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    EXPERIMENT 1

    AIM:

    To determine the no. of water molecules of crystallization in Mohrs

    salt provided standard K2Cr2O7sol (0.1N). Using diphenylamine as

    internal indicator.

    APPARATUS:

    Burette, burette stand, pipette, beaker, conical flask, funnel,

    measuring cylinder.

    CHEMICAL USED:

    Mohrs salt, H2SO4, H3PO3, Dipheyl amine, K2Cr2O7

    THEORY:

    This titration is a type of redox reactions. Here, the principle

    involved is that ferrous sulphate (FeSO4) present in Mohrs salt.

    [FeSO4(NH4)26H2O] is oxidized by potassium dichromate (K2Cr2O7)

    to ferric sulphate [Fe2(SO4)3] in the presence of dil. H2SO4using

    diphenyl amine [(C6H5)2NH2] as internal indicator. This reaction

    involved:

    Cr2O72-+ 14H++ 6e-2Cr3++ 7H2O

    [Fe2+Fe3++ e-] x 6

    --------------------------------------------------------------

    Cr2O72-+ 14H++ 6Fe2+2Cr3++ 6Fe3++7H2O

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    At the end point, all the ferrous ions (Fe2+) present in the solution get

    completely oxidized to ferric ions (Fe3+) by chromate ions (Cr2O72-).

    As soon as a slight excess of potassium dichromate solution is

    added, it brings about the oxidation of diphenylamine resulting in the

    formation of a blue coloured complex named diphenyl benzidine. At

    the end point a sharp change from colourful solution to deep blue

    solution is observed.

    Hoxidation with

    N N N

    Cr2O72-

    (Colourless) (Blue/Violet)

    Diphenylamine Diphenyl benzide

    OBSERVTION TABLE:

    SNo. Vol. of

    titrate taken

    (Mohrssalt)(ml)

    Burette

    reading

    (initial)(ml)

    Burette

    reading

    (final)(ml)

    Vol. of

    titrant

    (K2Cr2O7)used(ml)

    (Final-Initial)

    1 20ml 5.5 12.8 7.3

    2 20ml 12.8 20.3 7.5

    3 20ml 20.3 28.6 7.9

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    CALCULATIONS:

    Applying law of equivalence,

    N1V1= N2V2 N1= Normality at Mohrs Salt

    N2= Normality of K2Cr2O7

    V1= Volume of Mohrs salt

    V2= Volume of K2Cr2O7

    N1 x 20 =1

    10x V2

    N1 =2

    200=7.6

    200= 0.038

    Strength of anhydrated Mohrs Salt (y) = Normality x eq. wt.

    = N1x 284

    = 10.792

    Strength of hydrated salt = 20g/l (given)

    Strength of hydrated salt

    Strength of anhydrated salt=

    284 + 18

    284

    20

    =

    284+18

    284

    18x =20x284

    284

    18x =20x284

    10.79 284

    x = 13.46

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    RESULT:

    The no. of water molecules of crystallization in Mohrs Salt is 6.73

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    EXPERIMENT 2

    AIM:

    Determination of iron content in an iron are by titrating it against

    standard K2Cr2O7solution using potassium ferricyanide [K3Fe(CN)6],

    H2SO4, FeSO4as an external indicator.

    APPARATUS:

    Burette, burette stand, conical flask, white glazed tile, beaker, glass

    rod, measuring cylinder, funnel.

    CHEMICAL USED:

    K2Cr2O7, [K3Fe(CN)6], H2SO4, FeSO4

    THEORY:

    This estimation is based on the principle that the solution containing

    ferrous ammonium sulphate can be quantitatively titrated against

    standard K2Cr2O7solnin the presence of H2SO4using potassium

    ferrocynide as an external indicator.

    Oxides of ferrous sulphate present in Mohrs salt into ferric

    sulphate in the presence of dil H2SO4.[K3Fe(CN)6] is used as an

    external indicator gives a greenish blue colour due to formation of

    ferro-ferricyanide complex.

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    OBSERVATION TABLE:

    S.No. Vol. of

    titrate taken(Mohrs

    salt)(ml)

    Burette

    reading(initial)(ml)

    Burette

    reading(final)(ml)

    Vol. of

    titrant(K2Cr2O7)

    used(ml)

    (Final-Initial)

    1 20ml 0 10.1 10.1

    2 20ml 10.1 19.9 9.8

    3 20ml 19.9 30.2 10.3

    CALCULATIONS:

    Applying law of chemical equivalence,

    N1V1= N2V2

    N1 x 20 =1

    10x V2

    N1 =2

    200=

    10

    200= 0.05

    Strength of Fe2+in the soln= N1x eq.wt.

