EXPERIMENT NO: 1 DETERMINATION OF pH AIM: TO DETERMINE pH OF A GIVEN WATER SAMPLE INTRODUCTION: ‘The term pH refers to measure of hydrogen ion concentration in a solution and defined as the negative log of H’ ions concentration in water and wastewater. Values of pH, 0 to a little less than 7 are termed as acidic and values of pH a litle above 7 to 14 are termed as basic. When the concentration of H* and OH ions are equal then itis termed as neutral pHL. APPARATUS: pH meter, Beaker REAGENT: Buffer solutions of known pH value PROCEDURE: Three major steps are involved in the experiment. 1. Preparation of Reagents, 2. Calibrating the Instrument 3, Testing of Sample STEPS: * Perform calibration of pH meter using standard pH solutions. The calibration procedure would, depend on pHrange of interest. # Ina clean dry 100 ml beaker take the water sample and place it in a magnetic stirrer, insert the Teflon coatedstirring bar and stir wel. * Now place the electrode in the beaker containing water sample and check for the reading in pH meter, Wait untilyou get a stable reading. ‘© Take the electrode from the water sample, wash it with distilled water and then wipe gently with soft tissue. RESULT: pH of given water sample is, ENVIRONMENTAL SIGNIFICANCE: Determination of pH is one of the important objectives in biological treatment of the wastewater, In anaerobic treatment, if the pH goes below 5 due to excess accumulation of acids, the process is severely affected. Shifting of pH beyond 5 to 10 upsets the aerobic treatment of wastewater. In these eeecircumstances, the pH is generally adjusted by addition of suitable acid or alkali to optimize the treatment of the wastewater. pH value or range is of immense importance for any chemical reaction. A chemical shall be highly effective at a particular pH. Chemical coagulation, disinfection, water softening and corrosion control are governed by pH adjustment. Lower value of pH below 4 will produce sour taste and higher value above 8.5 a bitter taste. Higher values of pH hasten the scale formation in water heating apparatus and also reduce the germicidal potential of chlorine. High pH induces the formation of tri- halomethanes, which are causing cancer in human beings. Acidic solutions have pt Basic solutions have pH ‘alas less han 7 als greater than 7, eeeEXPEIMENT NO: 2 DETERMINATION OF ALKALINITIY & ACIDITY Al TO DETERMINE ALKALINITY OF A GIVEN WATER SAMPLE INTRODUCTION: Alki ity is primarily a way of measuring the acid neutralizing capacity of the water. In other words, its ability to maintain a relatively constant pH. The ability of natural water to act as a buffer is controlled in part by the amount of carbonate ion in solution. Carbonate ion and calcium ion both come from calcium igh levels of both carbonate or limestone. So water that comes in contact with limestone willscontain Ca” and CO ~ and have elevated hardness and alkalinity. PRINCIPLE: The alkalinity of water is a measure of how much acid it can neutralize. When a water sample that has a pH of greater than 4.5 is titrated with acid to a pH 4.5 end point, all OH", COs” and HCOs will be neutralized. For pH more than 8.3, add phenolphthalein indicator, the colour changes to pink colour. This, pink colour is due to presence of hydroxyl ions. If sulphuric acid is added to it, the pink colour di ippears ie. OH ions are neutralized. Then add mixed indicator, the blue colour appears. While adding acid, the colour changes to orange, this colour change indicates thatall the CO.” & HCOs has been neutralized. This is the end point. APPARATU! Burette, pipette, Conical flask, Beakers, Burette stand and Clamp CHEMICALS: Sodium carbonate, Standard Sulphuric acid, Phenolphthalein and Methyl orange indicator, Methyl red & Bromocresol green. PROCEDURE: ‘The procedure involves two phases. 