Analytical Chemistry Laboratory (11-BS104)

Laboratory Notes

Dr. K. Rajasekhara Prasad J. V. Shanmukha Kumar

K L University
Green Fields, Vaddeswaram Guntur (Dist.)

2011-12

Acknowledgements

We take this opportunity to thank all those who helped directly and indirectly in bringing this Analytical Chemistry manual. We thank Dr. V. Srinivasa Rao, Smt. T. Anupama Rashmi, Dr.M. Ashok, Ms. Ch. Rekha Devi, Smt. A.L. Lavanya, and Ms. S. Prasanthi for their valuable help in bringing out this manual to this form.

AUTHORS

Preface

The following materials were expressly written for the quantitative analysis course, Engineering Chemistry (11-BS103) at K L University, Green Fields. The information provided in this laboratory manual is required by the student for the performance of the laboratory work which represents a major part of the analytical chemistry.

The objective of the laboratory manual is to provide conceptual understanding of the principles involved in experimental work. Learning objectives for each experiment is given in the beginning of the experiment in the manual. For each experiment, list of review questions are included. Answering to these questions ensures learning of the process in terms of its application. Students are expected to answer all the review questions and to enter their observations in the manual itself. Students will be working individually once a week. At the end of the semester, students are expected to familiarize completely for using all the facilities in the analytical lab.

Authors

Table of Contents Expt. No. 1 2 2.1 2.2 2.3 2.4 2.5 2.6 2.7 2.8 2.9 3 3.1 3.2 3.3 4 Name of the Experiment INTRO TO VOLUMETRIC ANALYSIS E.g. Determination of strength of NaOH WATER ANALYSIS (QUANTITATIVE ANALSIS) Estimation of Total Hardness of water by EDTA method Estimation of alkalinity of water Determination of acidity of water sample Estimation of Dissolved Oxygen in water Determination of free CO2 in water sample Determination of total residual chlorine in water Determination of BOD of water sample Determination of Cu by complexometry Determination of Calcium in milk powder POLYMERS Preparation of Urea Formaldehyde resin Preparation of Phenol Formaldehyde resin Preparation of Nylon 6:6 ELECTROCHEMICAL ANALYSIS a) Preparation of buffers and standardisation of pH meter b) Determination the molarity of acid pH-metrically, provided suitable base Acid-Base titration by conductometry Determination of Specific and Equivalent conductivities of solutions Page No. 6 12 39 12 16 20 23 26 28 31 34 36 40 45 40 42 44 46 - 55

4.1

46

4.2 4.3

50 53

Safety precautions
Eye protection (minimum chemical splash goggles) must be worn at all times in the laboratory. Do not work in the laboratory unless a demonstrator or teaching assistant is present. To protect clothing from chemical damage, wear a lab apron or lab coat. Never taste any chemical unless instructed to do so and do not allow chemicals to come in contact with your skin. Do not through waste such as match sticks, papers, etc. into the sink. They must be thrown into the dust bin. Keep the water and gas taps closed when utilities are needed. If chemicals splash into someones eyes, act quickly and get them into the eye wash. Do not wait for the instructor. Incase of injury (cut, fire, burn, etc) notify the instructor immediately. Always remember, hot glass ware looks exactly the same as cold glassware, be careful what you touch 100C = 212F (boiling point of water)

General Instructions
Read the laboratory experiment and any suggested additional reading(s), before coming to lab. Do the assigned pre lab, exercises (if any). These generally cover any calculations or important observations which needed to be made. Make a list of questions regarding the experiment. A simple question can save hours of time in the lab. All data should be recorded in an observation note book. Do not use sheets of paper or 3 ring binders, as these pages can be quickly lost. It is some times necessary to modify lab procedures on the day of lab to obtain better results. Be prepared to adopt these changes. Clean your glass ware at the end of the period so that it will be ready for the next class. Lab instructors will some times discuss the important aspects of the lab with students individually or in small groups in an effort to help them get more out of the experiment. Keep your ears alert and you may here something that will help you out. Reagent bottles must never be allowed to accumulate on the bench. They must be replaced on the reagent shelves immediately after the use. Never carry out unauthorized experiments in the laboratory. If you are not sure about what to do, please ask the instructor. Lastly, it is important to follow the safety DOS and DO NOTS of the laboratory not only for your own safety but also for your classmates. Report the dangerous lab practices of others, you will be doing them (and yourself) a big favour.

Introduction to Volumetric Analysis

Chemical Analysis: It involves either qualitative determination of a given substance for the elements or radicals or quantitative estimation of substance given for the amount of substance present. Thus chemical analysis involves quantitative and qualitative analysis. Qualitative analysis: It involves the determination of the elements or radicals or compounds present in the given substance by the way of chemical test or physical methods. Quantitative analysis: It involves the determination of the exact amount of the substance or element present in a given substance. It consists of two major parts. i) Volumetric analysis and ii) Gravimetric analysis. 1) Volumetric analysis: It is the quantitative determination of a given substance by the determination of the volume of the solution of another substance which reacts chemically and instantly with that substance. 2) Gravimetric analysis: It involves the quantitative determination of the substance by weight determination of suitable substance after a chemical reaction of given substance. Volumetric analysis consists essentially of determination of volume of solution of accurately known strength which is required to react quantitatively with the solution of another substance to be determined. The weight of the substance to be determined is calculated from the volumes of standard unknown solutions by using loss of chemical equivalence or stoichiometry. The process of adding one solution of known concentration to another solution until the reaction is just completed is known as titration. The solution of accurately known concentration is known as std. solution. It consists of a definite number of moles of solute per 1 lt of solution. The solution of unknown concentration or the solution which is to be estimated is known as test solution. The stage in a titration where the reaction is just completed is known as end point. The substance of solution which indicates endpoint is known as indicator.

Generally it indicates end points either by colour change or precipitate formation or by any visible change. Usually a third solution is also used which is complimentary to both standard as well as test solutions. That means if the standard and test solutions are basic, third solution should be an acid. Similarly first two solutions are reducing agents, third one is used as oxidizing agent. Such a solution is known as intermediate solution or link solution. For a given chemical reaction volumetric method is chosen only if it satisfies the following conditions: 1. There must be chemical reaction between substance to be estimated and standard solution in equivalent proportion. 2. The reaction employed should be simple and it should be expressed in the form of chemical equation. 3. The reaction between the substances should be instantaneous or very quick. 4. There should be some means to detect the completion of reaction. 5. Reactants or the products should not be volatile. 6. There should not be any side reactions. The standard solutions are prepared from a compound which is considered to be a primary standard. Primary standard should possess the following qualities. 1. 2. 3. 4. It must be available in very pure form. It should not be effected by air or moisture. It should be pure during storage. It should have a high equivalent weight so that relatively large sample can be used.

Classification of Volumetric Titrations Volumetric Methods are classified into four categories. 1. Acid- Base Titration Ex.:- Titration of NaOH Vs H2SO4 2. Redox Titration Ex.:- Titration of Mohrs Salt Vs KMnO4 3. Precipitation Titration Ex.:- Titration of NaCl Vs AgNO3 4. Complexometric Titration Ex.:- Titration of Hard water Vs EDTA 1. Acid- Base Titration: These are the titrations involving an Acid solution and a Base solution. The titrations give sharp end points. The pH of the titrant gradually changes during the titration and at the end point it sharply changes. Thus a sudden change in pH is generally observed at the end point. A substance which has its pH range matching to the pH range of the titration is chosen as the indicator. Thus the end point is detected by the colour change by the indicator chosen.

Eg:- Methyl orange is used as an indicator in a weak base Vs strong acid titration where it shows colour change from pale yellow to pale pink at the end point. However, weak base Vs weak acid titrations are not performed. 2. Redox Titration: These are the titrations involving a reducing agent and an oxidising agent. The titrations give sharp end points. The redox potential of the titrant gradually changes. During the titration at the end point it sharply changes. Thus a sudden change in redox potential is generally observed at the end point. A substance which has its redox potential change matching with that of the titration is chosen as indicator. Thus the end point is detected by the colour change shown by the indicator chosen. Eg:- Diphenyl amine is used as an indicator in the estimation of Mohrs salt by using K2Cr2O7 where it shows colour change from colourless to bluish violet at the end point. 3. Precipitation Titration: These are the titrations involving a precipitate formation. Generally one of the products is insoluble in the solution and these precipitate a proper substance is chosen as an indicator. Eg:- Titration of Chloride ions using AgNO3 solution using Potassium chromate as an indicator. The colour change is from pale yellow to brick red at the end point. Silver chloride is the precipitate formed in the reaction. 4. Complexometric Titration: These are the titrations involving the formation of a complex. Generally one of the products is a water soluble complex. A proper substance is selected as the indicator. Eg:- Titration of the hard water against EDTA solution using EBT indicator. The colour change is from wine red to blue. Ca-EDTA complex and Mg EDTA complex are the complexes formed in the reaction.

Expt. No:

Date: ...

DETERMINATION OF STRENGTH OF NaOH Learning objectives: To learn about: the role of phenolphthalein in an acid base titration the amount of NaOH in a given solution.

Aim: Find the strength in g/L of given NaOH solution with the help of standard sodium carbonate solution (N/10) and intermediate solution of an acid. Chemicals required: A standard solution of 0.1 N Na2CO3 and HCl solution having approximate normality N/10. Apparatus required: Burette, pipette, 2 beakers, conical flask. Theory: The experiment involves two titrations. Part A: Standardisation of HCl solution: In the first titration, HCl (which is a secondary standard), is titrated against Na2CO3 to determine its exact normality. Rinse and fill the burette with the given HCl solution. Pipette out 10 ml of Na2CO3 in a conical flask and add a few drops of methyl orange. The solution turns orange colour. Titrate it with the HCl solution till a permanent red colour is obtained. Repeat the titrations to get 3 concordant readings. 2 HCl + Na2CO3 2 NaCl + H2O + CO2 Part B: Estimation of NaOH solution: Once the normality of HCl is known, the normality of given NaOH can be determined by titrating it with HCl using phenolphthalein indicator. Pipette out 10 ml of NaOH solution in a clean conical flask. Add a few drops of phenolphthalein indicator. The solution will turn pink. Titrate the NaOH solution with the HCl solution taken in the burette till the pink colour disappears. Repeat the titrations to get 3 concordant readings. HCl + NaOH NaCl + H2O

Observations: Part A: Standardisation of HCl solution: S.No. Volume of the solution taken in conical flask (ml) Burette Readings Initial reading (ml) Final reading (ml) Volume of the HCl solution used (ml)

1. 2. 3. Volume of the acid used = ------------ ml Use Normality equation and explain the terms clearly. Normality of HCl solution =

Calculation:

Part B: Estimation of NaOH solution: S.No. Volume of the solution taken in conical flask (ml) Burette Readings Initial reading (ml) Final reading (ml) Volume of the HCl solution used (ml)

1. 2. 3.

Volume of the acid used = ------------ ml Use Normality equation and explain the terms clearly. 10

Normality of NaOH solution = Calculation:

Strength of NaOH solution = Normality of NaOH x Eq. wt of NaOH = = Result: The strength of the given NaOH solution = ------------------ g/L Review Questions: 1. 2. 3. 4. 5. HCl is a primary standard or a secondary standard? Explain? Why anhydrous Na2CO3 is considered as primary standard? How an exact N/10 solution of NaOH can be prepared? Give the structure of phenolphthalein and Methyl orange? Apply modern quinoid theory to explain the action of phenolphthalein and methyl orange?

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Expt. No. .

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ESTIMATION OF HARDNESS OF WATER BY EDTA TITRATION METHOD (COMPLEXOMETRY) Learning Objectives: To learn about: Aim: To determine the total hardness of water using EDTA. Apparatus Required: Pipette, Burette, Conical flask, Wash bottle, Glazed tile. Chemicals Required: a) b) c) d) e) Standard Zinc salt solution EDTA solution Water sample Ammonium and Ammonium chloride buffer solution Eriochrome black T indicator Understand the hardness different types of hardness complexometric titrations structures of complexes formed in this titration role of buffer solution & EBT indicator

Theory: The method is based upon the fact that Ethylene diamine tetra acetic acid forms stable complex compounds with all metals particularly with di and polyvalent metals. For all practical purposes the hydrated disodium salt of the reagent is used which has the following formula: NaOOC H2C CH2COOH

N CH2 CH2 N HOOC H2C CH2COONa 12

When hard water is titrated against EDTA solution it forms stable complexes with Calcium and Magnesium ions in water. The titration is carried out in presence of EBT indicator at pH 10. It forms weak wine red coloured complexes with few of Calcium and Magnesium ions in water. When an excess drop of EDTA is added colour changes to blue.

M2+ + EBT -------------------------- M- EBT

Wine- red complex

M2+ + EDTA --------------------- M- EDTA

Stable- colourless complex

M-EBT + EDTA ----------------- M-EDTA + EBT

Wine red Blue

(M = Ca or Mg) Procedure:A) Standardisation of EDTA:Pipette out 10 ml of standard Zinc salt solution into a 250 ml conical flask. Add 2 ml of Ammonia and Ammonium chloride buffer solution and 2 to 3 drops of Eriochrome black- T indicator. Solution turns wine red in colour. Titrate with EDTA from the burette till the colour changes to blue. Note the final burette reading. Repeat the procedure until two concurrent readings are obtained. B) Determination of total hardness of water:Pipette out 50 ml of water sample into a conical flask. Add 2 ml of Ammonia and Ammonium chloride buffer solution and 2 to 3 drops of Eriochrome black T indicator. The solution becomes wine red in colour. Titrate with EDTA solution from the burette till the solution becomes blue. Note the final burette reading. Repeat the procedure until two concurrent readings are obtained.

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Observations and Calculations:A) Standardisation of EDTA:Molarity of Zinc salt solution M1 =

S.No.

Volume of Zinc salt solution V1 10 ml 10 ml 10 ml

Burette Readings

Volume of EDTA solution (b-a), V2

Initial (a) 1. 2. 3.

Final (b)

Use equation in terms of Molarity. Explain the terms clearly.

Molarity of EDTA solution =

Calculation:

B) Determination of Total hardness of water:Molarity of EDTA =

S.No.

Volume of water sample V3 50 ml 50 ml 50 ml

Burette Readings

Volume of EDTA solution (b-a), V4

Initial (a) 1. 2. 3.

Final (b)

14

1000 ml of 1M EDTA = 100 gms of CaCO3 V4 ml of M2 EDTA = V4 M2 100/ 1000grams of CaCO3 = --------- grams of CaCO3 50 ml of water contains = V4M2 100/ 1000 grams of CaCO3 = ------- grams of CaCO3 1000 ml of water contains = (1000 X) / 50 grams of CaCO3 = -------- grams of CaCO3 = -------- x 103 mg of CaCO3 = -----------Therefore, hardness of the given water sample = ------------ ppm of CaCO3

Calculation:

Result:Total hardness of given water sample is ..ppm of CaCO3 Review Questions: 1. 2. 3. 4. 5. 6. 7. 8. What is hardness of water? What are soaps? Why hard water does not lather with soap? What are carbonate and non-carbonate hardness? How hardness of water is expressed? What are the various units of hardness and how they are related to each other? What is EDTA? In what form EDTA is used? Give its structure? How does EBT acts as an indicator? What are the disadvantages of hard water?

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Expt. No..

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TO DETERMINE ALKALINITY OF A GIVEN WATER SAMPLE Learning Objectives: To learn about: the alkalinity species responsible for alkalinity different types of alkalinity role of methyl orange and phenolphthalein indicators in titration ill effects of alkalinity

Aim: To determine alkalinity of a given water sample. Theory: The knowledge of alkalinity of water is necessary for controlling the corrosion, in conditioning the boiler feed water (internally), for calculating the amounts of lime and soda needed for water softening and also in neutralizing the acidic solution produced by the hydrolysis of salts. In boilers fro steam generation, high alkalinity of water may not only lead to caustic embrittlement but also to the precipitation of sludges and deposition of scales. The alkalinity of water is due to the presence of hydroxide ion (OH -), carbonate ion (CO32-) and bicarbonate ion (HCO3-) present in the given sample of water. These can be estimated separately by titration against standard acid, using phenolphthalein and methyl orange as indicators. The chemical reaction involved can be shown by the equations given below: (i) (ii) (iii) [OH-] + [H+] H2O [CO32-] + [H+] [HCO3-] P M

[HCO3-] + [H+] H2O + CO2

The titration of the water sample against a standard acid upto phenolphthalein end-point shows the completion of reactions (i) and (ii) only. This amount of acid used thus corresponds to hydroxide plus one half of the normal carbonate present. The titration of the water sample against a standard acid to methyl orange end-point marks the completion of reaction (i), (ii) and (iii). Hence the amount of acid used after the phenolphthalein end-point corresponds to one half of normal carbonate plus all the bicarbonates; while the total amount of acid used represents the total alkalinity (due to hydroxide, bicarbonate and carbonate ions).

16

The possible combinations of ions causing alkalinity in water are: (i) OH- only, CO32- and HCO3 - only. (ii) OH- and CO32-, CO32- and HCO3 - together (iii) The possibility of OH- and HCO3 - ions together is not possible since they combine to form CO32- ions. OH- + HCO3 - CO32- + H2O Apparatus required: Burette, Pipette, conical flask, measuring flask, N/10 HCl, Phenolphthalein indicator, Methyl orange indicator. Procedure: Pipette out 20 ml of water sample into a conical flask. Add 1-2 drops of phenolphthalein. Rinse and fill the burette with N/10 HCl. Titrate the water sample in conical flask with N/10 HCl till the pink colour just disappears. Note down the reading and repeat to get three concordant readings. Again take 20 ml of the water sample in conical flask and add methyl orange indictor to it. Titrate it using N/10 HCl till a red colour is obtained. Record the observation and repeat to get three concordant readings. Observations: (a) Using Phenolphthalein: Normality of the acid used = N/10 S.No. Volume of the Burette Readings solution taken in titration flask Initial reading Final reading (ml) (ml) (ml) Volume of the titrant used (ml)

1. 2. 3. Volume of the acid used = ----------- ml

17

(b) Using Methyl Orange Normality of the acid used = N/10

S.No.

Volume of the Burette Readings solution taken in titration Initial reading Final reading flask (ml) (ml) (ml)

Volume of the titrant used (ml)

1. 2. 3. Calculations i) Phenolphthalein alkalinity in terms of CaCO3 equivalents: Use Equation in terms of Normality. Explain the terms clearly Concentration of water = Strength in terms of CaCO3 equivalents = Normality of water x Eq. wt of CaCO3 = Phenolphthalein alkalinity (P) = --------- X 1000 mg/L = ---------- X 1000 ppm. ii) Methyl orange alkalinity in terms of CaCO3 equivalents: Use Equation in terms of Normality. Explain the terms clearly Concentration of water = Strength in terms of CaCO3 equivalents = Normality of water x Eq. wt of CaCO3 = Methyl orange alkalinity or total alkalinity of water sample = ------- X 1000 mg/L = ------- X 1000 ppm

18

Calculation:

Result: Phenolphthalein alkalinity = ------------- ppm Methyl orange alkalinity = ------------ ppm Review Questions: 1. What is the significance of determining alkalinity in water? 2. Explain the action of phenolphthalein as an acid base indicator? 3. Why phenolphthalein is not a suitable indicator for titrating a weak base like NH4OH against a strong base? 4. How does methyl orange function? 5. Why methyl orange cannot be used as indicator for titrating weak acid, like acetic acid against a strong base?

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Expt. No..

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DETERMINATION OF ACIDITY OF WATER SAMPLE Learning Objectives: To learn about the acidity different types of acidity role of methyl orange and phenolphthalein indicators in titration ill effects of acidity

Aim: To determine the acidity of water sample. Apparatus Required: Pipette, Burette, Conical flask, Wash bottle, Glazed tile. Chemicals Required: NaOH, Methyl orange, phenolphthalein, and Na2S2O3. Theory: Measurement of acidity is important as acidic waters are corrosive and corrosion producing substances have to be controlled or removed. If the acidic waters are used for steam generation in boilers it results in corrosion and decreased efficiency of boiler. For mineral acids, the titration is carried to a pH of about 4.5 by using methyl orange indicator, giving a colour change from red to yellow. The acidity thus determined is called methyl orange acidity. Total acidity or phenolphthalein acidity is determined by carrying the titration to phenolphthalein end point of 8.3 (measuring mineral acids, organic acids and free CO2). The results are expressed as parts of equivalent CaCO3 per million parts of water. HCl + NaOH NaCl + H2O CH3COOH + NaOH CH3COONa + H2O CO2 + 2NaOH Na2CO3 + H2O

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Procedure: Phenolphthalein acidity: 1. Rinse and fill the burette with given normal NaOH solution. 2. Pipette out 100ml of the water sample in a conical flask and add drop of N/10 Na2S2O3 solution to destroy any residual chlorine. 3. Add 2-3 drops of phenolphthalein 4. Titrate the solution with NaOH solution till the appearance of pink colour. 5. Note the reading and repeat to get atleast three concordant readings. Methyl Orange Acidity: 1. Pipette out 100ml of the water sample in a conical flask and add one drop of N/10 Na2S2O3. 2. Add a few drops of methyl orange and titrate the solution with NaOH solution from the burette till the solution turns yellow. 3. Record the reading and repeat to get three concordant readings. Observations: Volume of water sample taken for each titration = 100ml Normality of NaOH solution = (c) Using Phenolphthalein: S.No. Volume of the solution taken in titration flask (ml) Burette Readings Initial reading (ml) Final reading (ml) Volume of the titrant used (ml)

1. 2. 3. Volume of the base used = (d) Using Methyl Orange

S.No.

Volume of the Burette Readings solution taken in titration Initial reading Final reading flask (ml) (ml) (ml)

Volume of the titrant used (ml)

1. 2. 3. 21

Volume of the base used = Calculations i) Phenolphthalein acidity in terms of CaCO3 equivalents: Use Equation in terms of Normality. Explain the terms clearly Concentration of water = Strength in terms of CaCO3 equivalents = Normality of water x Eq. wt of CaCO3 = Phenolphthalein acidity (P) = --------- X 1000 mg/L = ---------- X 1000 ppm. ii) Methyl orange acidity in terms of CaCO3 equivalents: Use Equation in terms of Normality. Explain the terms clearly Concentration of water = Strength in terms of CaCO3 equivalents = Normality of water x Eq. wt of CaCO3 = Methyl orange acidity or total acidity of water sample = ------- X 1000 mg/L = ------- X 1000 ppm Calculation:

Result: Phenolphthalein acidity = ------------- ppm Methyl orange acidity = ------------ ppm Review Questions: 1. What is source of Acidity in water? 2. What are the disadvantages of acidic water? 22

Expt. No. .

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DETERMINATION OF DISSOLVED OXYGEN IN THE GIVEN WATER SAMPLE Learning Objectives: To learn about: dissolved oxygen role and amount of dissolved oxygen iodometric titration role of starch indicator role of different reagents used in this titration

Aim: Determination of dissolved oxygen in the given water sample. Apparatus: Burette, Pipette, Conical flask, Beakers etc. Chemicals: Na2S2O3(N/40), MnSO4 solution, KI, Starch, Conc. H2SO4 Theory: Oxygen itself is not a pollutant in water, but its deficiency is an indicator of several types of pollution in water. Dissolved oxygen (DO) is determined by Winklers method or iodometric titration. The dissolved oxygen in water oxidizes KI and an equivalent amount of Iodine is liberated. This Iodine is titrated against a standard Hypo solution. However, since dissolved oxygen in water is in molecular state and is not capable of reacting with KI, therefore an oxygen carrier such as Manganese hydroxide is used. The method involves introducing a concentrated solution of MnSO4, NaOH, KI and azide reagent into the water sample. The white precipitate of Manganese hydroxide, which is formed is oxidized by oxygen in the water sample to give a brown precipitate of basic manganic oxide. This Manganic oxide in acidic medium dissolves and liberates free iodine from the added KI in an equivalent amount of dissolved oxygen in water sample. This liberated iodine is then titrated against hypo solution using starch as indicator. 23

Procedure: 1. 2. A known amount of sample water (250 ml) is taken in a stoppered bottle avoiding contact with air. Add 0.2 ml of manganese sulphate solution to it by means of a pipett, dipping the end well below the surface of water. Also add 2 ml of alkaline iodide- azide solution to it. Stopper the bottle and shake thoroughly. Allow the brown precipitate of manganic oxide formed, to settle down. When some portion of the liquid below the stopper is clear, add 2 ml of conc. H2SO4 with the help of pipette. Stopper and mix till the precipitate is completely dissolved. The characteristic brown colour of iodine is produced. Transfer 100 ml of the above solution into a 250 ml flask with a pipette. Titrate the liberated iodine with standardized sodium thiosulphate solution until the sample solution becomes pale yellow. Add 2 ml of starch solution. The solution will turn blue. Continue titration till the blue colour disappears. Repeat to get another reading.

3. 4.

5.

6. 7. 8.

Observations:Volume of the water sample taken for titration = 100 ml Observation Table Normality of Hypo =

S.No.

Volume of the solution taken in the titration flask (ml)

Burette Readings

Volume of the titrant used

Initial (a) 1. 2. 3. Calculations:Use equation in terms of Normality and Explain the terms. Concentration of Dissolved oxygen water sample =

Final (b)

24

Calculation:

Strength of dissolved oxygen in water = Concentration of water sample x eq. weight = ---------- x 8 gms per litre = --------------- ppm

Result: The amount of dissolved oxygen in water =

Review Questions: 1. State Henrys law for the solubility of a gas in a liquid? Outline the conditions under which the law is applicable? 2. Is dissolved oxygen necessary? 3. What is the effect of the presence of oxidizing impurities like NO2- and Fe3+ (if not removed) on the DO results? 4. How excess of Fe3+ can be removed? 5. How do reducing impurities such as Fe2+, SO32- and S2- effect the DO determination? 6. Why starch solution is added near the end point? 7. Why is the Na2S2O3 solution of N/40 strength selected for titration? 8. What are iodometric titrations? 9. Give the ionic equation showing reducing property of sodium thiosulphate? 10. With the help of above equation, find out the equivalent weight of sodium thiosulphate?

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Expt. No. .

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DETERMINATION OF FREE CO2 IN WATER SAMPLE Learning Objectives: To learn about: Formation of dissolved CO2 in water Effects of dissolved CO2 Removal of dissolved CO2

Aim: To determine free CO2 in a given water sample Apparatus Required: Burette, Pipette, Conical flask, Measuring flask. Chemicals Required: Water sample, Standard Na2CO3 solution, phenolphthalein indicator Theory: The CO2 content of a water sample is important as it contributes to the corrosion. Most natural waters contain dissolved CO2. It may enter water by absorption from atmosphere or may be produced by biological oxidation of organic matter with which water has been in contact, e.g., C6H12O6 + 6O2 6CO2 + 6H2O C6H12O6 2C2H5OH + 2CO2 CO2 is to be removed from municipal water supplies by aeration or by neutralization with lime; the choice of the method depends upon the amounts of free CO2 present in the sample. Free CO2 can be determined by titrating with a standard solution of NaOH or Na2CO3 with which it reacts to given NaHCO3 : CO2 + 2OH- CO32- + H2O CO2 + CO32- + H2O 2HCO3The completion of the reaction is indicated by the appearance of pink colour by using phenolphthalein as indicator. Procedure: 1. Pipette out 25ml of given water sample in a 250ml conical flask.

26

2. Add 2-3 drops of phenolphthalein indicator (presence of pink colour indicates the absence of CO2) and titrate against Na2CO3 solution until the pink colour persists for at least 30 seconds. 3. Take atleast 3 concordant readings and record the volume. OBSERVATIONS AND CALCULATIONS: Volume of water sample taken for each titration = 25ml. S.No. Volume of the water sample (ml) Burette Readings Volume of titrant (ml)

Initial (a) 1. 2. 3. Volume of Na2CO3 Solution used =

Final (b)

Use Normality equation and explain the terms clearly. Calculation:

Therefore, normality of the sample w.r.t CO2 = Strength Free CO2 Result: Amount of free CO2 present in given water sample = Review Questions: 1. What are the disadvantages of Dissolved CO2 in water? 2. How CO2 gets dissolved in water? 3. How Dissolved CO2 is removed? 4. How Carbon dioxide is formed during biological oxidation of organic matter? 27 = =

Expt. No..

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DETERMINATION OF TOTAL RESIDUAL CHLORINE IN WATER Learning Objectives: To learn about: Measure of the potability of water Role of chlorine in water purification How and why the Safe Water System project recommends testing of free chlorine

Aim: To determine the amount of total residual chlorine present in the given samples of chlorinated water by starch iodide method. Apparatus Required: Burettes, Pipettes, Erlenmeyer flask, Glazed tile, beakers. Chemicals Required: Concentrated glacial acetic acid, Potassium iodide, Starch indicator, Iodine solution 0.025N, Standard sodium thio sulphate solution (0.025 N). Theory: Chlorination of water supply is done to destroy or deactivate disease-producing micro-organisms. It will also improve the quality of water by reacting with ammonia, iron, manganese, sulphide and some organic substances. The residual chlorine is maintained in water to promote the primary purpose of chlorination. This method of determination depends upon the oxidising power of free and combined chlorine residuals. Chlorine will liberate free iodine from potassium iodide solution at pH 8 or less. The liberated iodine is titrated against standard sodium thiosulphate solution using starch indicator. Procedure: 1. 2. 3. 4. Take 25 ml of sample in an Erlenmeyer flask. Add 5 ml acetic acid to bring pH in the range 34. Add 1g of potassium iodide and mix thoroughly. Titrate with 0.025 N sodium thio sulphate solution until a pale yellow colour is obtained. 5. Add 1mL of starch solution and titrate until the blue colour disappears. Note down the volume of sodium thio sulphate solution added (V1). 6. Take a volume of distilled water corresponding to the sample used. Add 5 ml acetic acid, 1 g potassium iodide and 1mL starch solution. 28

7. If blue colour occurs, titrate with 0.025 N sodium thio sulphate solution until the blue colour disappears. Record the volume of sodium thiosulphate solution added (A1). 8. If no blue colour occurs, titrate with 0.025 N iodine solution until the blue colour appears (A2). Then titrate with 0.025 N sodium thiosulphate solution till the blue colour disappears. Record the volume of sodium thiosulphate solution added (A3). Note down the difference between the volume of iodine solution and sodium thiosulphate as A4. OBSERVATION AND CALCULATIONS: Chlorinated sample vs. Standard sodium thiosulphate solution (0.025 N) S.No. Volume of the water sample (ml) Burette Readings Volume of titrant (ml)

Initial (a) 1. 2. 3.

Final (b)

Distilled water vs. Standard sodium thiosulphate solution (0.025 N) S.No. Volume of the water sample (ml) Burette Readings Volume of titrant (ml)

Initial (a) 1. 2. 3.

Final (b)

Distilled water vs. Standard iodine solution (0.025N) S.No. Volume of the water sample (ml) Burette Readings Volume of titrant (ml)

Initial (a) 1. 2. 3.

Final (b)

29

Calculation

Residual chlorine in mg/L =

(V A1) or (V + A4) x N x 35.46 x 1000 mL of sample

=..........

Result Amount of total residual chlorine present in given water sample = Review Questions: 1. 2. 3. 4. 5. What is total residual chlorine? Why chlorine is added to water? What are the disadvantages of excess of chlorine present in water? What is the action of chlorine on pathogens? Why and how pH is adjusted between 3 and 4?

30

Expt. No..

Date:

DETERMINATION OF B.O.D OF WATER SAMPLE Learning Objectives: Gauge of the effectiveness of wastewater treatment plants. How far the source of water is polluted.

Aim: To determine the amount of B.O.D. exerted by the given sample(s). Apparatus Required: B.O.D. bottles 300mL capacity, B.O.D. incubator, Burette, Pipette, Air compressor, Measuring cylinder etc. Chemicals Required: Distilled water, Phosphate buffer solution, Magnesium sulphate solution, Calcium chloride solution, Ferric chloride solution, acid and alkali solution, Seeding, Sodium sulphite solution, Reagents required for the determination of D.O. Theory: The Biochemical Oxygen Demand (B.O.D.) of sewage or of polluted water is the amount of oxygen required for the biological decomposition of dissolved organic matter to occur under aerobic condition and at the standardised time and temperature. Usually, the time is taken as 5 days and the temperature 20C as per the global standard. The B.O.D. test is among the most important method in sanitary analysis to determine the polluting power, or strength of sewage, industrial wastes or polluted water. It serves as a measure of the amount of clean diluting water required for the successful disposal of sewage by dilution. The test has its widest application in measuring waste loading to treatment plants and in evaluating the efficiency of such treatment systems. The test consists in taking the given sample in suitable concentrations in dilute water in B.O.D. bottles. Two bottles are taken for each concentration and three concentrations are used for each sample. One set of bottles is incubated in a B.O.D. incubator for 5 days at 20C; the dissolved oxygen (initial) content (D1) in the other set of bottles will be determined immediately. At the end of 5 days, the dissolved oxygen content (D2) in the incubated set of bottles is determined. Then, mg/L B.O.D. = (D1 D2 ) P

31

where, P = decimal fraction of sample used. D1 = dissolved oxygen of diluted sample (mg/L), immediately after preparation. D2 = dissolved oxygen of diluted sample (mg/L), at the end of 5 days incubation.

Among the three values of B.O.D. obtained for a sample select that dilution showing the residual dissolved oxygen of at least 1 mg/L and a depletion of at least 2 mg/L. If two or more dilutions are showing the same condition then select the B.O.D. value obtained by that dilution in which the maximum dissolved oxygen depletion is obtained. Procedure: 1. Place the desired volume of distilled water in a 5 litre flask (usually about 3 litres of distilled water will be needed for each sample). 2. Add 1mL each of phosphate buffer, magnesium sulphate solution, calcium chloride solution and ferric chloride solution for every litre of distilled water. 3. Seed the sample with 12 mL of settled domestic sewage. 4. Saturate the dilution water in the flask by aerating with a supply of clean compressed air for at least 30 minutes. 5. Highly alkaline or acidic samples should be neutralised to pH 7. 6. Destroy the chlorine residual in the sample by keeping the sample exposed to air for 1 to 2 hours or by adding a few mL of sodium sulphite solution. 7. Take the sample in the required concentrations. The following concentrations are suggested: Strong industrial waste : 0.1, 0.5 and 1 per cent Raw and settled sewage : 1.0, 2.5 and 5 per cent Oxidised effluents : 5, 12.5 and 25 per cent Polluted river water : 25, 50 and 100 per cent 8. Add the required quantity of sample (calculate for 650 mL dilution water the required quantity of sample for a particular concentration) into a 1000 mL measuring cylinder. Add the dilution water up to the 650mL mark. 9. Mix the contents in the measuring cylinder. 10. Add this solution into two B.O.D. bottles, one for incubation and the other for determination of initial dissolved oxygen in the mixture. 11. Prepare in the same manner for other concentrations and for all the other samples. 12. Lastly fill the dilution water alone into two B.O.D. bottles. Keep one for incubation and the other for determination of initial dissolved oxygen. 13. Place the set of bottles to be incubated in a B.O.D. incubator for 5 days at 20C. Care should be taken to maintain the water seal over the bottles throughout the period of incubation. 14. Determine the initial dissolved oxygen contents in the other set of bottles and note down the results. 15. Determine the dissolved oxygen content in the incubated bottles at the end of 5 days and note down the results. 16. Calculate the B.O.D. of the given sample. 32

OBSERVATIONS: Sample Concentration No. Dissolved Oxygen content in mg/l B.O.D. in mg/l (5days 200C) Initial (D1) Final (D2) Bottle D.O. Bottle D.O. No. Value No. Value

Note: B.O.D. value in mg/l = (D1-D2)/P If concentrations is 0.1%, then P= (0.1/100=0.0001) and so on.
Sample Calculation

D1 = Initial Dissolved Oxygen = ...... mg/L D2 = Dissolved Oxygen at the end of 5 days = ...... mg/L P = Decimal fraction of sample used = ...... (D1 D2 ) P

Therefore, mg/L of B.O.D. =

= ......

Result: B.O.D in Mg/l (5days 200C) = Review Questions: 1. 2. 3. 4. What do you mean by B.O.D? What is BOD5 test? What is the significance of B.O.D determination? Why bad odour is developed in water if insufficient dissolved oxygen is present in water? 5. Give the formula to be applied for determining the BOD of a sewage water. 6. Correlate COD and BOD.

33

Expt. No:

Date:-...

ESTIMATION OF COPPER BY COMPLEXOMETRY

Learning Objectives: To learn about: Aim: To estimate the amount of Cu2+ present in given solution Principle: The small amount of copper can be estimated by using the complexometric titrations with EDTA, which forms a 1:1 complex. As the erio-T forms a very stable complex with Cu2+, it will not be released by EDTA. Therefore fast sulphate black, which forms relatively weak complex, can be used as indicator. The reaction is Cu2+ + H2EDTA2- [Cu-EDTA]2- + 2H+ complexometric titrations chemical reactions between various regents and indicator structures of complexes formed in this titration role of buffer solution

Procedure: Use the standard solution (0.05) EDTA solution. Pipette out 10 ml of Cu2+ solution into a clean conical flask. Add about 4 ml of water and 5ml of conc. ammonia solution. The solution gets intense blue colour. Add 3or 4 drops of the fast sulphon black indicator solution. The color of the solution changes to purple. Fill a clean burette with std. EDTA solution. Note down the initial readings of the burette and titrate the solution by adding EDTA solution drop by drop. Stop the addition of EDTA, when the color changes to bright green. Record the final reading and repeat the titrations till constant values obtained. Calculate the concentration of the copper solution and the amount of Cu2+ present in 100ml of the solution.

34

S.No.

Volume of Cu2+ solution 10 ml 10 ml 10 ml 10 ml

Burette reading Initial Final

Volume of EDTA solution

1. 2. 3. 4. Calculations:

Use Molarity Equation. Explain the terms clearly. Molarity of CuSO4 Solution =

Calculation:

Amount of Cu2+ present = Molarity of CuSO4 X 63.54 X (100/1000) = g/100ml. Result: Amount of Cu2+ present = .. g/100ml. Review Questions: 1. What are complexometric titrations? 2. Name the most important complexing agent employed into these titrations & write its structure. 3. How the equivalent point is detected in complexomteric titrations? 4. Give some examples of titrations involving EDTA as a complexing agent? 5. Which type of ligand is EDTA and what is a chelate? 6. Name the most widely used indicator used in EDTA titration and how does it act? 7. What is a buffer solution? 8. What is a direct complexometric titration? Give an example? 9. What is a back titration? Give an example? 10. What is the effect on end point with EBT indicator if the hard water sample does not contain Mg2+ ions? 35

Expt. No:

Date:-...

DETERMINAITON OF CALCIUM IN MILK POWDER

Learning Objectives: To learn about: Composition of milk powder complexometric titrations structures of complexes formed in this titration role of buffer solution & EBT indicator

Aim: To determine the percentage of calcium in milk powder. Apparatus Required: Pipette, Burette, Conical flask, Wash bottle, Glazed tile. Chemicals Required: Standard Zinc salt solution, EDTA solution, Milk solution, Ammonium and Ammonium chloride buffer solution, Mg-EDTA indicator, Eriochrome black T indicator. Theory: The method is based upon the fact that Ethylene diamine tetra acetic acid forms stable complex compounds with all metals particularly with di and polyvalent metals. For all practical purposes the hydrated disodium salt of the reagent is used which has the following formula: NaOOC H2C CH2COOH

N CH2 CH2 N HOOC H2C CH2COONa

When hard water is titrated against EDTA solution it forms stable complexes with Calcium and Magnesium ions in water.

36

The titration is carried out in presence of EBT indicator at pH 10. It forms weak wine red coloured complexes with few of Calcium and Magnesium ions in water. When an excess drop of EDTA is added colour changes to blue. M2+ + EBT M2+ + EDTA M- EBT
Wine- red complex

M- EDTA
Stable- colourless complex

M-EBT + EDTA M-EDTA + EBT

Wine red Blue

(M = Ca or Mg) Procedure:Part A: Standardisation of EDTA: Pipette out 10 ml of standard Zinc salt solution into a 250 ml conical flask. Add 2 ml of Ammonia and Ammonium chloride buffer solution and 2 to 3 drops of Eriochrome black- T indicator. Solution turns wine red in colour. Titrate with EDTA from the burette till the colour changes to blue. Note the final burette reading. Repeat the procedure until two concurrent readings are obtained. Part B: Titration of Milk Solution: Pipette an exact 50 mL aliquot of the milk solution into a 250 mL conical flask. Add about 2 mL of pH 10 buffer, 10 mL of Mg-EDTA Indicator solution and 3 drops of Eriochrome Black T indicator. Titrate with the standard EDTA solution until color changes from wine red to blue. Observations and Calculations:Part A: Standardisation of EDTA: Molarity of Zinc salt solution M1 =

S.No.

Volume of Zinc salt solution (ml) V1 10 ml 10 ml 10 ml

Burette Readings

Volume of EDTA solution (b-a), V2 (ml)

Initial (a) 1. 2. 3.

Final (b)

V2= Volume of EDTA solution ml 37

Use Molarity Equation and explain the terms. Molarity of EDTA = Calculation:

Part B: Determination of % calcium in milk solution: Molarity of EDTA solution =

S.No.

Volume of milk solution sample (ml) V3 50 ml 50 ml 50 ml

Burette Readings (ml)

Volume of EDTA solution (b-a), V4 (ml)

Initial (a) 1. 2. 3.

Final (b)

Volume of EDTA solution used, V4 =

ml

Use Molarity equation and explain the terms. Concentration of Milk solution = Calculation:

38

Amount of Calcium = Concentration of Milk x Eq. wt = % Calcium in milk powder = Amount of Calcium x (250/1000) x (100/w) = Where w is the weight of milk powder (given) dissolved in 250 ml of distilled water for preparing the solution of milk powder. Result: Percentage of Calcium in milk powder sample= % Review Questions: 1. What is the indicator used in this titration? 2. Why can Eriochrome Black T not be used directly as an indicator? 3. What is the color of the doubly ionized Eriochrome Black T indicator in slightly basic solution? 4. What is the purpose of adding NaOH solution dropwise to the Mg-EDTA mixture? 5. Is it possible to use the sodium salt of EDTA as a primary standard? 6. At what pH is the Ca titration carried out? 7. What are the conditional constants for Mg2+ and Ca2+ at the pH at which the titration is carried out?

39

Expt. No ..

Date:

PREPARATION OF U-F RESIN

Learning Objectives: To learn about: Aim: To prepare Urea- formaldehyde resin. Chemicals Required: Formaldehyde (40%), Urea and Conc. H2SO4. Theory: Amino resins are condensation products obtained by the reaction of urea or melamine with formaldehyde. Commercially important amino resins are Ureaformaldehyde, Melamine formaldehyde which are formed by the condensation polymerization reaction of Urea with aqueous Formaldehyde and Melamine with formaldehyde respectively. Reaction: H2N CO-NH2 Procedure: Take 20 ml of 40% Formaldehyde solution in a 100 ml beaker. Add about 10 gms of urea while stirring until a saturated solution is obtained. Add a few drops of Conc. H2SO4 stirring continuously during the addition. All of a sudden a voluminous white solid mass appears in the beaker. When the reaction is complete wash the residue with water and dry the product and calculate the yield of the product formed. Note: The reaction is sometimes vigorous and it is better to be little away from the beaker while the addition of the Conc.H2SO4 and until the reaction is complete. + 2HCHO ----------- U-F resin Cross-linked polymers Monomers required for the preparation of U-F resin Condensation reaction

40

Result: Yield = ..

Review Questions: 1. 2. 3. 4. 5. What are resins? What is Bakelite? What are the monomers of it? Define thermoplastic polymer and thermosetting polymer? What are the monomers of U-F resin? Preparation of U-F resin undergoes what type of polymerization?

41

Expt. No ..

Date:

PREPARATION OF PHENOL-FORMALDEHYDE RESIN Learning Objectives: To learn about The structure of Phenol-Formaldehyde Resin The monomers from which this resin produced The reactions by which Phenol-Formaldehyde resin is produced

Aim: To prepare Phenol-Formaldehyde Resin (Bakelite) Apparatus Required: Glass rod, beakers, funnel and filter paper Chemicals Required: Glacial Acetic acid, 40% formaldehyde solution, phenol, Conc.HCl Theory: Phenolic resins are condensation polymerization products of phenolic derivatives with aldehydes (like Formaldehyde, Furfural). It is prepared by condensing phenol and formaldehyde in the presence of acid catalyst. Procedure: 1. Place 5ml of glacial Acetic acid and 2.5ml of 40% Formaldehyde solution in a 500ml beaker and 2grams of Phenol. 2. Add few ml of Conc.Sulphuric acid into the mixture carefully. With in 5min a large mass of plastic is formed. 3. The residue obtained is washed several times with distilled water, and filtered. Product is dried and yield is calculated. Result: The weight Phenol-Formaldehyde =

42

Review Questions: 1. 2. 3. 4. Phenol Formaldehyde is also called as ___________ What do you understand by resin? Give main uses of Phenol-Formaldehyde Resin. What type of Co-Polymer is Phenol-Formaldehyde Resin?

43

Expt. No .. PREPARATION OF NYLON 6,6 Learning Objectives: To learn about The structure of nylons The different kinds of nylon and how they differ The monomers from which nylons are produced The reactions by which nylons are produced

Date:

Aim: To prepare Nylon6,6 Apparatus Required: Beakers, glass rod Chemicals Required: Hexa methylene di amine, adipoyl chloride, Cyclohexane Theory: For the preparation of Nylon 6,6 the method of interfacial condensation is used. The diamine is dissolved in water and diacid chloride is dissolved in an organic solvent like CCl4 or cyclohexane. The aqueous layer is poured on the top of organic layer carefully. Diamine is soluble in both the solvents and hence diffuses from aqueous layer to organic layer and reacts with the reactive diacid chloride at the interface to form the product. The polymer is removed with the help of a forceps and the process continues.

44

Procedure: 1. Add 15 mls of a 5% solution of 1,6 hexamethylenediamine in water to a small beaker. 2. Slowly pour 15 mls of the 5% solution of adipoyl chloride in cyclohexane down the side of this beaker so that the two layers do not mix. 3. Using a bent spatula or a small wire with a hook pull, out the polymer that forms at the interface of the two layers. (Do not touch the polymer with your bare hands). 4. Continue to draw out the nylon 6,6 fiber (see how long you can make one fiber). 5. Allow the polymer to dry then investigate its properties (strength, brittleness). 6. Mix any remaining solution to form nylon 6,6. Discard the polymer as instructed. Result: Weight of Nylon 6,6 polymer is _______ Review Questions: 1. Where is nylon 6/6 used as an end product? 2. Is nylon 6/6 a thermoplastic polymer or is it a thermoset polymer? 3. Is the synthesis of nylon 6/6 an addition polymerization or is it a condensation Polymerization? Discuss these two types of polymerization. 4. Is the synthesis of nylon 6/6 a chain-growth polymerization or is it a step-growth Polymerization. Discuss these two types of polymerization.

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Expt. No. .

Date..

(A) PREPARATION OF BUFFERS AND STANDARDISATION OF pH METER (B) DETERMINATION THE MOLARITY OF ACID PHMETRICALLY,PROVIDED SUITABLE BASE Learning Objectives: To learn about: Aim: To prepare buffers and standardization of pH meter Apparatus: pH meter with glass electrode, reference electrode, beaker, titration flask and pipette., etc. Chemicals Required: Buffer solutions of pH 4 and 9, micro burette, HCl, NaOH Theory: (A) All pH meters, have position for standardizing the glass electrode in a buffer solution of known pH. This is necessary because different electrodes have different asymmetric potentials. Once the adjustment has been made, so that the meter registers correctly the known pH of the buffer solution, the instrument gives the pH of the other solution without any calculation. (B) Measurements of pH is also employed to monitor the course of acid base titrations. The pH values of the solutions at different stages of acid base neutralization are determined and are plotted against the volumes of acid/alkali added. On adding a base to an acid the pH rises slowly in the initial stages pH= -log[H+] , then it changes most rapidly. However, the shape of the inflexion point(i.e., where the pH changes abruptly) and symmetry of the curve on its two sides, depends upon the ionisability of the acid and the base used and on the basicity of the acid and acidity of the base. pH the purpose for which pH is measured the importance of pH in various reactions

46

Procedure: Standardization of the instrument 1. switch on the instrument, wait for 10 to 15 min. so that it gets warned up. 2. Prepare the buffer solutions having pH=4 and pH=9(Buffer tablets BDH and EMerck are available). This can also be prepared in the laboratory. 0.05M solution Potassium Hydrogen Phthalate gives buffer solution of pH 4.008 at 250C, 0.01M solution of Borax gives a buffer solution of pH 9.18 at 250C. 3. Wash the calomel and glass electrodes(or combined electrode) with distilled water. 4. Take the buffer solution(pH=4) in a clean glass or polythene beaker. Lower the electrode so that they are immersed in the solution to a depth of about 1 inch. 5. Measure the temperature of the solution by thermometer and set temperature compensate control to this value 6. Set the pointer to 7 pH exactly by means of set zero control 7. Put the selector switch to proper pH range 0-7(because pH of buffer solution is 4) 8. Set the pointer to the known pH value of the buffer by turning the set buffer control. Now the standardization is done. 9. Put back the selector back to zero position Wash the electrodes with distilled water and standardize the pH meter by using a buffer solution of pH=9. Same procedure, as described above is followed, except now the selector switch put to a pH range of 7-14. Procedure for pH-metric titration 1. 2. 3. 4. 5. Standardize the pH meter Clean the electrodes by distilled water and wipe them with tissue or filter paper. Take 25ml of HCl solution in a 100ml beaker and immerse the electrodes. Set up a burette containing standard Sodium hydroxide solution Measure the temperature of the solution and set temperature compensate to this value. 6. Put the the selector to the expected pH range. 7. The reading shown on the scale of the meter is the pH value of the unknown solution. 8. Add NaOH solution gradually from the burette, 0.5ml at a time. Note the corresponding value from the meter. Near the end point add very small amount of NaOH as possible because change in pH will be very much appreciable because when the acid is neutralized, further addition of such a small amount as 0.01 ml raises the pH to about 9 or 10. 9. Put back the selector to zero position after pH measurements and before removing the electrodes from solution. Leave the selector in zero position when not in use. 10. Plot a graph between pH and volume of NaOH added. From this graph, determine the volume of NaOH required for the complete neutralization of HCl. 47

. Observation and Calculation: Plot a curve with pH value on Y-axis and volume of alkali added on X-axis. Sharp break in the curve corresponds to the equivalence point. Let the volume of the alkali at equivalence point is X ml. Temperature of the solution = S.No. 1 2 3 4 5 and so on Volume of NaOH added (ml.) 0.5 1.0 1.5 2.0 2.5 pH

Volume of NaOH required for complete neutralization of HCl = Use normality equation. Explain the terms Normality of HCl solution = Calculation:

Strength of HCl solution = M1 X 36.5 = . X 36.5 = Result: Strength of HCl is . Review Questions: 1. Define the term pH? 48

2. 3. 4. 5. 6. 7.

What is the effect of temperature on pH? What is the possible pH of pure water at 65C? What is the effect of dilution on pH of an acidic solution? What is the pOH of pure water at 25C? What chemicals would you use to make a buffer of pH 5 & 10? Name three electrodes which are usually employed to measure pH of a solution? Which one is most suitable? 8. Define a reference electrode?

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Expt. No..

Date:

Acid-base titration by Conductometric method (Demo)

Learning Objectives: To learn about: Conductometric titration Equivalence point of a titration Mobilities of ions the calibration of the conductometer

Aim: To find the concentration of an acid solution by titrating against NaOH solution conductometrically. Theory: Conductometry can be used to detect the equivalence point (end point) of a titration. This method is based upon the measurement of conductance during the course of titration. The conductance varies differently before and after the end point. This is due to the reason that electrical conductance of a solution depends upon the no. of ions present and their ionic mobilities i.e. speeds. When conductance values are plotted against volume of titrant added, two straight lines are obtained. The point of intersection of the lines gives the end point. Chemicals required: Conductivity bridge, conductivity cell, burette, pipette, 0.01N KCl solution, 0.1 N NaOH solution and approximately 0.01N HCl solution. Procedure: The conductivity measurements are made by making use of conductivity bridges or conductometers which are based upon the principle of Wheatstone bridge. Calibration of the Instrument: Switch on the instrument and wait for half a minute. Take the conductivity cell and connect it to the cell terminals on the instrument. Take 50 ml of 0.01 N KCl solution in a 100 ml beaker and place it on base plate of cell. Immerse the cell in the solution so that the platinum plates of the cell are completely immersed in solution. Select the proper conductance range by putting the multiplier switch in the proper range. Push the cal./meas switch to cal. Position 50

 Set temperature control at 25C and adjust calibration control to get 1000 on the screen position of decimal point. Measure the temperature of the standard solution and set the temperature control to the value of temperature. Now push the cal./meas switch to meas. Position. Adjust calibration control switch to get the desired value of conductivity of 0.01 KCl on the screen. After the calibration of the instrument remove the cell from KCl solution and wash with distilled water. Note: After the calibration, do not disturb the calibration control switch till the experiment is complete. B. Titration of HCl vs NaOH solution 1. Pipette out 50 ml of given HCl solution in a 100 ml beaker. 2. Immerse the conductivity cell in the solution so that the electrodes completely dip in solution. 3. Select the proper conductance range and put the ca/meas switch to meas position. 4. Measure the temperature of the sample solution and set the temperature control to the values of measured temp. 5. Note down conductance of the solution. 6. From the burette add 0.1 N NaOH solution in 0.5 ml lots. Mix the solution with the help of a glass rod carefully and note the conductance of mixed solution. 7. Keep on adding NaOH solution in 0.5 ml lots and note the conductance value till 10-12 ml of solution is added. 8. Plot a graph between observed conductance values along Y-axis against the volume of alkali added along X-axis. The point of intersection gives the amount of alkali required for neutralization of acid. Observations and Calculations: Volume of HCl taken = 50 ml Normality of NaOH solution = 0.1 N Observation Table S.No. 1 2 3 4 5 and so on Volume of NaOH added (ml.) 0.5 1.0 1.5 2.0 2.5 Observed conductance (ohm-1)

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Suppose volume of NaOH used at equivalence point = A ml Applying normality equation Calculation:

Result: Normality of given HCl solution is Precautions: 1. The solution taken in the burette should be about ten times stronger than that taken in the beaker so that the volume change of latter solution is negligible on the addition of the former solution. 2. After every addition of NaOH solution, the solution must be stirred thoroughly. Review Questions: 1. 2. 3. 4. 5. Define Ohms law? What is conductance and what are its units? What is cell constant? What is specific conductance and equivalent conductance? What is the effect of dilution on specific conductance and equivalent conductance? 6. State the principle on which the conductometer is based? 7. What is a conductivity cell? 8. Why ordinary water is unsuitable for conductivity measurements? What is conductivity water? 9. What is the effect of temperature on electronic and electrolytic conductance? 10. What are the advantages of conductometric titrations? N.

52

Expt. No..

Date:

DETERMINATION OF SPECIFIC AND EQUIVALENT CONDUCTIVITY OF A SOLUTION Learning Objectives: To Learn about Aim: To determine specific and Equivalent conductivities of solutions Apparatus: Conductivity Bridge(A.C.mains operated), Conductivity cell, Thermometer, Beaker, Burette, Pipette, Funnel. Chemicals: 0.01N KCl Solution, Distilled water. Theory: Specific conductance of a solution is the conductivity of a solution contain between two parallel electrodes which have cross sectional area 1cm2 and which are kept 1cm apart. If R is the resistance of a solution measured by cell having electrodes of cross sectional area a cm2 and l cm apart, specific conductance K of the solution is given by

Where C is the observed conductance and l/a is known as the cell constant. Thus to obtain the value of specific conductance, the observed conductance has to be multiplied by a certain factor known as cell constant. (the values of a and l are constant for a particular cell so l/a is constant and hence the name Cell constant. The cell constant i.e, the ratio l/a cannot be determined from the geometrical dimentions of the cell because the exact area of cross section of electrode or exact distance between them cannot be measured accuretly. Thus cell constant is determined by an indirect method. From the above equations

53

Or

Cell constant

--------------------(A)

For the determination of cell constant, a solution of known specific conductance is taken whose conductance is determined using the given cell. Thus cell constant can be determined using equation (iii). Solution of KCl of known concentration and known specific conductance are used for this purpose because , KCl strong electrolyte Procedure: 1. Wash the conductivity cell thoroughly with distilled water. 2. Rinse the conductivity cell repeatedly with KCl solution. 3. Take sufficient volume of KCl solution in a beaker and note down its temperature. 4. Connect the instrument to the mains and switch on the instrument using the power switch. Connect the electrode leads in the input sockets at the rear of the instrument. 5. Set the Function switch to check position and adjust the display to 1.000 with CAL control at the back panel. 6. Dip the conductivity cell in KCl solution and adjust the temperature knob of the conductivity bridge at the temperature of the KCl solution. 7. Move the Function switch to conductance position and range position to appropriate range. 8. Adjust the cell constant knob so that the display reads the known value of the KCl solution at that temperature 9. Bring the Function switch to Cell constant position and read the value of cell constant from the display window. 10. Substitute the cell constant value in the formula A given in the theory and calculate Specific conductance(K) of the solution. The mobility of K+ and Cl- is quite comparable.

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11. Substitute the Specific Conductance(K) value in the following formula and calculate Equivalent Conductance (v) of the solution. Equivalent Conductance, v = Specific conductance (K) Volume in ml (v) per gram equivalent of the electrolyte. The volume per gram equivalent of electrolyte is called dilution factor of the solution. If the concentration of the solution is c gram equivalent per litre then the volume containing 1 equivalent of the electrolyte will be V = 1000/c ml per gram equiv. Result: Measured Specific conductance = Measured Equivalent Conductance = Review Questions: 1. Define conductance, specific conductivity and equivalent conductivity. What are their units? 2. What is the relationship between specific conductivity, cell constant and conductance? 3. Why KCl is used as a standard for verification of cell constant?

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