Chemistry Lab Manual Acetr23
Chemistry Lab Manual Acetr23
Chemistry Lab Manual Acetr23
I SEMESTER
(ACER23 Academic Regulation)
Regd No:
Branch/ Section:
CODE OF CONDUCT
1. Students should report to the concerned lab as per the time-table schedule.
2. Students who turn up late to the labs will in no case be permitted to perform the
experiment scheduled for the day.
3. After completion of the experiment, certification of the concerned staff in-charge in the
observation book is necessary.
4. The record of observations along with the detailed experimental procedure of the
experiment performed in the immediate last session should be submitted and certified by
the staffmember in-charge.
5. The group-wise division made in the beginning should be adhered to, and no mix up of
students among different groups will be permitted later.
6. The components required pertaining to the experiment should be collected from the lab
assistants.
7. When the experiment is completed, students should clean the apparatus, carefully
disposethe leftover chemicals and disconnect the setup made by them and should return
all the components/instruments taken for the purpose.
8. Any damage to apparatus that occurs during the experimentation should be brought to the
notice of lab in-charge, consequently, the cost of the repair or new apparatus should be
brought by the students.
9. Students should be present in the labs for the total scheduled duration.
10. Students are required to prepare thoroughly to perform the experiment before coming to
Laboratory.
11. Procedure sheets/data sheets provided to the students’ groups should be maintained
neatlyand to be returned after the experiment.
L T P C
I Year – I SEM 0 0 2 1
CHEMISTRY LABORATORY SYLLABUS
Course Objectives:
Verify the fundamental concepts with experiments.
Course Outcomes (COs): At the end of the course, the student will be able to:
List of Experiments:
Reference:
"Vogel's Quantitative Chemical Analysis 6th Edition " Pearson Publications by J. Mendham,
R.C. Denney, J.D. Barnes, and B. Sivasankar
II. QUANTITATIVE ANALYSIS: It deals with the determination of how much of each
component or of specified component is present.
QUANTITATIVE CHEMICAL ANALYSIS IS FURTHER DIVIDED INTO TWO
TYPES:
Whenever two Substances react together, they react in the ratio of their equivalent mass. One
liter of a normal solution of a substance will react exactly with same volume of a normal
solution of another substance. In other words, equal volumes of equal normal solutions will
exactly react with each other. This result is stated in the form law of volumetric analysis. If V 1
mL of a solution of strength N1 is required or complete reaction by V2 mL of the second
solution of strength N2 then,
N1 V1 = N2 V2
If any three factors (V1, V2 & N1) are known, the fourth factor N2 can be calculated. The
following are theimportant formula used in all volumetric estimations
Mass of solute per liter of the solution = Equivalent mass x Normality
(a) TITRATION: It is a process of adding one solution from the burette to another in
the conicalflask, in order to complete the chemical reaction. Out of the two solutions one must
be standard.
(b) TITRANT: The reagent from the burette is called as Titrant.
(c) TITRAND (TITRATE): The substances being titrated is termed as titrand or titrates
(d) EQUIVALENCE POINT OR STOICHIOMETRIC END POINT: It is the point at
which the amount of reagent (Titrant) and substance (titrate) being determined are
chemically equivalent or it is the exact stage at which the chemical reaction involved in the
titration is just completed.
(e) END POINT: The point at which the reaction between Titrant and titrate is just
complete is called Endpoint or Equivalence point.
The determination of end point accurately is very essential in volumetric analysis. Generally,
the endpoint in the titration is detected by using an indicator.
(f) INDICATOR: chemical species which indicate the end-point by a sharp visual color
change is called indicator. There are three types of indicators. They are,
i. Internal indicators,
ii. External indicators and
iii. Self – indicators.
i. INTERNAL INDICATORS:
If one of the reacting solutions is in color, it acts as indicator in the titration. This kind of
indicator is called as Self-indicator. Ex: In the estimation of Mohr’s salt by KMnO4, KMnO4
acts as Self-indicator.
ACIDIMETRY AND ALKALIMETRY TITRATION:
Acidimetric refers to the titration of alkali with a standard acid and alkalimetry refers to the
titration of an acid with a standard alkali.
