LIST OF EXPERIMENTS

1. 2. 3. 4. 5.

Determination of percentage of iron in plane carbon steel. Determination of zinc in brass. Determination of the amount of copper in brass. Determination of presence of moisture in coal. Determination of percentage of nickel in steel alloy.

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. 2. 3. 4. Standard Ferrous ammonium Sulphate Solution (0.1) KMnO4 Solution. Dilute sulphuric acid 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 100ml conical flask Add 10ml Dilute sulphuric acid Titrate the solution slowly with KMnO4 solution from the burette until permanent 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 permanent pink colour persists in the solution Repeat the titration for CBR

Observation:
N1=__ V1=___ Wt. Of Steel=_____

Observation Table: Sr.No 1 2 3 CBR Volume Of KMnO4 Solution Used against (ML) Standard Steel

Calculation:
N1V1=N2V2 N2= 0.1X10 N1 N2=________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 in100ml 2. The percentage of iron ______________

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 of
lead (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 of zinc is calculated using stoichiometric relationship

Requirements: Chemicals:
1. 2. 3. 4. 5. Standard ZnCl2 solution.(0.01M) EDTA solution Ammonia Buffer solution. Eriochrome black T indicator. Brass solution

Apparatus:
Pipette, Burette, Conical Flask 100ml, Beaker 100ml, Funnel

Chemical Reaction:
EBT + Zn2+ (Blue) Zn- EBT (Pink)

Zn2+ + EDTA Zn EDTA (Stable) EDTA+ Zn EBT Zn -EDTA+ EBT (Blue)

Procedure: 1. Standardization of EDTA Solution:

i. Pipette out 10ml Standard ZnCl2 (0.01)in 100ml conical flask ii. 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 the colour changes wine red to blue. iv. Repeat the titration for CBR

2. Estimation of Zinc:
i. Pipette out 10ml brass solution in 100ml conical flask ii. 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 the colour changes wine red to blue. iv. Repeat the titration for CBR

Observation:
M1=__ V1=___ Wt. Of Brass=_____

Observation Table: Sr.No 1 2 3 CBR Calculation: M1V1=M2V2 M2= 0.1X10 M1 M2=________M M2V2=M3V3 M3= 0.1X10 M2 M3=________M Volume Of EDTA Solution Used against (ml) Standard Brass

1M EDTA = 65.38gm/1000ml N3 X 65.38 = ____gm/Lit

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 ______________

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 amount
of 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. 2. 3. 4. 5. 6. 7. Solution of brass alloy (free from other constituents) Potassium dichromate solution (0.1) Sodium carbonate (powder) Potassium thiocyanate Starch solution (indicator) Sodium thiosulphate Solution Potasium iodide (10% solution)

Apparatus:
Pipette, Burette, Conical Flask 100ml, Beaker 100ml, Funnel ,Rubber cork.

Chemical Reaction: 2CuSO4+4 KI=2CuI+I2+2K2SO4 I2+Na2S2O3=Na2S4O6+2 NaI 2CuSO4 = I2 = 2Na2S2O3

(1) . (2)

Procedure: 1. Standardization of Na2S2O3 Solution:

Pipette out 10ml Standard potassium dichromate solution in 100ml conical flask Add 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 of I2 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 to formation of Cu (OH)2. Add 10 ml potassium iodide 10% and shake the solution. The solution acquires brown colour due to the formation of I2 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 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.

Observation:
N1=__ V1=___ Wt. Of Brass=_____

Observation Table:
Sr.No 1 2 3 CBR Volume Of Na2S2O3 Solution Used against (ml) Standard Brass

Calculation: N1V1=M2V2 N2= 0.1X10 M1 N2=________N N2V2=N3V3 N3= 0.1X10 N2 N3=________N

1M Na2S2O3

= 65.35gm/1000ml

N3 X 65.35 = ____gm/Lit The given brass solution contains_____ gm of Copper The weight of alloy taken is___ gm % of iron =Weight of zinc in brass solution X 100 Weight of alloy taken

Result:
1. 2. The given brass solution contains ______________ gm Copper in100ml The percentage of Copper ______________

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, volatile material, 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. 2. 3. 4. 5. Coal sample Silica crucible Desicator Electronic Balance 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 C110 C exactly 1 hour. 4. Cool the crucible in desicator and weight it again. 5. Loss in weight is on account of the moisture.

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 ______________

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 as
indicator; 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 NiEDTA complex librating the free from the indicator by the colour changes from yellow to blue voilet

Requirements: Chemicals:
1. 2. 3. 4. 5. Standard ZnCl2 solution.(0.01M) EDTA solution Ammonia Buffer solution. Murexide indicator. Steel solution (Nickel Solution)

Apparatus:
Pipette, Burette, Conical Flask 100ml, Beaker 100ml, Funnel

Chemical Reaction:
Mur + Zn2+ (Pale Yellow) Zn - Mur (Pink) Zn2+ + EDTA Zn EDTA (Stable)

EDTA+ Zn Mur Zn -EDTA+ Mur (Pink) Mur + Ni2+ (Orange) Ni - Mur (Pink) Ni2 + EDTA Ni EDTA (Stable)

EDTA+ Ni Mur Ni -EDTA+ Mur (Pink)

Procedure: 1. Standardization of EDTA Solution:

i. Pipette out 10ml Standard ZnCl2 (0.01)in 100ml conical flask ii. Add 2ml Ammonia buffer and 2-3 drop of indicator. The solution acquires a pale yellow colour. iii. Titrate the solution with EDTA solution from the burette until the colour changes pale yellow to pink. iv. Repeat the titration for CBR

2. Estimation of Zinc:
i. Pipette out 10ml brass solution in 100ml conical flask ii. 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 colour changes orange to violet. iv. Repeat the titration for CBR

Observation:
M1=__ V1=___ Wt. Of Brass=_____

Observation Table:
Sr.No 1 2 3 CBR Volume Of EDTA Solution Used against (ml) Standard Brass

Calculation: M1V1=M2V2 M2= 0.1X10 M1 M2=________M 1M EDTA = 58.71gm/1000ml N3 X 58.71 = ____gm/Lit M2V2=M3V3 M3= 0.1X10 M2 M3=________M

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. ii. The given steel solution contains ________________ gm nickel in100ml The percentage of Nickel ______________