mbatech lab mannual 2012-13

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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 ______________