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CHEMISTRY

LAB MANUAL

Department of Chemistry

SRM University
Amaravati
2017-2018

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VOLUMETRIC TITRATION
AIM: Determination Strength of Hydrochloric Acid Using Sodium Hydroxide by Volumetric Titration.
Materials:
● 50 ml Burette with clamp
● Burette Stand
● porcelain tile
● 250 ml conical Flask
● Burette funnel
● 25 ml volumetric pipette
● Pipette bulb

Chemicals:
● Hydrochloric acid
● Sodium hydroxide
● Phenolphthalein indicator

Phenolphthalein:
a pH indicator. In acidic and neutral solutions, the indicator is colorless, but in a basic solution, the co
lor is a vibrant pink. The higher the pH is, the stronger the pink color is. The equivalence point will be
when the color is a very pale pink color. Keep your flask with acid and indicator over a white piece o
f paper to ensure you can see the color change.

Procedure:
Titrant: The solution of known concentration is also called the standardized solution.
the titrant is sodium hydroxide solution.

Burette:A long,cylindrical piece of glass that canbe used to determine small,accurate quantiti
es of a solution. A buret is controlled by a stopcock, a white Teflon piece that can be turned t
o deliver the solution. The markings on the buret are such that you must subtract the initial re
ading (where the titrant level is initially) from the final reading to determine the volume of ba
se delivered. The buret measures 2 digits after the decimal point accurately.
Volumetric pipette/pipette bulb: A thin glass tube with only one marking used to
measure a very specific volume of liquid. You will use a pipette bulb to draw the liquid into t
he pipette.
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● Pipette out 20 mL of HCl in a Conical Flask and fill the burette with NaOH Solution
● Add phenolphalein indicator 2-3 drops to the pippete out solution and start the
titration add NaOH Burette solution drop by drop to the conical flask solution
● HCl and NaOH both are colourless solutions. When the reaction completes the colour
less solution becomes pale pink colour.
● We do the titration 3 times.
Observation and Calculation:

Table 1 :- Volumetric Titration

Volume of HCl taken Volume of NaOH added (V2) (mL)


(V1) (mL) Intial Reading Final Reading

20
Plot a graph between conductance and volume of titrant (NaOH solution). Two intersecting lines will
be obtained (as given in the Figure 1) and the points of intersection of these lines represent the
equivalent point. Let, V2 be the volume of NaOH at the equivalent point (from graph) and the
strength of acid is M1 and strength of NaOH solution is M2 = 0.5(N).

Then, M1V1=M2V2

M1 = (V2×2/20) (N)

Result: The strength of the acid is ______ (N)

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CONDUCTOMETRIC TITRATION
AIM: Determination Strength of Hydrochloric Acid Using Sodium Hydroxide by Conductometric
titration.
Apparatus:
● Conductometer
● conductivity cell
● 100 ml beaker
● 20 ml pipette
● 50 ml burette
● Burette Stand
● porcelain tile
● Glass rod
Chemicals:
● Hydrochloric acid (HCl)
● Sodium hydroxide (NaOH)
● Potassium Chloride (KCl)
● Conductivity water or Distilled Water.
Theory:

Electrolytic conductivity is a measure of the ability of a solution to carry electric current. Electric
solutions conduct electric current by the migration of ions under the influence of directly proportional
to the potential difference (E) and inversely proportional to the resistance (𝜌) of the conductor.

i.e. I = E/R or, R = E/I

Where the resistance (R) is the hindrance provided by the solution. The resistance of any conductor
varies directly with the length and inversely with its area of cross-section.

R = 𝜌 x ( 𝜌/a)

Where, 𝜌 is the specific resistance and it is the resistance of a unit length of conductor of unit cross-
section. 𝜌/a is called cell constant. The reciprocal of specific resistance is called specific
conductance or conductivity.