PERMANGANOMETRY TITRATION:
(g)TITRATION ERROR: Ideally, the visible end point and the equivalence point should
coincide but in practice there is always a difference between the two, this difference is
calledthe titration error.
The substance should maintain its composition unchanged during storage and unaltered
inair during weighing; it is neither oxidized by air nor affected by carbon dioxide.
The total amount of impurities should not in general, exceed 0.01 – 0.02%.
It should have a high equivalent weight so that the weighing errors may be negligible.
The substance should be readily soluble in water under the conditions in which it is
MOLARITY (M):
Molarity is defined as the number of moles of solute present in one literof solution at given
temperature.
NORMALITY (N):
Normality is defined as the number of gram equivalents of solute present in one liter of
solution at given temperature.
An acid-base indicator is a substance which has one color in acidic medium and a completely
different color in the base medium. In fact, the change in color of an acid-base indicator does
not take place at a particular pH value but takes place within a small range of pH (usually about
2 pH units). This range of pH is known as “color change interval” of the indicator. This is
different for different indicators.
a. Self- indicators
b. External indicators
c. Redox indicators
3. PRECIPITATION TITRATIONS:
Titrations based upon the formation of insoluble precipitates when the reacting solutions are
brought together, such titrations are called precipitation titrations.
4. COMPLEXOMETRIC TITRATIONS:
The titrations involving the formation of complex compounds are called complexometric
titrations.
EDTA forms very stable metal chelates with many metals. To simplify the representation of
EDTA, reactions with various metals, it is assigned the formula H4Y. Hence the disodium salt
of EDTA written as Na2H2Y which gives the complex forming ion H2Y2- in aqueous
solution, the reaction with differentcations may be written as:
EDTA - STRUCTURE:
∆
Mg (HCO3)2 → Mg (OH) 2 + CO2 + 2H2O
Permanent hardness is due to the presence of chlorides and sulphates of calcium and
magnesium which can be removed by only chemical treatment.The sum of temporary hardness
and permanent hardness is known as total hardness. The hardness is expressed in ppm (parts
per million).Hardness of water can be expressed as CaCO 3 equivalents as it is highly insoluble
salt and its Molecular Weight is 100.
PRINCIPLE:
Hardness of water is determined by titrating a known volume of water sample with EDTA
using EBT as indicator in the presence of pH10 buffer. EDTA is a strong Complexing agent
reacts quantitatively with the metal ions to form soluble stable 1: 1 complex.
DETERMINATION OF TOTAL HARDNESS OF THE GIVEN WATER SAMPLE:
CALCULATION:
𝐌𝟏 𝐌𝟐 𝐕𝟐
𝐕𝟏 = 𝒏𝟐
𝒏𝟏
Where,
mL
When a few drops of the indicator EBT are added, it forms a wine-red complex with metal
ions.
M2+ + EBT [M – EBT] +2 Complex
(Blue color) (Wine Red color)
When the solution is titrated, EDTA reacts, preferentially with the free metal ions present in
the solution. Near the end point, when the free metal ions are exhausted in the solution, further
addition of EDTA dissociates the [M-EBT] Complex, consumes the metal ions and releases
free indicator, which is blue in color. Therefore, the color change is from wine red to blue.
is maintained at about 10, using pH 10 buffers. EDTA being insoluble in water, it is generally
METAL EDTA COMPLEX: EDTA is a hexadentate ligand and forms complexes with many
metal ions and the general structure of which is shown as follows.
PROCEDURE:
All the apparatus were washed with tap water and rinsed with Distilled water.
50 mL of the given water sample is taken into conical flask.
2 mL of pH 10 buffer solution is added and it is shaken well.
To these 2 drops of EBT indicator is added.
The contents are titrated with EDTA solution which is taken in burette until the color
change from wine red to clear blue.
The results are tabulated.
FACULTY SIGNATURE
Experiment No: Date:
The end point of the titration takes place when all the chloride ions reacts and precipitated.
Then slightly extra silver ions react with the chromate ions and form a brownish-red precipitate
of silver chromate.
2AgNO3 (aq) + K2CrO4 (aq) → Ag2CrO4(s) + 2KNO3 (aq)
Procedure:
Determination of chloride content of water.
All the apparatus were washed with tap water and rinsed with Distilled water.
