mbatech lab mannual 2012-13
TRANSCRIPT
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LIST OF EXPERIMENTS
1.Determination of percentage of iron in plane carbon steel2.Determination of zinc in brass.3.Determination of the amount of copper in brass.4.Determination of presence of moisture in coal.5.Determination of percentage of nickel in steel alloy.
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EXPERIMENT NO:Determination of percentage of iron in plane carbon steel.
Aim:To estimate the amount of iron (as %) in plane carbon steel alloy volumetrically
Principle:Plane carbon steel is an alloy of iron and carbon .To determine the amount of steel
alloy, the alloy can dissolved in dil. sulphuric acid to form iron sulphate and this
solution can titrate d with a standard KMnO4 solution .Then amount of iron in steel can
be calculated using stoichiometric relationship .
Requirements:
Chemicals:1. Standard Ferrous ammonium Sulphate Solution (0.1)2. KMnO4 Solution.3. Dilute sulphuric acid4. Steel solution.
Apparatus:Pipette, Burette, Conical Flask 100ml, Beaker 100ml, Funnel
Chemical Reaction:
2KMnO4+8H2SO4+10FeSO4K2SO4+2MNSO4+5Fe2 (SO4)3+8H2O
Procedure:
I)Standardization of KMnO4 Solution:Pipette out 10ml Standard Ferrous ammonium Sulphate Solution (0.1)in 100m
conical flask
Add 10ml Dilute sulphuric acid
Titrate the solution slowly with KMnO4 solution from the burette until permanen
pink colour persists in the solution
Repeat the titration for CBR
II)Estimation of Iron:Pipette out 10ml steel solution in 100ml conical flask
Add 10ml Dilute sulphuric acid
Titrate the solution slowly with KMnO4 solution from the burette until permanen
pink colour persists in the solution
Repeat the titration for CBR
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Observation:N1=__ V1=___ Wt. Of Steel=_____
Observation Table:
Sr.NoVolume Of KMnO4 Solution Used against (ML)
Standard Steel
1
23
CBR
Calculation:
N1V1=N2V2
N2= 0.1X10
N1N2=________N
N2V2=N3V3
N3= 0.1X10
N2
N3=________N
1N KMnO4 = 55.85gm/1000ml
N3 X 55.85 = ____gm/Lit
The given Steel solution contains_____ gm of iron
The weight of alloy taken is___ gm
% of iron = Weight of iron in steel solution X 100
Weight of steel taken
Result:
1. The given steel solution contains ________________ gm iron in100ml2. The percentage of iron ______________
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EXPERIMENT NO:
Determination of zinc in brass.
Aim: To estimate the amount of zinc (as %) in brass volumetrically(Complex metric titration)
Principle: The brass alloy of copper (60-80%) and zinc (20-40%) along with small amount oflead (0-2%). To estimate zinc in brass alloy, the other elements i.e. Cu, Pb and Fe
are also to be removed by precipitation method. The solution thus obtained which
free from all these constituents is then titrated with EDTA solution. The amount ofzinc is calculated using stoichiometric relationship
Requirements:
Chemicals:1. Standard ZnCl2 solution.(0.01M)2. EDTA solution3. Ammonia Buffer solution.4. Eriochrome black T indicator.5. Brass solutionApparatus:
Pipette, Burette, Conical Flask 100ml, Beaker 100ml, Funnel
Chemical Reaction:
EBT + Zn2+ Zn- EBT(Blue) (Pink)
Zn2+
+ EDTA ZnEDTA
(Stable)
EDTA+ Zn EBT Zn -EDTA+ EBT
(Blue)
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Procedure:
1.Standardization of EDTASolution:i. Pipette out 10ml Standard ZnCl2 (0.01)in 100ml conical flask
ii. Add 2ml Ammonia buffer and 2-3 drop of indicator. The solutionacquires a wine red colour.
iii. Titrate the solution with EDTA solution from the burette until thecolour changes wine red to blue.
iv. Repeat the titration for CBR2.Estimation of Zinc:
i. Pipette out 10ml brass solution in 100ml conical flaskii. Add 2ml Ammonia buffer and 2-3 drop of indicator. The solution
acquires a wine red colour.
iii. Titrate the solution with EDTA solution from the burette until thecolour changes wine red to blue.
