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# CHENNAI INSTITUTE OF TECHNOLOGY

## ENGINEERING CHEMISTRY LABORATORY MANUAL I & II

As per ANNA University syllabus (For First Semester B.E., / B. Tech.students common to all branches)

INDEX
S.NO
1

EXPERIMENTS
DETERMINATION OF TOTAL, PERMANENT , TEMPORARY HARDNESS OF WATER SAMPLE (EDTA Method ) ESTIMATION OF COPPER IN BRASS BY EDTA METHOD USING Fast sulphone black F indicator (or) Muroxide indicator ESTIMATION OF DISSOLVED OXYGEN IN WATER [winklers method] ESTIMATION OF CHLORIDE CONTENT IN WATER BY ARGENTOMETRIC METHOD [Mohrs Method] ESTIMATION OF ALKALITY IN WATER SAMPLE PHMETRY DETERMINATION STRENGTH OF HCl By NaOH CONDUCTOMETRIC TITRATION OF STRONGACID WITH STRONG BASE CONDUCTOMETRIC TITRATION OF MIXTURE OF ACIDS (HCl & CH3 COOH) CONDUCTOMETRIC PRECIPITATION TITRATION USING BaCl - NaSO ESTMATION OF FERROUS IRON BY POTENTIOMETRIC TITRATION

5 6

OF

8 9

10

S. NO

## VOLUME OF EDTA(V1) (ml)

1 2 3

CALCULATION Volume of standard hard water=20ml Volume of EDTA solution consumed, v1=ml 1ml of standard hard water contains 1mg of calcium carbonate 20ml of standard hard water consumes v1ml of EDTA ie., v1 ml of EDTA solution=20 mg of CaCO3 therefore 1ml of EDTA solution=20/v1mg of CaCO3 equivalent

## Step 2: TITRATION-2 Hard water sample Vs. std. EDTA

SI.no Volume of sample hard water (ml) 20 20 20 Burette readings (ml) INITIAL FINAL Volume of EDTA(ml)

1. 2. 3.

Calculation of the total hardness of the hard water Volume of hard water = 20ml Volume of EDTA consumed, v2........ml(titre value) 20 ml of the given hardwater sample consumes v2 ml of EDTA Ie,. 20ml of the given hard water sample contains 20/V1V2mg of CaCO3 Therefore 1000 ml of the given hard water sample cointains =20/V1V2mg of CaCO3 =1000V2/V1mg of CaCO3 =1000mg of CaCO3 ................................ =ppm Therefore total hardness of the given water sample of hard water =ppm.

## Step 3: TITRATION-3 Boiled hardwater sample Vs std EDTA

SI.NO Volume of boiled hard water(ml) 20 20 20 Burette reading(ml) INITIAL FINAL Volume of EDTA(V3)(ml)

1. 2. 3.

## Calculation of the permanent hardness of the hard water

Volume of the boiled hard water = 20ml Volume of the EDTA solution consumed, V3= ....................ml(titre value) 20ml of boiled hard water sample consumes V3 ml of EDTA Ie,. 20ml of boiled hard water sample cointains20/V1V31000/20mg of CaCO3 V3/V11000mg of CaCO3 ..1000mg of CaCO3 ........................ =mg of CaCO3 equivalent Therefore permanent hardness of hard water sample=.ppm.

## Step 4: Estimation of the temporary hardness of the hard water

Temporary hardness of the given sample of water }=total hardness-permanent hardness =- =..ppm.

EX.NO:1

## DETERMINATION OF TOTAL, PERMANENT , TEMPORARY HARDNESS OF WATER SAMPLE (EDTA Method - I)

AIM
To determine the total hardness, permanent hardness, temporary hardness in the given sample of hard water by EDTA method. A standard hard water and a EDTA solution are provided.

PRINCIPLE
Disodium salt of ethylene Diamine tetra acetic acid(EDTA) is a well known complexing agent. Its structure is shown in the figure 1 Disodium salt of EDTA is used to estimate the various hardness of the given hard water containing the Ca2+ and Mg2+ ions. When the EDTA is added to hard water , it reacts with calcium and magnesium present in hard water to form stable EDTA metal complexes. From the volume of EDTA consumed the hardness can be calculated. Eriochrome black-t is used as an indicator. The indicator forms a weak complex with the met al ions present in the hardwater and gives wine red colour.

Ca2

+EBT

Ca2+

EBT

Complex
Mg2+ Mg2+

When the EDTA is added into the hard, the metal ion forms a stable complex with EDTA by leaving the indicator. When all the metal ions are taken by EDTA from the indicator metal ion complex, the wine red colour changes into steel blue, which denotes the end point. The metal EDTA complex is stable at8-10. This pH range can be maintained by adding ammonical buffer (NH4Cl+NH4OH).

