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BS Chemistry All Practicals

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0% found this document useful (0 votes)
105 views113 pages

BS Chemistry All Practicals

Uploaded by

muskanarif641
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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INORGANIC LAB (SEMESTER-I)

CHEM-151 LAB
Experiment # 1
Standardize the given solution of NaOH
Apparatus required:
Titration flask, measuring cylinder, burette, burette stand, dropper,
funnel.
Chemicals Required:
Oxalic acid, NaOH, phenolphthalein indicator, distilled water

Experiment # 2
You are provided with 0.05 solution of H2 SO4 . How can you
determine its exact molarity. You are provided with 0.1 NaoH
Apparatus required:
Titration flask, measuring cylinder, burette, burette stand, dropper,
funnel.
Chemicals Required:
H2 SO4 , NaOH, phenolphthalein indicator, distilled water.
Experiment # 3
10 g of NaOH and NaCL mixture has been dissolved per dm3 of
solution. Calculate percentage purity of the mixture (molecular mass of
NaOH = 40g). You are provided with 0.1M HCl.
Apparatus required:
Titration flask, measuring cylinder, burette, burette stand, dropper,
funnel.
Chemicals Required:
HCl, NaOH, phenolphthalein indicator, distilled water.
Experiment # 04
Determine the solubility of KMnO4 at room temperature. You are
provided with 0.01M FeSO4 solution.
Apparatus required:
Titration flask, measuring cylinder, burette, burette stand, dropper,
funnel.
Chemicals Required:
KMnO4, FeSO4, distilled water
Experiment # 5
10g mixture of ammonium oxalate and ammonium sulphate dissolved
per dm3 of solution. How can you determine the percentage of each
compound in mixture. You are provided with 0.02M KMnO4.
Apparatus required:
Titration flask, measuring cylinder, burette, burette stand, dropper,
funnel.
Chemicals required:
Sample solution of ammonium oxalate and ammonium sulphate, H2SO4,
KMnO4, distilled water.
Experiment # 06
12g mixture of H2SO4 and oxalic acid dissolved in per dm3 of solution.
Find out the percentage composition of each compound if you are
provided with 0.02M KMnO4.
Apparatus required:
Titration flask, measuring cylinder, burette, burette stand, dropper,
funnel.
Chemicals Required:
Sample solution of H2SO4 and oxalic acid, KMnO4, H2SO4, distilled
water.
Experiment # 07
6.3g of H2Cr2O4.xH2O dissolved per dm3 of solution. Find the value of
‘x’ if you are provided with 0.02M KMnO4.
Apparatus Required:
Titration flask, measuring cylinder, burette, burette stand, dropper,
funnel.
Chemicals required:
Sample solution, conc. H2SO4, KMnO4, distilled water.
Experiment # 08
Determination of Cu(II) by using sodium thiosulphate as a standard
solution. (iodometrically)
Apparatus Required:
Titration flask, measuring cylinder, burette, burette stand, dropper,
funnel.
Chemicals Required:
Sample solution of copper sulphate, Sodium thiosulphate as a standard
soln., potassium iodide, iodine, starch.
Experiment # 09
Determination of Barium ions in the solution by gravimetric analysis.
Apparatus Required:
Beakers, funnel, hot plate, volumetric flasks, filter paper.
Chemicals required:
Potassium chromate, barium chloride, Hydrochloric acid HCl

MIXTURE ANALYSIS OR SALT ANALYSIS


ORGANIC CHEMISTRY (CHEM-161-LAB)
CONTENTS:
1. Qualitative analysis of compounds with different functional groups
2. Synthesis of organic compounds using as a tool for understanding
techniques like
o Reflux
o Distillation
o Filtration
o Recrystallization
o Yield calculation
3. Organic syntheses may include:
o Preparation of Benzanilide from Benzoyl Chloride
o Succinic Anhydride from Succinic Acid
o Phthalimide from Phthalic Anhydride
o Oximes and Hydrazones from Carbonyl Compounds
o An Ester from a Carboxylic Acid and Alcohol etc

1. QUALITATIVE ANALYSIS OF COMPOUNDS WITH


DIFFERENT FUNCTIONAL GROUPS

CHEMICALS AND REAGENTS

Functional groups:
1) Carboxylic acid 2) alcohol 3) Phenol. 4) Carbonyl 5)
Ester

Tests

 Sodium Bicarbonate

 Conc Ammonium Nitrate

 Ferric Chloride

 2 4 DNP.

 Hydroxylamine

 Feigel test (HCl. KOH)

Organic syntheses may include:

2. PREPARATION OF BENZANILIDE FROM BENZOYL


CHLORIDE

APPARATUS AND EQUIPMENTS

Conical flasks Volumetric flasks Pipette

Funnel Beakers Test tubes

Balance Spatula Water bath

Stirrer Filter paper

CHEMICALS AND REAGENTS


Aniline 05Ml Benzoyl Chloride 07mL 10%NaOH
45mL

3. SUCCINIC ANHYDRIDE FROM SUCCINIC ACID

APPARATUS AND EQUIPMENTS

Round bottom flask Reflux Condenser Pipes

Hot plate Magnetic stirrer Measuring


cylinder

Measuring balance Water bath Filter


paper

Beaker

CHEMICALS AND REAGENTS

Succinic acid Acetyl chloride Ether

Calcium chloride Ethanol

4. PHTHALIMIDE FROM PHTHALIC ANHYDRIDE

APPARATUS AND EQUIPMENTS

Round bottom flask Hot plate Stirrer or


glass rod

Porcelain dish Measuring balance Measuring


balance
CHEMICALS AND REAGENTS

Phthalic anhydride Ammonium carbonates Alcohol

5. AN ESTER FROM A CARBOXYLIC ACID AND ALCOHOL


(SYNTHESIS OF N-BUTYL ACETATE)
APPARATUS AND EQUIPMENTS
Round bottom flask Reflux Condenser Pipes

Hot plate Magnetic stirrer Measuring


cylinder

Beaker Water bath Filter paper

6. PURIFICATION OF AN ORGANIC COMPOUND BY


RECRYSTALLIZATION

APPARATUS AND EQUIPMENTS

Five test tubes Water Bath, Burner Test tube


holder

Stirrer Ice bath Erlenmeyer


flask

Filter paper Wire gauze Iron stand.

CHEMICALS AND REAGENTS


Crude substance 1.0g of unknown substance

Solvents (Acetone, Distilled water, Methanol, Ethanol and Chloroform).

7. REFLUX

APPARATUS AND EQUIPENTS

Round bottom flask Heating mantle Ring stand or


vertical support rod

Conical flask or funnel Magnetic stirrer Rubber tubing

Condenser Lotion or Vaseline

8. SIMPLE DISTILLATION

APPARTUS AND EQUIPMENTS

Distillation flask Condenser Thermometer

Iron stands Bunsen burner Receiving


flask

9. FILTRATION

There is several filtration methods.

 Simple or gravity

 Hot filtration
 Vacuum filtration

The selection of the appropriate method is typically dictated by the nature


of the experimental situation.

SIMPLE OR GRAVITY

Filter paper Funnel Erlenmeyer flask

Iron stand

HOT FILTRATION

Filter paper Stemless filter funnel Iron ring


clamp

Erlenmeyer flask Hot plate

VACUUM FILTRATION

Filter paper vacuum filter flask Iron clamp

Hirsch funnel or Buchner flask

PHYSICAL CHEMISTRY LAB


CONTENTS:

1. Determination of viscosity and refractive index of liquids


2. Determination of percent composition of liquid solutions
viscometrically
3. Determination of refractive index and molar refractivity
4. Determination of percent composition of liquid solutions by
refractive index
5. Determination of molecular weight of a compound by elevation of
boiling point (ebullioscopic method)
6. Determination of molecular weight of a compound by lowering of
freezing point (cryoscopic method)
7. Determination of heat of solution by solubility method
8. Determination of heat of neutralization of an acid with a base
9. Kinetic study of acid catalyzed hydrolysis of ethyl acetate.
10. Determination of partition coefficient of a substance between
two immiscible

1. KINETICS OF THE HYDROLYSIS OF ETHYL ACETATE

APPARATUS AND EQUIPMENT

Thermostat Beakers Pipettes

Burette Volumetric flasks titrimetric


flasks
Stop-clock

CHEMICALS AND REAGENTS

Solution of ethyl acetate(c= 0.04 moldm3

Solution of sodium hydroxide (c= 0.04 mol.dm3

Solution of hydrochloric acid (c= 0.04 mol.dm-3

Phenolphthalein

2. DETERMINATION OF HEAT OF NEUTRALIZATION OF


AN ACID WITH A BASE

APPARATUS AND EQUIPMENT

25ml Beaker Calorimeter Thermometers

Stops watch Pipette Stirrer

CHEMICALS AND REAGENTS

Ammonium nitrate (NH4NO3)

Ammonia (NH3)

Nitric acid (HNO3)

3. DETERMINATION OF HEAT OF SOLUTION BY


SOLUBILITY METHOD.

