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Laboratory Manual: Prepared by
Laboratory Manual: Prepared by
Laboratory Manual: Prepared by
Prepared By
Md. Imran Nur Manik
Lecturer
Department of Pharmacy
Northern University Bangladesh
Manual: Physical Pharmacy-I Lab
05.
d . of constant pH buffer.
Preparation 11 – 12
M
Bibliography and Some commonly used Lab Equipment. 12
Principle:
The concentration of a solution is defined as: the amount of solute present in a given amount of solution.
The concentration of a solution can be expressed as molarity, molality normality, mole fraction etc.
Molarity (M): Molarity is the number of moles of solute dissolved per liter of solution. It can be mathematically
expressed as, Moles of solute
Molarity( M )
Litre of solution
Example: Calculate the molar concentration of sodium sulphate (Na2SO4; MW=142 gm).That contains 2.8 gm of
Na2SO4 in 1500mL solution.
SOLUTION:
Moles of solute n
We Know That, Molarity( M ) or, M ...................( i )
Litre of solution V(in litre)
Here, Molecular mass of Na2SO4 = (232 + 32 + 164) gm=142 gm
M
Problem: Calculate the amount required to prepare 250 mL, 0.25M HCl. Purity of acid is 32%.
Normality (N): Normality is the number of gram equivalent (eq.) weights of solute (solu.) per liter of solution.
Equivalent mass (Eq. M.)/Gram equivalent Wight: Equivalent mass of a substance can be calculated
by dividing its molar mass per the number of active units in one molecule of this substance (k) thus:
The active unit in the acid-base reactions is the number of hydrogen ions liberated by a single molecule of an acid
or reacted with a single molecule of a base.
For e.g. 1 mole of NaOH (m.wt. = 40) can combine with 1 mole of hydrogen ion, therefore the equivalent weight
of NaOH is 40÷1=40 gm. Thus the concentration of 1N NaOH is same as 1M NaOH.
98
On the other hand H2SO4 has two ionisable hydrogen atoms; its equivalent mass will be, Eq.M. 49 g
2
Thus, the concentration of 1M H2SO4 is same as 2N H2SO4.
Problem: Calculate the amount required to prepare 0.1N H2SO4.Having density of 1.19 g/mL and 98%
purity.
Concentration can also be calculated by dilution method when the concentration and volume of one of the
two reactants is known.
Dilution: It is the addition of solvent to decrease the concentration of solute. The solution volume changes, but
the amount of solute remains constant.
M1V1 = M2V2
Initial values Final values
Problem: How to made 100 mL 0.1M NaCl from 5M NaCl solution?
Calculation:
All calculations are to be done as per the solutions to be made, needed for the experiment.
Apparatus: 5. Beaker i k
6. n
Measuring cylinder
Ma
1. Electrical balance
2. Pipette and pipette filler 7. Spatula
3. Funnel 8. Stirrer
4. Volumetric flask 9.
u r Permanent marker
Chemicals/Reagents: N
a n
Write all the reagents required to prepare the solutions (as per the solutions to be made for the experiment)
r
Experimental procedures: (Specimen)
Im
d .
Preparation of 1M 50 mL NaOH solution:
1. Weigh out accurately W gm (To be calculated) of NaOH.
M
2. Transfer it to 50 mL volumetric flask.
3. At first completely dissolve it with small volume of distilled water (DW).
4. Finally adjust the volume up to the 50 mL mark with DW Q.S.
Comments:
The term 'titrimetric analysis' refers to quantitative chemical analysis. It is carried out by determining the
volume of a solution of accurately known concentration, required to react quantitatively with a measured volume
of a solution of the substance to be determined. The solution of accurately known strength is called the standard
solution.
In titrimetric analysis the reagent of known concentration is called the titrant and the substance being
titrated is termed the titrand or analyte.
The process of adding the standard solution until the reaction is just complete is termed a titration, and
the substance to be determined is titrated. The point at which this occurs is called the equivalence point or the
theoretical (or stoichiometric) end point.
The completion of the titration is detected more usually, by the addition of an auxiliary reagent, known
as an indicator. After the reaction between the substance and the standard solution is practically complete, the
indicator should give a clear visual change (either a colour change or the formation of turbidity) in the liquid
being titrated. The point at which this occurs is called the end point of the titration.