Burette is rinsed and filled with Silver Nitrate solution, including burette nozzle
without air bubbles.
20 mL of water sample pipetted out into a clean conical flask.
2-3 drops of Potassium chromate (K2CrO4) indicator was added to the conical flask,
the solution turns into Light Yellow color.
The Resultant yellow color solution is Titrated against silver nitrate present in the
burette, turns into Permanent brick Red Color.
Repeated the titrations to get concurrent values.
Tabular column:
Calculations:
M1V1=M2V2
Result: -The amount of Chloride ion present in the given water sample is_ mg/lit
FACULTY SIGNATURE
Experiment No: Date:
The Nitrates present in water interfere with the estimation of dissolved Oxygen of water, since
these ions liberate Iodine from Potassium Iodide, Sodium Azide is added to remove nitrate.
2NaN3 + H2SO4 2HN3 + Na2SO4
HNO2 + HN3 N2O + N2 + H2O
Table: - Determination of D.O of water sample by titrating with Standardized Hypo
solution
N1V1= N2V2
N1 = Normality of Hypo = N
V1 = Volume of Hypo solution = Titre value with water sample (in mL)
N2 = Normality of Oxygen in water sample = ?
V2 = Volume of water sample = 50 mL
N1V1
N2 = V2
All the apparatus were washed with tap water and rinsed with Distilled water.
250mL of water sample is taken in a bottle having stopper to prevent possible contact
with air and is not agitated as there may be a change in the dissolved Oxygen
concentration.
2mL of Manganese Sulphate and 2mL of Alkaline Iodide- Azide solutions are added to
the water sample.
The contents in the bottle are shaken well and allowed to stand so that brown precipitate
of basic manganese oxide MnO (OH)2 (Manganic Hydroxide) settles down.
2mL of concentrated H2SO4 is added drop wise with stirring to dissolve the precipitates
and again allowed to stand for 5minutes.
Now 50mL of above solution is taken and titrated against standardized Hypo solution
till a pale-yellow color is obtained.
1-2mL Starch solution is added which turns the solution into blue color and titrated
against Hypo solution until blue color disappears.
The titrations are continued until 3 concurrent readings are obtained and the readings
are tabulated in Table.
FACULTY SIGNATURE
Experiment No: Date:
AIM: To determine the strength of strong acid (HCl) by titrating with strong base (NaOH)
conductometrically.
APPARATUS REQUIRED:
PRINCIPLE:
When an acid is added to an alkali the conductance of the solution is initially high because HCl is
a strong electrolyte and dissociates to give the fast-moving H + ions. However,when NaOH solution
is added to the HCl solution fast moving H + ions are replaced by the slow-moving Na + ions and
hence the conductance of the solution decreases. The conductance goes ondecreasing on the addition
of NaOH solution till whole of the H+ ions are replaced by Na+ ions.
After the end point has reached, further addition of NaOH results in increase in conductance, since
the OH- ions are no longer used up in chemical reaction. At the neutral point the conductance of the
system will have a minimum value from which the equivalence point can be determined. Therefore,
when the conductance of the solution is plotted against the number of mL of the base added two
curves are obtained. The point of intersection of the two curves gives the end point of the titration.
PROCEDURE:
All the apparatus were washed with tap water and rinsed with Distilled water.
50 mL of acid is taken in 100 mL beaker.
The titrating solution which is 10 times more concentrated than the acid is taken in a micro
burette and is allowedto run down in small quantities (0.5mL) and after each addition the
solution is well stirred and the conductivity is measured.
Calculations:
𝑵𝟐 𝑽𝟐
N1V1 = N2V2 N1 =
𝑽𝟏
Where N1= Normality of HCl solution = ?
𝑵𝟐 𝑽𝟐
N1 = 𝑽𝟏 =
GRAPH:
A graph is drawn with corrected conductance against the volume of NaOH added, and
the point of intersection of curves gives the equivalence point.
FACULTY SIGNATURE
Experiment No: Date:
POTENTIOMETRIC TITRATIONS BETWEEN STRONGACID AND
STRONG BASE
AIM: To determine the end point of an acid base reaction [HCl & NaOH] by potentiometer.
CHEMICALS REQUIRED: HCl solution (unknown), 0.1N NaOH solution and distilled
water.