APPARATUS AND EQUIPMENT


Thermostat Ten 125-ml Erlenmeyer flasks 250ml
beaker

5ml pipette 100ml graduated Cylinder 50ml


burette

100°C thermometer Funnel Safety bulb

Spatula Glass bar piece of glass


tube with rubber tube.

CHEMICALS AND REAGENTS

Oxalic acid

1N NaOH; KHP

phenolphthalein.

4. DETERMINATION OF MOLECULAR WEIGHT OF A


COMPOUND BY LOWERING OF FREEZING POINT
(CRYOSCOPIC METHOD).

APPARATUS AND EQUIPMENT

Large test tube 600mL beaker Clamp

Bunsen burner Thermometer Ring and ring


stand

CHEMICALS AND REAGENTS

Naphthalene
Sulfur

5. DETERMINATION OF MOLECULAR WEIGHT OF A


COMPOUND BY ELEVATION OF BOILING POINT
(EBULLIOSCOPIC METHOD)

LAND BERGER’S APPARATUS

A graduated inner tube with a hole in its side

A boiling flask which sends the Solvent vapors into the inner tube through
a nose head

An outer tube which receives solvent vapors coming out from the side
hole of the inner tube

A Beckmann’s thermometer which can read up to 0.01K

CHEMICALS AND REAGENTS

Suitable solvent and solute as suggested by instructor

Benzoic acid Urea oxalic acid

6. DETERMINATION OF PERCENT COMPOSITION OF


LIQUID SOLUTIONS BY REFRACTIVE INDEX

APPARATUS AND EQUIPMENT

Abbe’s refractometer Temperature controller Specific


gravity bottle

Thermometer Glass rod cotton glass


CHEMICALS AND REAGENTS

Alcohol or water

7. DETERMINATION OF REFRACTIVE INDEX AND MOLAR


REFRACTIVITY OF THE GIVEN LIQUID BY
REFRACTOMETER

APPARATUS AND EQUIPMENT

Abbe’s refractometer Temperature controller Specific


gravity bottle

Thermometer Glass rod cotton glass

CHEMICALS AND REAGENTS

Alcohol or water

8. DETERMINATION OF PERCENT COMPOSITION OF


LIQUID SOLUTIONS VISCOMETRICALLY

APPARATUS AND EQUIPMENT

Oswald viscometer Specific gravity bottle


Thermostat

Stops watch Thermometer

CHEMICALS AND REAGENTS

Distilled water
Given liquids: alcohols or ether

9. DETERMINATION OF PARTITION COEFFICIENT OF A


SUBSTANCE BETWEEN TWO IMMISCIBLE

LIQUIDS (BENZOIC ACID BETWEEN BENZENE


AND WATER)

APPARATUS AND EQUIPMENT

Separating funnels Reagent bottles Pipette

Burette Conical flasks

CHEMICALS AND REAGENTS

Benzoic acid Distilled water

Benzene Phenolphthalein

10. DETERMINATION OF VISCOSITY AND


REFRACTIVE INDEX OF LIQUIDS.

APPARATUS AND EQUIPMENT

Oswald’s viscometer Specific gravity bottle Thermostat

Stops watch Thermometer Beaker

Pipette

CHEMICALS AND REAGENTS

Distilled water Ethanol Glycerine


Semester IV
Analytical Chemistry Lab
CHEM-III Lab

1. Experiment: Determination of hardness of water using EDTA

Apparatus:
 Burette 25-30ml
 Glass funnel
 Pipette 1ml
 Volumetric Flask
 Dropper
 Measuring cylinder

Chemical Reagents:
 Water sample,
 EDTA
 Eriochrome Black-T
 NH4CL,
 Ammonia Buffer,
 Magnesium Carbonate,
 90% ethyl alcohol,
 Distilled water.

2. Experiment: Determination of chloride in tap water sample


Apparatus:
 Burette,
 Conical flask,
 Pipette,
 Measuring cylinder

Reagents:
 Potassium chromate indicator solution,
 Standard silver nitrate titrant.

3. Experiment: Gravimetric Analysis of Barium ions in given


solution
Apparatus:
 Beakers
 Hot Plate
 Funnel
 Volumetric Flash
 Filter Paper

Chemical Reagents:
 Potassium Chromate
 Barium Chloride
 Hydrochloric Acid
4. Experiment: Determination of Vitamin C (Ascorbic Acid)
using Iodometry

Apparatus:
 Titration Stand
 Pipette
 Conical Flash
 Burette
 Volumetric Flask
 Beakers
 Measuring cylinders

Chemical Reagents:

 Potassium Iodide
 Iodine
 Starch Powder
 Sample Solution

5. Experiment: Iodometric Determination fo Hydrogen Peroxide

Apparatus:
 Titration Stand
 Pipette
 Conical Flash
 Burette
 Volumetric Flask
 Beakers
 Measuring cylinders

Chemical Reagents:
 Potassium Iodide (10%)
 Acid Mixture
 Potassium Iodate Solution (0.1N)
 Starch Solution (10 g/L)
 Sodium Thiosulfate Solution (0.1N)

6. Experiment: Determination of Arsenic/Copper using


Iodometry

Apparatus:
 Titration Stand
 Pipette
 Conical Flash
 Burette
 Volumetric Flask
 Beakers
 Measuring cylinders

Chemical Reagents:

 Potassium Iodide
 Iodine
 Starch Powder
 Sample Solution

7. Determination of Nickel in a steel sample (Gravimetric)

Apparatus:
 3-Sintered Glass Crucibles; medium porosity (see instructor for these)
 3-400 mL beakers  3-Watchglasses and glass hooks
 1-Rubber Policeman and glass stirring rod
 Whatman No. 40 filter paper; medium porosity
 pH paper

Reagents:

 Unknown Ni ore sample


 Nitric Acid (concentrated)
 Hydrochloric Acid (concentrated)
 20% Tartaric Acid solution (prepared by student)
 1:1 Ammonium Hydroxide solution (prepared by student)
 1% alcoholic dimethylglyoxime solution
 Urea (solid, ACS reagent grade)
 Acidic AgNO3 (already prepared)

8. Determination of Bicarbonate in clinical sample (Blood) using


Back Titration

Apparatus:
 Titration Stand
 Pipette
 Conical Flash
 Burette
 Volumetric Flask
 Beakers
 Measuring cylinders

Reagents:
 0.1% phenol red in 0.003 M NaOH.
 M NaOH and 0.001 M HCL, (should be FRESHLY prepared)
 1% saline (NaCL).

EXPERIMENT 1: QUANTITATIVE & QUALITATIVE


ANALYSIS OF CARBOHYDRATES

Apparatus Required:
 Test tubes
 Dropper
 Test tube holder
 Beakers
 Spirit lamp
 Hot plate

Reagents Required:

Conc. Sulphuric acid


Molisch’s reagent 5% (5% alpha-naphthol solution in 95%
ethanol)
Carbohydrates (glucose, maltose)
Benedict’s solution
Iodine solution
Starch solution
Distilled water

EXPERIMENT 2: QUANTITATIVE AND QUALITATIVE


ANALYSIS OF PROTEINS

Apparatus Required:

 Test tubes
 Dropper
 Test tube holder
 Beakers
 Spirit lamp
 Hot plate

Reagent Required:

FOR NINHYDRIN TEST:

Ninhydrin solution
Amino acid solution

FOR BIURET TEST:

10% NaOH solution


1% copper sulphate solution
Protein solution

FOR XANTHOPROTEIC TEST:

Conc. HNO3
40% NaOH solution
Amino acid solution

FOR MILLIONS TEST:

Mercuric nitrate
Mercurous nitrate
Conc. HNO3
Distilled water

EXPERIMENT 3: QUANTITATIVE AND QUALITATIVE


ANALYSIS OF LIPIDS

Apparatus Required:

 Test tubes
 Dropper
 Test tube holder
 Beakers
 Spirit lamp
 Hot plate

Reagent Required:

FOR SOLUBILITY TEST

Olive oil
Chloroform
Distilled water

FOR SPONIFICATION TEST

20% KOH
Olive oil
FOR IODINE TEST

Oleic acid
Stearic acid
Hubl’s reagent

EXPERIMENT 4: EFFECT OF PH ON ENZYME ACTIVITY

Apparatus Required:

 Test tubes
 Stirrer
 Beakers
 Water bath
 Spectrophotometer

Chemicals Required:

0.1N HCl
Salivary amylase/commercial amylase
Soluble starch
Iodine
Potassium iodide
Distilled water
Na2HPO4
KH2PO4
EXPERIMENT 5: EFFECT OF TEMPERATURE ON ENZYME
ACTIVITY

Apparatus Required:

 Test tubes
 Test tube holder
 Beakers
 Glass rod
 Thermometer
 Water bath
 Spectrophotometer

Chemicals Required:

1% starch solution
1% amylase solution
Iodine solution
0.1N HCl solution

EXPERIMENT 6: DETERMINATION OF PH

Apparatus Required:

 Beakers
 Filter paper
 Funnel
 Glass stirrer
 Petri dish
 Conical flask
 Tripod stand
 Spatula

Chemicals Required:

Distilled water
2 different Sample

EXPERIMENT 7: PREPARATION OF BUFFERS

Apparatus Required:

 Beakers
 Glass rod
 Measuring cylinder
 pH meter

Chemicals Required:

Distilled water
Acid & its salt
Base & its salt

Semester v analytical chemistry


Experiment No 1-
separation of the given mixture of the cations using paper
chromatography
Principle
This experiment is based on the principle of paper chromatography
Introduction
The separation of chemical species is a critical step in many chemical
procedures and processes. Paper Chromatography is a quick and useful
technique for separating pigments and other substances.
Paper Chromatography Is used to separate the metal cations in an aqueous
mixture that possibly contains Fe3+, Ni2+, and Cu2+. On the same
chromatogram, we run known solutions of each of these cations. This is
done for comparative purposes, to identify the cations present in our
unknown mixture based on the chromatographic results, and to confirm
the method is indeed working correctly for this set of cations.
Apparatus required
 Chromatographic paper
 500ml Beaker
 Aluminum foil
 Forceps
 Ruler and led Pencil
 Capillary Tubes

Chemicals required
 Silver Nitrate
 Ferrous Nitrate
 Cobalt nitrate
 Copper Nitrate
 Potassium Iodide
 Hydrochloric Acid
 Butyl Alcohol

Experiment No 2-
3-Analysis of the composition of the mixtures of anilines by TLC

Principle
This experiment is based on the principle of thin layer chromatography
Introduction
TLC is a fast and very convenient technique for determining both the
identity and purity of a compound. In its simplest form, TLC is
accomplished by spotting a small amount of the test substance, dissolved
in an appropriate solvent, on a thin layer of absorbent that is backed by a
glass or plastic plate. The plate is placed in a closed jar (developing
chamber) that contains a small amount of solvent.

As the solvent moves up the plate by capillary action, wetting the dry
absorbent, the dissolved material (or materials) will move up the plate and
“partition” itself between the absorbent and the solvent that is moving up
the plate. The distance the compound moves in a particular solvent system
from the base of the plate (called the baseline) is a characteristic of the
compound just like the melting point or boiling point.

If we divide this distance by the distance the solvent moves, we get a


number called the Rf value (or Retention Factor). Though two compounds
may have the same Rf value, if we spot an unknown compound against a
known standard compound and the two compounds move the same
distance up the plate, we can be fairly sure that these two compounds are
the same.

Apparatus required
 TLC Plate
 Beaker 500ml
 Capillary tube
Chemicals required
 Ethanol
 Methylene Chloride

Experiment No 3-
Separation of sugars using paper chromatography

Principle
This experiment is based on the principle of paper chromatography.
Introduction
The separation of chemical species is a critical step in many chemical
procedures and processes. Paper Chromatography is a quick and useful
technique for separating pigments and other substances.
Paper Chromatography Is used to separate the metal cations in an aqueous
mixture that possibly contains Fe3+, Ni2+, and Cu2+. On the same
chromatogram, we run known solutions of each of these cations. This is
done for comparative purposes, to identify the cations present in our
unknown mixture based on the chromatographic results, and to confirm
the method is indeed working correctly for this set of cations.

Apparatus required
 Chromatographic paper
 500ml Beaker
 Aluminum foil
 Forceps
 Ruler and led Pencil
 Capillary Tubes

Chemicals required

 n-butanol;
 acetic Acid
 Distilled Water
 Volume Ratio (4:1:5)
 Ammoniacal Silver Nitrate (Spraying Agent)

Experiment No 4-
Deionization of water using ion exchange chromatography
Principle
This experiment is based on the principle of ion exchange
chromatography
Introduction
Ion exchange is a very powerful method to remove impurities, residues,
and contaminants from water.
For the ion exchange, substances are used that have a surface property
allowing ions to adhere very well (= so-called ion exchangers). These ion
exchangers are loaded with positively charged hydrogen ions H+ and/or
negatively charged hydroxide ions OH-.
+ -
These ions have a low charge ( ) ( ).
The higher the charge and the smaller the radius of an ion, the more the
ion is bound to the ion exchanger.
If the water to be treated is now passed through an ion exchanger with
positive and negatively charged ions, all positively charged cations in the
water are replaced with positively charged hydrogen ions (H+) and all
negatively charged anions in the water are replaced with negatively
charged OH ions (OH-). This means that the ion exchanger repels all
hydrogen and hydroxide ions and picks up the positive and negative ions
from the water. The H+ and OH- ions repelled by the ion exchanger now
combine to ultrapure, residue-free water outside of the ion exchanger.
This process takes place until the ion exchanger no longer can give off
any H+ or OH- Ions.

Apparatus required
 Columns
 Beakers
 Volumetric Flask
 Measuring Cylinder
Chemicals required
 Hydrochloric Acid
 Potassium Hydroxide
 Sodium chloride
 Cation resins
 Anion Resins
Experiment No 5-
Determine the lambda max of KMnO4 and K2Cr2O7 solutions and
verification of bear lambert’s law
Principle
Instrument
UV-Visible Spectrophotometer
Introduction
The primary objective of this experiment is to determine the concentration
of an unknown KMnO4 solution. prepare five known concentrations
(standard solutions). Each solution is transferred to a small, rectangular
cuvette that is placed into the Colorimeter or Spectrometer. The amount
of light that penetrates the solution and strikes the photocell is used to
compute the absorbance of each solution.

When a graph absorbance vs. concentration is plotted for the standard


solutions, a direct relationship should result. The direct relationship
between absorbance and concentration for a solution is known s Beer’s
law.

Determine the concentration of unknown sample solutions by measuring


their absorbance. By locating the absorbance of the unknown on the
vertical axis of the graph, the corresponding concentration can be found
on the horizontal axis. The concentration of the unknown can a so be
found using the slope of Beer’s law curve.