Principle
k
In titrimetry, chemicals used as reference solutions known as primary standards or secondary standards.
i
n
Primary Standards
Ma
A primary standard is a compound of sufficient purity from which a standard solution can be prepared by
N
n
A primary standard should satisfy the following requirements.
a
r
1. It must be easy to obtain, purify, dry (preferably at 110-120°C), and to preserve in a pure state.
Im
(This requirement is not usually met by hydrated substances, since it is difficult to remove surface moisture
completely without effecting partial decomposition.)
d .
M
2. It should be unaltered in air during weighing; that means, it should not be hygroscopic, oxidised by air, or
affected by carbon dioxide.
3. It should maintain an unchanged composition during storage.
4. It should be capable of being tested for impurities by qualitative and other tests of known sensitivity.
(The total amount of impurities should not, in general, exceed 0.01-0.02%)
(b) Complex formation reactions: Silver, Silver nitrate (AgNO3), Sodium chloride (NaCl), various metals
(e.g. Spectroscopically pure Zinc, Magnesium, Copper, and Manganese) and salts, depending upon the reaction
used.
(c) Precipitation reactions: Silver, Silver nitrate (AgNO3), Sodium chloride(NaCl), Potassium chloride (KCl),
and Potassium bromide(KBr) (prepared from potassium bromate).
Secondary Standards
Solutions that are prepared by standardisation against a primary standard are referred to as secondary standards.
It follows that, a secondary standard solution is a solution in which the concentration of dissolved solute has not
been determined from the weight of the compound dissolved, but by the reaction (titration) of a volume of the
solution, against a measured volume of a primary standard solution.
In the present experiment, NaOH solution is to be used secondary standard chemical and needs to be
This is a 1:1 titration therefore, one mole of base, will titrate one mole of acid.
i k
standardized by the primary standard chemicals. Here the primary standard chemical is KHP.
n
Ma
The end point of the solution would be determined by an indicator, phenolphthalein.
Reaction:
u r
N +Na+, K+
a n
r
Im
Phenolphthalein: Phenolphthalein exists in two tautomeric forms: (i) the benzenoid form which is yellow and
present in basic solution; and (ii) the quinonoid form which is pink and present in acid solution.
d .
M
Calculation (Sample): Full calculations required to make the reagents, for the experiment must be written down
2. 0.1 N 250 mL NaOH solution: Take 1 gm NaOH in a 250 mL volumetric flask. Completely dissolve
it with small portion of DW (e.g.125 mL). Finally adjusted the volume up to the 250 mL mark by Q.S. of distilled
water.
3. 0.5% 100 mL Phenolphthalein solution: 50 mL Ethanol+ 0.5 gm Phenolphthalein+ 50 mL DW.
Procedures:
= N
Precautions:
Comments:
Principle
An acid-base titration involves the addition of a titrant solution to an analyte solution. In titrimetry, chemicals used
as reference solutions known as primary standards or secondary standards.
A primary standard is a reagent that is extremely pure, stable, has no water of hydration, and has a high
molecular weight. A secondary standard solution refers to a solution that has its concentration measured by
titration with a primary standard solution.
The secondary standard chemicals are not absolute pure and may contain some impurities that come during their
synthesis. Therefore the secondary standard chemical should standardize by using the primary pure chemicals.
In the present experiment, NaOH solution is to be used secondary standard chemical and needs to be
standardized by the primary standard chemicals. Here the primary standard chemical is Oxalic acid. After being
standardized by the Oxalic acid, NaOH is to be used for the standardization of HCl.
Reaction:
1. H2C2O4 (aq) + 2NaOH (aq) ⇌ Na2C2O4 (aq) + 2H2O (l)
i k
2. HCl (aq) + NaOH (aq) ⇌H2O (l) + NaCl (aq)
n
Ma
Apparatus:
u r
Chemicals / Reagents:
1. Electrical balance
2. Spatula
N1. 0.1 N Sodium hydroxide (NaOH) solution
2. 0.1 N Oxalic acid (dihydrate) [H2C2O4.2H2O]
3. Volumetric flask
a n 3. 0.1 N Hydrochloric acid (HCl) solution
4. Measuring cylinder r 4. 0.5% Phenolphthalein indicator
5. Burette
6. Pipette and pipette filler Im 5. Distilled Water
7. Conical flask
8. Beaker d .
9. Funnel M
Calculation (Sample): Full calculations required to make the reagents, for the experiment must be written
down.
