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KUT TECHNICaL INSTITUTE

Department of Medical Laboratory Technique
First stage
Practical Analytical Chemistry
Prepared by: Riyadh Hussein Wali

2023-2024
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CONTINNT

SUBJECT PAGE NO.

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 LABORATORY NO. 1
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PRACTICAL GENERAL CHEMISTRY

LABORATORY GLASSWARE
Lecturers :
1 – Lecturer: Riyadh Hussein Wali
2 - Technical Training : Gufran Dawood

Study the table below. Be able to identify the name of each piece of equipment, as well as its
function or use in the laboratory.

Name Picture Use

Test tubes Use to make reactions.

Beaker Use to prepare,transport solution and make reactions

Conical used to transport, heat, store substance and make

flask reactions

Volumetric flask Flask calibrated to contain a precise volume at a

particular temperature. Used for precise dilutions
and creating standard solutions.

Brush Used to clean the inside of glassware

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Test tube rack Holding many test tubes

Funnel Used to pour liquids into containers with small

openings; also used to hold filter paper

Graduated Measuring specific amounts of liquids

cylinder

Spatula are small stainless steel, used for scraping,

transferring, or applying powders and
paste like chemicals or treatments.

Test tube clamp Heating contents in a test tube

Wash bottle Used to wash down specific pieces of equipment

with water or keep materials moist.

Graduated These Pipettes are calibrated in the factory to

pipette release the desired
quantity of liquid

Pastor pipets Used to measure and dispence very small amounts

of liquids.

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Burette Measuring specific amounts of liquids (often 5 of 5
determining amounts of acids or bases needed)

Dropper Used to obtain small amounts of liquids (not

precise)

Separatory \
funnel used in liquid-liquid extractions to separate the
components of a mixture into two immiscible
solvent phases of different densities.

Digital used for weighing substances to the

Balance milligram (0.001 g) level.

A water bath is laboratory equipment made from

Water bath a container
filled with heated water. It is used to incubate
samples in water
at a constant temperature over a long period of
time.

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LABORATORY NO. 2
PRACTICAL GENERAL CHEMISTRY
Reactions of Metal ion or cations (Group 1)
Lecturers :
1 – Lecturer: riyadh hussein wali
2 - Technical Training : gufran dawood

Group 1: Insoluble Chlorides

Most metal chloride salts are soluble in water; only Ag+, Pb2+, and Hg22+ form chlorides that
precipitate from water. Thus the first step in a qualitative analysis is to add about 6 M HCl
(general precipitate agent of cation), thereby causing AgCl, PbCl2, and/or Hg2Cl2 to precipitate.
If no precipitate forms, then these cations are not present in significant amounts.

It’s a white , metable and ductile metal ,its insoluble in H2SO4 and diluted hydrochloric acid but dissolve in
nitric acid (2:1)and in boiling conc.H2SO4
Ag + 2HNO3 = AgNO3 + NO2 + H2O
2Ag + 2H2SO4 =Ag2SO4 + SO4 + 2H2O

Reaction of silver ion (Ag+) found in silver nitrate (AgNO3)

1- with diluted hydrochloric acid (precipitate agent)

White , crudy precipitate of AgCl

AgNO3 + HCl =AgCl + HCl

wt.ppt

2 drop HCl
2drop AgNO3

wt.ppt(AgCl)

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The precipitate insoluble in water but soluble in diluted NH4OH and formation of complex7 ioofn5

AgCl + 2NH4OH = Ag(NH3)2Cl.H2O

Complex soluble salt
2- with Potassium chromate K2CrO4 (confirm reaction)
Red precipitate of silver chromate Ag2CrO4 insolube in acetic acid but soluble dil.HNO3

2 drop K2CrO4

2 drop of AgNO3

Red ppt.Ag2CrO4

Is bluish-gray metal , its readly dissolved by diluted nitric acid to produce Pb(NO3)2

3Pb + 8HNO3 =3Pb(NO3)2 + 2NO +4H2O

Reaction of lead ion (Pb++) found in lead nitrate Pb(NO3)2

1- with diluted hydrochloric acid (precipitate agent)

White precipitate of PbCl2 formed only in cold and not too diluted solution

Pb(NO3)2+ HCl =PbCl2 + HCl

wt.ppt

2 drop HCl
2drop Pb(NO3)2

wt.ppt
(PbCl2)

The precipitate is soluble in hot water but separated out again as needle when the solution is cooled
Solubility test for PbCl2
Add few drop of DW to precipitate and put it in boiling water (by use water bath) for 2min
With shaking the tube and observe disappear the precipitate

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2- with Potassium chromate K2CrO4 (confirm reaction)

yellow precipitate of lead chromate PbCrO4 insolube in NH4OH but soluble in alkali hydroxide

2 drop K2CrO4

2 drop of Pb(NO3)2

Yell. ppt.