Exactly 50 mL of the acid is pipetted out into a 100 mL beaker and it is saturated with
Quinhydrone and a Platinum electrode is dipped into the solution.
A calomel electrode is placed in the solution and the cell thus formed is connected to a
potentiometer.
The beaker is placed under a burette filled with standard Sodium hydroxide solution.
The alkali is added from the burette at the rate of 1mLfor rough titration and the
approximate end point is noted.
Then the titration is repeated by adding 0.1mLof the alkali near the end point and the
E.M.F is measured after each addition.
POTENTIOMETRIC TITRATIONS BETWEEN STRONG ACID AND STRONG BASE:
Pilot titration
GRAPH 1: EMF Vs. volume of NaOH: GRAPH 2: ∆E /∆V vs. volume of NaOH:
Volume of
E.M.F inmilli ∆𝐄 / ∆𝐕
S. No alkali (NaOH)(V in ∆V ∆E
volts (E)
mL)
Calculations:
Calculations:
𝑵𝟐 𝑽𝟐
N1V1 = N2V2 N1 = =
𝑽𝟏
Where,
N1= Normality of HCl solution = ?
V1= Consumed Volume of HCl solution = mL
N2= Normality of NaOH = 0.1N
V2 = Volume of NaOH = ___ mL (From Graph – End Point)
Strength of HCl, N1 = 𝑵𝟐 𝑽𝟐 =
𝑽𝟏
FACULTY SIGNATURE
Experiment No: Date:
PRINCIPLE:
Phenolic resins are condensation polymerization products of Phenolic derivatives with
aldehydes (like formaldehyde, furfural). It is prepared by condensing phenol with
formaldehyde in presence of acidic catalyst.
PROCEDURE:
All the apparatus were washed with tap water and rinsed with Distilled water.
5 mL of Glacial Acetic acid and 3 mL of 40% Formaldehyde Solution added into a
beaker.
2 grams of Phenol added to the beaker solution.
2-3 mL of Concentrated Sulfuric Acid solution into the beaker resultant solution.
Within five minutes a large mass of Plastic is formed.
The Resultant Residue is washed several times with distilled water and filtered.
The resultant product is dried and yield is calculated.
REPORT:
FACULTY SIGNATURE
Experiment No: Date:
DETERMINATION OF VITAMIN – C
AIM:
To determine the amount of Vitamin-C (ascorbic acid) present in given 100mL solutionusing
standard tri-iodide solution.
APPARATUS REQUIRED:
Burette, pipette, conical flask, burette stand, volumetric flask, measuring jar, white glazed tile
and wash bottle.
CHEMICALS REQUIRED:
Vitamin-C tablets / lemon juice / orange juice, 0.05N tri-iodide solution (potassium iodide+
potassium iodate), freshly prepared starch indicator and distilled water.
C6H8O6 + I2 → C6H6O6 + 2 HI
During The titration, presence of iodine is possible only when all the vitamin-C is completely
oxidized. Then left over iodine reacts with the starch to give blue color as the end point.
VITAMIN-C STRUCTURE:
PROCEDURE:
All the apparatus were washed with tap water and rinsed with Distilled water.
10 mL of Vitamin – C solution pipetted out into a conical flask.
2-3 drops of 1% freshly prepared starch indicator added to the conical flask.
Rinsed burette is filled with tri-iodide solution, including burette nozzle without air
bubbles.
The Resultant conical flask solution is titrated against burette containing tri-iodide
solution.
It turns into blue color.
Repeat the titration to get concordant values.
CALCULATION: Formula, N1 V1 = N2 V2
V2 - Volume of Vitamin-C = 10 mL
N1V1 = N2V2
𝑵𝟏 𝑽𝟏
N2 = 𝑽𝟐
The amount of Vitamin-C present in the given solution (100mL) is
FACULTY SIGNATURE
Experiment No: Date:
AIM:
To determine the strength of a sulfuric acid solution in Pb-acid battery by titration with standard
NaOH solution
PRINCIPLE:
Titration is the process, of determining the concentration of a substance in solution (The
analyte) by adding it to a standard reagent of known concentration (the Titrant) in carefully
measured amounts until a reaction of definite and known proportion is completed, as shown by
a color change or electrical measurement, and then calculating the unknown concentration. In
this experiment, sulfuric acid is titrated with sodium hydroxide.
2 NaOH + H2SO4 → Na2SO4 + 2 H2O
The titration is done in the presence of phenolphthalein indicator that is colorless in acid
solution but turns pink in basic solution. At the equivalence point, all of the analyte has reacted,
and only a tiny excess of Titrant has been added, just enough to change the color of the
indicator.
PROCEDURE:
All the apparatus were washed with tap water and rinsed with Distilled water.
The burette is rinsed with the given acid solution and filledwith same without air
bubbles, including nozzle.
10ml standard sodium hydroxide solution is pipetted outinto a clean conical flask
carefully. Two drops of phenolphthalein indicator are added directly to the contents
of conical flask.
The conical flask contents are titrated with given acid solution after noting the initial
reading.
The titration is continued till the color changes from pink to colorless. The final
reading of burette is noted.
A number of titrations are repeated for getting concurrent results.
CALCULATIONS:
Calculations:
N1V1 =N2V2
N2 = N1V1 / V2
FACULTY SIGNATURE
Experiment No: Date:
ESTIMATION OF Mn IN PYROLUSITE
PRINCIPLE:
MnO2 occurs in the nature in the form of pyrolusite. Pyrolusite is not only used as asource of
mangane4se but also as an oxidizing agent in many industrial processes. For such purposes, ore
is graded on the basis of its available oxygen content rather than on itspercentage of manganese.
The percentage of MnO2 is usually determined by treatment with an excess of acidified solution
of a reducing agent, oxalic acid. The excess of reducing agent isdetermined by titration with
standard KMnO4 where KMnO4 acts as a self-indicator with pale pink color as the end point.
PROCEDURE:
All the apparatus were washed with tap water and rinsed with Distilled water.
Rinsed burette and it is filled with KMnO4 solution.
0.25 g of pyrolusite sample is finely grounded and dissolved in 100 mL.
10 mL of Pyrolusite solution is pipetted out into a conical flask, 20 mL of Oxalic Acid
solution and 5 mL of Diluted sulfuric acid is added to the conical flask solution.
The conical flask contents were heated to about 600C to increase the rate of reaction.
The Resultant solution is titrated against KMnO4 solution until permanent pink color
is observed.
Titration was repeated with another sample of Pyrolusite
Amount of Mn present ion Pyrolusite can be calculated from the volume of oxalic acid
reacted equivalently with pyrolusite.
OBSERVATION AND CALCULATIONS:
Calculations:
N1V1 =N2V2
N1 = Normality of Pyrolusite = ?
N1 =N2V2/V1
FACULTY SIGNATURE
Experiment No: Date:
Chemicals Required:
Zinc nitrate hexahydrate (Zn (NO3)2.6H2O), Sodium carbonate (Na2CO3),
Ethanol (C2H5OH, 95%,).
Apparatus: Beakers, Measuring Jars
Procedure for Preparation of ZnO nanoparticles.
All the apparatus were washed with tap water and rinsed with Distilled water.
Two solutions are prepared
Solution A: 0.1 mol Zn (NO3)2.6H2O is prepared by dissolving 29.75g of Zinc nitrate
hexahydrate in 200 ml distilled water;
Solution B: 0.12 mol Na2CO3 is prepared by dissolving 12.72 g of sodium carbonate in
240ml distilled water.
After that solution A is added to solution B drop wise under vigorous stirring.
The white precipitate is collected by filtration and rinsed with distilled water three
times. The solid is then washed with ethanol and dried at 100°C for 6 h.
Finally, ZnO nanoparticles areobtained after annealing of the solid in air at 250, 300,
350, 400, 500, and 600°C for 2 h, respectively.
Characterization:
The optical properties of prepared ZnO NPs are analyzed by UV-visible
Spectrophotometer (Shimadzu, UV-2450). A broad absorption peak is observed in
each spectrum at 355-380 nm which is a characteristic band for the pure ZnO.
The FT-IR shows a broad absorption band related to Zn-O vibration band at 500 cm-1.
The SEM results show the formation of spherical shaped nano particles.
Report:--
FACULTY SIGNATURE