Ministry of Higher Education ‫وزارة التعليم العالي والبحث العلمي‬

Al-Rasheed University College ‫كلية الرشيد الجامعه‬

Pharmacy department ‫قسم الصيدلـــة‬

Practical
Analytical Chemistry

By
MSc. Farah A Hassan
MSC.Aseel S Mansoor

Supervised by
Prof. Dr. Suad Al-Sarraj
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

Important notes
Safety rules:

1. Always wash your hands before and after experiments. ( bring small
towel and a bar of soap with you)
2. Read all directions for the experiment carefully before beginning. Follow
all the directions exactly as written or explained by the supervisor.
3. Never perform unauthorized activities.
4. Never mix chemicals or other materials for fun.
5. Maintain a clean work area.
6. When an experiment is completed always clean up the glass ware and
working area and return all equipments to its proper place.
7. Never eat in lab ( DO NOT CHEW GUM )
8. Know the location of safety equipments (eg. Fire extinguisher) and how
to use it.
9. Always wear safety goggles when working with chemicals, burners, or
any substance or object that might injure eyes.
10.Wear your lab. coats as soon as you enter the lab. and keep it on the
whole time.(student NOT ALLOWED to enter the lab unless he has his
coat on)
11.Keep all lids closed immediately when a chemical is not being used.
12.Many chemicals and hazardous materials might be corrosive or even
poisonous . never touch, taste, or smell any chemical. If instructed to
smell the fumes in an experiment, gently wave a hand over the opening
of the container and direct the fumes tower the nose.
13.Dispose of all chemicals as instructed by the supervisor.
14.Take care not to spill any chemicals on you bench or in the lab. If spilling
does occur, notify the supervisor for clean-up directions.
15.Be careful if you work with acids and bases. Always pour acid into water
gradually when diluting the acid. NEVER pour water into acid.
16.Rinse any acids or bases off skin or clothing with water.
17.Never reach across a flame.

1
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

18.Pull back long hair and push up long sleeves if necessary.

19.Always point a test tube or bottle being heated away from you and
others.
20.Never heat chemicals in a closed container.
21.Always use a clamp, tong, or heat-resistant gloves when handling with
hot containers.
22.Use a wire screen to protect glassware when heating .
23.Never heat glassware that is not thoroughly dry.
24.Never use broken or chipped glassware. If glassware break notify the
supervisor.
25.Notify the supervisor immediately if you are cut or injured in lab. (For
first aid)
26.All sharp glass ware and broken glass are to be disposed of in the proper
container. ( notify the supervisor.)

2
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

Laboratory equipment

Glass rod

3
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

4
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

5
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

6
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

7
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

8
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

Analytical chemistry

Qualitative Quantitative
analysis analysis

The testing of a substance The analysis of a substance

or mixture of substances to to determine the amount and
determine the nature of proportions of its chemical
chemical constituents. constituents

So Qualitative analysis means just to detect the presence of a substance or more

in a sample(solute) while Quantitative analysis is the determination of the amount
of each substance in the analyzed sample.

Quantitative analysis:
Volumetric Analysis:
Volumetric or titrimetric analysis are quantitative analytical techniques which
employ a titration in comparing an unknown with a standard. In the titration, a
volume of standardized solution containing a known amount of reactant "A" is
added gradually to a sample containing an unknown amount of reactant "B". The
titration proceeds until reactant "B" is just consumed (fully reacted) . This is
considered as the equivalence point. At this point the number of equivalents of "A"
added to the unknown, equals the number of equivalents of "B" originally present in
the unknown solution.

9
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

A titration is a process for determining the amount of a chemical substance in

solution by measurement of the quantity of titrant required to react completely with
the chemical substance present in the unknown solution.
The Titrant is a standard solution which contain a certain weight of a chemical
compound in terms of its equivalent weight.
The solute is the compound that is dissolved completely in the solvent.

Standardization: It is a process whereby the concentration of a standard solution is

determined by titrating it with either primary standard or secondary standard.
Concentration in standard solutions must be expressed in unit of moles per liter.
A standard solution is a solution containing an exact known conc. of an analyte or
a substance such as primary standard.
A primary standard is a chemical compound which can be weighed easily, and is so
pure that its weight is truly represented the number of moles of the chemical
compound contained in one liter . A good example of this is Na2CO3.
Requirements of a primary standard solution:
1- Highly pure
2- Stabile (low reactivity)
3- Not hygroscopic
4- Highly soluble in the solvent used.
5- Non toxic
6- Not expensive and available

A Secondary standard is a solution of certain chemical compound that is not stable,

and must first be standardized before being used. A good example of this is NaOH
being used in titration with HCl.
The equivalence point It is the point where the amount of titrant is sufficient to fully
react with the analyte present in the unknown solution.
The end point is the point which is noticed immediately after reaching the
equivalence point.
Concentration of a chemical solution refers to the amount of solute that is dissolved
in a certain volume of solvent.
Normality: is the number of equivalent weights contained in one liter of solution
10
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

Molarity: is the number of gram molecular weights or the number of moles of

solute in one liter solution.
Formality: is the number of gram formula weights per liter of solution.