PbCrO4

3- Mecury Hg : not woke because its toxic

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LABORATORY NO. 3
PRACTICAL GENERAL CHEMISTRY
unknown of Metal ion or cations
Lecturers :

1 – Lecturer: riyadh hussein wali

2 - Technical Training : gufran dawood
Unknown
(Ag+ or Pb++ )

Put 3 drop of unk. In clean test tube

Add 2 drop HCl , mix well

Wt.PPT
AgCl or PbCl2

Add 4 drop DW

Put the tube in boiling water for 2 min

Insoluble ppt Soluble ppt

Ag+ Pb++

Unknown + K2CrO4 Add 2 drop K2CrO4

Red PPT Yell.ppt

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LABORATORY NO.4
PRaCTICaL GENERaL CHEMISTRY

Lecturers :
1 – Lecturer: riyadh hussein wali
2 - Technical Training : gufran dawood

Acid radical is negative part of acid such as

HCl  Cl –
HI  I –
H3PO4  PO4 -3
H2SO4  SO4 -2
H2C2O4  C2O4 -2
*The general precipitate agent of anion is AgNO3

1- chloride ion (use NaCl solution)

a-reaction with AgNO3 ( general reaction)
NaCl + AgNO3  AgCl + NaNO3
Wt. ppt

b-solubility test (confirm reaction)

AgCl insoluble in boiling water but soluble in NH4OH

AgCl + NH4OH  Ag(NH3)2Cl + 2H2O

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2- IODIDE ION (I -) use KI solution

a-reaction with AgNO3 (general reaction)
AgNO3 + KI  AgI + KNO3
Yell.ppt.

b- starch test (confirm reaction)

iodides are readily oxidized in acid solution to free iodide by a number of oxidizing agents
, the free iodide identified by the deep blue coloration produced with starch solution

KI +4HNO3  I2 + 2KNO3 + 2NO2 + 2H2O

Add 2 drop of starch

violet color compound

3- phosphate ion PO4 (use Na2HPO4)

a-reaction with AgNO3 (general reaction)
Na2HPO4 + 3AgNO3  Ag3PO4 + 2NaNO3 + HNO3
Yell.ppt.
b-reaction with FeCl3 (confirm reaction)
Na2HPO4 + FeCl3  FePO4 + 2NaCl + HCl
Pale yell.ppt
4- sulphate ion SO4-2 (use Na2SO4)

a-reaction with AgNO3(general reaction)

Na2SO4 + AgNO3  Ag2SO4 + 2NaNO3
Wt.ppt
b-reaction with Barium chloride (confirm reaction )
Na2SO4 + BaCl2  BaSO4 + 2NaCl
Wt.ppt
5- Oxalate ion C2O4 [use (NH4)2C2O4 ]
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a-reaction with AgNO3(general reaction)

(NH4)2C2O4 + 2AgNO3  Ag2C2O4 + 2NH4NO3
Wt.ppt

b-reaction with KMnO4 (confirm reaction)

decolorized the pink color of pot. Permanganate when warmed in acid solution with the
oxalate in (60-70 c)
(NH4)2C2O4 + H2SO4  H2C2O4 + K2SO4

2KMnO4 +3H2SO4 + 5H2C2O4  2MnSO4 + K2SO4 + 10CO2 +

8H2O
pink color colorless

6- Thiocyanite ion (SCN-)  not work because it toxic

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LABORATORY NO.5
PRACTICAL GENERAL CHEMISTRY
determination of anion in unknownsolution

Lecturers :
1 – Lecturer: riyadh hussein wali
2 - Technical Training : gufran dawood
Unknown

Cl , SO4 , C2O4 , I , PO4

2drop of unk. + 2 drop AgNO3

Mix well

White ppt yellow.ppt

AgCl or Ag2C2O4 or Ag2SO4 AgI or Ag3PO4

2drop unk + 2drop BaCl2 2drop unk + 2drop FeCl3

Wt.ppt No ppt. Pale yell.ppt No ppt.

SO4 or C2O4 Cl PO4 I

drop unk + 2drop KMnO4 + 2 drop H2SO4 2drop unk + 2drop HNO3 + 2 drop starch
70c

Violet color

colorless(C2O4) (SO4)violet I

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LABORATORY NO.6
PRACTICAL GENERAL CHEMISTRY
VOLUMETRIC ANALYSIS
Lecturers :
1 – Lecturer: Riyadh Hussein Wali
2 - Technical Training : Gufran Dawood

1- Neutralization Reaction :-
Titration of HCl with Borax
Theory
Borax (Na2B4O7 .10H2O) can be used as a primary standard since it does not

decompose under normal storage, it is readily obtained in a very pure form

(99.999% purity), it reacts with a known stoichiometry and can be weighed and used

directly.

In water, the salt dissociates:

Na2B4O7.10H2O → 2Na+ + B4O72- + 10H2O

and the anion is hydrolysed:

B4O72- + 7H2O → 4H3BO3 + 2OH-

The liberated hydroxide ions can be titrated with a strong acid

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Apparatus:
One 25 cm3 (or 50 cm3) burette, one funnel to fit the

burette, three 150 cm3 conical flasks, one wash bottle,

one white tile, one burette stand and one burette

clamp, access to an analytical balance, one weighing

bottle or 50 cm3 beaker.

Chemicals:

Na2B4O7.10H2O,

100 ml 0.1 N HCl,

1ml mthyl orange indicator.

Procedure

1- Fill the burette with HCl 0.1N to zero mark •

2-Place 10 ml of Borax into conical flask Methyl red

3-Add 2-3 drops of Methyl red indicator •

4- Titrate against HCl solution till the first color changed from
yellow to pink color (end point)

5- record the volume of HCl consumed in end point

Calculations

N(HCl) x V(HCl) = N(Borax) x V(Borax)

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LABORATORY NO. 7
PRACTICAL GENERAL CHEMISTRY
Oxidation reduction Reactions
Lecturers :
1 – Lecturer: Riyadh Hussein Wali
2 - Technical Training : Gufran Dawood

Titration of Oxalic acid with KMnO4

Theory –
KMnO is an oxidizing agent which works in acidic medium more strongly
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than alkaline medium. So, for quantitative analysis potassium

permanganate is generally used in acidic medium only.
We use sulphuric acid in this titration with KMnO to give acidic medium. The
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solution which contain KMnO in it is purple in colour. While the solution

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containing MnSO4 is colourless. Thus, potassium permanganate when

reacts with a reducing agent it works as self-indicator.
In the experiment, oxalic acid acts as a reducing agent
2KMnO4 +5H2C2O4 +3H2SO 2MnSO4 + K2SO4+10CO2+8 H2O

here in the above reaction, 2MnO4- reduced to Mn2+ while C O 2- oxidized to

2 4

CO2.

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Material Required –

Measuring flask, burette, burette stand, pipette, conical flask, funnel, water bath , oxalic
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acid, potassium permanganate solution, 1.0 M sulphuric acid.
Apparatus Setup – Potassium permanganate solution should be taken in the burette
and oxalic acid solution should be taken in conical flask.

Procedure :-
1. Rinse and fill a clean burette with potassium permanganate solution. Burette must
have a glass stop cock as rubber will get affected by permanganate ions.
2. Remove the air bubbles from the nozzle of the burette.
3. Take 10 ml of oxalic acid solution in a clean conical flask. Add 5ml of 1.0M
sulphuric acid in it.
4. Heat the solution up to 50-60℃ before titrating it with potassium permanganate
solution.
5. To increase visibility of the colour, keep the white tile below the conical flask.
6. Note the initial reading of the burette containing potassium permanganate.
7. Now start adding potassium permanganate through the burette in small quantity
into hot oxalic acid solution.
8. Keep swirling the contents of the flask slowly.
9. Initially purple (pink) colour of potassium permanganate is discharged on reaction
with oxalic acid.
10. When permanent pink colour appears, it indicates the end point.
11. Note down the upper meniscus of the burette containing potassium
permanganate.
12. Repeat the titration till three times to obtain 3 concordant readings.

Observation Table –
Burette
readings Volume of KMnO4 used
S.No. Volume of Oxalic acid in ml
V = (y-x) ml
Initial (x) Final (y)

1.
2.
3.

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Calculations –
The normality of potassium permanganate solution can be calculated by following
formula –
N1V1 = N2V2
N = normality of oxalic acid solution
1

N = normality of potassium permanganate solution.

2

V = volume of oxalic acid solution

1

V = volume of potassium permanganate solution

2

Result :- Molarity of potassium permanganate solution -

Precautions –
Following precautions should be taken while performing the experiment -
1. Always rinse the burette and take out the bubbles at nozzle of the burette.
2. Always rinse the burette and other flasks with distilled water before using.

3. KMnO is a dark colour solution so always use upper meniscus reading.

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4. Use sulphuric acid for acidifying the potassium permanganate. Don’t use HCl or
nitric acid.
5. Maintain the temperature of oxalic acid solution at 50-60’C.
6. Do not use rubber cork.
7. The strength of the solution should be taken till three decimals.
8. Never use burette with broken nozzle.
9. While noting reading at the end point, no drop should be hanging at the nozzle of
the burette.
10. End point should be detected carefully and precisely.
11. Pipette should be used carefully.

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LABORATORY NO.8
PRACTICAL GENERAL CHEMISTRY
COLORIMETRIC ANALYSIS
Lecturers :
1 – Lecturer: Riyadh Hussein Wali
2 - Technical Training : gufran dawood

Colorimetric Analysis :
is a method of determining the concentration of a chemical element or compound in a
solution with the aid of a color reagent

Beer’s law :
It states that the intensity of the colour is directly proportional to the
concentration of coloured particle in the solution.

Lambert’s Law :
It states that the amount of the light absorbed by a coloured solution depends
on the length of the column or the depth of the liquid

Lambert Beer ²s Law :-

The absorbance of light from substance is linear relationship with the
concentration & light bath .
Aαbc A= absorbance , Optical Density (O.D)
A =a b c a= constant b= light bath c= conc.
Conditions for application Lambert Beer s Law:-
1- The solution must be coloured .

2- The solution must be clear .

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3- The solution must be low conc.

4- The light must be monochromatic beam.

COLORIMETRY & SPECTROPHOTOMETRY

involves the measurement of color and is the widely used method for finding the
concentration of biochemical compounds. It Measures absorbance and
wavelength between 400 to 700 nm from the visible spectrum of light of the
electromagnetic spectrum.

When a ray of monochromatic light of initial intensity (Io) passes through a

coloured solution, some of the light is transmitted with intensity (I) and some is
absorbed

Maximum absorption curve :-

Is the curve that is explained the relation between Absorbance (A) & wave
length (λ) with the constant of concentration.
Is used to determination the wave length of colour solution.

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Standard curve :- 21 of

Is the linear relation between the absorbance and the concentration of the
colour solution with constant of wave length .is used to determination the
conc. of unknown solutions.
Preparation of calibration curve :-

An alternative procedure to find the concentration of ‘test’ of unknown solution sample

is to prepare a calibration curve, then read the concentration of the unknown.

Procedure :-
1- prepare three known concentrations of pot. Permanganate solution .

2- Place 3 ml of each concentration in a glass tube and label (St1, St2 & St3).

3- Read the absorbance of the standard by the spectrophotometer at 540 nm against

distilled water.

4- read the absorbance of unknown pot. Permanganate solution.

5- Draw a graph of calibration or standard curve with absorbance on Y-axis and

concentrations in on X-axis as in fig. below.

5-Find the concentration of the unknown solution ‘T’ from the curve.

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LABORATORY NO. 9
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PRACTICAL GENERAL CHEMISTRY

SEPARATION OF MIXTURE TECHNIQUES
Lecturers :
1 – Lecturer: Riyadh Hussein Wali
2 - Technical Training : Gufran Dawood

What is a mixture:
When two or more substances are mixed together but do not chemically combine. This
means they retain their original properties. This means they can be separated by physical
means.
What are the different techniques of separating mixtures?

1- MAGNETISM : depend on magnetic properties to separate the mixture.

Iron, nickel, and cobalt are examples of magnetic metals.
gold, silver, and aluminum are examples of non magnetic metals.

2- FILTRATION: depend on solubility properties used to separating insoluble solid from liquid
by passing a mixture through a porous material such as filter paper for example chalk from
water

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3- CENTRIFUGINGS: depend on sedimentation property where denser materials go to bottom

when centrifuged Example: Separate blood into cells(formed element) and plasma

4- EXTRACTION : depend on density(specific gravity) property , when Immiscible liquids do not

dissolve in each other; they form layers when placed in the same glassware. such as oil and
water can be separated by using a separating funnel.

5-DISTILLATION: this depend on boiling point property . Can be used to separate liquid from
liquid mixture (Ex.: alcohol from water) or solids from liquids (Ex.: water from salt) .This method
works because the substances that we are separating have different boiling points

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6- CRYSTALLIZATION: is based on the principles of solubility: compounds (solutes) tend to be

more soluble in hot liquids (solvents) than they are in cold liquids such as benzoic acid and

sugar

7-SUBLIMATION: is a process in which a solid turns directly into gas without passing into liquid
state. It depend on the principle that solids have a weak intermolecular force hence a higher
vapor pressure which converts it into directly vapor state.

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