Gram equivalent weight of H2C2O4 = (126.08 ÷ 2) gm = 63.040 gm
100 mL 0.1N H2C2O4 = {(63.0401000.1)÷ ÷1000 }gm = Y gm (for 100% pure H2C2O4)
2. 0.1 N 1000 mL NaOH solution: Completely dissolve 4.12 gm of NaOH (97%) in a1000 mL volumetric
flask with a small volume of DW. Finally adjust the volume up to 1000 mL mark by adding distilled water
Q.S.
3. 0.1N 100 mL HCl solution: Take 1.14 mL of HCl (32%) and completely dissolve it in 100 mL
volumetric flask in 100 mL DW.
4. 0.5% 100 mL Phenolphthalein solution: 50 mL Ethanol+ 0.5 g Phenolphthalein+ 50 mL DW.
Procedures:
1. Standardization of NaOH solution by Oxalic acid Solution:
Ma
= Strength of NaOH, S2 = ?
Im
b) Take 10 mL prepared 0.1N HCl solution in a conical flask.
c) Add 1-2 drops of Phenolphthalein indicator in the acid solution and titrate it with the NaOH solution,
.
until the colour of acid solution changes from colourless to faint pink.
d
M
d) Perform another two titrations and calculate the result.
= N
Result: The strength of HCl= N.
Precautions:
Comments:
Principle
A buffer solution is one which resists (or buffers) a change in its pH. If acid is added then, within reason, the pH
does not fall; if base is added, the pH does not rise. Buffers are usually composed of a mixture of weak acids or
weak bases and their salts and function best at a pH equal to the pKa of the acid or base involved in the buffer.
The equation that predicts the behaviour of buffers is known as the Henderson–Hasselbalch equation
(named after chemists Lawrence Joseph Henderson and Karl Albert Hasselbalch). It is derived as follows, by
considering a weak acid that ionises in solution.
[Salt]
pH pKa log
[Acid]
[Salt]
or, pKa pH log
[Acid]
Where, pKa=–log Ka; and Ka=Decomposition constant of acid.
An example of a buffer is a mixture of acetic acid and sodium acetate, which ionises and acts as follows:
CH3COOH⇌CH3COO– +H+
CH3COO–Na+⇌CH3COO– +Na+
i k
Apparatus: n
1. Electrical balance
2. Spatula Ma
3. Volumetric flask
u r
4. Measuring cylinder
5. Burette N
6. Pipette and pipette filler
a nFig. Mechanism of Buffer action of an acid buffer.
7. Conical flask
r
8. Beaker
9. Funnel Im
Chemicals / Reagents:
d .
M
1. 0.1 N Sodium hydroxide (NaOH) solution
2. 1% Acetic acid (CH3COOH) solution
3. 0.1 N Oxalic acid (dihydrate)[ H2C2O4.2H2O]
4. 0.5% Phenolphthalein indicator
5. Distilled Water
Calculation: Full calculations required to make the reagents, for the experiment must be written down.
Preparation of Reagents:
A. 1% 100 mL Acetic Acid Solution: Take 1 mL glacial acetic acid (100%) in a 100 mL volumetric flask, and
then adjust the volume up to 100 mL mark by adding distilled water.
B.0.1 N 1000 mL NaOH Solution: Completely dissolve 4.12 gm NaOH (97%) pellets in a 1000 mL volumetric
flask at first with a small portion of DW, and finally adjust the volume up to the mark by adding DW Q.S.
C.0.1 N 100 mL Oxalic Acid Solution: Completely dissolve 0.636 gm oxalic acid (99%) in a 100 mL volumetric
flask at first with a small portion of DW, and finally make the volume up to mark by adding distilled water Q.S.
Procedures:
1. Standardization of NaOH solution by Oxalic acid Solution:
u r
= N
N
The strength of NaOH = N. a n
r
Im
3. Determination of the strength of CH3COOH solution by NaOH solution:
a) Fill the burette with the standardized NaOH solution.
d .
b) Take 10 mL prepared Acetic acid (CH3COOH) solution in a conical flask.
c) Add 1-2 drops of Phenolphthalein indicator in the acid solution and titrate it with the NaOH solution,
M
until the colour of the acid solution changes from colourless to faint pink.
d) Perform another two titrations and calculate the result.