Specific conductance (𝜌) = 1/ 𝜌 = (𝜌/a) x (1/R)

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Conductance of electrolyte depends upon i) number of free ions, ii) changes on the free ions and iii)
mobility of the ions on the substitution of one ion by another of different mobility (speed of ions). So,
conductometric method can be used to determine the end point of ionic titrations like

i) acidimetric titration, ii) precipitation titration, iii) titration involving the formation of complex ion.
When hydrochloric acid solution (HCl) is titrated with sodium hydroxide solution (NaOH), the highly
mobile hydrogen ions (𝜌 °H+ = 350 ohm–1 cm–1) are progressively replaced by slower moving sodium
ions (𝜌°Na+ = 50 ohm–1 cm–1) and the conductance of the solution decreases. After the end point, the
conductance of the solution rises sharply due to the presence of excess, highly mobile hydroxide ion
(𝜌 °OH– = 198 ohm–1 cm–1).

Thus the neutralization of a strong acid by addition of a strong base leads to a minimum conductance
at the end points. This is due to the disappearance of H+ ions and their replacement by slower moving
Na+ ions of the base followed by the presence of highly mobile OH– ions after the end point.
Therefore, the nature of the plot (conductance of the solution versus volume of base added) will be as
given below:

Calibration:

● Calibration of the instrument done at room temperature.


● Switch on the conductivity meter
● Set the Function knob at check and Temperature at 250c Range Knob 2 m the value should be
0.00.

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● Set the Function knob at Cell Constant.
● Take 20 ml of KCl in a beaker and dip the conductivity cell in it set the value at 1.2886.
Precautions:

● Electrical connection should be made carefully.


● Temperature during the experiment should be kept constant as conductance depends on
temperature.
● Stirring should be done after each addition of titrant.
● To avoid the dilution effect, the concentration of the titrant should be 5-10 times more than
that of the solution to be titrated.
Procedure:

● HCl solution of unknown strength is provided.


● 0.5 (N) NaOH solution is provided.
● Rinse the conductivity cell a number of times with conductivity water or double distilled
water.
● Set the Function knob at Conductance and Temperature at 250c Range Knob 20 m.
● Pipette out 20 mL of HCl in a beaker and dip the conductivity cell in it, so that the cell should
dip completely in solution.
● Note the temperature of the sample solution and accordingly set the temperature control or
keep the cell in a thermostat at room temperature.
● Add small amount of NaOH solution (few drops) from burette, stir it and measure the
conductance after each addition.
● Take at least five readings beyond the end point.
Observation and Calculation:

Table 1:- Conductometric Titration

Volume of HCl taken Volume of NaOH added Conductance


(V1) (mL) (V2) (mL)

20
Plot a graph between conductance and volume of titrant (NaOH solution). Two intersecting lines will
be obtained (as given in the Figure 1) and the points of intersection of these lines represent the
equivalent point. Let, V2 be the volume of NaOH at the equivalent point (from graph) and the
strength of acid is M1 and strength of NaOH solution is M2 = 0.5(N).

Then, M1V1=M2V2

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M1 = (V2×2/20) (N)

Result: The strength of the acid is ______ (N)

Discussions:

● Normally, the coloured solution which cannot be titrated with volumetric method using
indicator can be titrated by the conductometric method.
● The conductometric titration method can be used in case of weak acid vs. weak base and also
in case of very dilute solutions.
● Near the end point, no special case is necessary as it is determined graphically.

PH METRIC TITRATION

AIM: Determination Strength of Hydrochloric Acid Using Sodium Hydroxide by PH Metric


titration.

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Apparatus:

● pH meter
● pH electrode
● 100 ml beaker
● 20 ml pipette
● 50 ml burette
● Burette Stand
● porcelain tile
● Glass rod
● Wash Bottle
Chemicals:
● 0.1N Hydrochloric acid (HCl)
● 0.25N Sodium hydroxide (Noah)
● Distilled Water.
● buffer of pH = 4 and 7

Theory:

pH of any solution is defined as (–log H+) and has values between 0–14. pH < 7 indicate
acidic solution, pH > 7 indicate basic solution and pH = 7 means neutral solution.