1. Preparation of reagents 2. Testing of water sample PREPARTION OF REAGENTS: ‘The following reagents are required to be prepared, © Sulphuric acid solution (0.02 N) © Phenolpthalein Indicator Mixed Indicator Sulphuric acid solution (0.02 N) ‘Take 500 ml of distilled water in a 1000 ml standard flask. Exactly measure 28 ml of concentrated eeesulphuric acid andadd slowly along the sides of the standard flask. Then make up the volume up to the mark. The strength of this solution is 1 N. For preparing 0.02 N sulphuric acid solution, exactly measure 20 ml of 1 N solution and make up to1000 ml in a standard flask, Phenolphthalein Indicator For preparing 0.02 N sulphuric acid solutions, exactly measure 20 ml of IN solution and make up to 1000 ml in astandard flask. Weight 1 gm of phenolphthalein and add 100 ml of 95% ethyl alcohol or 100 ml of distilled water. Mixed Indicator Dissolve 100 mg bromocresol green and 20 mg methyl red in 100 ml 95% ethyl alcohol or 100 ml of distilled water. TESTING OF WATER SAMPLE: Using a measuring cylinder exactly measure 100 ml of sample and pour it in a 250 ml of conical flask. Fill the burettewith 0.02N sulphuric acid, Add few drops of phenolphthalein indicator to the conical flask. If the contents in the conical flask turns pink then titrate it against 0.02N sulphuric acid till the pink colour disappears. Note down the titrate value (V.). The value of titration is 0.5 ml. This value is used in calculating the phenolphthalein alkalinity. To the same solution in the conical flask add few drops of mixed indicator and the solution turns blue. Continue the titration from the point where stopped. Titrate Lill the solution become red. The entire volume (V2) of sulphuric acid noted down and is accountable in calculating the total alkalinity. Repeat the titration from concordant values. Burette solution: Sulphuric acid solutionPipette solution: Sample Indicator: Phenolphthalein Indicator, Mixed Indicator CALCULATION: Calculation of Phenolphthalein Alkalinity Burette solution: Sulphuric solutionPipette solution: Sample Indicator: Phenolphthalein Indicator End point: Disappearance of pink colour eeeSr.No. | Volume of sample (ml) Burette reading (ml) __| Vol. of 0.02N Sulphuric acid (ml) Initial Final Phenolphthalein Alkalinity= Vol of Sulphuric acid (V;) x Normality x 50 x 1000/ Vol. of sample taken Caleulation of Total Alkalinity Burette solution: Sulphuric acid solutionPipette solution: Sample Indicator: Mixed Indicator End point: Appearance of red colour Sr.No. | Volume ofsample(ml) | Burette (mi)__| Vol. of 0.02N Sulphuric acid (ml) Initial Final ‘ol of Sulphuric acid (V2) x Normality x 50 x 1000/ Vol. of sample taken ENVIRONMENTAL SIGNIFICANCE: Large amount of Alkalinity imparts bitter taste in water. The principal objection of alkaline water is the reactions that can occur between alkalinity and certain cations in water. The resultant precipitate can foul pipes and other accessoriesof water distribution systems. a. Chemical coagulation of water and waste water - to neutralize acids produced during flocculation, the sample should be alkaline as otherwise further floc formation slowly ceases. b. Corrosion control: to control the corrosion due to acids, natural water is rendered to alkaline, cc. Effluents of wastewater: wastewater containing excess caustic (hydroxide) alkalinity is not to be discharged into natural water bodies or sewers.Alkaline Water Science: Water pH vs. Alkali PH: Measures the concentration of hydrogen ions e ] Alkalinity: Measures the ability of the water to neutralize acid ed oss |Alkaline ionized water has higher alkalinity than regular water| Alkaline water can neutralize stomach acid, RESULT: ‘Total Alkalinity present in water sample is :EXPERIMENT NO: 3 DETERMINATION OF HARDNESS IN WATER AIM: TO DETERMINE HARDNESS OF GIVEN WATER SAMPLEINTRODUCTION: Hardness is caused by divalent metallic cations. The principal hardness causing cations are calcium, ‘magnesium, strontiun sulphates, carbonates, bicarbonates, chlorides and nitrates. The hardness of water varies considerably ferrous and manganese ions. The major anions associated with these cations are from place to place. In general, surface water is softer than groundwater. The hardness of water reflects the nature of the geological formations with which it has been in contact. The total hardness of water is defined as the sum of calcium and magnesium concentrations, both expressed as calcium carbonate, in mg/l. Hardness are of two types, temporary or carbonate hardness and permanent or non-carbonate hardness. Temporary hardness is one in which bicarbonate and carbonate ion can be precipitated by prolonged boiling. Non-carbonate ions cannot be precipitated or removed by boiling, hence the term permanent hardness. IS value for drinking water is 300 mg/l as CaCOs. APPARATUS: ‘50 ml Burette, 20 ml Pipette, 250 ml Conical flask, 100 ml Beaker, 250 ml beaker, Glassfunnel. REAGENTS: EDTA solution, Standard CaCO3 solution, Eriochrome Black~T indicator, Buffer solution. THEORY: EDTA (Ethylenediamine tetra acetic acid) forms colorless stable complexes with Ca” and Mg™ ions present in water at pH = 9-10. To maintain the pH of the solution at 9-10, buffer solution (NH,CI + NH.OH) is used. EriochromeBlack-T (E.B.T) is used as an indicator. The sample of hard water must be treated with buffer solution and EBT indicator which forms unstable, wine-red colored complexs with Ca and Mg” present in water. APPARATUS: © Beaker © Burewte © Pipette © Conical flask © Measuring cylinder eeePROCEDURE: 1. Standardization of EDTA ( Pipette out 20 ml of standard hard water into a conical flask. Gi) Add 5 ml of buffer solution and few drops of Eriochrome Black-T. The indicator, which is originally bluecolor would acquire a wine-red color. i) Titrate with EDTA solution taken in the burette, tll the wine red color changes to blue which is the endpoint. Let the burette reading of EDTA be V2 ml 2, Determination of Total hardness Repeat the above titration method for sample hard water instead of standard hard water. Let the burette reading ofDTA be Vs ml. 3. Determination of Permanent hardness Take 100 ml of sample hard water in 250 ml beaker. Boil it o remove temporary hardness to about half of this volume and cool to room temperature, Filter through filter paper to remove insoluble CaCOs and MgCOs. Make up the volume to the original 100 ml by adding distilled water. Now pipette out 20 ml of this solution into a clean conical flask. Then repeat the process of titration steps as mentioned above. Let the burette reading of EDTA be Vs ml. OBSERVATIONS: 1, Standardization of EDTA. Sr.No. | Volume of hard water taken | Burette reading (ml) | Vol. of EDTA consumed (V;) (ml) (m) Tnitial | Final 2. Determination of Total Hardness Sr.No. | Volume of hard water taken (ml) Vol. of EDTA consumed (V;) (ml) 3. Determination of Permanent Hardness Sr.No. | Volume of hard water taken Burette reading (ml) Vol. of EDTA consumed (V:) (ml) Initial Final (m)CALCULATIONS: 1, Standardization of EDTA M,Vi = MV2 Where, Mi = Molarty of standard hard water Vi = Volume of standard hard water in Molarity of EDTA V2= Volume of EDTA consumed (burette reading) 2 Determination of Total hardness MLV2= MsVs Where, My = Total hardness of sample water V, = Volume of sample hard water in conical flask 3. Determination of Permanent hardness M:V2 = MsVs Where, Mr Permanent hardness of sample water Va = Volume of sample hard water in conical flask Note: Multiply Ms and Mz with 105 to covert hardnessinto parts per million (ppm), 4. Determi hardness tion of Temporary hardness Temporary hardness = Total hardness - Permanent RESULT: ‘Total Hardness present is a water sample is, ENVIRONMENTAL SIGNIFICANCE: Hard water is as satisfactory for human consumption as soft waters. Because of their action with soap, however, their use for cleansing purpose is quite unsatisfactory, unless soap costs are disregarded. Soap consumption by hard waters represents an economic loss to the water user. Sodium soaps react with multivalent metallic cations to form a precipitate, thereby losing their surfactant properties. In recent years these problems have been largely alleviated by the developments of soaps and detergents that do not react with hardness. Boiler scale, the result of the carbonate hardness precipitation, may cause considerable economic loss through fouling of water heater and hot water pipes. Change in pH in the water distribution systems may also result in deposits of precipitates. Bicarbonates begin to convert to the less soluble carbonates at pH values above 9.0. Magnesium hardness, particularly associated with the sulfate ion has a laxative effect on persons unaccustomed to it. Magnesium concentrations of less than 50 mg/l ate desirable in potable waters, although many public water supplies exceed the amount. Calcium hardness presents no public health problem, In fact, hard water is apparently beneficial to the human cardiovascular system. eeeGrains/Gallon {mg/L & ppm Classification Less than 1 Less than 17.1 1103.5 17.1 0.60 3.5 t0 7.0 60 to 120 7.00 10.5 120 to 180 10.5 and over | 180 and over Noe - one gain per gallon = 17-1 parts per milion (ppm) eeeEXPERIMENT NO: 4 DETERMINATION OF CHLORIDE IN WATER AIM: TO DETERMINE CHLORIDE IN A GIVEN WATER SAMPLEINTRODUCTION: Chlorides occur in all natural waters in widely varying concentration, the chloride content normally increases as the mineral content increases. Chloride ion may be present in combination with one or more of the cations of calcium, magnesium, iron and sodium. Chlorides of these minerals are present in water because of their high solubility in water. Each human being consumes about six to eight grams of sodium chloride per day, a part of which is discharged through urine and night soil. Thus, excessive presence of chloride in water indicates sewage pollution. IS value for drinking water is 250 to 1000 mg/l METHOD: ‘The Mohr Method uses silver nitrate for titration (normality: 0.0141) (method applicability: 0.15 to 10 ‘mg/L chloride ions). This corresponds to 1 mi of 0.0141 equals to 1 mg chloride in solution. The silver nitrate solution is standardized against standard chloride solution, prepared from sodium chloride (NaC). During the titration, chloride ion is precipitated as white silver chloride (Eq.1): Ag’ + Cl <=> AgCl (Solubility product constant, Kip=3«10"") (Eq.1) The indicator (potassium chromate) is added to visualize the endpoint, demonstrating presence of excess silver ions. Inthe presence of excess silver ions, solubility product of silver chromate exceeded and it forms a reddish-brown precipitate (Eq.2). This stage is taken as evidence that all chloride ions have been consumed and only excess silver ions have reacted with chromate ions: 2Ag! + CrOP <=> AgiCrO* (Ky=5x10" n-o----= (Eq. 2) APPARATUS: —_Burette, conical flask, pipette, measuring eylinder. REAGENTS: Potassium chromate indicator solution, standard silver nitrate titrant. STEPS: 1, Take 25 ml sample in a conical flask. Measure sample pH. 2. Add 1.0ml potassium chromate indicator solution, 3. Titrate with standard silver nitrate solution to pinkish yellow end point and note down volume of titrant used.Also measure sample pH. 4. Calculate chloride ion concentration using Eq. ( Chloride fon Concentration (mg/L) Where: A= volume of titrant used, = (AXN %35.45)"1000 / Veanpie ------(Eq. 3) eeeN is normality of silver nitrate (here we used N/71 or 0.0141 N), andV sanpc is volume of sample used (ml). RESULT: Chloride present in water sample is ENVIRONMENTAL SIGNIFICANCE: Chlorides in reasonable concentrations are not harmful to human. At concentrations above 250 mg/l they give a salty taste to water, which is objectionable to many people. For this reason, chlorides are generally limited to 250 mg/ 1 in supplies intended for public use. In many areas of the world where water supplies are scarce, source be containing as much as 2,000 mg/l are used for domest development of adverse effects, once the human system becomes adapted to the water. purposes without the ‘wor ——e e-toc ae eeeEXPERIMENT NO: 5 TOTAL SOLIDS (TS) AIM: TO DETERMINE TOTAL SOLIDS OF GIVEN SAMPLE. PRINCIPLE: Total solids are determined by evaporating a well mixed sample and dried to constant weight in an oven at 103 to 105°C and weighing the dry residue left. The increase in final weight than the initial weight of crucible indicates total solids, APPARATU! Crucible, Muffle furnace, measuring cylinder, weight balance, oven, desiccators, PROCEDURE: Take the weight of empty crucible Take 50 ml of given water sample in a crucible. Evaporate the sample at 103 to 105°C for 24 hrs. Rep p Again ignite the crucible for 15-20 minutes in a muffle furnace whose temperature is maintained to 550°Cuntil the constant weight is attained. Cool it. 5. Note down the weight of crucible with residue. OBSERVATION: 1. Weight of empty crucible (B): gm 2. Weight of empty crucible with residue (A): gm. CALCULATION: Total solids (TS) mg/l = {(A-B) x 1000 x 1000} / ml of sample (V), where,A: Final weight of the crucible with residue in gm B: Initial weight of the empty crucible in gm.V: Volume of sample taken in ml. RESULT:- ‘The amount of total solids determined from the given water sample is mg/l. ENVIRONMENTAL SIGNIFICANCE: Total solids determination is used to assess the suitability of potential supply of water for various uses. eeeEXPERIMENT NO: 6 TOTAL SUSPENDED SOLIDS (TSS) AND TOTAL DISSOLVED SOLIDS (TDS: AIM: ‘TO DETERMINE TOTAL SUSPENDED SOLIDS FROM GIVEN SAMPLE. PRINCIPLE: The residue which remains on filter paper after filtration. The dry weight of this residue is termed as total suspendedsolids. APPARATU! ‘Whatman filter paper no. 44, measuring cylinder, weight balance, oven, desiccator, funnel, tripod stand. PROCEDURE: 1, Take a tripod stand and put it on the table to which funnel is placed. 2. Take initial weight of Whatman filter paper as (Wi) 3. Now place the Whatman filter paper three folded on the funnel Pour the well mixed sample on the Whatman filter paper. Wait for some time so as to drain out the water sample completely. awe Now remove the Whatman filter paper and keep it in the oven, Care should be taken to see that the filterpaper should not be scratched. 7. Now take the final weight of the filter paper along with residue as (Ws). OBSERVATIONS: 1. Initial weight of Whatman filter paper (W:): gm. 2. Final weight of Whatman filter paper with residue (W2): gem. CALCULATION: Total suspended solids (TSS) mg/l = { (W2-W:) x 1000 x 1000 } / ml of sample (V)where, Wr: Initial weight of filter paper in gm Wo: Final weight of filter paper with residue in gm V = Volume of Sample taken eelRESULT: ‘The amount of total suspended solids determined from the given water sample is mg/l ENVIRONMENTAL SIGNIFICANCE: 1. Suspended solid material may be objectionable in water. Organic suspended are degraded anaerobically mayrelease obnoxious odors. 2. Measures the quality of the wastewater influent and effluent. 3. Extremely valuable in the analysis of polluted waters. APPLICATION OF DATA: 1. To evaluate the strength of domestic wastewater. 2. To determine the efficiency of treatment units. CONCLUSIO! ‘The amount of total suspended solids determined from the given water sample is mei TOTAL DISSOLVED SOLIDS (TDS) ‘TDS (mg/l) = TS- TSS ENVIRONMENTAL SIGNIFICANCE: 1__TDS stands for total dissolved solids, and represents the total concentration of dissolved substances in water. 2. An elevated total dissolved solids (TDS) concentration is not a health hazard. The TDS concentration is a secondary drinking water standard and, therefore, is regulated because it is more of an aesthetic rather than a health hazard. 3. High concentration produces hard water, which leaves deposits and films on fixtures and on the insides of hot water pipes and boilers Total Dissolved Solids a in - ‘per million = =a al Se lee ute tis | tr “uel see cme ah sa sarees a eeeEXPERIMENT NO: 7 DISSOLVED OXYGEN ‘TO DETERMINE DISSOLVED OXYGEN OF GIVEN SAMPLE. PRINCIPLE: DO rapidly oxidizes the divalent manganous to its higher valency which forms a brown hydrated oxide precipitate after addition of NaOH and KI. In the presence of iodide ions in an acidic solution the oxidized ‘manganese reverts to the divalent state and liberates Iodine from KI equivalent to the original DO content. The liberated odine is then titrated against Sodium thiosulphate solution with starch as an indicator. MnSO; reacts with alkali to form white precipitate Mn(OH): thus indicating absence of oxygen in the sample, REACTION: Mn*™ + 2(OH') > Mn(OH): (white) Mn’** + 2(OH) + 1/2 O2—+ MnO> (brown)+H:OMnO: + 21-4 4H Mn*™ +12 +2H:0 APPARATUS: BOD bottles (capacity 300 ml), burette, pipettes, conical flask, burette stands, tile, measuring cylinder, weight balance,glass rod, beakers. REAGENTS: Kkler’s A solution: Dissolve 48 gm tetra hydrate manganous sulphate in 100 ml distilled water. Filter if necessary. 2. Winkler’s B solution Dissolve 50 gm of NaOH and 15 gm of KI in 100 ml distilled water. 3. Starch indicator: Make a paste of 2gm L.R grade soluble starch powder in distilled water. Pour this solution in 100 ml distilledwater. Boil for few minutes. Cool the solution and then use. 4. Concentrated sulphuric acid 5, Standard sodium thiosulphate solution: Dissolve 24.82 gm NasS2O; in distilled water and make up to 1 liter. It becomes 0.1N. Take 250 mil of thissolution and make up to | liter with distilled water to prepare 0,025N. eeePROCEDURE: 1. Collect the sample in 300ml BOD bottle. 2. Add 2ml of Winkler’s A solution and 2m! of Winkler’s B solution well below the surface through the walls. Stopper immediately to remove air bubbles and mix carefully by inverting bottle up and down. Allow the brown precipitate to settle down leaving clear supernatant. wae ‘Add cone. Sulphuric acid drop by drop till precipitate digested. Restopper the bottle and mix by inverting several times for complete dissolution. A yellow colored solution appears. ‘Take 50 ml samples in conical flask. ‘Add few drops of starch indicator and titrate against 0.025N Na:S:0; solution. 10. Note down the reading until the color changes from blue to colorless. SOURCE: 1. Drinking water. 2. Tap water. OBSERVATIONS: 1. Inburette: 0,025 N sodium thiosulphate solution, 2. In conical flask: 50 ml sample + indicator. 3. Indicator: starch, 4. |. End point: blue to colorless. OBSERVATION TABLE: ‘Srno. Source se Difference Average CALCULATION: DO (mg/l) = (Vx70)/u Where, ‘V= mil of titrant used for DO determination (B.R.)u = ml of water sample taken 70 = correction factor RESULT: ‘The amount of dissolved oxygen determined from the given sample is ENVIRONMENTAL SIGNIFICANCE: mg/l eee1, A minimum DO of 4 to 6 mg/l is desirable for the survival of aquatic life; higher values of DO may causecorrosion of iron and steel. 2. High temperature, biological impurities, ammonia, nitrites, ferrous iron, chemi hydrogen sulphideand organic matter reduces DO values. 3. Drinking water should be rich in DO for good taste. APPLICATION OF DATA: 1. It is necessary to know DO levels to assess the quality of raw water and to check on stream pollution. 2. DO testis basis for BOD test which is an important parameter to evaluate organic pollution potential of waste. 3. DO testis used to control oxygen in boiler feed water. 4, DO test is used to evaluate the pollution strength of domestic and industrial waste. 5. Determination of DO in waste water is useful to identify the nature of biochemical reactions ‘whether aerobic oranaerobic. Wea eect ae) OT aka cud e aed sea ea Water Quality Good DO (ppm) at 20°C Slightly polluted Moderately polluted Heavily polluted Gravely polluted CONCLUSION: The Dissolved Oxygen derived from the given water sample is eee