    =2

    200x 56

    =1

    20x 56 = 2.8 g/l

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    % of Fe =56200

    x V2 x100

    (x = 20 given)

    = 2.8 x 5 = 14 %

    Hence % of iron in iron solnis 14%

    RESULT:

    The % of iron in iron solnis 14%.

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    Screw Pinch Cock

    B

    EXPERIMENT 3

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    0

    20

    40

    60

    80

    100

    120

    140

    160

    0 50 100

    Drops

    Composition of A in mixture

    Graph

    Linear (Graph)

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    The Redwood viscometer was made by Sir Boverton Redwood in about 1880.

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    EXPERIMENT 7

    AIM:

    To determine the type & extent of alkalinity of given water sample.

    APPARATUS:

    Burette, pipette, conical flask, beaker, measuring flask.

    CHEMICALS:

    Water sample, V/10 HCl, phenolphthalein and methyl orange

    indicator.

    THEORY:

    Alkalinity of water is mainly due to the presence of the following.

    (i) Hydroxides only(ii)

    Carbonates only

    (iii) Bicarbonates only(iv) Hydroxides and carbonates(v) Carbonates & bicarbonatesSince OH-& HCO3

    -ion cannot co-exist because both combine

    together to form carbonates.

    OH + HCO3- CO3

    2-+H2O

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    The extent of alkanity present in a water sample is determined by

    titrating the water sample (titrate) with a standard acid (titrant) using

    phenolphthalein indicator and alkalinity if found out in terms of

    CaCO3equivalent by using normality equation. This is called

    phenolphthalein alkalinity (P). At this point, complete neutralization

    of hydroxide and conversion carbonate to bicarbonate takes place.

    OH- + H+H2O -----(i)

    CO32- + H+HCO3

    - -----(ii)

    HCO3-+ H+H2O + CO2

    -----(iii)

    Now titrate the same alkality solnusing methyl orange indicator &

    alkalinity is calculated in terms of caco3equivalents. This alkalinity is

    called mothyl orange alkalinity, alkalinity due to diff. ions can be

    calculated. The results are summarized in the following table.

    Case I P=O NIL NIL M

    Case II P=1/2M NIL 2 PORM NIL

    Case III P1/2M (2P-M) 2 (M-P) NIL

    Case V P=M P=M NIL NIL

    INDICATORS: Phenol phtalien and methyl orange.

    END POINTS:Pink to colourless (phenolphthalein),

    Yellow to red (methyl orange)

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    OBSERVATIONS:

    (a) Reading using phenolphthaleinS.No. Vol. of soln

    titrate)token in

    the titration

    flask(ml)

    Burette reading Vol. of the

    titration

    used(V1-V1)

    Initial (V1) Final (V1) Final-Initial

    1 20 0 7 7

    2 20 11.5 18.2 6.73 20 22.5 29.0 6.5

    Mean=6.73

    (b) Reading using methyl orange

    S.No. Vol. Solntaken(ml) Initial Final Final-Initial

    1 20 7 11.5 4.5

    2 20 18.2 22.5 4.3

    3 20 29 33.2 4.2

    Mean=4.33

    CALCULATIONS:

    1. Phenolphthalein alkalinity in terms of CaCO3equivalentAcc. to Law of Equivalence,

    N1V1= N2V2

    (acid) (water)

    1/10(V2-V1) = N2x 20

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    N2 = 6.73/200 = 0.03365

    Strength in terms of CaCO3eq. = N2x eq. wt of CaCO3

    = 0.03365 x 50 = 1.6825 g/l

    P = 1.6825 x 1000 mg/l = 1682.5 mg/l

    = 1.6825 x 1000 ppm = 168.25 ppm

    2.Methyl orange alkanity in terms of CaCO3 equivalentAcc. to Law of Equivalence,

    N1 V1= N2 V2

    (acid) (water)

    1/10(V3-V1) = N2 x 20

    N2= 1/10 x (V3-V1)/20

    RESULT:

    Phenolphthalein alkalinity (P) = 1682.5ppm of CaCO3

    Methyl orange alkalinity (M) = 1082.5 ppm of CaCO3

    (To find out the alkalinity in terms of individual fans, find out to which

    case the values of P & M falls out from table, calculate the amount of

    individual ions as below.)

    Alkalinity due to OH-ions = 2P-M = 2282.5 ppm

    Alkalinity due to CO32-ions = 2(M-P) = 1200 ppm

    Alkalinity due to HCO3-ions = Nil

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    PRECAUTIONS:

    1. Phenolphthalein indicator should be added first & then methylorange.2. The vol. of indicator should be same in all observations.3. Constant shaking of solnmixture should be done.

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