## STEP 1 TITRATION I STANDARDISATION OF EDTA (Std Hard water Vs EDTA

The burette is washed with distilled water and then raised with a little amount of the given EDTA solution upto the zero level without air bubbles. Initial reading of the burette is noted. 20ml of standard hard water solution is pipetted out into a clean conical

flask. 5ml of ammonia buffer solution and 2ml of Eriochrome black-T indicator are added the solution turns in wine red in colour to steel blue colour is the end point. The final reading in the burette is noted. The difference in the burette reading gives the volume of the EDTA solution. The titration is repeated to get a concordant values. Let volume of EDTA bev2ml

## STEP 2 TITRATION-2 ESTIMATAION OF TOTAL HARDNESS OF HARD WATER

20ml of the hard water sample is pipette out into a clean conical flask. 5ml of ammonia buffer solution and 2 drops of Eriochrome Black-T indicator are added. The solution turns in wine red in colour. This solution is titrated against EDTA solution taken in the burette. The change of wine red colour into steel blue colour is the end point. The titration is repeated to get the concordant values. Let volume of EDTA bev2ml

## Step 3 TITRATION-3 ESTIMATION OF PERMANENT HARDNESS

100ml of the given sample iof hard water is taken in a clean 250 ml beaker and boiled for 10-15 minutes. It is then cooled and filtered. The filtrate is cooled and collected in a 100 ml standard flask. 20ml of this made up solution ispipetted out into a clean conical flask. 5ml of ammonia buffer solution and 2-drops of Eriochrome Black-T indicator are added. The solution turns in wine red in colour. This solution is titrarted against the EDTA taken in the burette. The change in colour from wine red to steel blue is the end point. The titration is repeated to get the concordant values. Let volume of EDTA be v3

## Step 4 Estimation of Temporary Hardness

Temporary hardness of the water sample is calculated by subtracting permanent from total hardness Temporary hardness=Total hardness-permanent hardness.

RESULT
1. Amount of the total hardness of the given sample of water=.ppm. 2. amount of permanent hardness of the given sample of water=..ppm. 3. amount of temporary hardness of the given sample of water=..ppm.

EX.NO:2

ESTIMATION OF COPPER IN BRASS BY EDTA METHOD USING FAST SULPHONE BLACK F INDICATOR (OR) MUROXIDE INDICATOR

AIM:
To estimate the amount of copper present in 100 ml of the given solution being supplied with standard solution of ZnSO4 of strength 0.01 M and an approximately 0.01 M EDTA solution

PRINCIPLE:
Brass is an alloy of 55% copper and 33% zinc. The purpose of alloying copper and zinc is to improve machinability and strength. Brass may also contain small amounts of lead, tin or aluminum. In this method, brass is dissolved in con. HNO3, so that copper present in the brass is brought into the solution in the form of cupric ions. Then the Cu2+ ions are determined by the usual complexometric method using EDTA in present of fast sulphone black-F indicator (or) Muroxide indicator. (i)FSB-F Cu2+ + FSB F [FSB F-Cu] complex Purple colour [FSB F-Cu] complex +EDTA Cu EDTA + FSB F (ii)Muroxide Cu2+ + Muroxige [Cu Muroxide] complex Orange colour [Cu Muroxide] complex +EDTA Cu EDTA + Muroixde Blue violet colour

PROCEDURE
Step I TITRATION I Standardisation of EDTA

The burette is washed well distilled water and rinsed with the small amount of given EDTA solution. It is then filled with the same solution upto the zero mark without the bubbles. The pipette is washed with distilled water and rinsed with small amount of

standard Zn2+ ion solution is pipetted out into a clean conical flask. 10 ml of ammonia buffer solution and 3-4 drops of Erichrome Black-T (EBT) Indicators are added. The solution turns wine red in colour and it is then titrated against EDTA taken in the burette. The change of wine red colour to steel blue colour is the end point. The final reading is noted. The titration is repeated to get concordant values. From the volume of EDTA consumed, strength of EDTA solution is calculated. Step 2 TITRATION II Estimation of copper (using FSB-F indicator)