iv. Repeat the titration for CBRObservation:
M1=__ V1=___ Wt. Of Brass=_____
Observation Table:
Sr.No Volume Of EDTA Solution Used against (ml)Standard Brass
1
2
3
CBR
Calculation:
M1V1=M2V2
M2= 0.1X10
M1
M2=________M
M2V2=M3V3
M3= 0.1X10
M2
M3=________M
1M EDTA = 65.38gm/1000mlN3 X 65.38 = ____gm/Lit
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The given brass solution contains_____ gm of zinc
The weight of alloy taken is___ gm
% of iron =Weight of zinc in brass solution X 100
Weight of alloy taken
Result:1. The given brass solution contains ________________ gm Zinc in100ml
2. The percentage of Zinc ______________
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EXPERIMENT NO:Determination of amount of Copper in brass.
Aim: To estimate the amount of Copper (as %) in brass
Principle: The brass alloy of copper (60-80%) and zinc (20-40%) along with small amountof lead (0-2%) and iron(0-1%). To estimate zinc in brass alloy, the other elements
i.e. Cu, Pb and Fe are also to be removed by precipitation method. The solution
thus obtained which free from all these constituents is then estimated for the
Cu2+ titrimetically by using iodimetric method. An excess of potassium iodide to
a copper solution maintained PH between (4-5.5). The reaction liberates an
equivalent amount of iodide. The amount of copper in brass is then calculated
using stoichiometric relationship
Requirements:
Chemicals:1. Solution of brass alloy (free from other constituents)2. Potassium dichromate solution (0.1)3. Sodium carbonate (powder)4. Potassium thiocyanate5. Starch solution (indicator)6. Sodium thiosulphate Solution7. Potasium iodide (10% solution)
Apparatus:Pipette, Burette, Conical Flask 100ml, Beaker 100ml, Funnel ,Rubber
cork.
Chemical Reaction:
2CuSO4+4 KI=2CuI+I2+2K2SO4 (1)
I2+Na2S2O3=Na2S4O6+2 NaI . (2)
2CuSO4 = I2 = 2Na2S2O3
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Procedure:
1. Standardization of Na2S2O3 Solution:Pipette out 10ml Standard potassium dichromate solution in 100ml
conical flaskAdd 5ml of dilute sulfuric acid, followed by the addition of 10 ml
potassium iodide 10% and shake the solution.
The solution acquires dark brown colour due to the formation ofI2
Cover the flask with rubber cork for 5 minutes in dark.
Add sodium thiosulphate solution from burette until the brown colour
fades and solution acquires pale yellow colour
Add 2ml starch solution. The solution becomes blue due to formation of
starch iodine complex.
Continue the titration till the greenish blue colour disappears and
solution becomes sea green colour.
Note down the end point and repeat the titration for CBR.
2.Estimation of Copper:Pipette out 10ml brass solution in 100ml conical flask
Add small amount of sodum carbonate. The solution turns turbid due toformation of Cu (OH)2.
Add 10 ml potassium iodide 10% and shake the solution.The solution acquires brown colour due to the formation ofI2Cover the flask with rubber cork for 5 minutes in dark.Add sodium thiosulphate solution from burette until the brown colour
fades and solution acquires pale yellow colour
Add 2ml starch solution. The solution becomes blue due to formation of
starch iodine complex.Continue the titration untill the blue colour begins pale.Add 10ml KCNS the blue colour becomes intense.Continue the titration as quickly as possible until the blue colour
disappears. The solution turns white due to formation of Cu2I2.
Note down the end point and repeat the titration for CBR.
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Observation:N1=__ V1=___ Wt. Of Brass=_____
Observation Table:
Sr.No Volume OfNa2S2O3 Solution Used against (ml)Standard Brass
1
2
3
CBR
Calculation:
N1V1=M2V2
N2= 0.1X10
M1
N2=________N
N2V2=N3V3
N3= 0.1X10
N2
N3=________N
1MNa2S2O3 = 65.35gm/1000ml
N3 X 65.35 = ____gm/Lit
The given brass solution contains_____ gm of CopperThe weight of alloy taken is___ gm
% of iron =Weight of zinc in brass solution X 100
Weight of alloy taken
Result:1. The given brass solution contains ______________ gm Copper in100ml2. The percentage of Copper ______________
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EXPERIMENT NO:Determination of presence of moisture in coal.
