CHAPTER I

PREFACE

1.1. Objectives
1. Understand the step by step of titrimetric analysis and can accurately perform
volumetric analysis or acidic-alkalimetric titration
2. Able to calculate equivalent point based on acid-base reaction, and can select
correct indicator for acidic-alkalimetric analysis
3. Able to determine the concentration of acid-base solution and its reaction with
standard solution
4. Able to correctly use laboratory apparatus and properly perform dilution
experiment

1.2. Principle
Acid neutralisation reaction by base or vice versa will form salt that suit the
nature of acid/base. This neutralisation reaction will be finished when the amount of
acid is equal with the amount of base, no excess. It can be determined by monitoring pH
value of salt. Visually, the use of indicator will indicate that the reaction is equivalent.
Permanently colour changing signifies that the reaction is above equivalent.

1.3. Basic Theory

The term ‘titrimetric analysis’ refer to quantitative chemical analysis carried out
by determining the volume of a solution of accurately known concentration which is
required to react quantitatively with a measured volume of a solution of the substance to
be determined (Jeffery et al, 1989).

Titration, by definition, is the addition of known concentration of base (or acid)

to a solution of acid (or base) of unknown concentration. Since both volumes of the acid
and base are known, the concentration pf the unknown solution is then mathematically
determined (Poulsen, 2010).

The earliest acid–base titrations involved the determination of the acidity or

alkalinity of solutions, and the purity of carbonates and alkaline earth oxides. Before
1800, acid–base titrations were conducted using H2SO4, HCl, and HNO3 as acidic
titrants, and K2CO3 and Na2CO3 as basic titrants. End points were determined using
visual indicators such as litmus, which is red in acidic solutions and blue in basic
solutions, or by observing the cessation of CO 2 effervescence when neutralizing CO32–.
The accuracy of an acid–base titration was limited by the usefulness of the indicator and
by the lack of a strong base titrant for the analysis of weak acids (Harvey, 2000).

One of the most common and straightforward means of comparison is by way of

titration, which consists of measuring the amount of a standard solution that reacts
 Figure 7.8 A buret, a long glass tube with marks on it and a stopcock
on the end, is used to measure the volume of standard solution added to a
sample during titration.

with a sample using the apparatus illustrated in Figure 7.8. As an example

consider a hospital incinerator with a water scrubbing system to clean exhaust gases.
Suppose it is observed that the scrub water contains hydrochloric acid from the burning
of chlorine-containing plastics and that this acid is corroding iron drain pipes, a problem
that can be eliminated by adding sodium hydroxide to neutralize the acid.

The amount of base needed may be determined by titration, a procedure in

which a measured volume of the hydrochloric acid-containing scrub solution is reacted
with a standard solution of NaOH,

HCl(aq) + NaOH(aq)  NaCl(aq) +H2O

until just enough base has been added to react with all the HCl in the measured
volume of sample. The point at which this occurs is called the end point and is shown
by an abrupt change in color of a dissolved dye called an indicator. Phenolphthalein, a
dye that is red in base and colorless in acid is commonly used as an indicator (Manahan,
2001).

The primary purpose of a titration is to measure an unknown amount of a

substance in a sample, as determined via a chemical reaction with a known amount of a
suitable reagent. We perform the titration to as certain when an equivalent amount of
the reagent has been added to the sample. When the amount of acid and alkali are just
equal,we have the equivalence point, from which we can determine the unknown
amount (Monk, 2004).
 CHAPTER II
WORK SCHEME

2.1. Work Scheme

1. Experiment: Titration of Strong Acid by Strong Base

HCL 0.1 M

Prepare 40 mL standard of NaOH 0.05 M and put into

Volumetric pippete. Write down the volume of solution.

Take 10 mL of 0.1 M HCl solution and put into

Erlenmeyer flask. Then add 20 mL of aquadest.

Add 3 drops of PP Indicator

HCL + PP Indicator

Slowly titrate the solution (approximately 1 drop per

second) and quickly stirred the flask. When the colour is
solution is changing into red, slower the titration
frequency until you have got permanent soft red. Record
the volume of solution that used.

If the permanent colour is too strong (bright/dark red),

repeat the procedure.(Strong colour indicates too much
titrant volumes above its end-point of titration)

Calculate HCl concentration based on this experiment.

