the student to ease the water level
measurement taking. Proper scale should be provided too in order to
make sure that the water level desired is correct.

2) The water volume added is not exactly the same as the theoretical volume
because it is hard to control the flow rate of the water and make sure that it is
exactly the same volume as what is required.
 Equipment like digital water flow rate controller could be used to make
sure that the volume obtained is correct.

3) The water tank is not cleaned properly at the end of each experiment. This
will affect the result obtained because if the tank is not cleaned thoroughly,
there are still some contaminated liquid present in the tank. When clean water
is being added in, it will be contaminated too when the water is blended with
the previous contaminated liquid which still left in the tank.
 The tank should be designed in a way that it can be taken out for
cleaning purpose and installed back again. By this way, the chance of
new water added being contaminated can be lessened.

Conclusion:

pH value of the solution will affect the conductivity of the solution. The lower
the pH value, the higher the conductivity. When amount of water increases with the
condition the amount of acid added constant, the conductivity will decreases due to
the increases of electric charge transmission distance. Besides, when the dissolved
oxygen in water increases, it will create an acidic medium which will increase the
conductivity. In conclusion, the objectives of the experiment are achieved.

Appendix
Figure 1: Graph for Experiment 1, water at level A

Figure 2: Graph for Experiment 1, water at level C


Figure 3: Graph for Experiment 2, with air

Graph for Experiment 2, with nitrogen gas

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