The pH of a solution can be measured accurately with the help of a pH meter. Measurement
of pH is employed to monitor the cause of acid-base titration. The pH values of the solution
at different stage of acid–base neutralization are determined and plotted against the volume of
alkali added on adding a base to an acid, the pH rises slowly in the initial stages as the
concentration of H+ ion decreases gradually. But, at the equivalence point, it increases
rapidly as at the equivalent point H+ ion concentration is very small. Then it flattens out after
the end point. The end point of the titration can be detected where the pH value changes most
rapidly. However, the shape of the curve depends upon the ionisability of the acid and the
base used and also on the acidity of base and basicity of the acid.

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Precaution:

● Electrodes must be immersed in the solution properly and sufficient time to be allowed
for the electrodes to obtain the temperature of the solution.
● pH meter should be calibrated before the experiment.
● Glass rod may be used or the solution be stirring from time to time during pH metric
titration
● Leave the selector in zero position where it is not in use.
Procedure:

● 0.25(N) NaOH solution is provided.


● HCl solution of unknown strength is provided.
● Switch on the instrument and wait for 10–15 minutes so that machine gets warmed
up.
● Put the Select Button Standard Temperature at 25 oc. The PH Meter show the value
‘000’.
● Prepare the buffer solution by adding buffer tablets of pH = 4 and pH = 7 in 100 mL
of water separately.
● Put the Select Button on PH
● Wash the electrode with distilled water. Then, dip the electrode in the buffer solution
(pH = 7) taken in a beaker. After Set the Switch to “mv” Position. It should read ‘000’
● We adjust the Calibration button only during pH electrode Calibration.
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● Wash the electrode with distilled water. Then, dip the electrode in the buffer solution
(pH = 4) taken in a beaker. After Set the Switch to “mv” Position. It should read ‘000’
● Clean the electrode with distilled water and wipe them with tissue paper or filter
paper.
● Take 20 mL of HCl solution in a 100 mL beaker and immerse the electrode in it. Set
the burette with NaOH solution. Put the selector at the expected range (0–7). The
reading shown on the scale of pH meter is pH value of the HCl solution.
● Add NaOH solution drop wise from the burette (maximum 1 mL at a time), shake the
solution well and note the corresponding pH values. Near the end point, volume of
NaOH added should be as small as possible because the acid is neutralized and there
will a sharp increase in pH values.
● Further addition of even 0.01 mL of NaOH, increase the pH value to about 9–10. Put
back the selector to zero position after pH measurement, and always keep the selector
at zero position when it is not in use.
Observation and Calculation:

Table 1: pH metric Titration

Volume of HCl taken Volume of NaOH added Conductance


(V1) (mL) (V2) (mL)

20

Plot a graph between pH and volume of NaOH added and find out the volume of NaOH
required (V2 mL) for complete neutralization of HCl from the graph. Then find out the
strength of HCl (N1) and strength of NaOH solution is M2 = 0.25N.

Then, M1V1=M2V2

M1 = (V2×2/20) (N)

Result: The strength of the acid is ______ (N)

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Determination of Hardness of Water using EDTA Method
AIM: Determination of Hardness of Water using EDTA Method.

APPARATUS:

● Burette
● Burette stand
● porcelain tile
● Pipette
● Pipette bulb
● Conical flask
● 250 mL graduated cylinders
● Standard flask
● Wash Bottle
● Beaker
CHEMICALS:
● Ammonium Chloride
● Ammonium Hydroxide
● EDTA (Disodium Salt of EDTA)
● Erichrome Black T
● Magnesium sulphate
INTRODUCTION:

Water that has high mineral content is known as Hard water. Hard water contains bicarbonate,
chlorides and sulphates of calcium and magnesium.

When treated hard water with soap, it gets precipitated in the form of insoluble salts of calcium and
magnesium. Hardness of water is a measure of the total concentration of the calcium and magnesium
ions expressed as calcium carbonate. There are two types of hardness

1. Temporary hardness
2. 2. Permanent hardness
Temporary Hardness is due to the presence of bicarbonates of calcium and magnesium. It can be
easily removed by boiling.
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Permanent Hardness is due to the presence of chlorides and sulphates of calcium and magnesium.
This type of hardness cannot be removed by boiling.