Result

2. Experiment: Titration of Strong Acid by Strong Base (Without Indicator)

HCL 0.1 M

Prepare 0.05 M standard of NaOH and put into

Volumetric pippete. Write down the volume of solution.

Take 10 mL of 0.1 M HCl solution and put into

Erlenmeyer flask. Then add 20–40 mL of aquadest.
Write down the pH value.
HCL + PP Indicator

Slowly titrate the solution using magnetic stirrer and pH

 meter. Read the pH value when add NaOH in variative
volume.

Stopped the titration, when pH meter show pH of 10.

Using graphic, determine at which volume is pH

equivalent = end-point of titration.

Calculate HCl concentration based on this experiment.

Compare the results.

Result

3. Experiment: Titration of Weak Base by Strong Acid

Sodium Carbonate 0.1 M

Prepare 10 mL of Sodium Carbonate 0.1M, and put the

solution into Erlenmeyer flask. Then, add 20-40 mL of
aquadest.

Add 5 drops of PP
Sodium Carbonate + PP Indicator

Slowly Titrate the solution using HCl standard solution

0.1 M until the colour of the solution is clear/colourless.
(As an alternative, concentration of HCl solution from
experiment I can be used as titrant).

Record the HCl volume needed for this experiment.

Add 3 drops of MO Indicator.

Sodium Carbonate + PP Indicator + MO
Indicator

Continue the titration using HCl 0.1 M, until the colour

of the solution changing into permanently soft red.

Record the HCl volume needed for second titration.

Calculate the concentration of Na2CO3 and HCO3 that

have been formed in this titration.
Result
 CHAPTER III
DISCUSSION

3.1. Observation Result

1. Experiment: Titration of Strong Acid by Strong Base

No. Observation Treatment Description/Reaction

1. Make the solution  Take 10 mL of 0.1 M HCl
solution and put into
Erlenmeyer flask.
 Add 20 mL of aquadest into
HCl solution
 Add 3 drops of PP Indicator

2. Titration process  Prepare 40 mL standard of

NaOH 0.05 M and put into
Volumetric pippete.
 Titrate the solution until the
color change into permanent
soft red.
 2. Experiment: Titration of Strong Acid by Strong Base (Without Indicator)

No. Observation Treatment Description/Reaction

1. Make the solution  Take 10 mL of 0.1 M HCl
solution and put into
Erlenmeyer flask.
 Add 20-40 mL of aquadest
into HCl solution
 Measure the pH value
20 mL = 1.84
40 mL = 1.91

2. Titration process  Prepare standard of NaOH

0.05 M and put into
Volumetric pippete.
 Slowly titrate the solution
using magnetic stirrer and pH
meter Read pH value when
add variative volume.
 Stopped the titration, when pH
meter show pH of 10
 pH value:
2.5 mL
2.5 mL = 1.93
5.0 mL = 1.99
7.5 mL = 2.06
10.0 mL = 2.16
12.5 mL = 2.30
15.0 mL = 2.48
1 mL
16.0 mL = 2.58
17.0 mL = 2.72
18.0 mL = 2.91
19.0 mL = 3.28
0.2 mL
19.2 mL = 3.49
19.4 mL = 3.95
19.6 mL = 5.35
19.8 mL = 6.59
 0.1 mL
19.9 mL = 7.79
20.0 mL = 7.99
0.2 mL
20.2 mL = 9.12
20.4 mL = 9.58
20.6 mL = 9.77
20.8 mL = 9.94
21.0 mL = 10

3. Experiment: Titration of Weak Base by Strong Acid

No Observation Treatment Description/Reaction

.
1. Prepare the solution  Prepare 10 mL of Sodium
Carbonate 0.1M, and put the
solution into Erlenmeyer flask.
 Add 20-40 mL of aquadest.
 Add 5 drops of PP

2. Titration Process  Slowly Titrate the solution

using HCl standard solution
0.1 M until the colour of the
solution is clear/colourless.
(As an alternative,
concentration of HCl solution
from experiment I can be used
as titrant).
 Record the HCl volume
needed for this experiment.
Volume: 6.9 mL
 Add 3 drops of MO Indicator
3. Second Titration Process  Continue the titration using
HCl 0.1 M, until the colour of
the solution changing into
permanently soft red.
 Record the HCl volume
needed for second titration.
Volume: 12.1 mL
3.2. Discussion
The fifth practicum of Enviromental Chemistry I subject which is held on
31 October 2017 at 8.00 am – 11.30 am in Measurement of solution based on
acid-base reaction (acidic-alkalimetric). Titrimetric analysis is a simple method,
which is cheap, has good endurance and accuracy, and thus has been widely
used in the analysis of chemical equivalent. However, since the reaction
occurred in this method is not specific, some precursor ions may disrupt the
accuracy of the analysis. Primarily, every groups of acid will reacts with any
groups of base. Therefore, on the analysis of specific acid/base, it has to be sure
that the solutions were not mixed with other compounds. In this method, some
amount of acid/base will be quantitatively reacted with standard solution. The
basis of calculation is mol equivalencies on stoichiometric reaction. So if,
reagent 1 is an analyte and reagent 2 is a standard (vice versa), the equations
were as follows:
V1 x M1 = V2 x M2
V1 x N1 = V2 x N2

It has to be noted that normality (N) will correlate with molaritas (M) as
much asionisation potential equal with proton (H+) or electron (e-) mol.

On titrimetric analysis, standard solution placed inside the burette (were

called titrant) were used to titrate the analyte (solution inside the erlenmeyer)
until it reach equivalent or end-point of titration. Equivalent point will indicate
the amount of acid/base in the analyte is equivalent with the amount of acid/base
from the titrant, thus the procedure has to be stopped and considered done. The
amount of the analyte will be calculated based on its equivalent with the
required mol titrant in this experiment.

The end of titration has to be clearly monitored to understand the

potential electricity turning point, extreme pH changing, potential, the formation
of turbidity, permanentbcolour changing, etc. Ideally, the end-point of titration
has to be equal with equivalent point. However, late monitoring of end-point,
may create big deviation on pH range or colour changing above standard limit.
Hence, it is important to choose indicator that appropriate with the nature of
reaction. Moreover, it also needs thorough and propermonitoring during
procedure.

Requirements criteria for good titrimetric analysis:

1. Reaction is occurred very fast/spontaneous between titrate and titrant
(e.g. most ionic reactions are meet the criteria).
2. Simple reaction that can be visualised in stoichiometric model
3. Equivalent point is easy to monitored using the nature of solution
(physically or chemically). Indicator can also be used for easier
monitoring.
4. The apparatus for volume measurement is in good condition and
calibrated
 Volumetric or titrimetric analysis is classified in 4 groups, i.e. acid-base
titration, redox titration, precipitation titration, and complexometric titration. In
this experiment, only acid-base titration will be performed. Acid-base titration
(acidic-alkalimetric analysis) is a titration method with the concept of acid
neutralisation by base or vice versa. Materials and apparatus for this experiment
are:

1. Apparatus include:
 Volumetric pipettes
 Pipette
 Cylinder glass
 Wash bottle
 Burette
 Beaker glass
 Spatulas
 Erlenmeyer flask 250 mL
 Stirrer
 pH meter
 Volumetric flask 100 mL

2. Materials include:
 Aquadest
 HCl 0.1 M
 NaOH 1 M
 Phenolphtalein (PP) Indicator
 Methyl Orange (MO) Indicator
 Sodium Carbonate 0.5 M

There are 3 experiment that we must do that day. First is, Titration of Strong
Acid by Strong Base. We should make the solution using 10 mL HCl 0.1 M. Take HCl
using Volumetric pippete and put in Erlenmeyer flask. After that, dilute using 20 mL
aquadest for decrease the pH value so it will easy for use to do titration process (find the
equivalent point) and add 3 drops PP as indicator of titration process. Take 40 mL
NaOH using Volumetric pippete and do the titration process with slowly. Monitor the
colour shifting until reach permanent soft red. The reaction of this titration process is:
NaOH + HCl ⇄ NaCl + H2O
In theoritical, 1 mol NaOH equivalent with 1 mol HCl. So, mol NaOH = mol
HCl when reach equivalent point. The formula is:
MHCl x VHCl = MNaOH x VNaOH
MHCl x 30 = 0.05 x 40
MHCl = 2/30
MHCl = 0.067 M
 Second is of Strong Acid by Strong Base without Indicator. Make the solution
using 10 mL HCl 0.1 M by Volumetric pippete. Put in Erlenmeyer flask and add 20 mL
aquadest for 2 times. Don’t forget to measure the pH value using pH meter. The pH
value is 1.84 (20 mL) and 1.91 (40 mL). Prepare the NaOH as titrant. Put the
Erlenmeyer flask in magnetic stirrer. It’s used to help us in titration process.Turn on the
magnetic stirrer and titrate the HCl with NaOH. Add NaOH with variant volumes. Read
the pH value using pH meter every addition of variant volumes of NaOH. Stop the
titration when pH meter show 10.

HCl + NaOH (mL) pH HCl + NaOH (mL) pH

2,5 1,93 19,4 3,95
5 1,99 19,6 5,35
7,5 2,06 19,8 6,59
10 2,16 19,9 7,79
12,5 2,3 20 7,99
15 2,48 20,2 9,12
16 2,58 20,4 9,58
17 2,72 20,6 9,77
18 2,91 20,8 9,94
19 3,28 21 10
19,2 3,49

From this data, we can make grahpic about correlation between volume (x) and
pH value (y).
 pH
12

10

8
pH
6 f(x) = 0.322445400566834 x Linear (pH)
R² = 0.859192778429552
4

0
0 5 10 15 20 25 From
this graphic,
we can conclude that when the volume of NaOH is increase, the pH changing higher.

Last experiment is Weak Base by Strong Acid. Prepare the titrate solution with
10 mL Na2CO3 0.05 M.Used Volumetric pippete and put in Erlenmeyer flask. Na2CO3
solution is colorless and no smell. Dilute with 20 mL aquadest and add 5 drops PP into
the solution, as indicator for equivalent point. The color will shift into pink. Take HCl
0.1 M using Volumetric pippete and do the titration process. Do this titration until the
color shifting into colorless. The volume of HCl that used is 6.9 mL.

After that, add 3 drops MO to the solution. Titrate the solution again using HCl
until the color shifting into permanent red brick. The volume of HCl that used in this
second titration is 12.1 mL. In weak base by strong acid, in theoritical, that will produce
acid salt. Good equivalent point, showed by indicator that shifting in appropriate neutral
pH. PP used to know the condition of HCl is equivalent with HCO 3 and they need
6.9mL HCl 0.1 M. Beside that, MO used to knowthe condition when Na 2CO3 equivalent
with HCl and they need 12.1 mL HCl 0.1 mL. The reaction is:

Na2CO3 + HCl + H2O ⇄ NaHCO3 + NaCl

Na2CO3 + 2HCl ⇄H2CO3 + 2NaCl
H2CO3⇄ H2O + CO2

When HCO3 equivalent with HCl in first titration, the formula is:

M HCl x V HCl(i)
−¿= ¿
V Na2CO 3
M HC O3

0 ,1 x6 , 9
−¿= ¿
30
M HC O 3

0 ,69
−¿= ¿
30
M HC O3
 −¿=0 ,02 3 M ¿
M HC O3

And when the reaction work fully Na2CO3 equivalent with HCl when th color
shift into red brick. SO, the total titration is condition that show equivalent. The formula
to find molarity of Na2CO3 is:

M HCl x V HCl Total

M Na2 CO3 =
V Na2 CO3

0 , 1 x (6 , 9+12 ,1)
M Na2 CO3 =
30

0 , 1 x 19
M Na2 CO3 =
30

1,9
M Na2 CO3 =
30

M Na2 CO3 =0.6333 M

CHAPTERIV
 CONCLUSION

4.1. Conclusion

Titrimetic analysis used manual and the point is mixed 2 solution that different
and one of them we know the concentration or we called it standard solution. The
titration will be end when the solution is equivalent. Equivalent is condition when the
indicator show the alteration into they limit. By using indicator, it will help us to know
the end point of titration. Indicators have different characteristic at each others.

To decide the concentration we can do when scond solution is equivalent.

Because, when the ratio of each solution, we can predict the other concentration using
V1 x M1 = V2 x M2. We can use Volumetric pippete to titrate the solution, beside used
burette. But, we just need to do this titration with carefully. pH meter used to measure
the pH value optimalically or we just can used indicator.

4.2. References

Harley, David, 2000, Titration Base on Acid-Base Reactions, Modern Analytical

Chemistry, United States, McGraw-Hill Companies, Page 278

Jeffery, G.H., J. Bassett, J.Mendham, R.C. Denney, 1989, Titrimetric Analysis, Vogel’s
Textbook Of Quantitive Chemical Analysis, United States, John Wiley &
Sons, Inc., Fifth Edition, Page 257

Manahan, Stanley, 2001, Standard Solutions and Titrations, Fundamentals of

Environmental Chemistry, Second Edition

Monk, Paul, 2004, Titration Analyses, Physical Chemistry, United Kingdom, John
Wiley & Sons Ltd, Page 263

Poulsen, Tracy, 2010, The Titration Process, Introduction to Chemistry, United State,
CK-12 Foundation, Pg 187

CHAPTER V
 QUESTION

5.1. Question and Answer

1. Write down the chemical reaction equations from experiment I and II, and
calculate the equivalent pH! Did the selection of indicator is correct? Explain!

Answer:
Experiment I:
NaOH + HCl ⇄ HCl + H2O
n NaOH = 0.05 x 40 = 2 mol
n HCL = 0.067 x 30 = 2 mol

NaOH HCL HCl H2O

M 2 mol 2 mol - -
R 2 mol 2 mol 2 mol 2 mol
S - - 2 mol 2 mol

Because this is strong acid and base acid reaction, the equivalent pH is 7
(neutralization)
Experiment II:
Na2CO3 + HCl + H2O ⇄ NaHCO3 + NaCl
Na2CO3 + 2HCl ⇄H2CO3 + 2NaCl
H2CO3⇄ H2O + CO2
n Na2CO3 = 0.63 x 30 = 18.9 mol
n HCL = 0.1 x 19 = 1.9 mol
Na2CO3 2HCl H2CO3 2NaCl
M 18.9 mol 1.9 mol - -
R 0.85 mol 1. 9 mol 0.85 mol 1.9 mol
S 18.05 mol - 0.85 mol 1.9 mol

H2CO3 ⇄ H+ + HCO3-

M HCO3- = 0.85/30 = 0.02 M

[H+] = √ Ka. Ma
[H+] = √ (4.3 x 10−7 ) x(2 x 10−2 )
[H+] = √ 8.6 x 10−9
[H+] = 2.93 x 10-4.5
 pH = - log [H+]
pH = - log 2.93 x 10-4.5
pH = 4.5 + 0.47
pH = 4.97

The PP and MO indicator that used in this practicum is correctly. PP used to

show the solution is shifting from base to neutral and MO show the shifting from
neutral to acid.

2. In experiment II, why do we need 2 types of indicators?

Answer:

Because there are a big pH changing from base to acid. Beside that, pH changing
trajectory indicator is limited, there is nothing cover vboth of them. So, we need
to use 2 indicators, PP for indicate from base to neutral and MO to indicate
neutral to acid.

3. Estimate the graphic chart from experiment II (mL titrant vs pH)!

Answer:

PP indicator

MO indicator

4. Give some examples on the application of acid-base titration in environmental

analysis!

Answer:

 Neutralization process or decrease the acidity level to water that have acidic
pH value using a substance that characteristic is base
 To know that environment is contamined or not

OFFICIAL LABORATORY REPORT

 ENVIRONMENTAL CHEMISTRY
“MEASUREMENT OF SOLUTION BASED ON
ACID-BASE REACTION (ACIDIC-
ALKALIMETRIC)"

NAME : MUHAMMAD RIFANI

NRP : 03211740000056
LECTURER : ARSETO YEKTI BAGASTYO, ST., MT., M.Phil., Ph.D.
LABORATORY’S ASSISTANT : KIKI GUSTINASARI, S.T.

ENVIRONMENTAL ENGINEERING DEPARTMENT

FACULTY OF CIVIL ENGINEERING, ENVIRONMENT AND GEOSCIENCE
SEPULUH NOPEMBER INSTITUTE OF TECHNOLOGY
2017