The given copper solution is made upto 100 ml in a standard flask. 20 ml of this solution is pipetted out into a clean conical flask. 10 ml of ammonia solution (or dil. Ammonia buffer) and 3-4 drops of fast Sulphone Black F (FSB-F) indicator are added. The solution turns purple in copper. The solution is titrated against standard EDTA solution taken in the burette. The change of colour into dark green colour is the end point. The titration is repeated to get concordant value. (OR) TITRATION II Estimation of Copper (using Muroxide indicator) The given copper solution is made upto 100 ml in a standard flask. 20 ml of this solution is pipette out into a clean conical flask. 5 ml of borate buffer solution and 3-4 drops of Muroxide indicator are added. The solution turns orange in colour. The solution is titrated against standard EDTA solution taken in the burette. The change of orange colour into blue violet colour is the end point. The titration is repeated to get concordant value. RESLUT: 1. 2. The amount of copper present in 100 ml of the given solution = ...gm Percentage of copper in the given brass sample =..%

Step I: TITRAETION I Standardisation of EDTA Standard Zn2+ solution Vs EDTA Volume of std Zn2+ Solution (V1) ml 20 20 20

Sl.No

## Volume of EDTA (v2) ml

1 2 3

Calculation of strength of EDTA solution Volume of std Zn2+ solution, Strength of Zn2+ solution, Volume of EDTA solution, Strength of EDTA solution, V1 =20 ml N1 = .M V2 N2 = ..ml = ?

According to the law of volumetric analysis V1N1=V2N2 N2= V1N1/V2 N2=20 ml X M/ ml Strength of EDTA solution (N2) = M

Sl.No

1 2 3

o o o

## Calculation of strength of EDTA solution

Volume of std copper solution, Strength of copper solution, Volume of EDTA solution, Strength of EDTA solution,

V1 N1 V2 N2

## =20 ml =? = ..ml = ..M

According to the law of volumetric analysis V1N1=V2N2 N2=V1N1/V2 N2= ml X M/20 Strength of copper solution (N2) = M

=gm

=.%

## EX.NO:3 Estimation of dissolved oxygen in water [winklers method]

AIM : To determine the amount of dissolved oxygen in the given water sample by winklers method , a standard solution of K2Cr2O2 of strength 0.01n is given. PRINCIPLE : Oxygen dissolved in water to the extent of 7-9 mgs/lit at a temperature range of 25 -350 C. The estimation of dissolved oxygen in water is useful in studying corrosion effect of boiler feed water and in studying water pollution . The amount of dissolved oxygen in water is estimated using winklers reagent (potassium bromide + potassium bromated ). Water sampel is collected carefully aeration/deaeration in ground stopperd flask . initially manganous sulphate and alkaline-iodide reagents are added and the reaction occur as follows
0

Mn2++2OH- Mn (OH)2(white) Mn(OH)2 + O2 Mno(OH)2 (yellow brown) The precipitate dissolves in concentrated sulphuric acid liberating iodine and the liberated iodine is titrated against Na2S2O3 MnO(OH)2+2H2SO4Mn(SO4)2 + 3H2O Mn(SO4)2 + 2KI MnSO4 + K2SO4 + I2 2 Na2S2O3 + I2 Na2S4O6 + 2NaI PROCEDURE :
TITRATION - 1 STANDARDIZATION OF SODIUM THIOSULPHATE

The burette is washed and rinsed with sodium thioosulphate solution . Then the burette is filled with given sodium thiosulphate solution . 20ml of 0.01n potassium dichromate solution is pipette out into a clean conical flask . To this 5ml of sulphuric acid and 15 ml of 5% potassium iodide are added . This is titrated against sodium thiosulphate solution . when the solution become straw yellow colour , starch indicator is added and then the titration is continued . The end is disappearance of blue colour and appearance of light yellow colour . the titration is repeated to get the concordant value .

## TITRATION 2 ESTIMATION OF DISSOLVED OXYGEN

100-150ml of water sample is taken in aiodine flask , 2ml of manganese sulphate and 2ml of alkali-iodide are added . Thje stopper is replaced and the flask is inverted and shaked several times for the rough mixing of reagents . The flask is left aside for some times . When half of the precipitate is setteled down , the stopper is removed and 2ml of conc. Sulphuric acid is added . The stopper is replacer and kept inverted for several times for complete dissolution of the precipitate . 100ml of this solution is pipette out and titrated against standard sodium thiosulphate solution . When the solution becomes light yellow starch indicator is added .The titration is repeated until the blue colour is disappeas . From the titire value the strength of dissolved oxygen is calculated and hence the amount of dissolved oxygen in the water sample is calculated RESULT : Amount of dissolved oxygen in tap water is = mgs/lit.

SI.NO

## Volume of sodium thiosulphate(ml)

Indicator

1. 2. 3.

