EXPERIMENT 1

AIM: To determine the no. of water molecules of crystallization in Mohrs salt provided standard K 2Cr2O7 sol (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, K 2Cr2O7 THEORY: This titration is a type of redox reactions. Here, the principle involved is that ferrous sulphate (FeSO4) present in Mohrs salt. [FeSO4(NH4) 2 6H2 O] is oxidized by potassium dichromate (K 2Cr2O 7) to ferric sulphate [Fe2 (SO4)3] in the presence of dil. H2SO4 using diphenyl amine [(C6H5 )2 NH2 ] as internal indicator. This reaction involved: Cr2O72- + 14H+ + 6e- 2Cr3+ + 7H2O [Fe2+ Fe3+ + e-] x 6

Cr2O 72- + 14H+ + 6Fe2+ 2Cr3+ + 6Fe3+ +7H2O

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

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.

H
oxidation with

N
Cr2 O 7 2(Colourless) Diphenylamine

N
(Blue/Violet) Diphenyl benzide

OBSERVTION TABLE: SNo. Vol. of Burette titrate taken reading (Mohrs (initial)(ml) salt)(ml) 20ml 20ml 20ml 5.5 12.8 20.3 Burette reading (final)(ml) Vol. of titrant (K 2Cr2 O7 ) used(ml) (Final-Initial) 7.3 7.5 7.9

1 2 3

12.8 20.3 28.6

CALCULATIONS: Applying law of equivalence, N1V 1 = N2V 2 N1= Normality at Mohrs Salt N2= Normality of K 2Cr2O 7 V1= Volume of Mohrs salt
1

V2= Volume of K 2Cr2O 7 x V2 = 0.038

N1 x 20 = N1 =
200

10 2 7.6

Strength of anhydrated Mohrs Salt (y) = Normality x eq. wt. = N1 x 284 = 10.792 284 + 18 Strength of hydrated salt = 284 Strength of anhydrated salt 20 284+18 = 284 18x = Strength of hydrated salt = 20g/l (given)

200

20 x 284 18x = 284 10.79

20 x 284 284 x = 13.46

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

EXPERIMENT 2
AIM: Determination of iron content in an iron are by titrating it against standard K 2Cr2 O7 solution using potassium ferricyanide [K 3Fe(CN)6 ], H2SO4, FeSO4 as an external indicator. APPARATUS: Burette, burette stand, conical flask, white glazed tile, beaker, glass rod, measuring cylinder, funnel. CHEMICAL USED: K 2Cr2 O7 , [K 3Fe(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 K 2Cr2 O7 soln in the presence of H2SO4 using potassium ferrocynide as an external indicator. Oxides of ferrous sulphate present in Mohrs salt into ferric sulphate in the presence of dil H2SO4.[K 3Fe(CN)6] is used as an external indicator gives a greenish blue colour due to formation of ferro-ferricyanide complex.

OBSERVATION TABLE: S.No. Burette Vol. of titrate taken reading (initial)(ml) (Mohrs salt)(ml) 20ml 20ml 20ml 0 10.1 19.9 Burette reading (final)(ml) Vol. of titrant (K 2Cr2 O7 ) used(ml) (Final-Initial) 10.1 9.8 10.3

1 2 3

10.1 19.9 30.2

CALCULATIONS: Applying law of chemical equivalence, N1V 1 = N2V 2

10 1

N1 x 20 =
200 2

N1 =

Strength of Fe2+ in the soln = N1 x eq.wt. =

200 20 1

200

10

x V2

= 0.05
2

x 56

x 56

= 2.8 g/l

% of Fe

= 2.8 x 5 = 14 %

200

56

x V2 x

100

(x = 20 given)

Hence % of iron in iron soln is 14%

RESULT: The % of iron in iron soln is 14%.

EXPERIMENT 3

Screw Pinch Cock

160 140 120 100 Drops 80 60 40 20 0 0 50 100 Composition of A in mixture Graph

Linear (Graph)

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

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) (ii) Hydroxides only Carbonates only

(iii) Bicarbonates only (iv) Hydroxides and carbonates (v) Carbonates & bicarbonates Since OH- & HCO3- ion cannot co-exist because both combine together to form carbonates. OH + HCO3CO32- +H2O

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 CaCO3 equivalent by using normality equation. This is called phenolphthalein alkalinity (P). At this point, complete neutralization of hydroxide and conversion carbonate to bicarbonate takes place. CO32- + H+ HCO3-----(i) -----(ii) -----(iii) OH- + H+ H2O

Now titrate the same alkality soln using methyl orange indicator & alkalinity is calculated in terms of caco3 equivalents. This alkalinity is called mothyl orange alkalinity, alkalinity due to diff. ions can be calculated. The results are summarized in the following table.

HCO3-+ H+ H2O + CO2

Case I Case II Case III Case IV Case V

P=O P=1/2M P<1/2M P>1/2M P=M

NIL NIL NIL (2P-M) P=M

NIL 2 PORM 2P 2 (M-P) NIL

M NIL (M-2P) NIL NIL

INDICATORS: Phenol phtalien and methyl orange. END POINTS: Pink to colourless (phenolphthalein), Yellow to red (methyl orange)

OBSERVATIONS: (a) Reading using phenolphthalein Vol. of soln titrate)token in the titration flask(ml) 20 20 20 Burette reading Vol. of the titration used(V1-V1) Final-Initial 7 6.7 6.5 Mean=6.73

S.No.

1 2 3 (b)

Initial (V1) 0 11.5 22.5

Final (V1) 7 18.2 29.0

Reading using methyl orange Vol. Soln taken(ml) 20 20 20 Initial 7 18.2 29 Final 11.5 22.5 33.2 Final-Initial 4.5 4.3 4.2 Mean=4.33

S.No. 1 2 3

CALCULATIONS: 1. Phenolphthalein alkalinity in terms of CaCO3 equivalent Acc. to Law of Equivalence, N1V1 = N2V2 (acid) (water) 1/10(V2-V1) = N2 x 20

N2 = 6.73/200 = 0.03365 Strength in terms of CaCO3 eq. = N2 x 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 equivalent Acc. 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

PRECAUTIONS: 1. Phenolphthalein indicator should be added first & then methyl orange. 2. 3. The vol. of indicator should be same in all observations. Constant shaking of soln mixture should be done.