Percentages :

1 % v/v = volume of solute / volume of solution X 100

2 % w/v = weight of solute / volume of solution X 100
3 % w/w = weight of solute / weight of solution X 100
= gram of solute / 106 gram of sample
4 ppm (part per million) = g of solute / 1000 kg of sample
= mg of solute / kg of sample
= mg of solute / L of sample

Density : is Mass per unit volume.

Density of water = 1 g / ml at 4oC
Specific gravity : it is the ratio of the density of a substance to the density of
water. So is a unitless value.
Equivalent weight : m.wt / valance no.
Valance no. is the number of hydrogens in acid
Or number of hydroxides in base
Or number of electrons in redox

11
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

Experiment ( 1 )
Acid base titrations
(Preparation and standardization of an acid (like HCl) and a base (like NaOH) )
a) Preparation of 0.1 N HCl (hydrochloric acid ) from concentrated HCl :-

s.g. X %w/w X 1000

NHCl =
𝑒𝑞 𝑤𝑡 𝑜𝑓 𝐻𝐶𝑙

s.g. of conc. HCl = 1.18

eq. wt. of HCl = 36.5 g
%w/w of HCl is obtained from the reagent bottle
‫ ؞‬N of concentrated HCl =12 ( why? )
To calculate the volume of concentrated HCl that should be taken to prepare 250 ml
of 0.1 HCl
N V of conc. HCl = NV of diluted HCl
12 X V1 = 0.1 X 250
‫ ؞‬V1 = 2.2 mL should be taken from conc. HCl and diluted with distilled water in
250 ml volumetric flask up to the mark, to obtain 0.1 N HCl

b) Standardization of prepared 0.1 N HCl solution

1- Fill the burette with 0.1 N Na2CO3 (primary standard ). ( 0.1 N Na2CO3
solution is prepared by weighing exactly 5.3 gm of Na2CO3 and diluted to
1000 ml with distilled water in a volumetric flask.
2- Transfer 10 ml of the prepared HCl solution into a conical flask by using a
bulb pipette.
3- Add 2 drops of methyl orange as an indicator . yellow color is obtained.
4- Titrate with Na2CO3 solution drop by drop from the burette into the conical
flask until a faint orange color is obtained.
5- The exact normality of HCl can be calculated from the equation
Na2CO3 + HCl → NaCl + H2O + CO2

12
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

N1 V1 = N2 V2

c) Preparation and standardization of 0.1 N NaOH solution :

1- Preparation of ≡ 0.1 N NaOH

Weigh 4 grams of NaOH dissolve in distilled water and dilute it up to one
liter.
2- Standardization of ≡ 0.1 N NaOH solution:
i. Transfer 10 ml of prepared NaOH solution to a conical flask
ii. Add 1-2 drops of phenolphthalein (phph) as an indicator.
iii. Fill the burette with the standard HCl solution.
iv. Add HCl drop by drop into the conical flask until the color of the
solution becomes faint pink
v. The exact normality of NaOH is obtained from
HCl + NaOH → NaCl + H2O
N1 V1 (NaOH) = N2 V2 (HCl)

13
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

Experiment ( 2 )
Analysis of sodium carbonate and sodium hydroxide mixture

A solution of sodium hydroxide always contain a small but variable amount of

CO2 fixed as sodium carbonate. The reaction with HCl can be expressed by the
following equation:
NaOH + HCl → NaCl + H2O .. .. .. .. .. .. .. .. .. .. (eq.1)
Na2CO3 + HCl → NaHCO3 + NaCl .. .. .. .. .. .. .. .. .. .. (eq.2)
NaHCO3 + HCl → NaCl + H2O + CO2 .. .. .. .. .. .. .. .. .. .. (eq.3)
Phenolphthalein end point represents the point at which all the hydrogen and half of
the carbonate have been neutralized (end point of eq1&2). Methyl orange end point
is obtained when all of three reactions are completed. Therefore it is a measure of
total alkali (hydroxide and carbonate).