20 20 20

0 0 0 Strach

Calculation : Volume of potassium dichromate Strength of potassium dichromate Volume of sodium thiosulphate Strength of sodium thiosulphate v1 = 20ml N1=0.01N V2 =.ml N2= ? V1N1=V2N2 N2=V1N1/V2 Strength of sodium thiosulphate = N2= 200.01/V2 =.. =.N

Step 2 :

## Estimation of dissolved oxygen Titration - 2

Water sample Vs sodium thiosulphate SI.NO Volume of Burette reading (ml) water sample (ml) Initial Final 100 100 0 Strach 2. 0 Volume sodium thiosulphate (ml) Indicator

1.

Calculation : Volume of sodium thiosulphate Strength of sodium thiosulphate Volume of water sample Strength of dissolved water sample V1 = . ml N1 = N V2 = 100ml N2 = ? V1N1=V2N2 N2= V1N1/V2 =ml..N/100

## Amount of dissolved oxygen in 1000mgs one litre of tap water

= normality eq.wt.of o2

= .N81000

=..mgs/lit

## 4. ESTIMATION OF CHLORIDE CONTENT IN WATER BY ARGENTOMETRIC METHOD [Mohrs Method]

AIM: To estimate the amount of chloride present in the given water sample, being supplied with standard solution of sodium chloride of strength .N and approximately N/20 solution of Silver Nitrate.

PRINCIPLE: Generally water contains chloride ions (Cl-) ions in the form of NaCl, KCl, CaCl2 and MgCl2. The concentration of chloride ions more than 250 ppm is not desirable for drinking purpose. The total chloride ions can be determined by argentometric method (Mohrs Method). In this method Cl- ion solution is directly titrated against AgNO3 using potassium chromate (K2CrO4) as the indicator. AgNO3 + Cl- AgCl + NO3At the end point, when all the Cl- ions are removed. The yellow colour of the chromate changes into reddish brown due to the following reaction. 2AgNO3 + K2CrO4 Ag2CrO4 + 2KNO3 (yellow) (reddish brown)

PROCEDURE: TITRATION I Standardisation of AgNO3 The burette is washed well with distilled water and rinsed with a small amount of AgNO3 solution. It is then filled with the same solution upto the zero mark without any air bubbles. The pipette is washed with distilled water and rinsed with a small amount of standard NaCl solution. 20ml of this solution is pipette out into a clean conical flask. 1ml of 2% K2CrO4 indicator solution is added and titrated against AgNO3 solution taken in the burette. The end point is the change of colour from yellow to reddish brown. The titration is repeated for concordant values.

STEP:2 TITRATION 2 Estimation of Chloride ion 20ml of the given water sample is pipette into a clean conical flask and 1ml of 2% K2CrO4 indicator solution is added. It is then titrated against standardized AgNO3 solution taken in a burette. The end point is the change of colour from yellow to reddish brown.

RESULT: (i) Amount of chloride ion present in the whole of the given water sample : .. gms /mgs/ppm. (ii) Amount of chloride ion present in the 100ml of the given water sample : .. gms /mgs/ppm.

SL.NO

## VOLUME OF AgNO3 (V2)(ml)

1 2 3

Calculation of the normality of silver nitrate Volume of Sodium Chloride Strength of Sodium Chloride Volume of Silver Nitrate Strength of Silver Nitrate V1 = 20 ml N1 = ..N V2 = ..ml N2 =...N

STEP:2

SL.NO

1 2 3

## VOLUME OF AgNO3 (V2)(ml)

Calculation of the normality of Water sample Volume of Water sample Strength of Water sample Volume of Silver Nitrate Strength of Silver Nitrate V1 = 20 ml N1 = ..N V2 = ..ml N2 =...N

According to Law of Volumetric analysis V1N1=V2N2 N1 = V2N2 / V1 = 20 .N / ml Strength of Water sample (Chloride ion) = N

CALCULATION OF AMOUNT OF THE CHLORIDE: Amount of the chloride ion present in 1 litre (1000ml) of the water sample = Equivalent weight of chloride ion sterngth of chloride ion Amount of the chloride ion present in 100ml of the given water sample = 35.65 Normality of the chloride ion 100/1000 = 35.65 ..100/1000 =gms.

## 5.ESTIMATION OF ALKALITY IN WATER SAMPLE

AIM
TO DETERMINE THE TYPE AND THE AMOUNT OF ALKALITY PRESENT IN THE GIVEN WATER SAMPLE .A STANDARED SOLUTION OF HYDROCHLORIC ACID OF STRENTH 0.1N

PRINCIPLE
Alkalinity is caused by the presence of hydroxide, carbonate and bicarbonate. There are five alkalinity conditions possible in a given sample of water, hydroxide only, carbonate only, bicarbonate only, combination of carbonate and hydroxide or carbonate and bi carbonate. The various alkalinities can be estimated by titrating with a standard acid is using phenolphthalein and methyl orange indicators successively.

(i)

## Phenolphthalein end point

Hydroxide alkalinity is completely neutralized and carbonate Alkalinity is partially neutralized during phenolphthalein end point.

OH- + H+ CO32- + H+

H 2O HCO3-

## (ii) Methyl orange end point

Bicarbonate neutralization occurs during methyl orange end point. HCO3- + H+ CO2 +H2O From the two titre values the different alkalinities are calculated. When, P=M, hydroxide alkalinity 2P=M, carbonate alkalinity P=0, bicarbonate alkalinity P<1/2M carbonate and bicarbonate alkalinity P>1/2M hydroxide and carbonate 2Co3 =2P HCO3- = M-2P CO32- = 2(M-P) OH- =2P-M Alkalinity values are expressed in terms of milligram per litre as calcium carbonate. PROCEDURE TITRATION 1 ( with phenolphthalein indicator) The burette is washed and rinsed with the given hydrochloric acid. Then the burette is filled with 0.1 hydrochloric acid. 20 ml of water sample is pipette out in a clean conical flask. A drop of phenolphthalein indicator is added. Pink colour is observed. This solution is titrated against the standard acid until pink colour is disappeared. The end point is noted. This titre value corresponds to phenolphthalein end point (P).

## TITRATION 2 (with methyl orange indicator)

S.NO RESULT OF [P] AND [M] 1. 2. 3. 4. 5. [P] = 0 [P] = [M] [P] =1/2 [P] > [M] [P] <1/2[M]
2-

OH

CO3

## O O 2[P]-[M] 2[M] 2[P] 2P

Few drops of methyl orange indicator is added to the same solution after the phenolphthalein end point. The titration is continued until the solution Becomes red orange. The total titre value is noted. This titre value corresponds to methyl orange end point (M).the titration is repeated for concordant values. From the titre values the amount of each alkalinity present in given water sample is calculated. RESULT Water sample contains the following alkalinity (i) Hydroxide alkalinity = ppm. (ii) Carbonate alkalinity = ppm. (iii) Bicarbonate alkalinity = ppm.

TABLE -2

S.no

## Methyl Orange end point [M]

1. 2.

20 20

CALCULATION
If the date satisfies the condition P>1/2 M (i) Volume of HCl required for [OH-] alkalinity = 2[P] [M] = 2 x - = . ml Volume of HCl required for [CO3-] alkalinity =2[M] 2[P] = 2x - 2 x =..ml HCO3- is not present.

(ii)

(iii)

NOTE:
1000 CC of 1N HCl = 1gm equivalent of CaCO3. 1000 CC of 1N HCl =50 gm of CaCO3.

## 1.calculation of OH- alkalinity

(V1) =Volume of HCl = (N1)=strength of HCl =0.1 N (V2)= volume of water sample = 20 ml (N2)={STRENGTH OF WATER SAMPLE(OH- ALKALINITY)} =? According to volumetric law : V1 N1 = V2 N2 V1 N1/V2=N2

N2=..ml x 0.1 N/ 20 =.N i.e., OH- alkalinity interms of CaCO3 equivalent= ..N x 50 x 103ppm

## ALKALINITY DUE TO OH ION = ppm 2.calculation of CO32- alkalinity

(V1)= Volume of HCl =.ml (N1)=Strength of HCl = 0.1N (V2)=Volume of water sample = 20 ml (N2)=strength of water sample (CO32- alkalinity)=? According to volumetric law V1 N1 = V2 N2 N2=V1 N1/V2 N2= ml x 0.1 N/20 =..N i.e,CO32- alkalinity interms of CaCO3 equivalent = . N X 50 X 103 ppm ALKALINITY DUE TO CaCO32- ION = ..ppm.

## PH METRY DETERMINATION OF STRENGTH OF HCL By NaOH AIM

To determine the strength of given HCL by pH metry , a standard solution of NaOH of 0.1 N is provided.

PRINCIPLE

Since the pH of the solution is related to the H+ ion concentration by the following formula. pH = -log [H+] measurement of pH of the solution gives the concentration of H+ ions in the solution. When NaOH is added slowly from the burette to the solution of HCL, the fast moving H+ ions are progressively replaced by slow moving Na+ ions . as a result pH of the solution increases. HCL + NaOH NaOH + H2O The increase in pH takes place until all the H+ ions are completely neutralized (upto the end point). After the end point , further addition of NaOH increases pH sharply as there is an excess of fast moving OH- ions.

MATERIALS REQUIRED
pH meter , glass electrode , beaker , standard N/10 NaOH , approximately N/10 HCL , burette , pipette , glass rod etc.,

PROCEDURE
The burette is filled with std. NaOH solution . exactly 20 ml of the given HCL solution is pipetted out into a clean beaker . it is then diluted to 20ml by adding distilled water . the glass electrode is dipped in it and connected with a pH meter.

TITRATION I
First a preliminary titration is carried out by adding std. NaOH solution in portions of 1 ml from the burette to the HCl solution taken in the beaker and pH of the solution is noted for each addition . this process is continued until atleast 5 readings are taken after the end point , and the range at which the end point lies is found out by plotting volume of NaOH added against pH (graph I).

TITRATION II
Another titration is carried out by adding std. NaOH solution in portions of 0.1 ml near the end point and pH of the solution is noted after each addition . the addition of NaOH is continued even after the end point for further 1 ml . the accurate end point is found out by plotting pH/v against volume of NaOH added (graph II) . from the end point , the strength of HCl solution and hence the amount of HCl can be calculated.

RESULT
1. Strength of the given HCL solution = N 2. Amount of HCL present in 1 litre of the solution = gms.

## TABLE I Titration of HCL (20 ml) Vs. NaOH

S.No.
1 2 3 4 5 Volume of NaOH 1 2 3 4 5 pH

6 7 8 9 10 11 12 13 14

6 7 8 9 10 11 12 13 14

TABLE II Titration of HCL (20 ml) Vs.NaOH Volume S.No of pH pH V Ph/v NaOH (ml)
(ml)

GRAPH GRAPH II

Ph pH/V

## Volume of NaOH (ml) (ml)

Volume of NaOH

CALCULATION
STEP I : calculation of strength of HCl
Volume of hcl , V1 = 20ml

## N1 = V2 = .. (titre value ) N2 = 0.1 N

According to the law of volumetric analysis , V1N1 = V2N2 N1= V2N2/V1 = ....N/20 Strength of HCL present in 1 liter of the given solution = ..N

## STEP II : calculation of amount of HCL

The amount of HCl present in 1000 ml of the given solution = ..NEq.wt.of HCl (36.5) =gms
CONDUCTOMETRIC TITRATION OF STRONG ACID WITH STRONG BASE

AIM To determine the amount of sodium hydroxide present in 250ml of the given solution by conductometric titration using standard hydrochloric acid of ..N

PRINCIPLE Solution of electrolytes conducts electricity due to the presence of ions. The specific conductance of a solution is proportional to the concentration of ions in it. The reaction between HCL and NaOH may be represented as, HCL + NaOH NaCl + H2O

When a solution of hydrochloric acid is titrated with NaOH, the fast moving hydrogen ions are progressively replaced by slow moving sodium ions. As a result conductance of the solution decreases. This decrease in conductance will take place as there is an excess of hydroxide ions. A graph is drawn between volume of NaOH added and the conductance of solution. The exact end point is intersection of the two curves. MATERIAL REQUIRED 1. 2. 3. 4. 5. 6. Conductivity bridge Conductivity cell Beaker Standard N/10 HCL Given NaOH solution Burette, pipette, glass rod etc.,

PROCEDURE The burette is filled with sodium hydroxide solution upto the zero level. 20 ml of the standard HCL is pipette out into a clean 100 ml beaker. The conductivity cell is placed in it and then diluted to 50 ml by adding conductivity water, so that the electrode are well immersed in the solution. The two terminals of the cell are connected with a conductivity bridge. Now 1 ml of NaOH from the burette is added to the solution, takes in the beaker, stirred for some time and then conductivity is measured. (The conductivity is going on decreasing upto the end point). This process is repeated until atleast five readings are taken after the end point has been reached.

Now the graph is plotted by taking volume of NaOH in the X-axis and conductance in the Y-axis. The end point is noted from the graph and the amount of NaOH present in 250 ml of the solution is calculated.

RESULT 1. The strength of given NaOH solution = ..N 2. The amount of NaOH present in 250 ml of the given solution = .gms

TABLE I Titration of standard HCL vs NaOH Volume of HCL taken = 20 ml Volume of NaOH added (ml) 0 1 2 Conductance (mho)

S.NO 1. 2 3

4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21

3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20

## cond point Equivalent

Volume of NaOH

Graph: conductance vs. volume of NaOH Step II Calculation of strength of NaOH Volume of HCL taken v1 = 20 ml Strength of HCL Volume of NaOH Strength of NaOH N1 = N v2= ml(titre value) N 2= ?

According to the law of Volumetric analysis V1N1 = V2N2 N2 = V1N1 / V2 = 20. Strength of NaOH = N Calculation of amount of NaOH The amount of NaOH present in 1000 ml of the given solution=40.N =gms The amount of NaOH present in 250 ml of the given solution = 40.N250/1000 =..gms

8

## ACIDS (HCl & CHCOOH)

AIM To determine the amount of a strong acid and a weak acid (HCL and CHCOOH) present in one litre of the given mixture of acid solution by Conductometric titration using standard NaOH of 0.1 N.

PRINCIPLE Solution of electrolytes conducts electricity due to the presence of ions. Since Specific conductance of a solution is proportional to the concentration of ions in it, Conductance of the solution is measured during titration. When the sodium hydroxide is added slowly from the burette to the solution, HCL (strong acid) gets neutralized first. Since the fast moving H ions are replaced by slow

moving Na ions, decrease in conductance take place until the end point is reached. HCL + NaOH Nacl + HO (Ist neutralisation).

After the complete neutralization of all HCL, the neutralization of CHCOOH starts, CHCOOH + NaOH CHCOONa + H0 (IInd neutrallisation).

Since CHCOOHNa is stronger electrolyte than CHCOOH, conductivity slowly increases until all CHCOOH is completely neutralized. When the end jpoint is reached, addition of NaOH will cause sudden increase in the conductance. This is due to the presence of fast moving OH ions. MATERIALS REQUIRED 1. Conductivity bridge N/10 2. Conductivity cell 3. Beaker 4. Standard

NaOH 5. Apporoximately N/10 HCL & CHCOOH glass rod etc., PROCEDURE

6. Burette, pipette,

The burette is washed well with water and rinsed with the given standard NaOH Solution. It is then filled with NaOH solution upto the zero level. 20 ml of the given Mixture of acids (HCL + CHCOOH) is pipette out into a clean 100ml beaker. The conductivity conductivity cell is placed in it and then diluted to 50 ml by adding

water, so that the electrodes are well immersed in the solution. The two terminals of the cell are connected with a conductivity bridge.

Now 1 ml of NaOH from the burette is added to the solution, taken in the beaker, Stirred for some time and then conductivity is measured. (The conductivity is going on decreasing upto the end point). This process is repeated until atleast five readings are taken after the end point (A) has been reached. After the end point, again NaOH is gradually added, which causes increase in Conductance. This increase in conductance is observed until the end point (B) is reached. After the second end point, sudden increase in conductance is observed on further Addition of NaOH. The reading (conductivity) is continuously measured for each Addition of NaOH and are tabulated. Now the graph is plotted between the volume Of NaOH Vs conductivity. From the graph the first end point (A) and the second end point (B) are noted. From the end points the amount of HCL and CHCOOH present in 1 litre of the mixture of solution is calculated. RESULT (i) (ii) The amount of HCl present in 1 litre of the given solution = .. gms The amount of CHCOOH present In 1 litre of the given solution = . gms

TABLE 1

TITRATION OF MIXTURE (HCl + CHCOOH) Vs NaOH S.No Volume of NaOH added(ml) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 Conductance

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22

step I calculation of strength of HCl volume of the mixture (HCl), V1 = 20 ml strength of the mixture (HCl), N1 = ..? volume of the NaOH, strength of the NaOH, V2 = .. (A) ml (Ist litre value) N2 = 0.1 N

According to the law of volumetric analysis, VN = VN N=VN/V=ml x 0.1 N/20 Calculation of amount of HCl The amount of HCl present in 1000 ml of the given solution = strength of HCl x Eq. wt of HCl =.. N x 36.5 =.. gms STEP II calculation of strength of HCl volume of the mixture (CHCOOH), V1 = 20 ml strength of the mixture (CHCOOH), N1 = ..? volume of the NaOH, strength of the NaOH, V2 = .. (A) ml (Ist litre value) N2= 0.1 N

Calculation of strength of CHCOOH The amount of CHCOOH present in 1000 ml of the given solution =..N x 60 =..gms =strength of CHCOOH x Eq.wt. of CHCOOH

## USING BaCl - NASO

AIM: To determine the amount of BaCl present in one litre of the given solution by conductometric titration using standard NaSO of 0.1N PRINCIPLE: Solution of electrolytes conducts electricity due to the presence of ions. Since specific conductance of a solution is proportional to the concentration of ions in it, conductance of the solution is measured during titration. In the precipitation titration, the ions are converted into insoluble precipitate, which will not contribute to the conductance. When NaSO is added slowly from the burette to the solution of BaCl, BaSO gets precipitated while the chloride ions remain unchanged. BaCl + NaSO BaSO + 2NaCl (unionized) The ions in the solution are replaced by free ions. Since the mobility

## ions, the conductance of the solution decreases.

After the end point, when all the ions are replaced, further addition of NaSO increases the conductance. This is due to the increase of Na and so ions in the solution. MATERIALS REQUIRED 1. 2. 3. 4. Conductivity bridge Conductivity cell Beaker Standard N/20 NaSO

5. 6.

## Approximately N/10 BaCl solution Burette, pipette, glass rod etc.,

PROCEDURE The burette is filled with NaSO solution upto the zero level. 20 ml of the given BaCl solution is pipette out into a clean 100 ml beaker. The conductivity cell is placed in it and then diluted to 50 ml by adding conductivity water. The two terminals of the cell are connected with a conductivity bridge. Now 1 ml of NaSO from the burette is added to the solution, taken in the beaker, stirred, and then conductivity is measured. This is continued upto the end point. (the conductivity is going on decreasing upto the end point). After the end point, again NaSO is gradually added and few more readings are noted. Thus the conductivity is continuously measured for each addition of NaSO and are tabulated. Now the graph is plotted between the volume of NaSO and conductivity. From the graph, end point is noted and hence the amount of BaCl present in 1 litre is calculated.

RESULT The amount of BaCl present in 1 litre of the given solution = . gms.

## ESTMATION OF FERROUS IRON BY POTENTIOMETRIC TITRATION

AIM
To estimate the amount of ferrous iron (fe2+ ) present in whole of the given Solution potentiometrically. A standard solution of potassium dichromate of strength 0.1 N is provided.

PRINCIPLE
Potentiometric titration depend on measurements of emf between reference electrode and an indicator electrode. When a solution of ferrous iron is titrated with a solution of potassium dichromate, the following redox reaction takes place. 6Fe2+ + Cro2- + 14H+ 6Fe3+ + 2Cr3+ +7HO During this titration fe2+ is converted into fe ,whose concentration increases.At the end point , there will be a sharp change due to sudden removal of all fe2+ ions. The cell is set up by connecting this redox electrode with a calomel electrode as shown below Hg/HgCl , KCl//fe2+ , fe3+ /pt A graph between emf measured against the volume of kcro added is drawn and the end point is noted from the graph.

MATERIAL REQUIRED
1.potentiometer 2. Pt electrode 3.Satured calomel electrode 4. Standard kcro solution 5. Given ferrous iron solution.

PROCEDURE
The given ferrous iron solution is made upto 100ml in a standard flask. 20ml of this made up solution is pipette out into a clean 100ml beaker. About 10ml of dil HSO and 20ml of distilled water are added in it. A platinum electrode is dipped into the solution. This electrode is then coupled with a

saturated calomel electrode and the cell is introduced into potentiometric circuit. The std KCrO solution is taken in the burette and is added.

TITRATION-I
First a preliminary titration is carried out by adding std. KCrO solution in portion of 1 ml and the emf of the cell is measured after each addition. The addition of KCrO is connected even after the end point and the range at which end point lies is found out by plotting volume of KCrO added against emf (graph 1)

TITRATION II
Another titration is carried out by adding std. KCrO solution in portion of 0.1 ml near the end point and the emf of the cell is measured after each addition. The addition of KCrO is continued even after the end point for further 1 ml. the accurate end point is determined by plotting Vs volume of KCrO added (graph-2) from the end point , the strength of ferrous iron solution and hence its amount can be calculated.

RESULT
The Amount of ferrous iron present In 100ml of the given solution is = gms.

## Volume of ferrous iron solution =20 ml

S.NO
1. 2. VOLUME OF KCrO (ml) 0 1 EMF (VOLTS)

## CALCULATION OF STRENGTH OF FERROUS IRON SOLUTION

Volume of ferrous iron solution , V=20ml Strength of ferrous iron solution N=? Volume of KCrO,V=.m Strength of kCrO, N=0.1N According to the law of volumetric analysis VN=VN N=vxN/20 N= .mlx0.1N/20 Strength of ferrous iron solution N=..N

## Calculation of amount of ferrous iron

The amount of ferrous iron present in 1000ml of the solution =Nx55.85

## The amount of ferrous iron present In 100ml of the given solution

=..Nx55.85x100/1000gms

=gms