PRINCIPLE:

A water sample is buffered to pH 10.1 and taken in to a conical flask. If an indicator dye like EBT,
when added to a solution containing Calcium and Magnesium ions, the color of the solution turns to
wine red.

EDTA, the titrant, complexes with Magnesium and Calcium ions, removing them from association
with the indicator.

When all the Mg and Ca are complexed with EDTA, the indicator will turn blue. This is the end point
of the titration.

PRECAUTIONS:

● Here we are handling ammonia solution so necessary precaution should be taken for
preventing the inhalation.
● It causes irritation if inhaled.
● Do not pipette out the buffer solution using either measuring cylinder, automatic pipette (or)
pipette with a sucker.
● Always store EDTA solution and buffer solution in a plastic or resistant glass container.
● Discard the buffer solution if it is turbid or if it is stored for a very long period of time.
PROCEDURE:

PREPARATION OF REAGENTS:

Buffer Solution preparation:

● Switch on the Electronic balance, keep the weighing pan, set the reading to zero.
● Measure 50 mL of distilled water and transfer it to the beaker
● Weigh 1.179g of EDTA
● Now the weight is 1.179gms
● Transfer the contents to the beaker having 50 mL of distilled water and dissolve it thoroughly.
● Weigh 16.9g of ammonium chloride.
● Add it to the contents in the beaker. And dissolve it thoroughly.
● Weigh 780mg of magnesium sulphates and transfer it to the beaker.
● Measure 143 mL of Ammonium hydroxide solution using measuring cylinder and add it to
the contents in the beaker.

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● Place the funnel over the 250mL standard flask and transfer the dissolved contents from
beaker
● Make the volume upto 250mL mark by adding distilled water. Transfer the buffer solution to
a clean reagent bottle labelled as buffer solution. This buffer solution is used to maintain the
pH of water sample between 9 and 10.
Erichrome Black T:

● Weigh 0.5g of Erichrome black T


● Transfer it to 100mL standard flask using funnel
● Add distilled water in the standard flask and make the volume exactly up to 100 mL mark
● Put the lid and shake the contents well
● Transfer the solution to a clean reagent bottle named EBT
Standard EDTA Solution (0.02 M):

● Switch on the Electronic balance, keep the weighing pan, and set the reading to zero.
● Weigh 3.723g of EDTA sodium salt
● Transfer the entire content to 1000 mL standard flask
● Fill with distilled water up to 1000 mL mark
● Put the lid and shake the contents well.
● For easy handling take the EDTA solution in a 250 mL beaker.

TESTING OF WATER SAMPLE:

● Pipette 20mL of water sample and transfer it to a clean 250mL conical flask.
● Add 2mL of Ammonia buffer solution to the water sample so that the pH will be maintained
between 9 and 10.
● Add few drops of EBT indicator to the conical flask and the sample turns to wine red in
color.
● Before starting the titration rinse the burette with few mL of EDTA. Fill the burette with
0.02M EDTA solution and adjust to zero then fix it in burette stand.
● Titrate the sample against the EDTA solution in the burette till all calcium and magnesium
ions present in the sample reacts with the EDTA. The appearance of blue colour indicates that
all Ca & Mg ions
● are complexed with EDTA and forms a metal EDTA complex i.e., the end point of the
titration.
● Note down the burette reading
● Repeat the titration for concordant values
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CALCULATION:

S. No. Volume of Burette Reading Volume of


Sample EDTA(Ml)
Initial Final

1.

2.

3.

Determination of the strength of the given KMnO4 solution using standard


oxalic acid solution

AIM:

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Determination of the strength of the given KMnO4 solution using standard oxalic acid solution.