Procedure :
1- Transfer 20 ml of unknown sample solution (containing a mixture of NaCO3
and NaOH) to 100 ml volumetric flask. Dilute it up to the mark with distilled
water.
2- Transfer 10ml from the diluted sample solution into a conical flask, add 1
drop of phenolphthalein indicator.
3- Fill the burette with the standard HCl solution.
4- Titrate the unknown solution with the standard HCl till the color changes
from pink to colorless. The volume of HCl used = (m). used to neutralize the
other half of carbonate present in the solution (eq 3)
5- Add 1drop of methyl orange. The solution becomes yellow.
6- Continue the titration with HCl till the color of the indicator changes from
yellow to pale orange. The volume of HCl= (M).

14
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

Calculation :
(M-m) is the volume of HCl required to neutralize half of CO32- present in the
unknown solution
2(M-m) is the volume of HCl required for all CO32- present in the unknown
solution
M- [2( M-m)] is the volume of HCl required for all OH-(hydroxide ion) present in
the unknown solution
𝑊𝑡.
NV= 𝑋 1000
10

For Na2CO3:
2(M-m) × NHCl = Wt. CO32- / 53 × 1000
‫ ؞‬wt. CO3= × 10 = wt. of CO32- in 100 ml of diluted unknown
Wt. × 10 × 5 = wt of CO32- in 100 ml of concentrated unknown
For NaOH:
𝑤𝑡.𝑁𝑎𝑂𝐻
M- [2(M-m)] × NHCl = × 1000
40

Wt. (OH-) × 10 = wt of NaOH in 100 ml of diluted unknown solution

Wt. (OH-) × 10 × 5 = wt of NaOH in 100 ml of concentrated unknown solution

15
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

Oxidation – reduction reactions

(Redox Reactions )
Chemical reactions in which transfer of electrons occurs in an element are known
as oxidation-reduction, or redox reactions. Oxidation involves the loss of electrons
by a specimen, and reduction the gain of electrons.
In any oxidation-reduction reaction, the number of electrons lost by the one
element is equal to the number of electrons gained by the other.
Oxidizing agents readily gain electrons that comes from the reducing agents. For
example Permanganate ion functions as an oxidizing agent in acid, being reduced to
Mn2+
MnO4- + 8H+ + 6e- ↔ Mn2+ + 4H2O
In case of iron been a reducing agent, Fe+2 (iron II) is itself oxidized to (iron III).
Fe2+ ↔ Fe3+ + e-
The equivalent weight in redox-reactions is equal to the m wt. divided by
number of electron gained or lost .
𝑀 𝑤𝑡.
Eq. wt. =
𝑁𝑜.𝑜𝑓 𝑒𝑙𝑒𝑐𝑡𝑟𝑜𝑛𝑠 𝑔𝑎𝑖𝑛𝑒𝑑 𝑜𝑟 𝑙𝑜𝑠𝑡

16
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

Experiment ( 3 )
Preparation and standardization of about ≅ 0.1 N KMnO4
1- Preparation of ≅ 0.1 𝑁 KMnO4 solution.
A. Dissolve 0.8 gm of solid KMnO4 in 50-100 ml of distilled water
B. Heat the solution on a hotplate for 10 minutes at 70- 80 oC.
C. Cool the solution to room temperature , then add 2.5 ml of
concentrated sulfuric acid. (acidification)
D. Complete the volume up to 250ml by distilled water. Stopper the
volumetric flask and mix well. Store the solution in the dark.( it might
decompose by light)
2- Standardization of KMnO4 solution against sodium oxalate standard solution.
A. Filter the previously prepared KMnO4 solution through glass wool
(why?).
B. Fill the burette with the 0.1 N sodium oxalate solution, add 5 ml of
concentrated H2SO4 .
C. Transfer 10ml of filtered KMnO4 solution to a conical flask .
D. Heat the sodium oxalate solution to 65 oC. and put it in the burette
E. Titrate KMnO4against sodium oxalate st. solution. The end point is the
first permanent pink color.
2MnO4- + 5C2O4= + 6 H+ ↔ 2Mn 2+ + 10 CO2 + 8H2O
Calculation :
N1 V1 (KMnO4) = N2 V2 (Na2C2O4)

