Experiment No: 01 Name of the Experiment:

Determination of the alkalinity of the water sample by the neutralization titration.

Principle:
Water samples containing measurable OH- and or CO32- ions turn pink to phenolphthalein indicator. This water becomes color less at pH below 8.4, when titrated with acid to covert

theses ions to HCO3- form. Again, water with only HCO3- can be titrated to the critical pH
level of 5.3 with acid by using yellow to faint orange color change of methyl orange indicator. Both of the indicators are used for determining total alkalinity, expressed as ppm of CaCO3 and also the concentrations of OH-, CO32- and HCO3- ions in Water samples. CO32- + H+ = HCO3HCO3- + H+ = H2CO3

Materials:
Burette (25ML), pipette (10ML), funnel, conical flask (250ML), measuring flask (100ML), beaker (250ML), spatula, burette stand etc.

Reagents:
H2so4, Na2CO3, Phenolphthalein, Methyl orange indicator.

Reagent Preparation:
0.1N H2SO4 Solution: 2.8 ml H2SO4 (95-98% Sp. gravity=1.84) was taken into 1 litre volumetric flask and it was diluted to 1000ml mark of the flask. Methyl orange indicator Solution: 500mg methyl orange was dissolved as free add powder in distilled water and it was diluted to 1L.

Procedures:
The burette was rinsed with distilled water and then rinsed with 0.1N H2SO4 by pipette. The burette was clamped and it was filled with 0.1N H2SO4 solution up to mark.

H2SO4 solution was standardized by Na2CO3 solution. The sample (say 200ml) was taken into 250ml of conical flask and 5 drop of phenolphthalein was added into the solution. If the solution become colored then we proceeded with step (a) . If not, we will go directly on to step 1 with 0.1N H2SO4 until the color disappeared. The number of ml of adding used was recorded. 5 drops of Methyl orange indicator solution was added to the sample and was titrated with 0.1N H2SO4 to a light pink (pH=4.5) color, as required by the sample composition.

Table of Data :
Volume of H2SO4 in ml. added from burette No. of Observation Initial reading of burette in ml. 1. 2. 3. 19 19.6 20.3 19.6 20.3 21.1 Final reading of burette in ml .6 .7 .8 Difference between burette reading in ml

Calculation :
Average volume of H2SO4 Alkalinity as CaCo3 = = 350 mg/L mg/L mg/L = 0.7ml

Here,
A = volume of H2SO4 N = normality of H2SO4 ml of sample = 10 ml

Result :
The alkalinity of the water sample is 350 mg/L.

Experiment No: 02
Name of the Experiment: Determination of the acidity of the water sample by neutralization titration of the free CO2 in the water sample.

Principle:
By neutralization titration acidity of the sample of water can be determined. In this process 0.1 N NaOH is used as titrate. Phenolphthalein is used as the indicator. 5 drop Phenolphthalein indicator will be added with 100 ml of sample water and then titrated by 0.1 N NaOH. The ending point of the reaction is light pink color of the solution.

100 ml sample + 5drop Phenolphthalein + add NaOH (0.1 N) =Light pinc color (End point)

Materials:
Burette (25ml), Pipette (10ml), Funnel, Conical flask, Measuring flask (100ml), Beaker (250ml), Burette stand etc.

Reagents:
NaOH, Phenolphthalein, Bromophenol blue, standard potassium hydrogen thalate.

Reagent preparation:
Dissolve 2.5gm phenolphthalein into 250 ml 95% ethyl alcohol and 250 of distilled water added.

Procedure:
The burette was rinsed with distilled water and then rinsed with 0.1 N NaOH by pipette. (2)The burette was clamped and filled with 0.1 N NaOH solution up to mark. The NaOH solution was standardized by standard potassium hydrogen phthalate solution. Then it was titrated with 0.1 N NaOH solutions until a permanent pink color appears.

Table of Data:
Volume of NaOH in ml, added from burette. No. of Observation Initial reading of Final reading of Burette in ml Burette in ml Difference between burette reading in ml

16.3

16.9

0.6

16.9

17.6

0.7

17.6

18.3

0.7

Calculation:
Average of burette reading = (0.6+0.7+0.7) / 3 ml = o.7 ml Acidity as CaCO3 = = = 35 ml Free CO2 = = = 30.8 ml
Here, A=Volume of NaOH N= Normality of NaOH

Result:
The acidity of water sample is 35 ml/L; The quantity of free CO2 in water is 30.8 ml/L.

Experiment No: 03 Name of the experiment:

Determination of the dissolved oxygen (DO) of the water sample by the iodometric titration (Winker method)

Principle:
Manganous (Mn2+) ions form manganous hydroxide Mn(OH)2 under highly alkaline condition. In order to avoid loss of oxygen from the water sample it is fixed by its reaction with manganese(II) hydroxide which is covered rapidly and quantitively to manganese (III) hydroxide: 4Mn(OH)2 + O2+ 2H2O = 4Mn(OH)3 The brown precipitate obtained dissolves on acidification and oxidizes iodide ions to iodine: Mn(OH)3 + I- + 3H+ = Mn2+ + I2 + 3H2O This I2 estimated by titration with sodium thiosulphate (Na2S2O3) indicates the amount of DO in water sample. 2S2O32- + I2 = S4O62- + 2IThis means that 4 moles of thiosulphate correspond to 1 mole of dissolved oxygen. The main interference in the process is due to the presence of nitrates (especially in waters from sewage treatment). This is overcome by treating the original water samples with sodium azide, which destroys any nitrate when the sample is acidified: HNO3 + HN3 = N2 + N2O + H2O

Materials:
Manganous sulphate (MnSO4.4H2O), KOH, KI, NaN3, Starch and sodium thiosulphate (Na2S2O3)

Procedure:
(a) Laboratory Preparation: Manganous Sulphate solution: Dissolve 120gm MnSO4. 4H2O (or 100gm MnSO4.2H2O or 91gm MnSO4.H2O) in distilled water and dilute to 250ml. Alkali-iodide-acid reagent: For a saturated or less than saturated sample; Dissolve 700gm KOH and 150gm KI in distilled water and dilute to 1L. Add 10gm NaN3 dissolved in 40ml distilled water. Starch solution: Dissolve 2gm laboratory-grade soluble starch and 0.2gm salicylic acid as a preservative, in 100ml hot distilled water. Standard sodium thio-sulphate titrant: Dissolve 6.025gm Na2S2O3.5H2O in distilled water and add 0.4gm NaOH and dilute to 1000mL. Standardize with biiodate solution. (b) Field work: Add 1 ml MnSO4 solution followed by 1ml alkali-iodide-azide reagent to the sample collected in a 250 to 300ml BOD bottle. Stopper carefully to exclude air bubbles and mix by inverting bottle a few times. When precipitate has settled sufficiently to leave clear superannuate above the manganese hydroxide flock, add 1.0ml conc. H2SO4. Re-stopper and mix by inverting several times until dissolution is complete. Titrate a volume corresponding to 200mL original sample after correction for samples loss by displacement with reagents. Titrate sample (10ml) with 0.025 Na2S2O3 solution to pale straw color by adding a few drops of starch solution and continue titration to first disappearance of blue color.

Experiment No: 04
Name of The Experiment: Determination of water hardness by complexometric (EDTA) titration.

Principle:
Water hardness due to Ca+ and Mg+ is expressed as mg/L CaCo3 (ppm) The total of Ca+ and Mg+
2H2Y.2H2O

( purity 100.0

0.5%).

If the sample does not contain magnesium, Mg-EDTA is added to the titration flask to provide a sharp end point with Eriochrome Black T, since calcium does not form a sufficiently strong chelate with the indicator to give a sharp end point.

Equations:
Ca2+ + H2Y2- = CaY2- + 2H+ Ca2+ + MgY2- = CaY2- + Mg2+ End point: Mg2+ + HIn2- = MgIn- + H+ MgIn- + H2Y2- = MgY2- + Hin2- + H+

Preparation of reagents:
1. Buffer Solution: Dissolve 16.9gm Ammonium Chloride (NH4Cl) in 143ml conc. Ammonium hydroxide (NH4OH) into 250 ml flask. Dissolve 1.179gm disodium salt of ethylenediaminetetraacetic acid dehydrate ( analytical reagent grade and 644 mg magnesium chloride (MgCl2.6H2O) in 50 ml distilled water. Now this solution is added to 16.9 gm Ammonium Chloride (NH4Cl) and 143ml conc. Ammonium hydroxide (NH4OH) with mixing and is diluted to 250 ml with distilled water. 2. Indicator Solution: Eriochrome Black T : 0.5gm dye ( Sodium salt of 1-(hydroxyl- 2- napthylazo)- 5- nitro-2napthol- 4- sulfonic acid) in 2- methoxymethanol (also called ethylene glycol monomethyl ether) is dissolved.

3. Standard EDTA titrant (0.01M): 3.723gm analytical reagent grade disodium ethylenediaminetetraacetic acid dehydrate, also called Ethylenedinitrilo tetracetic acid disodium salt ( EDTA) is weighed and diluted to 1000ml. This solution is standardized against standard calcium solution. 4. Standard calcium solution: 1.0 gm anhydrous CaCo3 powder is weighed into a 500 ml Erlenmeyer flask. A funnel on the flask neck is placed, then at a time 1+1 HCL is added until all CaCO3 is dissolved. 200 ml distilled water is added and boiled for a few minutes to expel CO2. After cooling a few drops of methyl red indicator is added and is adjusted to the intermediate orange color by adding 3N NH4OH or 1+1 HCL as required. Then it is transferred quantitavely and diluted to 1000ml with distilled water. 1ml= 1.00 mg CaCO3

Procedure:
A sample volume is selected that requires less than 15 ml EDTA titrant and complete titration within 5 minutes measured from time to buffer addition. Appropriate (10ml) sample is diluted to about 50 ml with distilled water in a porcelain casserole or other suitable vessel. 1-2 ml buffer solution is added. Usually 1 ml will be sufficient to give a pH of 10.0 to 10.1 1-2 drops indicator is added Standard EDTA titrant is added slowly, with continuous stirring, until the last reddish tinge disappears. The last few drops are added at 3-5 seconds intervals. At the end point the solution is normally blue.

Experiment No: 05 Experiment Name:

Determination of the amount of chloride (Cl) in water by Mohr Titration

Principle:
The Mohr method employs a solution of silver nitrate as the titrant and potassium chromate as the indicator. In a neutral or slightly alkaline solution, potassium chromate can indicate the end point of the silver titration of chloride. Ag + Cl = AgCl The end point cannot be detected visually unless an indicator capable of demonstrating the presence of excess Ag+ is present. As the concentration of chloride ions approaches extinction, the silver concentration increases to begin form a reddish-brown precipitate. Ag + CrO4 = Ag2CrO4 Since an excess of Ag+ is need to produce a visible amount of Ag2CrO4 , the indicator error or black must be determined and subtracted from all the titration.

Apparatus:
Erlenmeyer flask, 250ml, pH meter, Burette, Pipette, Beaker etc.

Chemicals:
Potassium chromate (K2CrO4), Silver nitrates(AgNO3) , Sodium chloride (NaCl) etc.

Reagent Preparation:
Potassium chromate indicator solution: Dissolve 12.50gm K2CrO4 in a little distilled water. Add AgNO3 solution until a define red precipitate is formed. Let stand 12h. Filters, and dilute to 250ml with distilled water. Standard silver nitrate titrant; 0.0141M (0.0141N): Dissolve 2.395g AgNO3 in distilled water and dilute to 1000ml. 1.00ml =0.5mg Cl. Store in a brown bottle.

Standard sodium chloride, 0.0141M (0.0141N): Dissolve 824.0mg NaCl in distilled water and dilute to 1000ml.

Procedure:
10 ml of the sample was taken into 250ml conical flask. Sample pH was adjusted to 7 to 10 with H or NaOH . 1.0ml K2CrO4 indicator solution was added. A titration was titrated with standard AgNO3 titrant to a pinkish yellow end point. AgNO3 titrant was standardized and established reagent blank value by the titration method. The indicator blank correction was not more than 0.03-0.1ml of silver nitrate and was deducted from the volume of silver nitrate used in titration. Then the titration was repeated with two further 10ml portions of NaCl solution.