ACID-BASE TITRATION

(NEUTRALIZATION TITRATION)

BY
Prof. Amol S. Jagdale
Assistant Professor
MVP’s College of Pharmacy, Nashik
 The Early History of Acid—Base Concepts
 The word acid derives from Latin acere, meaning sour. Bases
were referred to as alkali in early history and that word derives
from Arabic al-qili, the ashes of the plant saltwort, rich in
sodium carbonate.
 What are some uses/applications of acid–base titrations?

 They provide precise measurements.

 While manual titrations disadvantage are
 tedious (time consuming) ,
 more sample require
 chances personal error are more.
 ADVANTAGES OF AUTOMATED TITRATORS
 While automated titrators are often used that titrations
 can perform effortlessly,
 Accurately
 Precisely.
 Selectively
 Specifically
 Requires very low sample
 No need to use visualized indicator
 The increased efficiency and accuracy of automated instrumentation makes manual titrations
progressively more obsolete.
 Also, as regulatory requirements increase and audits become more commonplace, the cost of
continuing to do manual titrations will outweigh the cost of upgrading your lab to an automated
 Acid–base titrations are important in a number of
industries.
 Acid–base titrations are used in the
 food industry to determine fatty acid content,
 Acidity of fruit drinks,
 Total acidity of wines,
 Acid value of edible oils,
 Acetic acid content of vinegar (10% aq. acetic acid solution)
 They are used in biodiesel production to determine the acidity of waste vegetable
oil, one of the primary ingredients in biodiesel production; waste vegetable oil must
be neutralized before a batch may be processed to remove free fatty acids that
would normally react to make soap instead of biodiesel.
 Ammonia is very toxic to aquatic life; aquaria test for ammonia content.
 In the plating industry, boric acid concentration in nickel plating solutions is determined.
 In the metal industries, acid in etching solutions is determined.
 In the environmental arena, alkalinity or acidity of city and sewage water is determined.
 In the petroleum industry, the acid number of engine oil is determined, and acetic acid in
vinyl acetate.
 In the pharmaceutical industry, sodium hydrogen carbonate in stomach antacids is
determined.
 Acid–base titrations can be used to determine the percent purity of chemicals.
 The saponification value of carboxylic acids is used to determine the average chain
length of fatty acids in fat, by measuring the mass in milligrams of KOH required to
saponify the carboxylic acid in one gram of fat.
 Strong Acid versus Strong Base—The Easy Titrations

 An acid–base titration involves a neutralization reaction in which an acid is reacted with an equivalent
amount of base.
 By constructing a titration curve, we can easily explain how the end points of these titrations can be
detected.
 The end point signals the completion of the reaction. A titration curve is constructed by plotting the pH of the
solution as a function of the volume of titrant added.
 The titrant is always a strong acid or a strong base.
 The analyte may be either a strong base or acid or a weak base or acid In the case of a strong acid versus a
strong base, both the titrant and the analyte are completely ionized.
 An example is the titration of hydrochloric acid with sodium hydroxide:
 The equivalence point reaction is theoretically
complete
 The H and OH combine to form H2O, and the
+ −

other ions (Na+ and Cl−) remain unchanged, so

the net result of neutralization is conversion
of the HCl to a neutral solution of NaCl. The
titration curve for 100mL of 0.1 M HCl titrated
with 0.1 M NaOH is shown fig.
 The calculations of titration curves simply
involve computation of the pH from the
concentration of the particular species
present at the various stages of the titration
pH transition ranges and colors of some common
indicators.
 PREPARATION AND STANDARDIZATION OF SODIUM HYDROXIDE SOLUTION I.P

Sodium Hydroxide, 1 M:
PREPARATION:
Dissolve 42 g of sodium hydroxide in sufficient carbon dioxide-free water to produce
1000 ml. Standardise the solution in the following manner.
STANDARDIZATION:
Weigh accurately about 5 g of potassium hydrogen phthalate, previously powdered
and dried at 120° for 2 hours, and dissolve in 75 ml of carbon dioxide-free water. Add
0.1 ml of phenolphthalein solution and titrate with the sodium hydroxide solution until
a permanent pink colour is produced.
Factor formula:
1 ml of 1 M sodium hydroxide is equivalent to 0.2042 g of C8H5KO4.
Storage:
Store in bottles with well-fitted suitable stoppers which prevent access to atmospheric carbon
dioxide. Volumetric solutions of sodium hydroxide must be restandardise frequently. Solutions
of lower concentrations are prepared by quantitatively diluting accurately measured volumes of
0.1 M sodium hydroxide with sufficient carbon dioxide-free water to give the desired
concentration.
 Requirement: Other than Glasswares:
 Chemicals:  Burette Stand,
 NaOH (Pellatts),  Clamp,
 Oxalic Acid/Potassium Hydrogen Phthalate,  White Tile/White Thick Paper,
 Phenolphthalein Solution (1.0 % Methanolic)  Watch Glass
 Solvent:  Permanent Marker,
 Distilled Water/ Water (Freshly Boil and warm water should  Glass wool,
be used to prevent interference of Dissolved CO2 Which can  Spatula
form Na2CO3 as basic Interference which may get titrated  Butter Paper
 Filter Paper
with the primary standard used e.g. Oxalic Acid, Potassium
 Tissue Paper (Soft)
Hydrogen Phthalate
Glasswares: Safety Requirements for students
 Burette (25 mL/ 50 mL) ,  Gloves
 Pipette (1 mL),  Goggle.
 Graduated Volumetric Flask (100 mL)
 Conical Flask (25 mL/100 mL)
 Measuring Cylinder (50 mL)
 Glass Funnel
 Glass Rod
Note:
1.Water which can be used as solvent for the preparation 0.1 N aq. NaOH solution should be free
from dissolved CO2 gas, which can form Na2CO3 as basic Interference which may get titrated with
the primary standard used e.g. Oxalic Acid, Potassium Hydrogen Phthalate in the standardization.
(You can make water free from dissolved CO2 gas by heating around 70-80 oC then once water
heated cover the vessel in which it is heated once temperature of water comes to room
temperature use it)
2. Do filtration of prepared aq. NaOH solution prior to standardization by use of primary standard
substance.
3. The prepared aq. NaOH solution must be filter by use of Glass Wool (Do not use ordinary filter
paper for filtration of aq. NaOH solution because NaOH highly alkaline/basic which causes
decomposition of filter paper which can contain cellulose)
 2. Preparation of Phenolphthalein Solution (1.0 % Methanolic)
Weigh accurately 0.01g (10 mg) of Phenolphthalein powder dissolve in 10 mL of Methanol.

Note:
1. Phenolphthalein is white colour powder.
2. It turns colourless in acidic solutions and pink in basic solutions.
Procedure:
Weigh accurately oxalic acid in between 0.100-0.120 g (100-120 mg), transfer in to 250 mL conical flask to that add 15 mL
of Distilled water once dissolved completely to that add 1-2 drop of Phenolphthalein solution as indicator and titrate with
prepared aq. NaOH Solution drop wise, shake conical flask clockwise until it becomes faint pink.
Factor formula:
Each mL of 0.1 N aq. Sodium hydroxide solution = 0.0063 g of Oxalic acid (C 2H2O4.2H2O)
Burette reading (mL) of x N aq. Sodium hydroxide solution= Sample Weight (g) of oxalic acid

x N aq. Sodium hydroxide solution= Burette reading (mL) x 0.0063 g of Oxalic acid
0.1 x Sample Weight (g) of oxalic acid
 Note:
Put the burette reading (B.R) and sample weight(g)in the lower factor formula and do cross multiplication.

FACTOR FORMULA:

Each mL of 0.1 N aq. Sodium hydroxide solution = 0.0063 g of Oxalic acid (C 2H2O4.2H2O)

15.8 mL of x N Sodium hydroxide solution= 0.100 g of oxalic acid (C2H2O4.2H2O)

x N Sodium hydroxide solution= 1x 0.1 x 0.100/15.8 x 0.0063

=0.01/0.0756

=0.01/0.09954

=0.1005N
Note:
1. Oxalic acid must be dried in oven at 105oC to remove moisture content (water) or adsorbed gases on to
the surface of oxalic acid. If drying is not done before weighing of sample (oxalic acid) so due to presence
of moisture content or adsorbed gases on to the surface of sample the weight of sample may get added
depending on how much amount of moisture content present in sample for e.g. if non-dried sample is used
if weight taken is 120 g (120 mg) if 5 mg moisture present in such case the actual weight of sample is 120-
5= 115 mg. Here due to presence moisture content error (i.e. determinate/systematic error) may get added
which can affect the accuracy result.
2. Calibrated volumetric glassware must be used to minimize error in the standardization procedure.
3. The end point has been reached when the pale pink colour of the phenolphthalein persists for 30
seconds.
3. During weighing NaOH pellet use watch glass. (place small size watch glass on weighing balance and add
NaOH pellet over it once weighed immediately transfer to conical flask and rinse surface of watch glass with
solvent to prevent weight loss. (For preparation of 0.1 N/M aq.NaOH solution 0.400 g (400 mg) of NaOH pellet
are required).

Do not use butter Paper/filter paper because NaOH pellet are hygroscopic which can absorb moisture and due
to that it may get adhere to surface of paper which may lead to weight loss of NaOH.

4. Exothermic reaction take place during solubilisation of NaOH (Heat get released because NaOH is strong
base i.e. highly alkaline. ( Care must be taken when preparing concentrated solutions of sodium
hydroxide because of the large amounts of heat released so keep beaker containing water in to cold water
bath then add NaOH in beaker with constant stirring with help of glass rod)
5. Avoid direct contact of NaOH solution to the skin which may lead to irritation. If accidently in contact

with skin/tongue/eye repeatedly wash with water.

6. Once Burette is filled with aq. NaOH Solution must consider lower meniscus (in case of coloured

solution Upper meniscus must be considered)

7. Use white tile/ thick white paper as background for correct visualization of end point detection i.e.

colour change take place from colourless to pink. (Place tile/ thick white paper on the surface of burette

stand)
 Observation Table:
Sr.No. Weight of Burette Reading (mL) End Point
sample/analyte taken
(g) Initial Final Difference

Colourless
1 to faint pink
2
Sr.No.
3 Weight of Burette Reading (mL) End Point
sample/analyte Initial Final Difference
taken (g)
Colourless
1 0.100 0.00 15.8 15.8 to faint
2 0.120 15.8 31.7 15.9 pink

Note: 3 0.125 31.7 47.6 15.8

1. If Sample weight is different as per above observation table you must do calculation separately in each case
Sr.No. Weight of Burette Reading (mL) End Point
sample/analyte
Initial Final Difference
taken (g)
Colourless
1 0.100 0.00 15.8 15.8 to faint
pink
2 0.115 15.8 31.7 15.9