17
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

Experiment ( 4 )
Iodometric titration
determination of copper as CuSO4
procedure :
1- Weigh about 0.6-0.8 gm of CuSO4. Dissolve the sample in 25 ml distilled
water. Add 2ml of concentrated H2SO4 or 2 ml of 5N HCl. (for
acidification).
2- Transfer the solution quantitatively to a Stoppard flask. Add enough water to
make the volume up to 50 ml .
3- Add 1-2 gm of KI (or 15 ml of 10% KI)
4- Titrate the librated iodine against standard 0.1N sodium thiosulfate(Na2S2O3)
solution until the color of the solution is light yellow. Add 5 ml of starch
mucilage as indicator and continue the titration until the bluish color changes
to yellowish white.
5- Add 1 gm of ammonium thiocyanate (NH4)SCN , mix well , continue the
titration with Na2S2O3
6- . drop by drop, until the color disappears and the precipitate becomes white .
2 Cu2+ + 4 I- → 2CuI↓ + I2
I2 + 2S2O32- → S4O62- + 2I-

N1 V1 (Na2S2O3) = Wt. of Cu2+ / eq. wt. × 1000

18
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

Experiment ( 5 )
Complexometric titration

A. Determination of total hardness in tab water:

1- Transfer 50 ml of tab water into a conical flask .
2- Add 10 ml of buffer 10
3- Add 0.2 gm of [ Eriochrome black –T ] as an indicator.
4- Titrate against 0.01F EDTA solution until the color of the solution
changes from red to blue.
Note: CaCO3 represents the total hardness of H2O

V M EDTA = Wt of CaCO3 / m wt. × 1000

M wt. of CaCO3 = 100
ppm CaCO3 = wt of CaCO3 / 50 × 106
B. Determination of calcium-hardness
1. Transfer with a pipette 50 ml of tab water into a conical flask
2. Add 2 ml of buffer 12
3. Add 0.2 gm of murexide indicator, and titrate against 0.01 F EDTA
until the color changes from pink to violet
𝑤𝑡.𝑜𝑓 𝐶𝑎2+
V M EDTA = × 1000
𝑎𝑡 𝑤𝑡
Atomic wt. of Ca2+ = 40
ppm = Wt. of Ca2+ / 50 × 106

C. Determination of Magnesium – Hardness

V EDTA total - V EDTA,Ca 2+ = V EDTA,Mg 2+
V EDTA,Mg 2+ × M EDTA = wt of Mg2+ / 50 × 1000
Atomic wt. of Mg2+ =24
ppm (Mg 2+) = wt of Mg2+ /50 × 106

19
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

Experiment ( 6 )
Precipitation titrations
Determination of chloride by the mohr method

The chloride ion is titrated with standard silver nitrate solution (AgNO3), silver
chloride (AgCl) is formed as a precipitate. The end point is the appearance of brick-
red color of silver chromate (AgCrO4)
NaCl + AgNO3 → AgCl ↓ + NaNO3
2AgNO3 + K2CrO4 → Ag2CrO4 + 2KNO3
Procedure:
1- Transfer 10 ml of unknown solution containing KCl or NaCl into a conical
flask.
2- Add 1 ml of K2CrO4 as an indicator.
3- Titrate with the standard 0.1 N silver nitrate solution, slowly, until a faint
reddish color appears
Calculations:

𝑤𝑡 𝑜𝑓 𝐶𝑙 −
N × V AgNO3 = × 1000
𝑒𝑞 𝑤𝑡.

Weight of chloride in a liter of solution=

N × V AgNO3 × 35.46/ 1000 × 1000/10

Standardization of AgNO3 solution :

1- Transfer 10 ml of silver nitrate solution AgNO3 into a conical flask.
2- Add 10 ml of K2CrO4 indicator and titrate slowly with standard 0.1N NaCl
solution until a faint color is formed.
N V AgNO3 = N VNaCl

20
Ministry of Higher Education
Al-Rasheed University College
Pharmacy Department

Experiment ( 7 )
Determination of ferrous Iron in Mohr's salt
FeSO4.(NH4)2SO4.6H2O
Procedure:
1- Dissolve the sample in distilled water. Transfer 50 50 ml volumetric flask,
complete the volume up to mark and mix well.
2- Transfer 20 ml of the sample solution to a conical flask, add 5 ml of
concentrated H2SO4
3- Titrate against standard KMnO4 solution. The end point is faint pink
MnO4- + 5 Fe2+ + 8H- ↔ Mn2+ + 5Fe3+ + H2O

Calculations:
𝑤𝑡.𝑜𝑓 𝑚𝑜ℎ𝑟 ′ 𝑠 𝑠𝑎𝑙𝑡
N1 V1 = × 1000
𝑒𝑞.𝑤𝑡.
Wt. of mohr's salt= gm in 20 ml of solution
55.85
Wt of ferrous iron = wt. of mohr's salt × × 2.5
392.14
= gm Fe2+ in the sample

Note:
M wt. of mohr's salt = 392.14
Eq. wt. of Fe2+ = atomic wt. = 55.85

21