Aim: Determination of moisture presence in given coal sample.
Principle:Coal is a fossil fuel which occurs in layers in the earths crust. It has been formed
by partial decay of plant materials accumulated millions of years ago and further
altered by the action of heat and pressure. Coal is an important solid fuel. The
composition of coal varies widely and hence it is necessary to analyses and
interprets the results from the points of view of commercial classification, price,
fixation and proper utilization. The quality of coal is ascertained by two types of
analysis.
Proximate analysis which includes the determination of moisture, volatilematerial, ash and fixed carbon.
Ultimate analysis which includes estimation of carbon, hydrogen, sulphur,
nitrogen and oxygen.
Moisture is generally determined by heating a known quantity of air-dried coal
from 105 C-110 C for about one hour and calculates the loss of weight as
percentage.
Requirements:
1.
Coal sample2. Silica crucible3. Desicator4. Electronic Balance5. Oven
Procedure:
1. Weight the empty crucible. Note the weight.2. Take 1 gm coal sample in it .again weight it accurately. . Note the weight.3. Heat the crucible without lid in an oven maintained at a temperature of 105 C-
110 C exactly 1 hour.
4. Cool the crucible in desicator and weight it again.5. Loss in weight is on account of the moisture.
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Observation:
Weight of empty crucible =
Weight of crucible with coal sample (approx 1gm) =
Weight of sample =
Weight of crucible with coal sample after heating =
Loss of weight =
Calculation:
Percentage of moisture=loss of weight
Weight of coal sample X 100
%=______________
Result:
The percentage of moisture is in coal ______________
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EXPERIMENT NO:Determination of Nickel in steel alloy.
Aim: To estimate the amount of nickel (as %) in steel alloy volumetrically
Principle: The nickel solution is titrated against EDTA at pH 10-11 using murexide asindicator; the free nickel ions are first complexed with EDTA. Then the nickel
ions from the nickel-murexide complex are displaced to from the more stable Ni-
EDTA complex librating the free from the indicator by the colour changes from
yellow to blue voilet
Requirements:
Chemicals:1. Standard ZnCl2 solution.(0.01M)2. EDTA solution3. Ammonia Buffer solution.4. Murexide indicator.5. Steel solution (Nickel Solution)Apparatus:
Pipette, Burette, Conical Flask 100ml, Beaker 100ml, Funnel
Chemical Reaction:
Mur + Zn2+
Zn - Mur Zn2+
+ EDTA ZnEDTA
(Pale Yellow) (Pink) (Stable)
EDTA+ Zn Mur Zn -EDTA+ Mur
(Pink)
Mur + Ni
2+
Ni - Mur Ni
2
+ EDTA NiEDTA(Orange) (Pink) (Stable)
EDTA+ Ni Mur Ni -EDTA+ Mur
(Pink)
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Procedure:
1.Standardization of EDTASolution:i.Pipette out 10ml Standard ZnCl2 (0.01)in 100ml conical flask
ii.Add 2ml Ammonia buffer and 2-3 drop of indicator. The solutionacquires a pale yellow colour.
iii.Titrate the solution with EDTA solution from the burette until thecolour changes pale yellow to pink.
iv.Repeat the titration for CBR2.Estimation of Zinc:
i. Pipette out 10ml brass solution in 100ml conical flaskii. Add 2ml Ammonia buffer and 2-3 drop of indicator. The solution acquires a
pale orange colour.
iii. Titrate the solution with EDTA solution from the burette until the colourchanges orange to violet.
iv. Repeat the titration for CBRObservation:
M1=__ V1=___ Wt. Of Brass=_____
Observation Table:
Sr.NoVolume Of EDTA Solution Used against (ml)
Standard Brass
1
2
3
CBR
Calculation:
M1V1=M2V2
M2= 0.1X10M1
M2=________M
M2V2=M3V3
M3= 0.1X10M2
M3=________M
1M EDTA = 58.71gm/1000ml
N3 X 58.71 = ____gm/Lit
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The given steel solution contains_____ gm of Nickel
The weight of alloy taken is___ gm
% of iron =Weight of nickel in brass solution X 100
Weight of alloy taken
Result:i. The given steel solution contains ________________ gm nickel in100ml
ii. The percentage of Nickel ______________