Apparatus required
 Beakers
 Volumetric flasks
 Cuvette or sample holder
Chemicals required
 KMnO4
 K2Cr2O7
 Distilled water

Experiment No 6-
Separation of amino acids using TLC
Principle
This experiment is based on the principle of thin layer chromatography
Apparatus required
 TLC Plate
 Beaker 500ml
 Capillary tube
Chemicals required
 Ethanol
 Methylene Chloride
 Amino acids sample solution
Experiment No 7-
Determination of aspirin and caffeine by UV-visible spectrometer
Principle
Acetylsalicylic acid forms a color complex with iron chloride that can be
determined using colorimetry. The complex ion formation occurs in two
steps in 1st step aspirin reacts with NaOH to form salicylate dianion .in
second step acidified iron ion addition results in appearance of violet color
complex. The concentration is measured by uv-visble spectrophotometer
Apparatus required
 UV-Visible Spectrophotometer
 Flask
 Pipette
 Beaker ‘

Chemicals required
 Aspirin
 NaOH

Experiment No 8-
Determination of the stoichiometry of a metal complex by visible
spectrometry
Principle
This experiment is based on UV-Visible spectroscopy
Apparatus required
 Beakers
 Volumetric Flask
 Pipette
 Cuvet

Chemicals required
 Distilled water
 Standards of known concentration

BS 5th organic semester


EXPERIMENT # 01
SYNTHESIS OF BENZILDENEACETOPHENONE
3(CHALCONE) FROM BENZALDEHYDE 1 AND
ACETOPHENONE 2.
CHEMICALS REQUIRED:
 Benzaldehyde  NaOH solution
 Acetophenone  Ethanol
APPARATUS :
 Conical flask  Glassrode
 Condenser  Filter paper
 Beaker  Round bottom flask
 Pipette
EXPERIMENT # 02
SYNTHESIS OF DIBENZALACETONE 3(1,5 DIPHENYL, 1,4
PENTADIENE-3-ONE)FROM BENZALDEHYDE AND
ACETONE 2
CHEMICALS REQUIRED:
 Benzaldehyde  Acetone
 Ethanol  NaOH solution
APPARATUS :
 Conical flask  Beaker
 Condenser  Pipette
 Glassrode  Round bottom flask
 Filter paper
EXPERIMENT # 03
PREPRATION OF SCHIFF BASE USING THE
BENZALDEHYDE AND ANILINE
CHEMICALS REQUIRED:
 aniline  benzaldehyde
 ethanol  HCL/H2SO4

APPARATUS :
 conical flask  magnetic stirrer
 beakers  filter paper
 round bottom flask  pipette
 condenser  glassrode
 hot plate

EXPERIMENT # 04
SYNTHESIS OF AMIDE FROM ANILINE AND
BENZOYLCHLORIDE
CHEMICALS REQUIRED:
 ANILINE  MgSO4
 PYRIDINE  DCM( dichloromethane )
 BENZOYL CHLORIDE  HCL/H2SO4

APPARATUS :
 Hoteplate  Filter paper
 Magnetic stirrer  Beakers
 Round bottom flask  Separating funnel
EXPERIMENT # 05
SYNTHESIS OF BENZONINE FROM BENZALDEHYDE
CHEMICALS REQUIRED:
 benzaldehyde  ethanol
 potassium cyanide(KCN)
APPARATUS :
 Hoteplate  Magnetic stirrer
 Round bottom flask  Beakers
 Filter paper  Separating funnel

EXPERIMENT # 06
SYNTHESIS OF BENZIL FROM BENZONIN
CHEMICALS REQUIRED:
 Benzonin  Ice cold water
 Nitric acid  Nitric acid
 Ethanol
APPARATUS :
 Hoteplate  Magnetic stirrer
 Round bottom flask  Beakers
 Filter paper  Separating funnel
EXPERIMENT # 07
SYNTHESIS OF BENZILIC ACID FROM BENZIL

CHEMICALS REQUIRED:
 benzil  HCL
 potassium hydroxide  ethanol
APPARATUS
 round bottom flask  filter paper
 pipette  round bottom flask
 hotplate  china dish
 condenser  stands
EXPERIMENT # 08
POLARIMETER USED TO MEASURE THE OPTICAL
ACTIVITY
CHEMICALS REQUIRED:
 suagr(maltos)
 water
APPARATUS :
 polarimeter

SEMESTER-V COURSE
PHYSICAL CHEMISTRY CHEM-271 LAB.
Experiment no.1
Equilibrium constant of the KI + I2 = KI3 reaction.
Apparatus Required:
Beakers, Separating funnel, Wash bottle, Burette, Clamp, Volumetric
flask
Chemicals Required:
Solid iodine, 0.1M KI, 0.05M sodium thiosulphate, Starch indicator,
Distilled water, Hexane (organic solvent)
Experiment no.2
Kinetics of saponification of ethyl acetate.
Apparatus Required:
Conductometer, Conductivity cell,Burette, Pipette, Conical flask,
beakers.
Chemicals Required:
Ethylacetate solution (N/25), NaOH (N/25) Analytical Lab 7th
semester Physical Chemistry Lab 5th semester 3, Acetic acid
(N/10), Oxalic acid
Experiment no.3
Acid catalyzed hydrolysis of sucrose.
Apparatus Required:
Polarimeter, Sodium-vapor lamp, Thermostat and circulating pump,
Two water-jacketed polarimeter tubes, Two #3 rubber stoppers; pure
sucrose, Three 25-ml pipettes.
Chemicals Required:
100 ml of 4 M hydrochloric acid, 100 ml of 4 M monochloroacetic
acid;
Experiment 4:
Study of the adsorption isotherms of acetic acid-charcoal system.
Apparatus Required:
6 boiling flasks (250 ml), 6 Erlenmayer’s flasks (250 ml), 6 funnels, 3
burettes (50 ml), 3 10 titrimetric flasks, 3 pipettes, Holders for funnel,
Holders for burettes IX. Filtering paper,Wessels for weighing coal,
Spoon, Rubber stoppers
Chemicals Required:
Solution of acetic acid (c = 1 mol dm-3 ),
Solution of NaOH (c = 0.2 mol dm-3 ), Activated charcoal,
Experiment 5:
Determination of activation energy for the acid catalyzed hydrolysis
of ethyl acetate.
Apparatus Required:
Thermostat, pipettes, Burette, Volumetric flasks, Titrimetric flasks,
Stop watch.
Chemicals Required:
Solution of ethyl acetate (c = 0.04 mol dm-3 ), Solution of sodium
hydroxide (c = 0,04 mol.dm-3 ), Solution of hydrochloric acid (c = 0,04
mol.dm-3 ), Phenolphthalein.
Experiment 6:
Determination of partial molar volumes.
Chemicals Required:
Sodium chloride,
Apparatus Required:
Mettler density meter, Fiive 50-ml stoppered flasks, A constant
temperature bath set to 25.0°C.
Experiment 7:
Characterization of the given compound by UV-Vis spectroscopy.
Apparatus Required:
UV/VIS spectrophotometer, Polystyrene cuvettes, 2 100 mL volumetric
flask, 1000 μL micropipette, 100 μL pipet, Hot plate, 1 10 mL graduated
cylinders, 6 10 mL volumetric flasks, 2 125 mL Erlenmeyer flasks or
150 mL beakers
Chemicals Required:
I. Solid KMnO4

SEMESTER 5TH INORGANIC CHEMISTRY


EXPERIMENT.NO.1

PREPARATION OF TETRAMINE COPPER SULPHATE:

APPARATUS:

 Filter paper  Measuring Cylinder


 China dish  Spatula
 Funnel  Beaker
 Conical Flask
CHEMICALS:

 CuSO4.5H2O  Ethanol
 Conc HNO3  Distilled water

EXPERIMENT.NO.2

PREPARATION OF POTASSIUM TRIOXALATO CHROMATE


TRIHYDRATE

APPARATUS:

 Beaker  Filter paper


 Conical flask  Hot plate
 Magnetic stirrer  Tri pod stand
 Funnel
CHEMICALS:

 Potassium chromate  Ethanol


monohydrate  Distilled water
 Oxalic acid dihydrate  Potassium dichromate

EXPERIMENT.NO.3

PREPARATION OF POTASSIUM TRIOXALATO ALUMINATE

APPARATUS:

 Beaker  Funnel
 Filter paper  Pipette
 Burette  Conical flask
 Hot plate  Weighing balance

CHEMICALS:

 Aluminum sulfate  Potassium permanganate


 Sodium hydroxide  Distilled water
 Oxalic acid

EXPERIMENT.NO.4

PREPARATION OF CIS-POTASSIUM DIOXALATO


DIAQUACHROMATE

APPARATUS:

 Weighing balance  Conical flask


 Bunsen burner  Tripod stand
 Conical flask  Watch glass
 Funnel
 Water bath  Glass rod
 Wire gauze
CHEMICALS:

 Oxalic acid  Ethanol


 Potassium dichromate
EXPERIMENT.NO.5

DETERMINATION OF ZINC AND CADMIUM BY


COMPLEXOMETRIC TITRATION

APPARATUS:

 Burette  Conical flask


 Pipette  Standard flask
 Funnel  Measuring Cylinder
 Burette stand  Weighing bottle

CHEMICALS:

 EDTA solution  Distilled water


 Calcium carbonate  Erichrom black T indicator
 Zinc sulphate solution  Buffer solution

EXPERIMENT NO.6

SPECTROPHOTOMETRIC DETERMINATION OF IRON

APPARATUS:

 Cuvette  Volumetric flask


 Spectrophotometer  Micropipette

CHEMICALS:
 Iron solution  Hydroxyl amine
 Distilled water  o-phenanthroline solution

EXPERIMENT NO.7

SPECTROPHOTOMETRIC DETERMINATION OF Mn

APPARATUS

 Cuvette  Volumetric flask


 Spectrophotometer  Micropipette

CHEMICALS

 Buffer  Fe-Mn powder


 Aqua regia  2-hydroxy-3-methoxy
 Chloroform benzaldehyde

EXPERIMENT.NO. 8

SPECTROPHOTOMETRIC DETERMINATION OF NICKEL

APPARATUS

 Cuvette  Volumetric flask


 Spectrophotometer  Micropipette
 pH meter

CHEMICALS

 Ethanol  Buffer solution


 Dimethyl formamide  2-amino acetophenone
 Sodium acetate isonicotinoyl hydrozone
 Distilled water

EXPERIMENT NO.9

CHROMATOGRAPHIC SEPARATION OF TRANSITION


METALS

APPARATUS:

 Chromatographic paper  Ruler


 Capillary tube  Pencil
 Plastic wrap
CHEMICALS:

 Eluting solvent
 Developing solvent
 Transition metal cations

Unknown mixture of transition metal


APPLIED CHEMISTRY LAB SEM-VI
Experiment#1
MEASUREMENT OF WATER HARDNESS WITH EDTA
TITRATION
Apparatus Required:
 Water sample  Dropper
 Burette 25-30ml  Burette
 Glass funnel  Iron stand
 Pipette 1ml  Measuring cylinder
 Flask
Chemicals Required:
 EDTA  Magnesium Carbonate
 Eriochrome Black-T  90% ethyl alcohol
 NH2Cl  Distilled water
 Ammonia Buffer

Experiment#2
ESTIMATION OF TOTAL SOLID IN WATER
Apparatus Required:
 Evaporating Dish  Graduated Cylinders
 Water Bath  Dish Tongs
 Oven  Gooch Crucibles
 Desiccators  Filter paper
 Analytical Balance  Vacuum Pumps
70
 Crucible tongs
Chemicals Required:
 Sample
 Distilled water

Experiment#3
ESTIMATION OF CHLORIDE IN WATER
Apparatus Required:
 Burette  Pipette
 Iron stand  Measuring cylinder
 Dropper  Beaker
 Conical flask
Chemicals Required:
 Potassium chromate indicator solution
 Sample
 Distilled water
 Sodium Chloride
 Standard silver nitrate as a titration agent.

Experiment#4
ESTIMATION OF FERROUS AND FERRIC IONS IN DRINKING
WATER BY REDOX REACTION
Apparatus Required:
 100 ml standard flask
 Burette
 Conical Flask

71
 20 ml Pipette
 Simple balance with weights
 Iron stand
Chemicals Required:
 K2Cr2O7  H2SO4
 SnCl2  Ortho phosphoric acid
 HgCl2  Diphenylamine
 HCl  Distilled water
 Ferric ion solution

Experiment#5
ESTIMATION OF CAPSICUM OIL BY SOXHLET
EXTRACTION
Apparatus Required:
 Soxhlet glassware  Iron stand
 Condenser  Clamp
 Aluminum foil  Funnel
 Round bottom flask  Separating funnel
 Hot plate  Beaker
 Magnetic Stirrer
Chemicals Required:
 Capsicum
 Ethanol

Experiment#6
ESTIMATION OF CLOVE OIL FROM CLOVES
Apparatus Required:

72
 Heating mantle  Separating funnel
 Round bottom flask  Beaker
 Biomass flask  Voil
 Condenser  Measuring cylinder
Chemicals Required:
 Clove buds (Syzygium aromaticum)
 96% N-hexane
 100% Acetic acid glacial
 99.9% Ethanol
 99.0% Acetone

Experiment#7
PREPARATION OF LIQUID DETERGENTS
Apparatus Required:
 Dropping pipette  Heat resistant mat
 Measuring cylinders  Ice bath
 Beakers  Hot plate
 Glass rod  Filter flask
 Spatula  Funnel
 Bunsen burner  Filter papers
 Tripod and gauze
Chemicals Required:
 Castor oil
 Ethanol
 Sodium hydroxide solution, 5 M
 Sodium chloride, 10 g
 Concentrated sulfuric acid
 Purified water (distilled or deionised)
73
Experiment#8
STUDY OF KINETICS OF DISSOLUTION OF MAGNESIUM
METAL IN DILUTE HCl
Apparatus Required:
 Conical flask (100 cm3)
 Single-holed rubber bung and delivery tube to fit conical flask
 Trough or plastic washing-up bowl
 Measuring cylinders
 Clamp stand, boss and clamp
 Stopwatch
 Graph paper
Chemicals Required:
 Magnesium ribbon cut into 3 cm lengths
 Dilute hydrochloric acid, 1M

Experiment#9
ESTIMATION OF MANGANESE IN STEEL
Apparatus Required:
 UNICAM UV/VIS Spectrophotometer
 Volumetric flask
 Beakers
 Pipette
 Measuring cylinder
 Cuvette
Chemical Required:

74
 Ni (NO3)2 .6 H2O
 Murexide
 Distilled water
 KMnO4

Experiment#10
ESTIMATION OF FERRIC IRON IN CEMENT
Apparatus Required:
 UNICAM UV/VIS Spectrophotometer
 Volumetric flask
 Beakers
 Pipette
 Measuring cylinder
 Cuvette
Chemicals Required:
 Stock Fe solution (0.050 mg Fe+3/ ml)
 1 M ammonium acetate (NH4C2H3O2), buffer to maintain pH = 3.5
 10% Hydroxylamine HCl (NH3OHCl), reducing agent
 0.3% o-phenanthroline (C12H2N2)
 10 drops 3 M H2SO4

FUEL CHEMISTRY LAB EXPERIMENT CHEM-6TH SEM

75
EXPERIMENT.NO.1
DETERMINATION OF MIXTURE CONTENTS OF COAL
APPARATUS:
 Oven  Weighing balance
 Desicator  Petri dish
 Spatula  Crucible
CHEMICALS:
 Coal sample

EXPERIMENT.NO.2
DETERMINING OF ASH CONTENT IN COAL SAMPLE
APPARATUS:
 Crucible  Furnace
 Coal sample  Weighing balance
CHEMICALS.
 Coal sample

EXPERIMENT NO. 3
DETERMINATION OF VOLATILE MATTER IN COAL
SAMPLE
APPARATUS:
 Crucible  Dessicator
 Furnace  Weighing balance
CHEMICALS:

76
 1g moisture free coal sample

EXPERIMENT.NO.4
DETERMINATION OF FIXED CARBON IN COAL SMPLE
APPARATUS:
 Furnace  Dessicator
 Crucible  Weighing balance
CHEMICALS:
 Coal sample

EXPERIMENT NO. 5
DETERMINATION OF SULPHUR IN COAL
APPARATUS:
 Coal sample  Filter paper
 Beakers  Funnel
 Bomb calorimeter  Stirrer
CHEMICALS:
 BaCl2  Coal sample
 Distilled water  H2SO4

EXPERIMENT NO. 6
DETERMINATION OF HYDROGEN AND NITROGEN IN COAL
APPARATUS:
 Kjeldahl flask  Distillation flask

77
 Condenser  Conical flask
 Bunsen burner  Beaker
 Iron stand
CHEMICALS:
 H2SO4  NaOH
 Coal sample  Distilled water

EXPERIMENT NO 7
DETERMINATION OF SULPHATED ASH IN LUB OIL
APPARATUS:
 Bunsen burner  Spatula
 Evaporating disk  Pipette
 Iron stand
 Measuring balance
CHEMICALS:
 Lubricating oil
 H2SO4
 Distilled water

EXPERIMENT.NO.8
DETERMINATION OF ASH CONTENT IN PETROLEUM
PRODUCTS
APPARATUS:
 Crucible  Weighing balance
 Furnace
CHEMICALS.

78
 Petroleum sample

79
SEMESTER VI

PHYSICAL CHEMISTRY

CHEM 371 LAB

Experiment:

Spectroscopic determination of Cu percentage in the given


sample.

Apparatus:

 Spectrophotometer
 Cuvettes
 Paper wipes

Reagents:

A set of Cu2+ (Aqueous copper (II) sulphate solution ) Standards (


5g/L , 4g/L , 3g/L, 2g/L, 1g/L)

80
Experiment

To determine the effectiveness of an extraction of I2 solution by


using Solvent Extraction method.

Apparatus:

 Separating funnel
 Beakers/containers
 Iron stand

Reagents:
 Aqueous solution (iodine in water)
 Organic solvent

Experiment

Determination of molecular weight of a polymer by viscosity


method.

Apparatus:

 Viscometer
 Stopwatch
 Rubber tube
 Specific gravity bottle

Reagents:

 Distilled Water

81
 Polymer solution

Experiment

Determination of percentage composition of KMnO4/ K2Cr2O7


in a given solution by spectrophotometry.

Apparatus:

 Spectrophotometer
 Cuvettes
 Paper wipes

Reagents:

A set of sample solution


 2ppm
 4ppm
 6 ppm
 8 ppm
 10 ppm
 Blank

82
Experiment:
Evaluation of pKa value of an indicator (Bromothymol Blue) by
spectrometric method.

Apparatus:
• Cuvets
• 10-mL graduated cylinder
• pH meter and electrodes
• 1-mL pipette • 5-mL pipet
• scanning spectrophotometer
• 12, 25-mL volumetric flasks

Reagents:
• bromothymol blue solution (0.1% in 20% ethanol)
• hydrochloric acid (concentrated)
• KH2PO4 solution (0.10 M)
• Na2HPO4 solution (0.10 M)
• sodium hydroxide solution (4 M)

• Cuvets
• 10-mL graduated cylinder
• pH meter and electrodes
• 1-mL pipette • 5-mL pipet
• scanning spectrophotometer
• 12, 25-mL volumetric flasks

83
Reagents:
• bromothymol blue solution (0.1% in 20% ethanol)
• hydrochloric acid (concentrated)
• KH2PO4 solution (0.10 M)
• Na2HPO4 solution (0.10 M)
• sodium hydroxide solution (4 M)

Semester VI
Organic Chemistry Lab
CHEM-361 LAB

1. Experiment: Nitration of Nitrobenzene to Meta-


dinitrobenezene

Apparatus:
 Round Bottom Flask
 Beakers
 Reflux Condenser
 Stirrer
 Hot plate
 Funnel
 Iron stand
 Measuring Cylinder

Reagents:
 Conc. HNO3
 Conc. H2SO4
 Nitrobenzene

84
2. Experiment: Sulphonation of Aniline

Apparatus:
 Round Bottom Flask
 Water bath
 Beakers
 Stirrer
 Iron stand
 Measuring Cylinder
 Funnel
 Filter paper

Reagent:
 Aniline
 Con. H2SO4
 NaOH
 Water
 Decolourizing carbon

3. Experiment: Oxidation of Benzaldehyde


Apparatus:
 Conical Flask,
 Round Bottom flask,
 Beaker

85
 Filter Paper
 Condenser
 Stirrer
 Stand,
 Funnel

Reagent:
 Benzaldehyde
 KmnO4
 Anhydrous Na2CO3
 Na2SO3

4. Experiment: Oxidation of Cyclohexanol to cyclohexanone

Apparatus:
 Round Bottom Flask
 Beaker
 Measuring cylinder
 Pipette
 Thermometer
 Glass Rod
 Iron Stand
 Iron ring
 Cold Water bath
 Hot plate
 Separatory funnel
 Distillation apparatus

Reagents:
 Cyclohexanol

86
 Bleach
 Glacial Acetic Acid
 Na2CO3
 Nacl
 DCM
 Sodium Bisulfate (NaHSO3)
 Sodium Hypochlorite

5. Experiment: Preparation of benzoic acid and benzyl alcohol


from benzaldehyde using Cannizzaro’s reaction

Apparatus:
 Beaker
 Funnel
 Separatory Funnel
 Measuring cylinder
 Filter paper

Reagents:
 Benzaldehyde
 NaOH
 Ethyl Acetate
 Na2SO4
 HCl

Determination of chloride.
Apparatus:
 Test tube
 Burner
87
 Test tube holder
 Volumetric flask
 Spatula
 Measuring cylinder
Required chemicals:
 Nacl salt
 K2Cr2O7
 Conc.H2SO4
 NaOH
 Acetic acid
 Lead acetate
 Distilled water
(2)
Determination of bromide:
Apparatus:
 Test tube
 Burner
 Test tube holder
 Volumetric flask
 Spatula
 Measuring cylinder
Required chemicals:
 KBr salt
 Conc.HNo3
 CCl4
 Distilled water
(3)
Determination of iodide.
Apparatus:

88
 Test tube
 Test tube holder
 Volumetric flask
 Spatula
 Measuring cylinder
Required Chemicals:
 NaI salt
 NaNo2
 CCl4
 CH3COOH
 Distilled water
(4)
Determination of Nitrate.
Apparatus:
• Test tube
• Test tube holder
• Volumetric flask
• Spatula
• Measuring cylinder
Required Chemicals:

 NH4No3 salt
 FeSO4
 Dil.H2SO4
 Conc.H2SO4
 Distilled water

(5)
Determination of acetate:
Apparatus:

89
 Test tube
 Test tube holder
 Volumetric flask
 Spatula
 Measuring cylinder
Required Chemicals:
 CH3COONa salt
 C2H5OH
 Conc.H2SO4
 Distilled water
(6)
Determination of oxalate:
Apparatus:
• Test tube
• Test tube holder
• Volumetric flask
• Spatula
• Measuring cylinder
Required chemicals
 Na2C2O4 salt
 Dil.H2SO4
 Mg.powder
 Resorcinol
 Conc.H2SO4
 Distilled water
(7)
Determination of sulphate:
Apparatus:
 Test tube

90
 Burner
 Test tube holder
 Volumetric flask
 Spatula
 Measuring cylinder
Required Chemicals:
 Na2SO4 salt
 Dil.HCl
 Bacl2
 Conc.HCl
(8)
Determination of borate:
Apparatus:
• Test tube
• Burner
• Test tube holder
• Volumetric flask
• Spatula
• Measuring cylinder
• Platinum wire
Required Chemicals:
 Na2B4O7.10H2O salt
 Lead acetate
 Distilled water
(9)
Determination of phosphate:
Apparatus:
• Test tube
• Burner
• Test tube holder
• Volumetric flask
• Spatula

91
• Measuring cylinder
Chemicals:
 AlPO4
 Conc.HNO3
 Ammonium Molybdate
(10)
Iodometric titration with potassium iodate:
Apparatus:
 Glass beaker
 Burette with PTFE stopcock
 Ring stand
 Burette clamp
 Glass funnel
 Erlenmeyer flask
 Measuring cylinder
 Volumetric flask
 Dropper
Required Chemicals:
 Potassium iodate
 Potassium iodide
 H2SO4.soln
 Starch indicator
 Sodium thiosulfate
 Distilled water
(11)
Determination of % age purity of KBr using Fluoresceine as
indicator.
Apparatus:
 Glass beaker

92
• Burette with PTFE stopcock
• Ring stand
• Burette clamp
• Glass funnel
• Erlenmeyer flask
• Measuring cylinder
• Volumetric flask
• Dropper
Required Chemicals
 KBr
 AgNO3
 Fluorescein indicator
 Distilled water
(12)

Determination of strength of NaCl given solution by AgNO3 using


Fluorescein as indicator.
Apparatus:
 Glass beaker
• Burette with PTFE stopcock
• Ring stand
• Burette clamp
• Glass funnel
• Erlenmeyer flask
• Measuring cylinder
• Volumetric flask
• Dropper
• Electronic balance
• Spatula
Required chemicals:
 Nacl

93
 AgNO3
 Fluorescein indicator
(13)
Spectrophotometric determination of cerium.
Apparatus:
 Spectrophotometer A unicam SP8-200 spectrophotometer
equipped with 1cm glass cells was used
 pH meter
 Volumetric flask
 Measuring cylinder
 Spatula
 Electronic balance
Required Chemicals:
 Methyl thymol blue solution
 Cerium(lll) nitrate hexahydrate
 Disodium oxalate
 Potassium cyanide
 Glycine stock solution
 Nacl
 NaOH
(14)
Percentage determination of barium in barium nitrate by
gravimetric method
Apparatus:
 Beakers
 Measuring cylinder
 Hot plate
 Funnel
 Conical flask
 Whatmann filter paper
 Oven

94
 Petri dish
Required chemicals:
 Barium nitrate
 K2CRO4
 Distilled water

(15)
Separation and of heavy metals from concentrated smelting
wastewater by solvent extraction
Apparatus:
 Hot plate
 Condensers
 Round bottom flask
 pH meter
 Conical flask
 Magnetic stirrer
 Separating funnel
 Beakers
Required chemicals:
 Concentrated smelting waste water
 2-hydroxy-5-nonylacetophenone oxime (Mextral 84H)
 bis(2,4,4 -trimethylpentyl)-phosphinic acid (Cyanex 272) in an
aliphatic diluent (DT-100)

BS 7th Semester Analytical Lab-2 (major lab)


Experiment # 01
Gravimetric determination of Ni(II) using DMG reagent.
Apparatus required:

95
Gooch crucible, beakers 500ml, watch glass, graduated cylinder,
stirring rods, wash bottles, funnel filter paper, iron stand.
Chemicals Required:
Unknown nickel solution, 6M HCl soln., 6M NH3 soln., conc. NH3,
0.1M AgNO3, 1% dimethyl glyoxime (DMG) in 95% ethanol.

Experiment # 02
Determination of major oxides in Portland cement.
Apparatus required:
Weighing balance, furnace, beakers, measuring cylinders, ashless
filter papers, crucibles, volumetric flasks, funnel, burette.
Chemicals Required:
Conc. HCl, ammonium chloride, ammonium oxalate, ammonium
nitrate, ammonia soln. salicylic acid, methyl red indicator, buffer soln.
(Ph 4, 10)

Experiment # 03
Preparation Of Standard thiosulphate solution and determination of
hypochlorite in a commercial bleach product.
Apparatus Required:
2L beakers, 1L storage bottle, three 250 ml flasks, pipette, 10ml
graduated cylinder, tripod stand, burners.
Chemicals Required:
6M HCl, KI, I2, Na2CO3, Na2S2O3.5H2O, soluble potato starch, H2SO4
(3M), liquid bleach.
Experiment # 04

96
Determination of Aluminium in an unknown sample by back
titration.
Apparatus Required:
Burette, beakers, volumetric flasks, funnel, weighing balance, titration
flask, water bath, pipette, sucker.
Chemicals required:
0.01 M EDTA, buffer solution, 0.01M ZnSO4, Erichrome black T
(EBT), unknown sample.
Experiment # 05
Determination of Al2O3 percentage in Portland cement by back
titration.
Apparatus required:
Beakers, volumetric flask, burette, funnel, weighing balance, titration
flask, pipette, water bath.
Chemicals required:
0.01 M EDTA, buffer solution, EBT indicator, 0.01 M ZnSO4, cement
sample.
Experiment # 06
Apparatus required:
Burette, iron stand, 200ml volumetric flask, 20ml pipette, measuring
cylinders, 250ml conical flask, funnel, weighing balance.
Chemicals required:
Different samples containing vitamin C, 0.005 M iodine solution,
distilled water, starch solution.
Experiment # 07
Determination of CO2 in soft drink.
Apparatus Required:

97
Erlenmeyer flask, burette, beaker, pipette, measuring cylinder,
volumetric flask, weighing balance, thermometer.
Chemicals required:
1M NaOH, phenolphthalein indicator, soft drink sample, 0.05 M
oxalic acid.
Experiment # 08
Preparation of Biodiesel
Apparatus required:
Beaker, hot plate, petri dish, foil, thermometer, magnetic stirrer,
separating funnel,, measuring cylinder.
Chemicals required:
Vegetable oil/coconut oil, methanol, NaOH/KOH.
Experiment # 09
Determination of free fatty acids in oil sample
Apparatus required:
Burette, iron stand, volumetric flask, pipette, funnel, weighing
balance, conical flask, separating funnel, measuring cylinder.
Chemicals required:
Oil sample, 50% butanol, 0.1 M NaOH, 0.01 M oxalic acid,
phenolphthalein indicator, distilled water.
Experiment # 10
Determination of barium ions in the given solution by gravimetric
analysis.
Apparatus required:
Beakers, funnel, hot plate, filter paper, volumetric flask.
Chemicals required:
Potassium chromate, barium chloride, hydrochloric acid.
98
Experiment # 11
Separation of spinach plant pigments by column chromatography.
Apparatus required:
Volumetric flask, measuring cylinder, burette as column, spatula,
funnel, cotton, hot plate, petri dish, pestle mortar, conical flask.
Chemicals required:
Sand, silica, n-hexane, acetone, sample solution (spinach plant
extract), tetrachloromethane.
Experiment # 12
Solvent extraction of caffeine from coffee
Apparatus required:
Measuring cylinder, beaker, burette stand, watch glass, water bath,
funnel, separating funnel.
Chemicals Required:
Magnesium sulphate, dichloromethane, distilled water, coffee, sodium
carbonate.
Experiment # 13
Thin layer chromatography of extracted sample of caffeine
Apparatus required:
Beaker, TLC plate, lead pencil, measuring cylinder, UV-lamp,
pipette, hot plate, ruler, round bottom flask.
Chemicals required:
Extracted coffee, ethyl acetate, acetic acid, methanol.
Experiment # 14
Gravimetric analysis of Zn+2 by anthranilic acid
Apparatus required:

99
Volumetric flask, round bottom flask, round bottom flask measuring
cylinder, hot plate, drying oven.
Chemicals required:
ZnCl2, conc. HCl, anthranilic acid, sodium bicarbonate.
Experiment # 15
Separation of metal ions by paper chromatography
Apparatus required:
Measuring cylinder, capillary tube, chromatographic paper,
chromatographic tank.
Chemicals required:
Lead nitrate, mercury nitrate, cadmium nitrate, ethanol, potassium
dichromate, distilled water.
Experiment # 16
Determination of ß-carotene from carrot.
Principle:
Solvent extraction
Apparatus required:
Hot plate, stirrer, pipette, sucker, separating funnel, water bath,
volumetric flask, spectrophotometer.
Chemicals required:
Crushed carrot, distilled water, diethyl ether, methanol
Experiment # 17
Determination oif unknown concentration or %age composition of
KMnO4 by spectrophotometer.
Apparatus required:
Measuring cylinder, burette, volumetric flask, spectrophotometer,
pipette, sucker.
100
Chemicals required:
KMnO4, distilled water.
Experiment # 18
Apparatus required:
Funnel, china dish, cotton, burner, tripod stand.
Chemicals required:
Nephtalene, anthracene, camphor, distilled water.

Extraction of plants using hydrodistillation.


Appatarus:
Weigning balance, Clevenger apparatus (heating mantales, 1000ml
round bottom flask, condenser), separating funnel, funnel stand
Chemicals
Anhydrous sodium sulphate.
Extraction of essential oil from spices (zeera)
Apparatus:
Pestle mortar, weighing balance, round bottom flask, condenser,
heating mantals, cold water, supply filter paper, separating funnel.
Chemicals
Ethyl ethanoate, spices (zeera), anhydrous magnesium sulphate/
anhydrous calcium chloride (1-2g), water
Extraction of essential oil by steam distillation.
Apparatus:
Steam distillatory, heater
Chemicals: water
Determination of Iodine value of oil sample.
101
Apparatus:
Glass stoppered iodine flask 9250ml), cylinder, burett in oil samplee
Chemicals:
Carbon tetrachloride, 15% potassium iodide soln. (15g/100ml), 0.1N
Na2S2O3.5H2O (25g/L), Starch (1g in 100ml boiling soln.), wijis soln.
(dissolve separately resublimed iodine (8g) & iodine tetrachloride
(7.5g) in glacial acetic acid by warming on a water bath, mix the two
solns. And dilute to 1L with glacial acetic acid in cold.

Determination of saponification value of given sample

Apparatus:

Conical flask, beaker weighing balance, dropper, Reflux, condenser,


boiling water bath, glass pipette, burette.

Chemicals:

Alcoholic KOH (0.2805g/100ml of 95% ethanol V/V), HCl (0.5N),


phenolphthalein indicator

Determination of free fatty acid (FFA) in oil sample

Apparatus:

Conical flask, beaker weighing balance, dropper, Erlenmeyer flask,


cylinder

Chemicals:

102
Oil sample, ethyl alcohol 95%, phenolphthalein indicator 1%,
isopropyl alcohol, NaOH (0.1M), neutralized isopropyl alcohol.

Determination of % free fatty acid (FFA)and acid value of


biodiesel

Apparatus:

Conical flask, beaker, dropper

Chemicals:

Ethanol, phenolphthalein indicator, NaOH (4g/L)

Determination of peroxide value of oil sample

Apparatus:

Weighing balance, burette, iodine flask, Erlenmeyer flask 250 ml with


stopper, stop watch

Chemicals:

Chloroform, cyclohexane, conc. Formic acid, glacial acetic acid,


isooctane, methanol, starch, sodium thiosulphate soln., 0.01/L(0.01N)
or 0.1 mol/L 0.1N thyodene, potassium iodide, distilled water,
saturated potassium iodide solution in deionized water freshly
prepared, the soln. must remained saturated and kept protected from
light, Starch Soln. 1% = soluble starch 10g in deionized water, 1000
ml with heating formic acid, 3ml is added to stabilized the solution.

Sodium thiosulphate solun.; the soln. kept to be in the dark and to be


prepare freshly

103
Solvent mixture I: glacial acetic acid : chloroform (3:2)

Solvent mixture II: glacial acetic acid : cyclohexane (3:2)

Solvent mixture III: glacial acetic acid a; isooctane (3.2)

Preparation of standard molar, molal, normal soln., % ppm %


ppb soln.

Apparatus:

Weighing balance, beaker, conical flask, pipette, burette, dropper,


measuring cylinders.

Chemicals:

HCl, NaOH, C2H5OH, NaCl, distilled water.

Preparation of 1 dm3 of 0.1 acetate buffer having pH 5.2

Apparatus:

pH meter, beaker, pipette, vol. flask, glass rod, standard buffer,


weighing balance.

Chemicals:

Acetic acid, sodium acetate, distilled water

Preparation of 1 dm3 of 0.1 M phosphate having pH 7

Apparatus:

pH meter, beaker, pipette, vol. flask, glass rod, standard buffer,


weighing balance.

104
Chemicals:

Disodium hydrogen phosphate, sodium dihydrogen phosphate.

Determination of dissociation constant of weak acid using


potentiometer

Apparatus:

pH meter, beaker, pipette, vol. flask, glass rod, standard buffer,


weighing balance.

Chemicals:

0.1 M acetic acid, 0.1 M NaOH, distilled water.

Calibration of pH meter and determination of pH of buffers


prepared from acetic acid and sodium acetate

Apparatus:

pH meter, beaker, pipette, vol. flask, glass rod, standard buffer,


weighing balance.

Chemical:

Standard buffer, acetic acid, sodium acetate, water

Determine the strength of HCl soln. by titrating it against the


NaOH soln using potentiometer.

Apparatus:

pH meter, beaker, pipette, vol. flask, glass rod, standard buffer,


weighing balance.

105
Chemicals:

HCl soln., 0.1M NaOH, standard buffer

Determine the strength of acetic acid soln. by titrating it against


NaOH soln. using potentiometer

Apparatus:

pH meter, beaker, pipette, vol. flask, glass rod, standard buffer,


weighing balance.

Chemicals:

acetic acid soln., water, buffer

Semester 8th :
Experiment No 1:
Determination of fat content in milk
Apparatus Required:
 Beakers
 Butyrometer
 Measuring Cylinder
 Centrifuge
 Water Bath
 Hot Plate
Chemicals Required:
 Milk Sample
 Alcohol (Ethanol or Methanol)
 Sulphuric Acid

106
Experiment No 2:
Quantification of Protein
This experiment is based on UV-Visible spectroscopy
Apparatus Required:
 Beakers
 Weighing Balance
 Measuring Cylinder
 UV-Visible spectrophotometer
Chemicals Required:
 Standards solution of protein samples

Experiment No 3:
Quantification of reducing sugars and total sugars
Apparatus Required:
 Burette
 Beakers
 Weighing Balance
 Conical Flask
 Measuring Cylinder
Chemicals Required:
 Fehling solution
 Sugar Sample
Experiment No 4:
Water analysis for drinking purpose (Hardness of water)
Apparatus Required:
Burette
107
Pipette
Titration Stand
Beakers
Conical Flask
Chemicals Required:
Soap solution (wanklyn solution)
Experiment No 5:
Determination of the Caffeine
Principle:
It is a solvent extraction based on the solubility of compounds
Apparatus Required:
 Beakers
 Separating Funnel
 Hot Plate
 Pipette
 Filter Paper
 Funnel
Chemicals Required:
 Coffee Sample 10g
 Sodium Carbonate 4g
 Distilled Water 100ml
 Chloroform 15ml
 Magnesium Sulfate

Experiment No 6:
Determination of Heavy Metals in Food Sample
Principle:
This experiment is base on the UV-Visible spectroscopy
108
Apparatus Required:
 Titration stands
 Beakers
 Volumetric Flasks
 Weighing Balance
 Papeete
UV-Visible spectrophotometer
Chemicals Required:
 Food Sample
 Lead nitrate
 Cadmium chloride
 Mercurius Chloride
 Lead Nitrate
 Salts of other Heavy metals
 Distilled Water

Experiment No 7:
Determination of citric acid in juices
Principle
This experiment is based on acid-base titration.

Apparatus Required:
 Titration stands
 Dropper
 Conical Flask
 Burette
 Pipette
 Beakers 200 ml
 Volumetric Flask
Chemicals Required:
109
 Sodium Hydroxide 40g
 Oxalic Acid 6.3g
 Lemon juice solution 10ml

Experiment No 8:
Determination of ascorbic acid
Principle
This experiment is based on redox titration. The purpose of this
experiment is to determine the concentration of vitamin C in a solution
by redox titration. Vitamin C also known as Ascorbic acid is an
essential antioxidant needed by the human body. As iodine is added
during the titration the oxidation of the ascorbic acid occurs and it is
oxidized to the dehydroascorbic acid and the iodine is reduced to the
iodide ions
Ascorbic Acid + I2 --------- 2 I- + dehydroascorbic Acid
The reduction of the iodine to the iodide ions occurs as long as there is
ascorbic acid present. As all the ascorbic acid is oxidized the excess
iodine is free to react with the starch and form a blue-black starch iodine
complex which is the

Apparatus Required:
 Titration stands
 20ml pipette
 Conical Flask
 Burette

110
 10ml and 100ml measuring cylinders
 Beakers 200 ml
 Volumetric Flask (100 ml and 200ml)
Chemicals Required:
 Potassium iodide 2.0 g
 Iodine 1.3 g
 Starch Powder 0.25 g

Experiment No 9:
Determination of the iodine value of the edible oil
Iodine value is the number of the unsaturation of the tested sample. The
iodine is quantitatively adds to the double bonds which can be
accurately measured, it is the number of the grams of the iodine which
add to the 100 grams of the fats.

Apparatus Required:
 Burettes
 Measuring cylinder
 Hot Plate
 Weigh Balance
 Beaker 100ml
 Spatula
 Water Bath
Chemicals Required:
 Carbon tetra chloride
 Potassium iodide solution
 Wijs solution
 Sodium thiosulphate solution

111
Experiment No 10:
Determination of Acid value of the edible oil
Principle:
The acid value is determined by the directly titrating the oil or fat in
an alcoholic medium against potassium hydroxide or sodium
hydroxide.
The acid value is defined as the number of the milligrams of the
potassium hydroxide required to neutralize the free fatty acids present
in the one gram of the fat
It is relative measure of the rancidity as the free fatty acid formed
during the decomposition of the triglycerides. the value is also
expressed as the percent of free fatty acids calculated as the oleic acid,
lauric acid p or palmitic acid
Apparatus Required:
 Burette
 Measuring Cylinder
 Hot Plate
 Weighing Balance
 Spatula
 Water Bath
Chemicals Required:
 Potassium Hydroxide
 Phenolphthalein Indicator
 Ethanol
 Oil Sample

Experiment No 11:
Finger print analysis by AgNO3

112
Apparatus Required:
 Googles
 Gloves
 Protective Clothing
 Spray Bottle
 Magnifying Glass
Chemicals Required:
 Paperc with fingerprint
 3% Silver Nitrate Solution
Experiment No :
Extraction of DNA from saliva
Apparatus Required:
 Centrifuge Tubes
 Pipette
 Beakers
 Measuring Cylinder ‘
Chemicals Required:
 Saliva Sample
 Salt
 Distilled Water
Missing Practical:
1-Calibration of the HPLC system as per requirement of the
British or US pharmacopeia
2-Analysis of Binary Mixture of pharmaceutical dosage by HPLC

113

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