Apparatus:

● Electronic weighing Balance


● Burette
● Burette stand
● porcelain tile
● Pipette
● Pipette bulb
● Conical flask
● Standard flask
● Wash Bottle
● Beaker
● Funnel
● Glass rod
● Spatula
● Tripod stand
● Wire gauge
● Bunsen burner
● Test tubes
Chemicals:

● Oxalic acid
● Potassium Permanganate
● Dilute sulphuric acid
Procedure:

Preparation of standard solution of oxalic acid [250 ml M/10 (0.1 M) solution]


● Using an electronic balance, first weigh exactly 3.15g of oxalic acid crystals in a weighing
bottle.
● Transfer these into a 250ml beaker.
● Then wash the weighing bottle 2 or 3 times with distilled water and transfer all the washings
into the beaker.
● Dissolve the oxalic acid crystals in the beaker by gentle stirring with a clean glass rod.
● When the oxalic acid crystals in the beaker are completely dissolved, transfer the entire
solution from the beaker into a 250ml standard flask through a funnel and a glass rod.
● Wash the beaker 2 to 3 times with distilled water and transfer all the washings into the
standard flask.

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● Finally wash the funnel thoroughly with distilled water to transfer the drops of the solution on
the sides of the funnel into the standard flask.
● Add enough distilled water to the standard flask so that the level is just below the calibration
mark on it.
● Add the last few drops of distilled water with a pipette until the lower level of the meniscus
just touches the mark on the standard flask.
● Stopper the measuring flask and shake gently to make the solution uniform throughout.
Determination of strength of given KMnO4
● Take a burette and wash it with distilled water.
● Rinse and fill the burette with the given KMnO4 solution and set the initial burette reading as
zero.
● Clamp it vertically to the burette stand.
● Rinse the pipette with water and then with the given oxalic acid solution.
● Then pipette out 20ml of the given oxalic acid solution into a conical flask and add one test
tube (~20ml) full of dil.H2SO4 into it.
● Heat the contents of the conical flask to 60-70°C.
● Titrate it against the KMnO4 solution taken in the burette till the colour of the solution in the
conical flask changes from colourless to light pink.
● Note down the final burette reading.
● Repeat the titration until concordant values are obtained.

Observation
The readings are recorded in a tabular form as shown and the molarity of the given KMnO 4 solution
can be calculated using the molarity equation.

burette reading burette reading


SI. No Volume of KMnO4 (in ml)
Initial Final

The Result
Then,

M1V1/n1=M2V2 /n2

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Amount of KMnO4 solution

Q = GMW x M1(V1 )ml 1000 /

The strength of the given KMnO4 solution = ............g/litre

Iodometric Determination of Vitamin C

AIM:
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Iodometric Determination of Vitamin C

APPARATUS:

● Burette
● Burette stand
● porcelain tile
● Pipette
● Pipette bulb
● conical flask
● Standard flask
● Wash Bottle
● Beakers

CHEMICALS:
● Solid Potassium iodide(KI)
● 0.3 M Sulphuric acid
● 0.04 M Sodium thiosulphate
● 0.01 M Potassium iodate(KIO3)
● Ascorbic acid(Vitamin C)
● Starch Indicator

PROCEDURE:

● Starch indicator will be provided


● Solid potassium iodide will be available
● 0.3 M H2SO4 will be available
● 0.04 M Sodium thiosulfate solution will be provided
● 0.01M KIO3 Solution will be provided.
Standardizing the Thiosulfate Solution

● Collect 250 mL of the thiosulfate solution. You must use the same solution for the entire
experiment.
● Pipet 25.00 mL of the KIO3 solution into each of 3 Erlenmeyer flasks. Using the
calculated KIO3 solution concentration, calculate the volume of titrant (thiosulfate)

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required assuming that the thiosulfate concentration is 0.04 M. This gives the
approximate endpoint.
● Add 1 g of KI and 20 mL of 0.3 M sulfuric acid solution to each flask.
● Titrate the triiodide with the thiosulfate solution until the brown solution becomes pale
yellow. Then add 2 mL of the starch indicator solution and titrate until the violet color of the
starch‐iodine complex just disappears. This is the endpoint.
● Repeat this procedure for a total of three precise titrations.
Analyzing the Vitamin C:

● Refill the burette with the thiosulfate solution


● Pipet 25.00 mL of the Ascorbic acid solution
● Pipet 25.00 mL of the KIO3 solution
● Add 1 g of KI and 20 mL of 0.3 M sulfuric acid solution to flask
● Titrate the triiodide with the thiosulfate solution until the brown solution becomes pale
yellow. Then add 2 mL of the starch indicator solution and titrate until the violet color of the
starch‐iodine complex just disappears. This is the endpoint.
● Repeat this procedure for a total of three precise titrations.
● Calculate the average mass of vitamin C.

Caluculation:

burette reading burette reading


SI. No Volume of Na2s2o3(in ml)
Initial Final

Result:
Then,

Estimation of Iron Content of the given Solution using Potentiometer

AIM: Estimation of Iron Content of the given Solution using Potentiometer.

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Apparatus:
● Potentiometer
● Calomel Electrode
● Platinum Electrode
● 250 ml beaker
● 20 ml pipette
● 50 ml burette
● Burette Stand
● porcelain tile
● Glass rod
CHEMICALS:

● Ferrous Ammonium Sulphate


● 2.5 M Sulphuric Acid
● 0.1 N Potassium DiChromate (K2CR2O7)
PRINCIPLE:

Potentiometric titration is the titration in which potentiometric measurements are carried out in order
to fix the end point. In this method, the interest is with the change in electrode potential, rather than
with an accurate value for the electrode potential in a given solution. In a potentiometric titration, the
change in cell e.m.f. occurs most rapidly in the neighbourhood of the end point. The Fe(II) –K2Cr2O7
redox system is represented as

Fe2+ + 4H2SO2+ K2Cr2O7 → Fe3+ + K2SO4 + Cr2(SO4)3 + 4H2O +3 (O)

The determining factor is the ratio of the concentrations of the oxidised and the reduced forms of the
iron species.

For the reaction,

Oxidised form + ne- → Reduced form,


The potential E acquired by the indicator electrode at 25oC is given by,

0.0591 𝑛𝑛
E = E o+ 𝑛𝑛𝑛[ ]
𝑛 𝑛𝑛𝑛

where Eo is the standard Reduction Potential of the system. Thus the potential of the immersed
electrode is controlled by the ration of these concentrations. During redox reactions, the potential

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changes more rapidly at the vicinity of the end point. The indicator electrode is usually a bright
platinum wire or foil, the oxidising agent is taken in the burette. The cell can be represented as,

Calomel| |Fe3+,Fe2+/Pt.

Here Pt is the indicator electrode and calomel is the reference electrode.

PROCEDURE:

● 0.1 N K2Cr2O7 is Provided filled the burette.


● Pipette out 20 ml of Ferrous Ammonium Sulphate into a beaker
● Pipette out 25 ml Sulphuric acid in that beaker.
● A platinum electrode is dipped into this solution, and it is coupled with a calomel electrode
through a salt bridge. The resulting cell is connected to the potentiometer. Standard K2Cr2O7
solution is added from the burette, to this solution, insteps of 1 ml and the emf is recorded
after each addition. At the end point, there is a jump in emf due to the absence of Fe2+. The
approximate range of the end point is determined. The experiment is repeated by adding the
titrant in steps of 0.1 ml near the end point. A graph is plotted between emf, E and the volume
of dichromate added. The inflexion point gives the volume of titrant at the end point.
The first derivative (𝛥E/𝛥V vs. Volume of titrant) and the second derivative (𝛥E2/𝛥2V vs.
Volume of titrant) curves give the exact volume of dichromate required for the reaction.
From the plot of E vs. Volume of titrant, potential at the equivalent point is obtained.

CALACULATION:

S. No. Volume of EMF 𝛥E 𝛥E/𝛥V Vmean


K2Cr2O7 ml

1.

2.

3.

RESULT: The amount of iron present in the whole of the given solution is __________ g.

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