= N
The strength of CH3COOH = N.
1) Take 40 mL 1% Acetic acid solution and 20 mL standardized NaOH solution in a 100 mL beaker and
mix them very well.
2) Then measure the pH of the buffer solution using a pH meter.
[Salt]
pKa pH log ................................................................................................................(1)
[Acid]
Volume of NaOH Strength of NaOH
Here, the concentration of Salt, [Salt]
Total Volume
Volume of CH3COOH Strength of CH3COOH
And the concentration of Acid, [Acid]
Total Volume
Volume of Remaining CH3COOH Strength of CH3COOH
In the present experiment concentration of Acid, [Acid]
Total Volume
Thus from the equation(1 ) we get
Volume of NaOH Strength of NaOH i k
n
Ma
pKa pH log Total Volume
Volume of Remaining CH3COOH Strength of CH3COOH
Total volume
u r
N
a n
Result: The pKa value of the solution =
r
Precautions: Im
d .
Comments: M
Principle:
A solution which resists changes in pH when small quantities of an acid or an alkali are added to it, is called
buffer solution. Most of the buffer solutions usually consist of a mixture of weak acid and one of its salts or a
weak base and one of its salts. The resistance to a change in pH is known as buffer action. A buffer solution
contains large and equal concentrations of an acid and its conjugate base. The pH of this solution is
approximately equal to the pKa of the acid. Addition of small amounts of acid or base results in the mopping up
or the release of protons by the conjugate base or the acid as necessary, which keeps the solution pH constant.
TYPES OF BUFFERS
Buffers are classified into following types
1. Simple Buffers:
Simple buffers are categorized into three different ways.
A) Salts of weak acid and a weak base
Example: Ammonium acetate-CH3COONH4, Ammonium cyanide-NH4CN.
B) Proteins and amino acids.
C) A mixture of an acid salt and a normal salt formed from polybasic acid
i k
Example: Na2HPO4 and Na3PO4
n
2. Mixed Buffers Ma
Example: CH3COOH +CH3COONa, H2CO3 +Na2CO3 u r
Acidic Buffer: A solution of weak acid and its salt with strong base.
N
Basic Buffer: A solution of weak base and its salt with strong acid.
Example: NH4OH+NH4Cl, NH4OH+NH4NO3
a n
r
3. Natural Buffers
Im
A solution is said to be naturally buffered if it contains buffering compounds
.
as it exists in nature. Blood is an example of a naturally buffered solution.
d
M
Fig.Citric acid monohydrate
Fig. pH meter
Apparatus: Chemicals/Reagents:
1. Electrical balance 1. 0.1 M Na-Acetate (CH3COONa) solution
2. Spatula 2. Citric acid (monohydrate)
3. Volumetric flask 3. Distilled Water
4. Conical flask
5. Beaker
6. Measuring cylinder
7. pH meter
8. Stirrer
Calculation: Full calculations required to make the reagents, for the experiment must be written down.
Preparation of Reagents:
0.1 M 100 mL CH3COONa Solution: Completely dissolve 1.374 gm CH3COONa (99%) in a 100 mL volumetric
flask with a small amount of DW. Later on adjust the volume up to the mark by adding distilled water Q.S.
Procedures:
1. Take 100 mL 0.1 M CH3COONa solution in a 250 mL beaker.
2. Carefully submerge the detector of pH meter into the CH3COONa solution.
3. Take the reading of pH meter.
4. Now add crystalline citric acid (C6H8O7.H2O) to the CH3COONa solution with continuous stirring by
the stirrer.
5. Carefully submerge the detector of pH meter into the solution.
6. Take the reading of pH meter simultaneously while adding citric acid.
7. Continue the step 4 until the pH is adjusted to 6 or above.
i k
n
Table-1: Data for pH adjustment:
No. of observation pH of CH3COONa Solution Ma pH of final solution
1 u r
N
Result: The pH value of the solution=
a n
Precautions: r
Comments:
Im
d .
M
Bibliography: