IPC - Jawaharlal Nehru Engineering College, Aurangabad

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Jawaharlal Nehru Engineering College. Laboratory .... If no oxygen is present the manganous ion reacts with the hydroxide ion to form white ppt. If oxygen is ...
Jawaharlal Nehru Engineering College

Laboratory Manual

INDUSTRIAL POLLUTION CONTROL

For

BE Year Chemical Engg Students

FOREWARD

It is my great pleasure to present this laboratory manual for Final year Chemical engineering students for the subject of industrial pollution control keeping in view the vast coverage required for visualization of concepts of industrial pollution control in Chemical industries .

As a student, many of you may be wondering with some of the questions in your mind regarding the subject and exactly what has been tried is to answer through this manual.

Faculty members are also advised that covering these aspects in initial stage itself, will greatly relieve them in future as much of the load will be taken care by the enthusiastic energies of the students once they are conceptually clear.

LABORATORY MANNUAL CONTENTS

This manual is intended for the students of Final year Chemical Engineering branch in the subject of Industrial pollution control. This manual typically contains practical/Lab Sessions related in Industrial pollution control Chemical industries covering various aspects related the subject to enhanced understanding.

We have made the efforts to cover various aspects of the subject covering various actually used in industry Industrial pollution control will be complete in itself to make it meaningful, elaborative understandable Chemical concepts and conceptual visualization.

Students are advised to go thoroughly through this manual rather than only topics mentioned in the syllabus as practical aspects are the key to understanding and conceptual visualization of theoretical aspects covered in the books.

Good Luck for your Enjoyable Laboratory Sessions

Prof. M. R. Gaonkar Chemical Engineering Department

SUBJECT INDEX 1. To determine Ph measurement 2. To determine total so;ids and volatile matter 3. To determine hardness 4. To determine alkalinity 5. To determine dissolved solids 6. To determine BOD 7. To determine COD 8. To determine Chlorides 9. To determine turbidity 10. Conduction of Viva-Voce Examinations. 11.

Submission

12.

Evaluation and Marking Systems

DOs and DON’T DOs in Laboratory:

1.

Do not handle any equipment before reading the instructions/Instruction manuals.

2. Wear Apron before conducting experiment.

3. Handle Chemicals, equipments and glass wear carefully.

4. Strictly observe the instructions given by the teacher/Lab Instructor.

5. Be careful about moving part of any equipment.

6. Clean all equipments and glassware after use.

Instruction for Laboratory Teachers::

1.

Submission related to whatever lab work has been completed should be done during the next lab session.

2. The promptness of submission should be encouraged by way of marking and evaluation patterns that will benefit the sincere students.

PRACTICAL NO 1 (2 HOURS) AIM: To measure the pH value of the given sample(by any one method). APPARATUS: pH meter , pH paper, beaker, solutions CHEMICALS: Buffer solution, sample solution. THEORY: PROCEDURE: USING Ph meter 1. Calibrate the electrodes with standard buffer solution. 2. Rinse the electrodes with std buffer solution. 3. Dip the electrodes into the sample solution (25ml) taken in 100ml beaker and wait upto 1 min for steady reading. 4. Note down the reading. 5. Repeat this procedure for other given unknown samples. USING pH PAPER 1. Take ph paper from the strip. 2. With dry hands dip the paper in the solution 3. Compare the resulting colour with the standard colour strip. 4. Note the ph values. 5. Repeat procedure for different unknown samples. FIGURE: OBSERVATION: SAMPLE NO

RESULT:

Ph readings

REMARKS

PRACTICAL NO 2 :(2 HOURS) AIM: To measure the fixed solids,volatile solids and total solids in the given effluent sample water. APPARATUS: Pipette, crucible, weight box, heater/burner,whatman paper. CHEMICALS: Effluent/waste water sample solution. THEORY: PROCEDURE: 1. 2. 3. 4. 5. 6.

Weigh the empty crucible. Add 20 ml of given effluent water sample which is filtered into the crucible. Weigh the crucible with sample water. Evaporate the sample till there is no water droplets in crucible. Cool and weigh the crucible with residue it contains fixed solids and volatile solids. Tilt the crucible and slightly expose it to the flame for few seconds till the residue color changes to brown or black. 7. Cool the crucible and take its weight. This contains fixed solid.

FIGURE: OBSERVATIONS: 1. 2. 3. 4. 5. 6.

Weight of empty crucible=W1= gm Weight of empty crucible + sample = W2 = Weight of empty crucible + residue = W3 = Weight of total solids = W3 –W1= gm Weight of fixed solids= W4= gm Total volatile solids =w5= W3-W1-W4 =

RESULT : Fixed solids, Volatile solids, Total solids in

gm gm

gm

mg/lt.

`

PRACTICAL NO 3: (2 HOURS) AIM: To determine the hardness of the given sample. APPARATUS: Beaker, Burette,Pipette, Conical flask. CHEMICALS: Erichrome black T INDICATOR, Std EDTA solution ,Sample solution. THEORY: FIGURE: PROCEDURE: 1. 2. 3. 4.

Take 10ml of given sample in a conical flask. Add 2-3 drops of buffer solution to the sample. Add 1-2 drop of EBT indicator. Shake well and titrate against EDTA solution from burette end point red to blue.

