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Experiment no.

Aim: To Determine pH and acidity of given water sample.


Apparatus required: Digital pH meter

Chemicals Required: Buffer solutions of various pH.


pH is the negative log 10 of hydrogen ion concentration in a solution .pH meter employs two electrodes, an indicator glass electrode and a calomel reference electrode or may have a combined glass and reference electrode .pH meter also have a temperature compensation system to avoid the difference arising due to the different temperature. pH = - Log 10[H+] = Log10 1 [H+] Ionic product of water is 1x 10-14 at 250 C therefore neutral solution will have 1x10-7 ions of H+ and OH- each pH scale range from 0 to 14 with 7 as neutral ,below 7 being acid and above 7 as alkaline.

Principle:

Procedure:
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. Switch on the instrument. Dip the electrode in 7 pH buffer solution. Set the temperature electrode in accordance with temperature of buffer solution. Select the function switch to pH position and adjust calibrate Knob until the display precise pH value of buffer solution i.e. 7.00 pH. Now put function selector switch to stand by. Remove electrode from the buffer solution wash with distilled water. Dip the combined electrode in to another buffer solution of pH 4 value. Set the Temperature 0C control to the temperature of the selected buffer solution. Set the function selector switch to thepH position .Adjust slope correction knob until the display of pH value of selected buffer solution say 4.00 on display. Check that correct reading is obtained with both solutions without further adjustment. Remove the electrode from buffer solution, wash with distilled water and dip in the solution under test or given water sample. Set the Temperature 0C control to the temperature of test solution. Set function selector switch to the pH position. The instrument will display pH value of test solution. Note down the readings of the pH Meter.

Aim: Determination of Acidity.


Chemicals required:
1. Sodium hydroxide,0.05N 2. Methyl orange indicator 3. Phenolphthalein indicator

Glass wares Required: Burettes, pipettes, conical flask, Beakers, droppers, titration stand. Principle: Acidity of water is the capacity to neutralize a strong base to a fixed pH. It is caused by
the presence of strong mineral acid, weak acid, and hydrolysing salts, of strong acids. However in natural unpolluted fresh waters, the acidity is mostly due to the presence of free co2 in the form of carbonic acid. Acidity can be determined by titrating the sample with a strong base such as NaOH using methyl orange or phenolphthalein as indicator.

Procedure:
1. Take 100 ml of colourless sample in a conical flask and add 2-3 drops of methyl orange indicator. 2. If the solution turns yellow ,the methyl orange acidity is absent .In case the contents turns pink, titrate with 0.05 N NaOH . At the end point colour changes from pink to yellow. 3. Now add a few drops of the phenolphthalein indicator to the sample and titrate further with NaOH until the contents turn pink to yellow. 4. Now add a few drops of the phenolphthalein indicator to the sample and titrate further with NaOH until the contents turns pink.

Calculation:
Methyl Orange acidity (mg/l) as CaCO3 = AXN of NaOH X1000X50 Ml sample Phenolphthalein Acidity (mg/l) as CaCO3 = BXN of NaOH X1000X50 Ml sample Total Acidity to pH 8.3 = (A + B) XN of NaOH X1000X50 Ml sample A= volume of NaOH used with phenolphthalein in titrating the sample to pH 3.7. B= volume of NaOH used with phenolphthalein in titrating sample from pH 3.7 to pH 8.3.

Experiment No. Aim: Determination of alkalinity and its species.


Chemicals required:
1. 2. 3. 4. Hydrochloric acid (0.05%) Methyl orange indicator (0.05%) Phenolphthalein indicator Sodium carbonate.

Glasswares used: Burette, pipette, conical flask

Principle:
Total alkalinity is the measure of the capacity of the water to neutralize a strong acid. The alkalinity in the water is generally imparted by the salts of carbonates, bicarbonates, phosphates, nitrates, borates, silicates etc.togather with hydroxyl ions in Free State. Total alkalinity, carbonatesand bicarbonates can be estimated by titrating the sample with strong acid (Hcl/H2S04), first to pH 3 using phenolphthalein as an indicator and then further to pH between 4.2 and 5.4 with methyl orange .in first case the value is called as phenolphthalein alkalinity (PA) and in second case, it is called as total alkalinity (TA). Value of carbonates, bicarbonates and hydroxyl can be computed from these two types of alkalinity.

Procedure:
1. Take 100 ml of sample in Erlenmeyer flask and add 2 drops of phenolphthalein indicator. 2. If solution remains colourless then, PA=0, then total alkalinity is determined by adding 2-3 drops of methyl orange to sample and titrate it with 0.1N Hcl until colour changes to pink. This is the total alkalinity (TA). 3. If colour changes to pink after addition of the phenolphthalein, titrate it with 0.1N HCl until colour disappear at the end point .This is the phenolphthalein alkalinity.

4. Now add 2-3 drops of methyl orange to the same sample and continues the titration further until yellow colour changes to the pink colour at the end point .This is the total alkalinity (TA).

Calculation:
PA as CaCO3, mg/l = (A X Normality) of Hcl x !000x50 Ml of sample TA as CaCO3, mg/l = (B X Normality) of Hcl x !000x50 Ml of sample Where, A = ml of Hcl used with only phenolphthalein. B = ml of total Hcl used with phenolphthalein and methyl orange. PA = phenolphthalein alkalinity. TA = Total alkalinity.

Table: value of OH- ions, CO3-, HCO3- from the value of phenolphthalein and total alkalinity.
Result of titration P =o P < 1/2T P = 1/2T P > 1/2T P=T OH alkalinity CaCO3 0 0 0 2p - T T as CO3 alkalinity CaCO3 0 2P 2P 2(T-P) 0 as HCO3 alkalinity CaCo3 T T-2P 0 0 0 as

P = Phenolphthalein alkalinity T = Total alkalinity

Experiment No. Aim: Determination of solids: Total, dissolved and suspended.


Apparatus required =
1. 2. 3. 4. 5. 6. Hot Air Oven/ Hot plate Silica/ porcelain evaporating dish. Filtrations assembly Filter paper Crucible Beaker

1. Total solid: Principle:Total solids are determined as the residue left after evaporation of unfiltered sample.

Procedure:1. Take an evaporating dish of suitable size and weight. 2. Evaporate 250-500 ml unfiltered sample in the evaporating dish on a water bath. 3. Take the final weight of the dish after evaporation of the sample. Calculation: total solids g/l = A-BX 1000 V Where, A = Final weight of dish in (g). B = Initial weight of dish in (g). V = Volume of sample taken in ml.

Total dissolved solid:Principle: filtered sample. Total dissolved solids are determined as the residue left after evaporation of the

Procedure:1. Take an evaporating dish of suitable size and weight. 2. Evaporate 250 -500 ml filtered sample in evaporating dish on water bath. 3. Take final weight of dish after evaporation.

Calculation:TDS, g/l = Where, A-B X1000 V A = Final weight of dish in (g). B = Initial weight of dish in (g). V = Volume of sample taken in ml.

Total suspended solids (TSS):Determination of total suspended solids is done by taking difference between total solids and total dissolved solids.

TSS = TS-TDS.

Experiment No. Aim: - Determination of chlorides.


Chemicals required: - 1. Silver nitrate solution (0.02N)
2. Potassium chromate solution (5%)

Glassware: - flask, burette, beakers, pipettes, dropper. Principle:Silver nitrate reacts with chloride to form very slightly soluble white ppt. of AgCl.At the end point when all the chloride get precipitated free silver ions react with chromate to form silver chromate of reddish brown colour.

Procedure:
1. Take 50 ml of sample in Erlenmeyer flask. 2. Add 2 ml of k2 cr2 o4 solution. 3. Titrate against 0.02 N AgNO3 until persistent red tinge appears.

Calculation:Chlorides, mg/l = (ml X N ) of AgNO3 X1000 X35.5 ml of sample

Experiment no. Aim: - Determination of residual chlorine and chlorine dose. Chemicals required:1. 2. 3. 4. Glacial acetic acid Potassium iodide Sodium thio sulphate Starch indicator

Glass wares used:1. 2. 3. 4. Erlenmeyer flask (500ml) Measuring cylinder (5ml) Dropper Stirring Rod

Principle:Chlorine is primarily added to the waters for destroying harmful microorganisms. Presence of excess chlorine intensifies the taste and odour of many other compounds such as phenol etc. It may be harmful to many aquatic organisms in combination with ammonia. Chlorine is the strong oxidising agent and liberates iodine from potassium iodide .the liberated iodine is equivalent to the amount of chlorine and can be titrated against sodium thiosulphate using starch as an indicator

Procedure:1. Take 100ml of sample in an Erlenmeyer flask and add 5 ml of glacial acetic acid 2. Add approximately 1g of KI crystals and mix thoroughly with a stirring rod for about 15 minutes keeping it away from direct sunlight. 3. Add a few drops of starch indicator and titrate against 0.025 N sodium thio sulphate until the contents turns colourless from blue.

Calculation:Residual Chlorine .mg/l = ml x N of titrant x1000x35.5 Ml sample

Experiment No. Aim: - Determination of hardness (different types).


Chemicals required:1. 2. 3. 4. EDTA solution Buffer solution. Erichrome Black T Sodium sulphide solution

Principle: Hardness is generally caused by calcium and magnesium ion present in water .Polyvalent ions of some other metals like strontium, iron, aluminium, zinc and manganese etc are also capable of precipitating the soap and thus contributing to the hardness .however concentration of these ions is very low in natural waters, therefore hardness is generally measured as concentration of only calcium and magnesium as calcium carbonate, which are far higher in quantities over other hardness producing ions. Calcium and magnesium form a complex of wine red colour with Erichrome black T at pH 10.0 + 0.1. The EDTA has got a stronger affinity towards Ca++ and Mg++ therefore by addition of EDTA, the former complex is broken down and a new complex of blue colour is formed.

Procedure:1. Take 50-100ml of sample in a conical flask. 2. Add 1ml of buffer solution to it. 3. If sample is having higher amount of heavy metals Add 1 ml of Na2S solution. 4. Add 100-200mg of Erichrome Black T indicator the solution turns wine red. 5. Titrate the contents against EDTA solution .At the end point colour changes from wine red to blue.

Calculation:Hardness as mg/L CaCO3 = ml EDTA used X1000 ml sample

Calcium:Principle: Many indicators such as ammonium purpurate, calcon etc form a complex with only calcium but not with magnesium at higher pH. As EDTA is having a higher affinity towards calcium; the former complex is broken down and a new complex is formed .however EDTA has a property to combine with both Ca++ and Mg++therefore, magnesium is largely precipitated as its hydroxide at sufficient higher pH.

Requirements:1. EDTA solution 2. Sodium hydroxide solution 3. Murexide indicator.

Procedure:1. Take 50 ml of sample in Erlenmeyer flask. If the sample is having higher alkalinity, use smaller volume diluted to 50 ml. 2. Add 2 ml of NaOH solution in the sample. 3. Add 100-200mg of Murexide indicator, a pink colour develops. 4. Titrate against EDTA solution until pink colour changes to purple for better judgement of end point; compare the purple colour with distilled water blank titration.

Calculations:Calcium, mg/L = x X400.8 Mlofsample Where x = volume of EDTA used.

Magnesium:Calcium and magnesium form a complex of wine red colour with Erichrome Black T at pH 10.0.The EDTA has got a stronger affinity for Ca++ and Mg++; the former complex is broken down and a new complex of blue colour is formed .the value of mg++ can be obtained by subtracting the value of calcium from total of Ca++ and Mg++.

Calculation:Magnesium, mg/L = Y X = = (y- x) X400.8 Mlofsample EDTA used in hardness determination. EDTA used in calcium determination for same volume of the sample.

Mg++ =

Total Hardness- calcium hardness X 0.244.

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