OBSERVATION TABLE: SNO

BURETTE READING

CALCULATIONS: CaCO3 in sample = 1000XBR/Volume of sample RESULT:

PRACTICAL NO 4: (2 HOURS) AIM: To determine the alkalinity of the given sample. APPARATUS: Beaker, Burette,Pipette, Conical flask. CHEMICALS: Sample water, phenolphthalein, sulfuric acid, methyl orange. THEORY: FIGURE: PROCEDURE: 1. 2. 3. 4. 5. 6. 7.

Prepare 0.01 N sulfuric acid solution. Take 10 ml of sample in conical flask. Add 2 drops of phenolphthalein indicator. Titrate the solution in flask(if pink in colour) against sulfuric acid till it becomes colorless. Note the burette reading. Add 2ml of methyl orange indicator to the titrated sample(colourless sample) If sample becomes yellow in colour titrate with 0.01N sulfuric acid till the color changes to orange. 8. Note the burette reading. 9. Repeat procedure for 2 samples and for tap water samole.

OBSERVATION TABLE: SNO

BURETTE READING

CALCULATIONS: CaCO3 in sample = 1000XBR/Volume of sample RESULT:

PRACTICAL NO 5: (2 HOURS) AIM: To determine the quantity of dissolved oxygen present in the given sample. APPARATUS: Beaker, Burette, Pipette, Conical flask. CHEMICALS: Sample water, manganous sulphate, alkaline iodide reagent, starch indicator, stdN/40 sodium thiosulphate, conc sulphuric acid. THEORY: PROCEDURE: 1. Take 20 ml in a 300ml BOD bottle. 2. Add 2ml of manganous sulphate in sample and 2ml of alkaline iodine solution to the BOD bottle. The tip of the pipette should be below the liquid level while adding these reagents. 3. Stopper the bottle with care to exclude air bubbles and mix by repeatedly inverting the bottle 23 times. 4. If no oxygen is present the manganous ion reacts with the hydroxide ion to form white ppt. If oxygen is present it forms brown colour. 5. Allow thw precipitate to settle completely leaving a clear supernatant liquid. 6. Carefully remove the stopper and add 2 ml of sulfhuric acid conc by the sides of the bottle. 7. Stopper the bottle and mix thoroughly until dissolution is complete. 8. Titrate the sample immediately with o.1 N sodium thiosulphate solution using starch indicator (blue to colourless) 9. Record the amount of sodium thiosulfhate used.

OBSERVATION: SAMPLE NO

Burette reading (ml)

Calculation: D.O = 0.2x1000X B.R/ volume of sample Result:

PRACTICAL NO 6: (2 HOURS) AIM: To determine the quantity of B.O.D present in the given sample. APPARATUS: Beaker, Burette, Pipette, Conical flask. CHEMICALS: Sample water, manganous sulphate, alkaline iodide reagent, starch indicator,0.1N sodium thiosulphate, conc sulphuric acid. THEORY: PROCEDURE: 1. 2. 3. 4. 5. 6.

Take 20 ml in a 300ml BOD bottle. Analysis for dissolved oxygen on 1 st day. Take the sample and keep it in the incubator for 5 days at 30degree temperature. Analyse the D.O of the sample after 5 days. Calclulate the DO on the 5 th day. Calculate the BOD.

OBSERVATION: 1. 2. 3. 4. 5. 6. 7. 8.

D.O on the 1st day: Volume of sample : Normality of sodium thiosulphate: Burette reading: D.O On the 5th day: Volume of sample : Normality of sodium thiosulphate: Burette reading:

SAMPLE NO

Burette reading (ml)

Calculation: D.O = 0.2x1000X B.R/ volume of sample B.O.D =DO 1-DO5 Result:

PRACTICAL NO 7: (2 HOURS) AIM: To determine the quantity of C.O.D present in the given sample. APPARATUS: Beaker, Burette, Pipette, Conical flask , reflux condenser, heater CHEMICALS: Sample water,K2Cr2O7, Mercuric sulfate, H2SO4 , ferroin indicator, 0.2N ferrous ammonium sulphate. THEORY: PROCEDURE: 1. 2. 3. 4. 5. 6. 7.

Take 10ml sample in 500ml round bottom reflux flask. Add 20 mg sulfamic acid and 250 mg of mercuric sulfate to the sample in the flask. Add 5 ml of std potassium dichromate solution in the flask. Add 15 ml of sulfuric acid reagent slowly. Adjust the condenser on the flask and strat cooling water. Reflux for 1 hour and cool the mixture. Titrate 10 ml of cooled sample with 0.2N ferrous ammonium sulfate solution using ferroin indicator. 8. Repeat for blank reading of distilled water 9. End point is gree-blue-brown.

Oberservation: SAMPLE NO

Burette reading (ml)

Calculation: C.O.D = (A-B)X 1000XN/Volume of the sample A- B.R for distilled water B- -B.R for sample N- normality of ferrous ammonium sulphate

Result:

PRACTICAL NO 8: (2 HOURS) AIM: To determine the quantity of Chlorinity present in the given sample. APPARATUS: Beaker, Burette, Pipette, Conical flask , measuring cylinder. CHEMICALS: Sample water, tap water, AgNO3, K2Cr2O7 THEORY: PROCEDURE: 1. 2. 3. 4. 5. 6.

Prepare 0.01 N Silver nitrate solution. Take 20ml of sample in clean conical flask. Add 0.5 ml of K2Cr2O7 indicator to the sample flask. Titrate sample with silver nitrate till colour changes Note reading Repeat procedure for tap water.

Oberservation: SAMPLE NO

Burette reading (ml)

Calculations: Chloride content in sample: 1000XB.R/Vol of sample

Result: