Submission of Proposal under Star College · Web viewA method involving systematic study of performance of a process is called scientific method. Various types of experiments of routine

Submission of Project Booklet under Star College Scheme

Contents

Section A:

Manual for GLP & Green Chemistry

Section B:

SOP for various instruments used under ‘DBT star college’ scheme

Section C:

Manual for (Laboratory Staff)

Preparation of:

i. Standard solutions,

ii. Lab reagents,

iii. Chemicals required for various C.T.

Section D:

Projects for U.G. students under ‘DBT star college’scheme

D – 1Projects for F.Y.B.Sc. students

D – 2Projects for S.Y.B.Sc. students

D – 3Projects for T.Y.B.Sc. students

---------------------------------------------------------------------------------------------------------------------|| Hindi Vidya Prachar Samiti’s RAMNIRANJAN JHUNJHUNWALA COLLEGE || Page 93 of 280


Section A

Manual for

Good Laboratory Practices

GLP & Green Chemistry



GENERAL CHEMICAL ANALYSIS AND . EXPERIMENTATION

Chemistry is a branch of science which deals with the study of matter, its physical and chemical

property, its composition the physical and chemical changes which it undergoes and the energy

that accompany these properties. Chemistry can be used in industry, medicine, agriculture and

environmental science.

INDRODUCTION TO CHEMISTRY LABORATORY

A chemical laboratory is a place where necessary equipments chemicals and adequate facilities

are provided to test certain concepts, theoretical knowledge obtained in classroom and from the book.

Carefully established scientific methods are crucial for all these. A method involving systematic

study of performance of a process is called scientific method. Various types of experiments

of routine or project work are carried out in a chemistry laboratory using scientific methods.

SCIENTIFIC METHODS INVOLVE:


1 Object 2 apparatus

3 experimentation 4 observation5 hypothesis 6 verification7 prediction 8 new experiments9 modification


DEMONSTRATIONS

In the initial stages, the experiments would be performed by the teacher and demonstrated to the students. The

main purpose of the demonstration is to make the students aware as how some of the apparatus is

used and precautions to be followed while doing the experiments.

EXPERIMENTATION BY THE STUDENTS

Most of the experimerts are done by the students themselves. This gives them the confidence to

do the work-themselves and get the results. For this, it is essential that the students should follow

the rules meticulously laid down to work in laboratory.

RULES TO BE FOLLOWED WHILE WORKING IN CHEMISTRY LABORATORY

1. Know the work in advance. Come prepared for it.

2. Bring all the necessary articles with you. Viz. duster, match box, rough journal, manual,

dropper, test tube holder.

3. Reach the laboratory at allotted time

4. Occupy your allotted seat. Wear the apron.

5. Listen to the practical exercise (work) to be done very carefully. Note down the

instructions as to how to proceed with the experiment.

6. Follow the instructions very carefully. Do not deviate from them.

7. Handle the apparatus and the equipments carefully. Ensure that the apparatus you are

going to use is clean.

8. Ensure that you use the labeled chemicals. Replace them at their respective place after

use.

9. Clean the apparatus after using it and replace it to its original place.



10. Record your observation very carefully and meticulously. If you find any difficulty in

taking the reading resort to be help of your teacher. Do not cook up the results to get the

correct answer.

11. Show the procedure and the results to your teacher as soon as you complete the work.

MAINTENANCE OF RECORD

1. A neat and systematic recording of the experimental reading in the practical file is very

important.

2. Follow the instructions as to how a particular experiment is to be recorded in the notebook.

SAFETY RULES AND PRECAUTIONS TO BE OBSERVED

While working in a laboratory following safety rules are to be observed.

1. Wear eye protection and laboratory coat.

2. Do not eat or drink in the laboratory.

3. Never perform an unauthorized experiment.

4. Handle glass apparatus very carefully.

5. Follow proper procedure while heating liquids. While heating the liquids in a test tube,

keep the mouth of test tube in the direction away from you. Keep the test tube shaking all the

time while heating. It does not allow the boiling liquid to spurt out of the test tube.

6. Never inhale vapour directly.

7. While diluting acid always add acid to water, and never pour water to acid.

8. If a glass tubing or a thermometer is to be inserted in a rubber cork, lubricate the glass and

protect your hand with a towel. Use gentle twisting.

9. Use dropper and test tube holder.

10.Do not smell or taste the chemicals.

11. Learn & be familiar with the fire extinguisher procedure provided in the

laboratory.---------------------------------------------------------------------------------------------------------------------

|| Hindi Vidya Prachar Samiti’s RAMNIRANJAN JHUNJHUNWALA COLLEGE || Page 97 of 280


12. Never heat volatile inflammable chemicals directly on flame for e.g. if alcohols are heated

directly, its vapours will catch fire.

13. Do not throw porcelain piece, match stick, and filter paper etc. in the sink.

14. Avoid leaving Na metal exposed to air or throwing it in sink. This may lead to fire in the

lab.

15. Never heat graduated glass apparatus over a flame.

16. Wear half sleeved clothes, Hair should be tied back .

17. Be alert & follow discipline, orderliness in lab.

HOW TO DEAL WITH ACCIDENTS

1) Inform the teacher immediately in case of emergency or accident, even if you think it is

aminor one.

2) Burns: wash with clean water. Do not rub the affected portion.

3) Acid burns: wash with water and dilute solution of NaHCO3 and then with running

water.

4) Alkali burns: wash the affected portion with dilute solution of CH 3C00H and then

withrunning water.

5) Eye Injury: do not rub the eyes. Splash the eyes with clean water.

6) Cuts: wash with plenty of free slowing water. Apply tincture Iodine.

7) Gas leak: Try to switch off gas supply from mains.

8) electric shock: Try to switch off the electric current/mains immediately. Keep youself

away from the affected area.

SAFETY SYMBOLS AND THEIR MEANINGS

1 Irritant: substances that can make your skin go red or blister



2Toxic: Substances that are poisonous and can kill a person.

e.g. Cl2

3Highly Inflammable: Substances that catch fire easily. e.g.

C2H5OH

4Harmful: Substances that may cause pain and discomfort.

e.g. CuSO4

5Oxidizing: Substances that help others burn more strongly.

e.g. Ammonium nitrate

6Corrosive: Substances that will the damage skin and eyes.

They can damage even wood and metal. e.g. NaOH

7 Irritant: substances that can make your skin go red or blister

8Toxic: Substances that are poisonous and can kill a person.

e.g. Cl2

REFERENCES

1) Vogel's Textbook of quantitative inorganic analysis

J. Bassett R.C. Denney, G.H. Jeffery, J. Mendham, 4th ed. ELBS.

2) Chemistry by Richard Harwood, Cambridge Univ. Press.

3) Methods of teaching chemistry

K. S. Kumar, K. Ramakrishna, D. B. Rao, Discovery Publishing, New Delhi. 6.

4) Laboratory Manual Science & Technology

R. S. Mittal, R. R. Mishra, S. C. Maheswary and Yash Pal, Arya publication, CBSE

5 ) Practical Chemistry for B. Sc.Students



O. P. Pandey, D. N. Bajpai, S. Giri, S. Chand & Co. Ltd.

6) Franck Secondary Science Practicals

Y. P. Purang, Stalin, Malhotra. Ed. Franck Bros & Co., Published NCERT

INSTRUMENTAL AND QUANTITATIVE ANALYSIS (CONDUCTOMETRY)

CONDUCTOMETRY

1 . P r inc ip l e

2.Apparatus a) Cell & C e l l Constant

b) Conductometer

3. Standardisation

4. Working

5. Graphical method and determination of Equivalence point



6. Advantages and Limations

7 . Precaut ions



POTENTIOMETRY

1 . Principle

2. Apparatus - a)Indicator electrodes / Reference / electrode

b) Potentiometer

c) Salt bridge

3. Standardisation

4. Working

5. Graphical method and determination of equivalence point.



6. Advantages and Limitations

7. Precautions



pH-METRY

1. Definition of pH, Buffer

2 . P r i n c i p l e

3. Apparatus a) cell

b) pH meter

4. Standardisation

5. W o r k i n g

6 . Graphical method and determination of equivalence point


8.P recau t ions



COLORIMETRY AND SPECTROPHOTOMETRY

1 . P r inc ip l e

2. Distinguish between colorimeter and Spectrphotorneter

3. Apparatus a) Cuvette

b) Colorimeter / Spectrophotometry

4. Standardisation

5. Working

6. Graphical method




8. Precaution



QUANTITATIVE ANALYSIS

1. Standard solution :

a) Definition:

b) Ways of expressing concentration:

2. Primary and secondary standards :

3. Steps involved in the preparation of primary standards solution:

a) Determining the amount of primary standards to be weighed:

From the chart, note the weight of the substance to be weighed & the final volume to which it

is to be diluted.

b) Weighing on watch glass :

i. Watch glass should be thoroughly dry (both the sides):

ii. Do not weigh on paper (use only watch glass)

iii. Filter paper will absorb the mixture. Solid particles may get attached to the filter paper.

iv. Watch glass should be covered with 'dry funnel. (Collect the substance in the centre of the

watch glass).

v. While recording the final reading doors of the balance should be closed. Record the weight in

the rough journal and not on a paper or hand.

vi. Maintain the balance and balance room clean.

c) Transferring substance in a beaker:---------------------------------------------------------------------------------------------------------------------



Transfer the substance in breaker with jet of water from wash bottle

taking care that all the solid particles is transferred in the beaker. Then, wash watch glass with

minium amount of water with washings transfered in the beaker

d) Dissolving the solute completely by stirring with glass rod:

e)Transferring in a standard measuring flask through funnel :

Transfer the clean solution through funnel with the help of glass rod in to the standard flask.

Wash the beaker 2-3 times using 5-10cm3 of water each time. Wash glass rod & then

funnel & All these washings must be transferred in the standard flask.

f) Diluting to final volume:

Add water directly up to 2 cm3 less than marking and then the final dilution should be done drop wise

with the help of the glass dropper. Lower meniscus should tocuh the marking on the standard

flask.

4. Volumetric titration:

Check, the burette should not leak.

Burette: Wash, rinse & before adjusting zero marking on the burette, make sure that there is no

air bubble. Lower meniscus should touch the zero marking on the burette. Pipette: Wash, rinse &

pipette out the solution with dry index finger kept on the pipette. Transfer the solution from the

pipette to the flask without blowing the pipette. indicator: Add constant amount of indicator for

each titration (2-3 drops). Observe the colour change on the background of clean white tile.

Before starting the titration, remove the funnel.

5. Errors &Accuracy:

Observe all the precautions explained in the earlier part to ensure that there are no procedural

errors and that will ensure the accuracy. Report the constant burette reading,



QUALITATIVE ASPECTS IN INORGANIC PREPARATION

1) PRECIPITATION:

a) Precipitating agent:

to be added slowly with constant stirring Add the required quantity as given in procedure.

b)Maintenance of pH:

Proper pH should be maintained as given in the procedure to ensure complete precipitation.

c) Technique:

d) Use the proper amount of reagent. Precipitant should be added slowly with

constant stiffing. Use sufficient amount of reagent in required quantity as given in the

procedure,

2) DIGESTION:

a) Use of water-bath:

Digest the ppt for a given time as mentioned in the chart. During digestion do not remove

the glass rod.

b) Completion of precipitation :

After digestion, check complete precipitation by adding some more precipitating agent

3) FILTRATION :

Technique :

Precipitate to be filtered through whatman paper using suction pump

4) WASHING :

a) Solvent for washing:

Depending on the solubility of the ppt. proper wash liquid should be used as given in the

chart, water, is the preferred wash liquid for the precipitate provided precipitate Is Insoluble

in water



5) DRYING:

Drying temperature

110°C to 130°C for ppt. which are formed from organic solvents. Dry for 20.30 mins,

6) COOLING

Use desiccators to dry the substance i.e to absorb the moisture, It contains anhydrous CaCl2

Always keep the desiccators closed.

7) WEIGHING

Transfer the dried cooled product on the previously weighed watch-glass, to find the

weight of the product.



QUALITATIVE ASPECTS IN ORGANIC EXPERIMENTS

1. PHYSICAL CONSTANT DETERMINATION :

a. Melting point :

a) Boiling point:

2. RECRYSTALISATION TECHNIQUE:

a. Choice of solvent :

b. Procedure :

3. DRYING METHODS:



4. BULK SEPARATION:



QUALITATIVE ASPECTS IN GRAVIMETRIC ANALYSIS

1. REMOVAL OF IMPURITY:

To estimate the given metal ion in the presence of other metal ion as impurity, it is necessary to

remove the impurity by precipitating with suitable reagents.

a. Passing of H2S (jf any): Use a clean glass tube (not glass rod) for passing H2S.

(Use beaker for passing H2S gas)

b. Time ofpassing H2S:

Not less than 2-3 minutes. The glass tube through which H2S is passed, should be

washed with water & the washing must be collected in the beaker.

c. Removal of H2S and concentration: Remove H2S completely and

concentrate the solution to half of its initial quantity.

2. PRECIPITATION:

a) Precipitating agent:

To be added slowly with constant stirring. Add the required quantity as given in

procedure.

b) Maintenance of pH:

Proper pH should be maintained as given in the procedure to ensure complete

precipitation.

c) Technique:

Use the proper amount of reagent. Precipitant should be added slowly with constant

stirring Use sufficient amount of reagent in required quantity as given in the

procedure.

3. DIGESTION:

a) Use of water- bath:



Digest the ppt. for a given time as mentioned in the chart. During digestion do not remove

the glass rod.

b) Completion of precipitation:

After digestion, check complete precipitation by adding some more precipitating agent.

4. FILTRATION:

a) Technique:

Precipitate to be filtered through sintered glass crucible using suction pump.

b) Porosity of crucible:

Depending on the size of ppt. crucible of the proper porosity_Ooulci be used like G3, G4 as mentioned in the

chart.

5. WASHING:

a) Solvent for washing:

Depending on the solubility of the ppt, proper wash liquid should be used as given in the chart.

b) Technique:

Do not add wash liquid up to the upper end of the crucible, it should cover 3/4th of the crucible. Allow the wash

liquid to drain as completely as possible before adding next washing.

c) Elimination of CI- , s042- PO43- :

Check removal of CI- after 4 washings. Don't check after each Washing. SO42- PO43-are removed prior to Cl-

therefore, removal of Cl- ensures removal of SO41-8, PO43-

6. DRYING:

Drying temperature

1 10°C to 130°C for ppt. which are formed from organic solvents. Dry for 1 hour.---------------------------------------------------------------------------------------------------------------------



7. COOLING:

Use desiccators to dry the substance i.e. to absorb the moisture. It contains anhydrous CaCl2 Always keep

the desiccators closed.

8. WEIGHING:

Never weigh the hot crucible. Record the weight of the crucible with ppt. in the same rough journal.

Again keep the crucible in the oven for 20 minutes. If second weight is les then that should be the weight

recorded

9. ERRORS IN GRAVIMETRIC ANALYSIS:

Observe all the precautions explained in steps no. 1 - 8 which will ensure that there are no errors.



GR EEN C HEM IS TR Y

PRINCIPLES:

1) Need of alternative pathways for chemical reaction and usage which doesn't

produce waste.

2) If waste is formed, it should be non- toxic, pollution free and degradable.

3) Synthesize products with maximum effect a per requirement and least harmful to human

and environment

4) Catalytic reagents are renewable whereas stoichiometric ones are wasteful and polluting

5) Reaction vessels should be strong enough to minimize the potential of chemical accident.

6) Accidental spillage of hazardous by-product should be prevented by properly monitoring

them

7) Production Of compounds with multi-functional group should be minimized as it involves

use of many reagents and hence generation of more by-products.

8) Rate of production should be a according to the availability of feedstock/raw-material for

maintenance of ecological balance.

PRACTISING GREEN CHEMISTRY IN LAB

1) Use minimum organic solvents (like acetone alcohol) for cleaning, rinsing dissolving etc.

2) Avoid them as far as possible in first place itself. Wherever possible water should be

used for all above purposes.

3) Dry the apparatus in air. (Avoid use of heat for drying and prevent thermal pollution).

If required, filter papers can be used.

4) As far as possible, dilute solutions should be used instead of solids.

5) Minimum amount (as required) of dilute solution should be prepared avoiding wastage.

6) All the required arrangement of test (for quantitative analysis) should be done and then

burner should used for short required time period only.

7) Burner should be kept off as and when possible (match box or gas lighter



should always be kept handy)

8) Micro-techniques should be followed wherever possible:

i. Small test tubes to be used

ii. Cavity of tile to be used in colour tests not involving heat.

iii) Even capillary tubes can be used in various tests.



Section B

SOP for Various Instruments



SOP FOR COLORIMETER

Insert the plug in mains socket and switch the power ON .Allow the instrument to

warm up for about 5min.

1)Zero Adjustment : Rota te s lowly the wavelength se lec tor knob. Insert the test

tube filled with solvent in its place. Adjust the "Zero adjustment knob till the pointer

comes to zero.( zero reading of transmittance).

2)100% Adjustment :Rotate slowly the wavelength selector knob ti l l desired

wavelength is selected. Do not disturb the filled test tube. Adjust the "100%"

knob till the pointer comes to 100.

Repeat steps 1 & 2 above.

The instrument is now calibrated for use.



SOP FOR CONDUCTOMETER

1) Switch the instrument on about 10-15 minutes before starting the experiment.

2) Keep the conductivity cell dipped in distilled water for about 10-15 minutes. Connect

its terminals to the cell terminals seen on the conductivity meter.

3) Confirm that the instrument has been properly standardized.

4) Take the sample solution whose conductance is to be measured, in a 100cm3 beaker.

5) Remove the conductivity cell from distilled water. Wipe it clean gently with a filter paper

and dip it into the sample solution.

6) Wait for about one minute. Check that the standard switch is kept at up position.

7) Rotate slowly the range selector knob till the display shows maximum number of

significant figures.

8) Note down the reading shown in the display with an exponent of (-3).This is the

conductance of the sample.

SOP FOR POTENTIOMETER

1) Switch on the instrument and let it to warm up for about 10 to 15 minutes.

2) Switch on to standardization mode.

3) Now display must read standard potential1.018V.

4) If it does not read so, use screw driver and adjust it to 1.018 V.

SOP FOR pH METER



1) Switch on the instrument and let it to warm up for about 10 to 15 minutes.

2) Adjust the temperature knob to room temperature.

3) Rinse the electrode with distilled water before dipping in different solution and handle it

carefully as it is fragile.

4) Standardization of the instrument can be done by using the following buffers of pH =

4.00, 7.00 and 9.2.

5) First adjust buffer of pH= 4.00 followed by 9.2 any variation in pH of 4.00 and 9.2 value

can be adjusted using slope knob. Intercept knob is used to adjust a buffer value of 7.00.

6) Once it is standardized do not disturb the slope/intercept knob.



S O P F O R D I G I T A L F L A M E P H O T O M E T E R ( D F P ) C L - 4 1 0

The DFP consists of two units: 1. Main Unit (MU) & 2. Compressor Unit.(CU)

Operating Instructions :

1. Connect the gas tube from LPG cylinder to a fuel gas inlet located on LHS of MU

2. Connect the air tube from compressor to automiser of MU.

3. Connect CU to 230V electric main, switch on the electric supply and set the o/p pressure to 0.5

kg/cm2, using the knob provided alongside.

4. Dip the-automiser capillary tube in the beaker containing distilled water,

5. Connect a pipe at the base of MU for the drainage. The other end of the pipe may be kept in a

plastic mug.

6. Open (rotate anticlockwise) the Fuel Gas Valve (FGV) of the MU by approximately half turn.

7. Switch on the LPG cylinder regulator and immediately ignite the flame through the ignition

window.

8. Watch the flame through the flame view window. Do the fine adjustments of fuel flow with the

help of FGV to get a stable flame having well defined cones.

9. Connect MU to electric main & switch on the power supply to make the digital display

on.

10. Turn the Set FS knobs (both coarse & fine) as well as Set zero knobs (both coarse &fine) to

maximum clockwise position and sensitivity switch to high position.

11. Select the appropriate filter ( Na or K) with the help of filter selector of the MU.

12. Feed distilled water to the atomizer and wait for at least 30 sec.

13. Rotate Set zero (coarse) knob slowly till readout of the digital display approaches to zero.

Adjust Set zero (fine) knob to achieve precise zero setting.

14. Replace D/W with the standard solution of highest ppm and adjust the full scale deflection

to 100, with the help of Set FS coarse & fine knobs as well sensitivity switch.

15. The standard solutions of lower concentrations are then introduced in turn, and their respective

emission intensities are recorded. Note that in between any two solutions, D/W must be

aspirated and zero background emission intensity must be checked.---------------------------------------------------------------------------------------------------------------------



16. Unknown solution is finally introduced and its emission intensity is recorded.

17. After the completion of estimation, feed the distilled water to the atomizer & aspire it for

about 2 minutes to wash out remaining from the mixing chamber, atomizer etc.

18. Switching off the instrument:

i. First close the gas cylinder regulator.

ii. After the flame goes off, close the FGV (turn clockwise to maximum) of the MU.

iii. Switch off the power supply to MU.

iv. About two minute later, switch off the power supply to CU.



SOP FOR SPECTROPHOTOMETER CL-350

Operating Instructions

1. Plug-in the cable to electric main and switch on the instrument.

2. Allow the instrument to warm up for 15 minutes.

3. The display shows:

Operating mode

1. Single wavelength 2. Multi wavelength 3.Scan 4. Time scan

4. Select the required mode, say single wavelength by pressing 1.

5. Feed the desired wavelength, say 440 and press the ENTERkey.

6. This gives the following display:

1. ABS 2. % T 3.Conc.

Select the required output, say ABS by pressing 1.

7. This gives the chosen desired display. If correct press ENTER. (Else press BACKto go

to step 3).

8. Wait for the display: PUT REFERENCE......................

9. Then place the cuvette containing blank solution in the path of the light beam & then press

ENTER.

10.Wait for the display: PUT SAMPLE...................

11.Then place the cuvette containing standard solution in the path of the light beam and

then press ENTER.

12.Record the absorbance reading.

13.Press ENTERand wait for the display: PUT SAMPLE.......................

14.Replace the standard solution by another standard solution and press

ENTERtorecord the reading.

15.Repeat steps 13 & 14 to record the absorbance of remaining solutions.

***********************



Preparation of 1 N Solution of various chemicals

Name Weight / Volume

Acetic acid 57 cm3 CH3COOH in one liter water

Ammonium hydroxide 67 cm3 NH4OH in one liter water

Ferrous ammonium sulphate392 gm FAS + conc. H2SO4 in one liter

water

Ferrous sulphate 278 gm FeSO4 in one liter water

Hydrochloric acid 100 cm3 HCl in one liter water

Iodine 127 gm I2 + 200 gm KI in one liter water

Nitric acid 62 cm3 HNO3 in one liter water

Oxalic acid 63 gm H2C2O4 in one liter water

Potassim carbonate 63 gm K2CO3 in one liter water

Potassium dichromate 49 gm K2Cr2O7 in one liter water

Potassium hydroxide 56 gm KOH in one liter water

Potassium iodide 166 gm KI in one liter water

Potassium oxalate 92 gm K2C2O4 in one liter water

Potassium permangnate 32 gm KMnO4 in one liter water

Sodium bicarbonate 84 gm NaHCO3 in one liter water

Sodium carbonate 53 gm Na2CO3 in one liter water

Sodium hydroxide 40 gm NaOH in one liter water

Sodium thiosulphate 248 gm Na2S2O3 in one liter water



Succinic acid 59 gm (CH2COOH)2 in one liter water

Sulphuric acid 28 cm3 H2SO4 in one liter water



Preparation of various 0.1 N Solutions

Name Weight / Volume

Acetic acid 5.7 cm3 in one liter water

Ammonium hydroxide 6.7 cm3 in one liter water

Ferrous ammonium sulphate 39.21 gm in one liter water

Hydrochloric acid 10 cm3 in one liter water

Iodine 12.7 gm + 20 gm KI in one liter water

Nitric acid 6.2 cm3 in one liter water

Oxalic acid 6.33 gm in one liter water

Potassium dichromate 4.93 gm in one liter water

Potassium hydroxide 5.6 gm in one liter water

Potassium iodide 16.8 gm in one liter water

Potassium permangnate 3.16 gm in one liter water

Silver nitrate 17 gm in one liter water

Sodium carbonate 5.3 gm in one liter water

Sodium chloride 5.85 gm in one liter water

Sodium hydroxide 4 gm in one liter water

Sodium thiosulphte 24.82 gm in one liter water

Succinic acid 5.9 gm in one liter water

Sulphuric acid 2.8 cm3 in one liter water



MAIN TABLE REAGENT SOLUTION

Sr. NO. Preparation of dilute solutions required for side shelf

1Acetic acid CH3COOH

200 cm3 of conc. Acitic acid dissolve in one liter water

2Ammonium acetate CH3COONH4

40 gm of solid dissolve in one liter water

3Ammonium chloride NH4Cl


4Ammonium hydroxide NH4OH

200 cm3 of liquor ammonia in one liter water

5

Ammonium molybedate (NH4)2MoO2

Add mixture of 38 gm Ammonium molybedate and 25 gm Ammonium nitrate

to 62 cm3 conc HNO3 and make it one liter water.

6Ammonium oxalate (NH4)2C2O4

20 gm of solid dissolved in one liter water

7Ammonium sulphide

200 cm3 of ammonium hydroxide + 800 cm3 water and pass H2S gas

8Barium chloride BaCl2


9Barium nitrate BaNO3


10Calcium chloride CaCl

55 gm of solid dissolved in one liter water + 55 cm3 conc.HCl

11Cobalt nitrate CO(NO3)2


12Copper sulphate CuSO4


13 Di sodium phosphate Na2HPO4




14Ferric chloride FeCl3

50 gm of solid dissolved in one liter water + 10 cm3 conc HCl

15Hydrochloric acid HCl

800 cm3 water + 200 cm3 of conc. HCl

16Iodine solution I2

25 gm of iodine crystal and 50 gm KI dissolve in one liter water

17Lead acetate

70 gm of solid dissolved in one liter water + 10 cm3 acetic acid

18

Mercuric chloride HgCl2

17 gm of solid dissolved in one liter water in case insoluble dissolve in HCl

conc. 1.5%

19Nitric acid HNO3

800 cm3 water + 200 cm3 of conc. HNO3

20Potassium chromate K2CrO4


21Potassium chromate K2Cr2O7


22Sodium hydroxide NaOH


23Sulphuric acid H2SO4

900 cm3 water + 100 cm3 of conc. H2SO4



SIDE TABLE REAGENT SOLUTION

Sr. NO. Reagents required for various tests

1

2:4 DNP

5 gm of 2:4 DNP dissolve in 50 cm3 conc. H2SO4 make up to one liter with

methanol and filter if necessary.

2

Ammonium carbonate

Dissolve 160 gm of ammonium carbonate in the mixture of 140 cm3 of ammonia

and 860 cm3 of water

3Ammonium nitrate


4Ammonium thiocynate


5Bromine in chloroform

2 cm3 of liquid bromine in 98 cm3 of chloroform

6Bromine in potassium bromide

30 gm of bromine and 100 gm of KBr in one liter of water

7Bromine water

30 gm of bromine and 100 gm of KBr in one liter of water

8Calcium hydroxide

30 gm of solid dissolved in one liter water (use supernatant solution)

9Carbon tetrachloride

Carbon tetrachloride solution

10

Chlorine water

Add conc. HCl from separating funnel to round bottom flask containing KMnO4

delivery tube pass the gas formed to distilled water

11Chloroform

Chloroform solution

12 Dimethyl glyoxime



1 gm of solid dissolved in 100 cm3 of methanol / ethanol

13

Fehlings A

70 gm of copper sulphate dissolved in one liter water. Add dil H2SO4 drops if

necessary for clear solution

14

Fehlings B

Add mixture of 350 gm of sodium potassium tartarate and 100 gm of NaOH to

one liter water

15Ferric chloride (Alcoholic)

44 gm of ferric chloride dissolved in one liter methyl alcohol

16

Ferrous sulphate

10 gm of ferrous sulphate in little amount of water add 10 cm3 dil H2SO4 and

dilute to 100 cm3 with water

17Methyl red

1 gm in 100 cm3 methanol

18Methylene blue

0.1 gm in 100 cm3 water

19

Molybdate A

Dissolve 45 gm of ammonium molybdate in mixture of 40 cm3 of liquor ammonia

and 60 cm3 of water and add 120 gm of ammonium nitrate make up the volume to

one liter with water.

20

Molybdate B

Dissolve mixture of 38 gm of ammonium molybdate and 25 gm of ammonium

nitrate in 62 cm3 of conc HNO3 and make the volume up to one liter with water

21Sodium hydroxide in α – napthol

10 gm of α – napthol in 100 cm3 of 10% NaOH solution

22Sodium hydroxide in β – napthol

10 gm of β – napthol in 100 cm3 of 10% NaOH solution

23 Nesselers reagent



Add 10% KI solution to 5% HgCl2 solution till a precipitate form get just dissolve

and then add equal volume of 5% KOH solution to it

24 Oxine reagent

2 gm of solid in 100 cm3 of acetic acid

25Phenyl hydrazine

25 gm of substance in one liter of water

26Picric acid

50 gm of picric acid in 100 cm3 of ethanol

27Potassium ferricynide

55 gm of solid in one liter of water

28Potassium ferrocynide

53 gm of solid in one liter of water

29Potassium hydroxide (alcoholic)

10 gm of KOH in 100 cm3 of 50% ethanol

30Potassium iodide

5 gm of KI in 100 cm3 of water

31Potassium permangnate

3 gm of potassium permangnate in one liter of water

32Silver nitrate

5 gm in 100 cm3 of distilled water

33Silver sulphate

5 gm in 100 cm3 of water

34Sodium nitroprusside

10 gm of solid dissolve in one liter of water

35

Stannous chloride

3 gm of stannous chloride in 40 cm3 of conc. HCl and make up the volume up to

100 cm3



Section D

Projects for U.G. students

D – 1 Projects for F.Y.B.Sc. studentsD – 2 Projects for S.Y.B.Sc. studentsD – 3 Projects for T.Y.B.Sc. students



D – 1Projects for

F.Y.B.Sc. students



Project: 1

Aim:

Acidity of carbonated drinks

Experiment:

To determine the acidity of various carbonated drinks.

Requirements:

1. Cans of carbonated drinks,

2. pH meter

3. Bottle of 9.2 pH reference

4. Bottle of 4.0 pH reference

Procedure:

1. Standardize the pH meter with pH 4 and pH 9.2

2. Pour the 50 cm3 of the carbonated drinks in 100 cm3beakers.

3. Allow it to degas some time.

4. Measure the pH of each carbonated drinks.

Result:


Sr. No. Name of carbonated drink pH

1 Coke

2 Diet Coke

3 Thums up

4 Pepsi

5 Limca

6 Sprite


Project: 2

Aim:

To study the action of heat on hydrated copper sulphate crystals.

Procedure:

1) Take about 1.0 g of blue copper sulphate crystals in a test tube.

2) The test tube is fixed to a clamp and kept in an inclined position.( this is done to ensure

that any water vapour that condences on the upeer parts of the test tube does not trickle

back into the test tube) .

3) White anhydrous copper sulphate is placed ( in a watch glass ) below the open end of the

test tube.

Observation:

1) The blue solid in the test tube slowly turns white.

2) A mist of water droplets form on the upper cool portion of the test tube.

3) The white copper sulphate in the watch glass turns blue as the drops of water trickle

down onto it.

Conclusion:

Copper sulphate looses its water of crysallisation when heated and becomes white. On adding

water to anhydrous copper sulphate, copper sulphate once again recombines with a certain

amount of water and regains its blue colour.

Part-2

On very strong heating ,the white anhydrous copper sulphate decomposes to form black copper

oxide . Two colourless gases are liberated. The gases are acidic sulphur dioxide and neutral

oxygen.

CuSO4 . 5 H2O CuSO4 + 5 H2O

2 CuSO4 ---- 2 CuO + 2 SO2 + O2



Note.

Students are expected to study following

1.thermal decomposition of ferrous sulphate (7H2O) , sodium carbonate decahydrate , copper

carbonate , Zinc carbonate .



Project: 3

Aim:

A comparative study of L.R and A.R grade Na2CO3.

Experiment:

To determine the percentage purity of L.R and A.R grade sodium carbonate.

Requirements:

Sodium carbonate, 1M HCl, Methyl orange.

Procedure:

1) Weigh accurately 1.0 g of Na2CO3 and dissolve it in 25 cm3 of distilled water.

2) Titrate the above solution with 1M HCl using methyl orange as an indicator.

3) End point will be yellow to pink.

4) Repeat the procedure to get constant burette reading

Observation:

Part –I: L.R grade sodium carbonate sample.

Constant Burette reading = ____________ (A) cm3

Part –II: A.R grade sodium carbonate sample.

Constant Burette reading = ____________ (B) cm3

Calculation:

Part –I:

1 cm3 of 1M HCl = 0.05299 g of Na2CO3



A cm3 of 1M HCl = A X 0.05299

1

= ‘ X’ g of Na2CO3

% purity = X x❑1001

= ______________ % W/W

Part –II:

1 cm3 of 1M HCl = 0.05299 g of Na2CO3

B cm3 of 1M HCl = B X 0.05299

1

= ‘ Y’ g of Na2CO3

% purity = ' Y' x1001

= ______________ % W/W

Result:



Project: 4

Easy Identification of Adulteration in Food Materials

1. Turmeric

a. Turmeric is adulterated with Metanil yellow, to identify this, turmeric powder is

added to water & few drops of hydrochloric acid is added.

b. Redish color is developed.

c. If the turmeric powder is pure, this color disappears after few minutes.

d. If the turmeric powder is adulterated with Metanil yellow, the red colour remains

unchanged.

Observation:

Inference:

Adulterated/ Non-adulterated.

2. Sweets (Made of Mava)

a. Take a small piece of sweet and add about 1 ml of hydrochloric acid to it.

b. If purple colour develops then it indicates that the sweet is adulterated with metanil

yellow.



Observation:

Inference:


3. Pulses

a. Many times the pulses are coloured with metanil yellow.

b. To identify coloured pulses put a small quantity of pulses in water & add

hydrochloric acid. If yellow colour develops then it indicates that the pulses are

adulterated with metanil yellow.

Observation:

Inference:


4. Edible oil

1. Take about 1-2 ml of oil in a test tube and add 5 ml so alcoholic KOH solution

to it. Keep it in water bath with intermediate shaking



2. If the edible oil is adulterated with crude oil, two layers are observed. If pure the

oil dissolves in the alcoholic solution of KOH.

Observation:

Inference:




Project: 5

Aim:

To determine gravimetrically loss in weight of mild steel samples in 3 M and 6 M Hydrochloric

acid

Requirements:

Mild steel sample, Hydrochloric acid(3 M and 6 M),Acetone etc.

Procedure:

1. The two mild steel samples were washed with distilled water then with acetone and clean

with cotton.

2. Weigh the samples accurately.

3. Both the weighed samples kept in separate test tubes containing 5 ml of 3M and 5 ml Of 6

M HCl respectively for two hours.

4. After two hours the samples were taken out wash with water clean with cotton and weighed

accurately.

Observation:

samples Weight of samples

Before keeping in HCl After keeping in HCl

A __________ g ________g in 3M HCl

B __________ g ________ g in 6M HCl



Calculation:

1) For 3M HCl:

a) Loss in weight of sample A = (weight of sample ‘A’ before keeping in 3M HCl -

weight of sample ‘A’ after keeping in 3M HCl )

b) % loss in weight in 3M HCl = loss in weight ×100

Weight of sample ‘A’ before keeping in HCl

2) For 6M HCl:

c) Loss in weight of sample B = (weight of sample ‘B’ before keeping in 6M HCl -

weight of sample ‘B’ after keeping in 3M HCl )

d) % loss in weight in 6M HCl = loss in weight ×100

Weight of sample ‘B’ before keeping in HCl

Result:

1) loss in weight :

I) For 3M HCl = _______g

II) For 6M HCl = _______g

2) %loss in weight :

III) For 3M HCl = _______%

IV) For 6M HCl = _______%



D – 2Projects for

S.Y.B.Sc. students



Project: 1


1. Tea Powder

1) Many times ,used tea is coloured and sold in the market.

2) To identify this ,spread the tea powder on tissue paper and sprinkle some water on it

3) If the tea powder is coloured the colour spreads on tissue paper and adulteration can

be identified.

Observation:

Inference:

Adultrated/ Non-adultrated.

2. Dry red chilli

Many times Rhodamine B is used to colour Dry red chilli.

1) Take a red chilli from the sample and rub the outer surface with a piece of cotton

soaked in liquid paraffin. The sample is adulterated if the Cotton turns red.

Observation:

Inference:


3. Coffee powder

1) Coffee powder is adulterated with the dry seeds of tamarind. To identify this

adulteration, add the coffee powder to water.

2) The pure coffee powder settles at the bottom and the adulterated tamarind seeds

settle at the bottom.---------------------------------------------------------------------------------------------------------------------



Observation:

Inference:


4. Powdered sugar

1) Powdered sugar is adulterated with washing soda or baking soda.

2) If HCl is added to this , frothing indicates adulteration.

Observation:

Inference:




Project: 2

Aim:

To analyse the given sample of limestone for it’s loss on ignition

Theory:

Limestone mainly contains CaCO3 besides small amount of silica, Fe, Al, Ti etc. The loss on

ignition i.e. loss in weight due to loss of CO2 can be determined by heating a known quantity of

the ore in a muffle furnace at about 10000C for about 90 minutes to constant weight.

CaCO3 CaO +2 CO

Procedure:

1. Dry the limestone ore in an oven by heating it at 1100C for about 60 minutes.

2. Weight accurately one g of the dried sample in a previously weighted silica crucible.

3. Heat the crucible and it’s contents slowly on a burner for about 30 minutes.

4. Transfer the hot crucible along with it’s contents to a muffle furnace and heat it for

about 60 minutes.

5. Remove and cool crucible. Then weigh. Continue the heating and cooling procedure till

constant weight is obtained.

6. As CaO residue is hygroscopic in nature, for cooling each time the crucible should

be transferred to a desiccators. This weight can be used for calculating loss on

ignition.



Project: 3

Aim:

To determine the amount of calcium present in the given Sample. (Ostocalcium)

Requirements:

EDTA, 2N HCl, Ammonia buffer, Mordant black –II indicator.

Procedure:

1) Prepare 0.1 M EDTA solution (Dissolve 3.725 g EDTA in 100 cm3 of standard flask, with

distilled water)

2) Weigh accurately 0.400 g of sample (ostocalcium)& transfer it to a 250 cm3 conical flask.

3) Add 15 cm3 of dil. HCl and 100 cm3 of distilled water stir the solution to dissolve the

sample completely.

4) Add 15 cm3 of ammonia buffer and 5-6 drops of mordant black-II solution as indicator.

5) Titrate immediately with 0.1 M EDTA till colour changes sharply from pink to permanent

blue.

Calculation:

Calcium content=M ×V ×0.04W

Where, M = Molarity of EDTA

V = Volume of 0.1 M EDTA

W = Weight of the sample

Result:

Amount of calcium present in the given sample =_______



Project: 4

Aim:

To determine percentage of chloride present in the given sample (Soup powder)

Requirements:

a. Silver Nitrate (0.1N)

b. Potassium Chromate indicator 5% (W/V)

Procedure:

1) Weigh accurately 0.500 g sample (Soup powder) & transfer it to conical flask.

2) Add 75 cm3 of distilled water & stir the solution for 10 minutes.

3) Add 1 cm3 of potassium chromate indicator and titrate with 0.1N silver nitrate solution to

the first appearance of brick red colour.

Calculation:

% of chlorideexpressed as NaCl=N × V × 5.8443w

Where, V= Volume of silver nitrate consumed in the reaction

N = Normality of the silver nitrate solution

w = Weight of the sample taken

Result:

% of chloride present in the given sample = _____________



Project: 5

Fractional Distillation Experiment

Aim:

To separate a nearly ideal solution of cyclohexane (bp 81° C) and toluene (bp 111° C) using

simple and fractional distillation.

Theory:

Distillation is the most common method used to separate and purify liquids.

The process consists of heating a liquid to its boiling point and the vapors are passed through the

condenser. The condensate is then collected.

The vapor pressure of a liquid is defined as the pressure that is exerted by a liquid at the given

temperature. This force is due to the molecules escaping from the liquid’s surface into the gas

phase.

The boiling point of a liquid is that temperature at which the vapor pressure is equal to the

pressure of the surroundings. The boiling point of a liquid is determined by placing a

thermometer in the vapor.

The temperature of the vapor will remain constant throughout the distillation if the vapor is pure.

The boiling point at a given pressure is a characteristic property of the pure compound.

Procedure:

1. Set up the simple distillation assembly using fractionating column apparatus on sand bath

as per the demomnstration, using a 100 ml round bottom flask.

2. Lubricate the ground glass joints with silicone grease. Get the distillation assembly

checked by your teacher.

3. Add a boiling chip before heating the solvents.

4. Add 30 ml of cyclohexane and 30 ml of toluene to your distillation flask.

5. Heat the distillation assembly on medium flame.

6. Heat the round bottom flask on the sand bath until the distillate drops at a regular rate of ---------------------------------------------------------------------------------------------------------------------



approximately 1 drop per second. ( boiling range 78-83° C)

7. Measure volume of cyclohexane collected.

8. After cyclohexane has been distilled out, the vapour temperature will rise & toluene will

start distilling. ( boiling range 109-114° C)

9. Record the temperature as the distillate starts to collect in the test tube/ flask.

10. Never distill to dryness!

11. Allow the apparatus to cool until it is comfortable to handle distillate.

Result:

1. Volume of cyclohexane collected = ------- cm3

2. Boiling range of cyclohexane = ------ ° C

3. Volume of toluene collected = ------- cm3

4. Boiling range of toluene = ------ ° C



Project: 6

POTENTIOMETRY

Aim:

To determine amount of HCl in the given solution potentiometrically. (Using quinhydrone

electrode)

Requirement:

Potentiometer, Calomel electrode, Platinum electrode, salt bridge, 0.1 N NaoH, HCl.

Procedure:

1) Dilute given solution to 100 cm3 with distilled water. Pipette out 10cm3 diluted solution

2) In a 100cm3beaker. Set up the cell as given

SCE II quinhydrone electrodeI Pt

3) Add 0.5 cm3 of 0,1 NaOH from burette, stir the solution well and record emf of the

solution. Repeat this till negative emf is obtained.

4) Plot E VS V and ∆E VS ∆V to determine equivalence point and calculate the amount of

HCl in the given solution.



Project: 7

POLARIMETER

Aim:

To determine the amount of fructose in the given sample solution.

Requirement:

Polarimeter, Fructose injection / powder, 5M Ammonia, Distilled water.

Procedure:

1) To an accurately measured volume containing (approximately 5.0 g) fructose, add 2

cm3of 0.5 M ammonia and sufficient water to make the volume 100 cm 3. Mix well

2) And allow to stand for 30 mins. Determine optical rotarion in a 2 dm tube.The observed

rotation in degrees multiplied by 0.5427 represents the weight in gm of Fructose C6H12O6

in the volume taken for assay.



Project: 8

Synthesis of acetanilide

Aim:

To prepare acetanilide from aniline using Microwave

Requirements:

Aniline, Acetic anhydride, conc. H2SO4

Procedure:

Take about 1 cm3 of aniline in a 150 cm3 dry conical flask. Add about 2 cm3 of acetic anhydride

and two drops of conc. H2SO4. Heat the mixture using a microwave for 1 min. cool and pour the

contents in 20 cm3 of ice cold water in a beaker with constant stirring to obtain crystals of

acetanilide. After 5 mins. filter the crystals, wash with water, recrystallise with hot water, dry

and determine its m.p.

Reaction:

Result:

Melting point of the product = _________0 C (expected m.p. 1140C)



D – 3Projects for

T.Y.B.Sc. students



Project: 1

ACETYLATION OF PRIMARY AMINE

(Preparation of acetanilide)

Conventional Procedure:

Non-green Components:

Use of chlorinated solvent like CH2Cl2

Pyridine is also not eco-friendly

Acetic anhydride leaves one molecule of acetic acid unused (not atom-economic)

Alternative Green Procedure:

Chemicals Required:

Aniline - 10 ml (10.2 g)

Glacial acetic acid - 30 ml

Zinc dust - 0.5 g

A mixture of aniline (10 ml) and zinc dust (0.5 g) in acetic acid (30 ml) in a 100 ml round bottom

flask was heated over a gentle flame using water condenser. Heating was continued for about 2

hrs. The reaction mixture was then carefully poured in cold water (100 ml) in a 250 ml beaker

with cooling and vigorous stirring. The shining crystals of acetanilide were separated slowly.

After 15 min. the acetanilide crystals were collected by filtration. The solid crystals were washed

over the Buchner funnel with water and the product was dried (yield, 10 gm). It was crystallized

in boiling water. (If necessary, decolorizing charcoal may be used), m.p. 114 ̊C.



Yield: 10 g (91%)

Analysis: Using TLC

Green Context:

Avoids use of acetic anhydride (usage banned in some states, due to its utility in narcotic

business), Minimizes waste by-products, Avoids hazardous solvent.

Mechanism:



Project: 2

Aim:

Analysis of ferrous gluconate tablets

Ferrous gluconate tablet contain not less than 90.0 percent and not more than 105.0 percent of

the stated amount of ferrous gluconate, C12H22FeO14,2H2O

Usual Strength:

300 mg (300 mg of ferrous gluconate is approximately equivalent to 35 mg of ferrous iron )

Tests:

Ferric Iron - weigh accurately a quantity of the powder prepared for the assay,containing

about5.0 g of ferrous gluconate, in a stoppered flask, dissolve as completely as possible without

the aid of heat in a mixture of 100 ml of freshly boiled and cooled water and 10 ml of

hydrochloric acid, add 3 g of potassium iodide, close the flask and allow to stand in dark for 5

minutes. Titrate the liberated iodine with 0.1 M sodium thiosulphate using starch solution, added

towards the end point of the titration, as indicator. Repeat the operation the operation without

the substance under examination. The difference between the titrations represents the amount of

iodine liberated by the ferric ion. Not more than 11.2 ml of 0.1 M sodium thiosulphate is

required.

Assay:

Weigh and powder the 20 tablets. Weigh accurately a quantity of the powder containing about

1.0 g of ferrous gluconate , dissolve in a mixture of 140 ml of water and 60 ml of 1 M sulphuric

acid and titrate with 0.1 M cerric ammonium sulphate, using ferroin as indicator, until the red

colour disappears.

1 ml of 0.1 M cerric ammonium sulphate, is equivalent to 0.04822g of C12H22FeO14, 2H2O.

Storage:



Store protected from light.

Labelling:

The label states the quantity of the active ingredient both as the amount of ferrous gluconate and

in terms of the equivalent amount of ferrous iron in each tablet.



Project: 3

Aim:

Analysis of cyanocobalamin Injection.

Vitamin B12 injection

Cyanocobalamin Injection is sterile solution of cyanocobalamin in water for injections

containing sufficient acetic acid or hydrochloric acid to adjust the pH to about 4. It may contain

suitable buffering agents.

Cyanocobalamin injection containnot less than 95.0 percent and not more than 110.0 percent of

the stated amount of anhydrous cyanocobalamin,C63H88 CoN14O14P.

Usual Strength:

The equivalent of 500μg and 1 mg of anhydrous cyanocobalaminper ml.

Assay:

Carry out the following procedure protected from light

The Dilute the injection if necessary , with water to produce a solution containing not more than

equivalent of 0.0025 percent w /v of anhydrous cyanocobalamin and measure the absorbance at

about 361 nm. Calculate the content of C63H88 CoN14O14P taking 207 as the specific absorbance

at 361 nm.

Storage:

Store protected from light in single dose or multiple dose containers.

Labelling:

The label states the strength in terms of the equivalent amount of anhydrous cyanocobalamin, in

a suitable dose-volume.

Project: 1



Project: 4

SPECTROPHOTOMETRIC STUDY OF THE REACTION OF POTASSIUM IODIDE WITH POTASSIUM

PERSULPHATE

Aim:

To determine the order and rate expression of the reaction of potassium iodide with potassium

persulphate spectrophotometrically.

Theory:

The rate of a reaction can be followed spectrophotometrically if one of the reactants or products

absorbs light strongly and distinctly from the other reactants and products. The rate of the

reaction is represented by the slope of the line in a graph of absorbance vs. time. A reaction

is first order if an increase in concentration produces the same increase in rate, that is, if doubling

the concentration of a reactant doubles the rate, the reaction is first order in that reactant. If

doubling the concentration of a reactant causes a four fold increase in the rate, then the reaction

is second order in that reactant. If doubling the concentration causes an eight fold increase in

rate, then the reaction is third order in that reactant.

In the reaction between KI and K2S2O8, the triiodide produces a yellow solution that

absorbs light in the 350 nm region. The reaction is as follows:

Thus, the absorbance increases as more of the triiodide ion is produced. From the graph of

absorbance versus time, the slope of the line for a reaction is the rate of that reaction.

Equipment/Materials:

0.02 M KI solution, 0.02 M K2S2O8 solution, distilled water, spectrophotometer, cuvettes, 10

mL graduated pipette, 2 small test tubes, parafilm, tissue paper, etc.


S2 O82− + 3 I− → 2 SO

4 2− + I3−


Procedure:

1. Switch on the spectrophotometer and set the wavelength to 350 nm.

2. Place 2 ml of KI and 2 ml of distilled water into a cuvette to serve as blank. Cover with a

piece of parafilm and invert several times to mix.

3. Insert the blank into the spectrophotometer. Set the absorbance to zero.

4. Place the required amount of KI and water into a cuvette and place the required amount of

potassium persulphate into a small test tube (as given in the following table).

Set – 1 Set – 2 Set – 3 Set – 4

Vol. KI (cm3) 1 2 1 2

Vol. H2O (cm3) 2 1 1 0

Vol. K2S2O8 (cm3) 1 1 2 2

5. Quickly pour the contents of the test tube into the cuvette (start the timer immediately at the

instant the liquid are mixed). Cover the cuvette with parafilm and invert three times.

6. Insert the cuvette in the sample compartment. Record the absorbance every 15 seconds in the

data table. Consider the absorbance at time 0 to be 0.

7. When the run is complete, remove the cuvette and clean thoroughly.

8. Repeat steps 4-7 for remaining three sets of solutions. Only mix up the components for one

set at a time.

9. Plot absorbance versus time and determine the slope of each run. Plot all the graphs on the

same piece of paper (use a different colour of ink for each set).



Data table:

Time (s)ABSORBANCE

Set – 1 Set – 2 Set – 3 Set – 4

0

15

30

45

60

75

90

105

120

Calculations:

[KI] [K2S2O8] Rate (slope of the graph)

Set – 1

Set – 2

Set – 3

Set – 4

The concentrations can be calculated by using the formula M1V1= M2V2

Once the concentrations of each reactant and the rate of the reaction are known, the order

of each reactant can be calculated using the following formulae:


yx Rate 3

Rate1= ( [ S2 O

82− ]3

[ S2 O82− ]1 )Rate 2

Rate1= ( [ KI ]2

[ KI ]1 )


Thus, order of the reaction with respect of KI is ‘x’ and

with respect to K2S2O8 is ‘y’. The, overall order

of the reaction is ‘x+y’.

Results:

1. Overall order of the reaction is ………….

2. Rate expression, Rate =


Rate expression= [ KI ]x [ K 2 S2O8 ]y


Project: 5


1. Ingredient : green vegetables, Adultrrant : Malachite Green

Green vegetables like Bitter Gourd, Green Chilly and others Malachite Green Take a small part of

the sample and place it on a piece of moistened white blotting paper. The impression of color on

the paper indicates the use of malachite green, or any other low priced artificial color.

Observation:

Inference:


2. Ingredient : Coriander powder , Adulterant: Saw Dust

Take a little amount (a half of tea-spoon) of the sample. Sprinkle it on water in a bowl. Spice

powder gets sedimented at the bottom and saw-dust floats on the surface.

Observation:

Inference:


3. Ingredient: Coffee powder, Adulterant: Cereal starch ,

Take a small quantity (one-fourth of a tea-spoon) of the sample in a test tube and add 3 ml of

distilled water in it. Light a spirit lamp and heat the contents to colouri2e. Add 33 ml of a solution of

potassium permanganate and muratic acid (1:1) to decolourize the mixture. The formation of

blue colour in mixture by addition of a drop of 1% aqueous solution of iodine indicates adulteration

with starch.



Observation:

Inference:


4. Ingredient : Milk, Adulterant : Urea

Take tea spoon of milk in attest tube , add ½ tea spoon of soyabean powder. Mix up the contents

thoroughly by shaking the test tube. After 5 minutes dip a red litmus paper in it. Remove the

paper after ½ minute. A change in colour from red to blue indicates the presence of uera in it.

Observation:

Inference:


5. Ingredient : Iodised salt , Adulterant : Common salt.

Cut a piece of potato, add salt sample and wait for a minute and add 2 drops of lemon juice. if

salt is iodised,blue colour will develop. In case ofcommon salts, there will be no colour.

Observation:

Inference:


6. Ingredient - Processed food, sweets & syrups,Adulterant : Rhodamine B.



Take half teaspoon of the sample in a test tube. Pour 3 cm3 of carbon tetrachloride and shake

the test tube to mix well. If the food contains Rhodamine B, then first the mixture turns

colorless and addition of a drop of hydrochloric acid brings the color back

Observation:

Inference:




Project: 6

Estimation of Calcium in Milk

Equipment Required:

1. Single channel flame photometer

2. Calcium filter

Blank Preparation:

2.5ml of diluted hydrochloric acid, 2.0ml 10% lanthanum chloride, make up to 100ml

with distilled water to give reagent blank.

Standard Preparation:

Place 1.249gm A.R. calcium carbonate in approximately 50ml H20, adding dropwise

concentrated hydrochloric acid until calcium carbonate is dissolved (should take about 10ml).

This will give 500 ppm stock calcium standard.The stock solution should be diluted to give

standards of 2.5, 5.0, 7.5 and 10 ppm Ca2+

Sample Preparation:

Place 4gm (accurately weighed) of milk in a dry silica crucible. Ash sample at 500-525°C

oven. When cool, dissolve ash in 5ml of 1:4 diluted concentrated hydrochloric acid. Transfer to

100ml volumetric flask; make up to mark. Filter through Whatman filter paper, pipette 50ml of

filtrate into 100ml volumetric flask. Add 2ml of 10% lanthanum chloride. Make up to mark with

distilled water.

Method:

1. Spray reagent blank, set zero

2. Spray 10 ppm standard set full scale

3. Reset zero

4. Spray intermediate standards, note readings, construct calibration curve



5. Spray test samples and note readings

This gives you calcium in parts/million of calcium for milk. If percent calcium required multiply

Ca2+ ppm sample reading by 0.025 = percent Ca2+ in milk. Normal level for milk is

approximately 0.11%.

Result:

The Ca content in given milk sample is-----------ppm.



Project: 7

Aim:

Extractive Spectrophotometric determination of Nickel using dimethyl glyoxime.

Theory: Dimethyl glyoxime gives a scarlet red precipitate with nickel in alkaline medium.

Nickel(II) dimethylglyoximate is slightly soluble in chloroform and other organic solvents.

Since the solubility of Nickel(ll) dimethylglyoximate in water is much less than in chloroform,

small amounts of nickel can be effectively be extracted. The optimum pH range for the

extraction of nickel complex is 7 to 12 in the presence of citrate. The nickel complex in

chloroform absorbs at 366 nm and can be determined spectrophotometrically.

Requirements:

1. Standard Nickel ion solution : Dissolve 0.135 g of nickel ammonium sulphate

(A.R.) NiSO4.(NH4)2SO4.6 H2O in small quantity of distilled water and dilute to

1 dm3 in a standard measuring flask. 1 cm3 of this solution contains 20 vg of

Ni(II).

2. Dimethyl glyoxime reagent: Dissolve 0.500 g of dimethyl glyoxime in 250 cm3

of ammonia solution and dilute to 500 cm3 with distilled water.

Procedure:

I. Calibration Curve:

1) Transfer 2.5, 5.0,7.5,10.0, and 12.5 cm3 of standard nickel solution ( 20 pg/ cm3) in five

different standard measuring flasks and add 5 g of citric acid in each flask.

2) Add distilled water to make up the volume to 100 cm3 and add dilute ammonia solution

to obtain PH 7.5

3) Cool and transfer each solution to a separate 250cm3 separating funnels.

4) Add 20 cm3 DMG solution. Shake well and after standing for 1-2 minutes, add 10 cm3 of

chloroform to it.

5) Shake individually every funnel for 1 minute. Allow the phases to settle. Separate the

yellow chloroform layer in each case and collect it in 25 cm3 standard measuring flask.



6) Repeat the extraction of aqueous phase with additional 10 cm3 of chloroform and collect

the chloroform extract in the same 25 cm3 standard measuring flask.

7) Dilute each solution to the mark with chloroform.

8) Measure absorbance of each solution at 366 nm against blank reagent.

9) Constuct a calibration curve from the above readings.

II. Estimation of unknown Ni(II) solution.

1) Dilute the supplied sample solution of unknown concentration to 250 cm3 with distilled

water.

2) Transfer 10 cm3 of the diluted solution in a 250 cm3 beaker.

3) Treat the solution in the same manner as explained earlier.

4) Determine the concentration of nickel ion in the sample solution with the help of

calibration curve.

III Observation Table

Flask

No.

Volume of (cm3) Concentration of

Ni+2 ions in pg/ 25

cm3

AbsorbanceStandard

nickel

0.1 %

DMG

Final

0 0.0 20 25 0.01 2.0 20 25 4.02 4.0 20 25 6.03 6.0 20 25 12.04 8.0 20 25 16.05 10.0 20 25 20.06 10.0

( Sample)

20 25 (Unknown)

Graph:

Plot a graph of concentration of nickel in µg against absorbance and determine

concentration of sample.

Calculations: The amount of nickel present in 10 cm3 of the given sample solution ( from

graph) = x µg.

10 cm3 of the diluted sample solution = x µg of Ni(II)---------------------------------------------------------------------------------------------------------------------



250 cm3 of the diluted sample solution = 25 x µg of Ni(II)

Amount of Ni(II) present in the given solution = 25 x µg = (25 x) 10-3 mg.

Result:

Amount of Ni(II) present in the given solution =



Project: 8

N – Acetylation of aromatic primary amine

Aim:

To prepare acetanilide from aniline.

Theory:

Replacement of active hydrogen of –NH2 group by an acyl group (-COCH3) is called N-

acetylation of primary amine. Acetylation can be carried out by using acetic anhydride or acetyl

chloride.

Reaction:

Procedure:

1) Place the given quantity of aniline, 4ml of acetic anhydride and a drop of conc. H2SO4 in

250ml conical flask.

2) To the aniline solution add 3cm3of acetic anhydride with constant stirring.

3) Heat the reaction mixture on boiling water bath for 15-20 min pour the contents into 50cm3

of ice cold water.

4) Filter the solid product with suction pump or common. Wash with cold water.

5) Recrytallize the product from hot distilled water.

6) Dry and weight and determine m.p. of the purified product.



Observation & Calculation:

Density of aniline = 1.023 g/cm3

Weight of product = _________ gm

Theoretical Yield:

93gm of aniline gives 135gm of acetanilide

V ×1.023 g=135×V ×1.02393 = __________________(Y)g of acetanilide.

Value of V (in cm3) will be supplied.

Percentage Yield:

Y gm of product corresponds to 100% yield

X g ---------------- ¿100× X

Y = ______________ Z %

Rf value¿Distance travelled by soluteDistancetravelled by solvent

Result:

1) Melting point of the product = ____________0 C

2) Weight of product =_____________ g

3) Theoretical yield =_____________ g

4) Percentage yield =_____________%

5) Rf value (Match) given product = _____________



Project: 9

PREPARATION OF CARBON NANOTUBES FROM GRAPHITE POWDER

Requirments:

Graphite Powder (99.95% purity,45µm, Aldrich), Nitric acid(fuming), Sulfuric acid (AR Grade),

Potassium chlorate (KClO3), Ultra-sound sonicator, etc.

Procedure:

Add slowly 5.0 g. of graphite to a mixture of fuming nitric acid (25 cm3) & sulfuric acid (50

cm3) over a period of 30 minutes. After cooling the mixture down to 50C in an ice bath, add 25 g

of potassium chlorate slowly with stirring for 30 minutes. Heat the solution upto 70 0C for 24

Hrs*. and then place in the air for 3 days. Most graphite precipitate at the bottom, but some

reacted carbons float. Transfer the floating carbons into DI water. Stir the solution for 1 hour and

filter it immediately. Dry the tubes and analyse. Characterize the CNT’s with the help of SEM,

TEM results.

*Modifications to be tested with the procedure:

Ten times reduction in the time of heating by following a tech. of heating (at 70 0C) + ultra-

sonication of the reaction mixture.

Observation:

Conclusion:

A cheap and simple chemical method for producing CNT’s ( with an approx. diameter of 14-

18nm) in liquid solution at 70 0C without any pressure treatment.



Project: 10

Aim:

Determination of solubilities of inorganic solid in water at different temperatures (Greener

approach)

Apparatus/ Instruments:

Analytical balance with accuracy of ±0.0001g, A grade standard flasks of capacity 5 ml, 10 ml

and 25 ml (three number of eachBorosil make with certificate), small size glass funnels to fit in

these flasks, wash bottle, Fine stainless steel spatula ( 5 numbers),thermostat with accuracy

±0.01°C, Thermometer with accuracy ±0.01°C, graduated test tubes.Glass distillation apparatus,

Hot air drier for chemical apparatus(handy).

Chemicals:

Solid KCl, distilled water, distilled acetone for drying

Procedure:

1. Weigh about 1.0000g, 3.0000g and 10.0000g of solid and add in 5 ml, 10 ml and 25 ml

dry standard flasks respectively by butter paper. This makes 20%, 30% and 40%

mixtures. Add distilled water in small increments by wash bottle and shake the flask

carefully in order to dissolve the solid.Dilute the flaskafter the equilibrium has

established. Check in which flask it has remained insoluble.

2. Insert the flasks in thermostate at 10.00°C and 20.00°C higher temperatures

3. Select the pilot solubility percentage range in which solid remains soluble at room

temperature as well as 10.00°C and 20.00°C higher temperatures.

4. Determine accurate solubility by further selecting appropriatepercentages(by adding

0.0500g )of above solid at room temperature and at 10.00°C and 20.00°C higher

temperatures.



5. Collect all KCl solutions in a container. The water evaporates and KCl solid can be

reused or can be used for preparing saturated KCl solution. Plot the graph of temperature

Versus solubility.

Observations and Calculations:

Sr.

No.

Temperature Weight of KCl

(w)

Volume of

water(V)

Solubility (w/V) g/cm3

1

2

3

Result:

1. The solubility of KCl in water is _______ g/cm3 2. The nature of graph_______



Project: 11

Spectrophotometric Determination of Iron in Vitamin Tablets

Principle:

In this experiment, iron from a vitamin supplement tablet is dissolved in hydrochloric acid and

thenreduced to Fe+2with hydroquinone:

While freshly-dissolved Fe+2in aqueous solution is nearly colorless, we can impart an intense

redcolor by a stoichiometric reaction of Fe+2with three molecules of o-phenanthroline:

The complex, which is often written as Fe(phen)3+2, has a maximum in its absorption spectrum

close to 510 nm (the literature value for λmax is 508 nm.) Measuring the solution’s absorbance

at

λmax is therefore an accurate method of determining Fe concentration.

Both standard solutions of Fe(phen)3+2and a solution with Fe from vitamin tablet has to be

prepared, and measure their absorbance on Spectrophotometer/Colorimeter. Construction of a

calibration curve will allow you to determine both the molar absorptivity of the Fe(phen)3+2

complex, and the milligrams of Fe in vitamin tablet.

Experimental Procedure



A. Reagents required:

Hydroquinone: Solution containing 10 g/L in water.(90mM)

Sodium citrate: 25 g/L in water.(96mM)

o-Phenanthroline: 2.5 g in 100 mL of ethanol and 900 mL of water. (The ethanol helps

dissolve the rather non-polar o-phenanthroline.),13.87mM

Stock Fe+2(nominally 0.04 mg Fe/mL): Prepare by dissolving 0.28 g of reagentgrade

Fe(NH4)2(SO4)2·6H2O in water in a 1L volumetric flask containing 1 mL of98 wt %

H2SO4.0.714mM .

B. Wet Chemistry Procedures

1. Place one tablet of an iron-containing vitamin (note which brand you use and the nominal

mass of iron per tablet) in a 100-mL beaker and boil gently with 25 mL of 6 M HCl for

15 min. Filter the solution directly into a 100-mL volumetricflask using qualitative filter

paper. Wash the beaker and filter paper several times withsmall portions of water to

complete a quantitative transfer. If some insoluble bits make itthrough the filter paper, re-

filter solution before proceeding. Allow the solution tocool, dilute to the mark, and mix

well. (Note that is important to let the solution cool beforediluting, since volumetric flask

marks are accurate only at room temperature.) Dilute 5.0mL of this solution to 100.0 mL

in a fresh volumetric flask. If the label indicates that thetablet contains <15 mg of Fe, use

10.0mL instead of 5.0 mL. This is our unknownsolution.

2. Pipette 10.0 mL of the Fe+2stock solution into a beaker and measure the pH with indicator

paper accurate to the nearest pH unit. Add sodium citrate solution 1 drop at a time until a

pH of ~3.5 is reached. It will require at least 3.5 mL.

3. Pipette a fresh 10.0-mL aliquot of the Fe+2stock solution into a 100 mL volumetric flask

and add the same number of drops of citrate solution that was required in Step 2. Add 2.0

mL of hydroquinone solution and 3.0 mL of o-phenanthroline solution, dilute to the mark

with water, and mix well by inverting at least 20 times. Then prepare three more standard

solutions with 5.0, 2.0, and 1.0 mL aliquots of Fe+2stock solution, and prepare a blank

solution containing no Fe+2. All five solutions, including the blank, should contain 2.0 mL ---------------------------------------------------------------------------------------------------------------------



of hydroquinone solution and 3.0 mL of o-phenanthroline solution. The goal is to make

the matrix in all five solutions as similar as possible. However, add sodium citrate

solution in proportion to the volume of Fe+2solution. (For example, if 10 mL of Fe+2stock

requires 7 mL of citrate solution, 5 mL of Fe+2stock requires 3-4 mL of citrate solution.)

4. Take a 10.0 mL aliquot of your unknown solution (which is made in Step 1) and find out

how many drops of citrate solution are needed to bring the aliquot’s pH up to ~3.5.

5. Transfer a fresh 10.0mL aliquot of unknown solution to a 100 mL volumetric flask. Add

the required amount of citrate solution determined in Step 4. Then add 2.0 mL of

hydroquinone solution and 3.0 mL of o-phenanthroline solution; dilute to the mark and

mix well.

6. Let the solutions stand for at least ten minutes before making any

absorbancemeasurements.

C. Spectroscopic Measurement:

To each solution (unknown sample and standard solutions) at 510 nm using

Spectrophotometer/ Colorimeter.

D. Data Analysis

1. Make a graph of absorbance versus the molarity of Fe in the four standards. Plot all

twelve points on one graph. Be sure that you have accurately calculated all dilution

factors. Calculate the slope (m), and y-intercept (b).

using, A= ε × C× l ( beer –lamberts law.

2. Using the slope of your calibration curve and the assumption that the cuvette path length

is exactly 1.00 cm, calculate the molar absorptivity ε of Fe(phen)3+2at λmax (molar

absorptivity ε literature value of 11000 M-1cm-1.)

3. Using the equation of your calibration curve to determine the molarity of Fe in your

unknown solution.

Result:---------------------------------------------------------------------------------------------------------------------



Given vitamin tablet contains______________µg/ml iron.

Molar absorptivity of (ε) of Fe(phen)3+2 = _______ /µ. cm



Project: 12

TRANSESTERIFICATION REACTION

(Synthesis of biodiesel)

Introduction:

This experiment focuses on synthesis of diesel fuel from vegetable oil. The mechanism involves

a transesterification reaction, the process of transforming one type of ester into another type of

ester.

Green reaction:

Chemicals required:

Vegetable oil - 100 ml

Methanol - 20 ml

Sodium hydroxide - 3 pellets

Green Procedure:

The finely ground anhydrous NaOH was added into pure (99% or higher purity) methanol (20

ml) in a 250 ml Erlenmeyer flask and stirred vigorously until all the NaOH was dissolved. The

pure vegetable oil (100 ml) was warmed to about 40 oC in a 250 ml beaker. The warmed up oil

was poured into the methoxide solution with continuous stirring. At first the mixture would

become cloudy, but should soon two layers would separate. This was stirred for 15-20 minutes.



The contents of the flask were transferred into a 250 ml separatory funnel. The mixture will

separate into two different layers. The glycerol will fall to the bottom, and the methyl ester

(biodiesel) will float to the top. Allow the experiment to sit for an hour. The stopcock of the

separatory funnel was opened and the glycerol was allowed to drain into a small beaker.



Project: 13

Synthesis of schiff’s base using Microwave

Aim:

To prepare schiff’s base from aniline and benzaldehyde using microwave and compare its yield

with that of conventional method.

Requirements:

Aniline, benzaldehyde,lime juice.

PROCEDURE:

Take about 2 cm3 of aniline and 2 cm3 of benzaldehyde in dry conicalflask, add about 5-6 drops

of fresh lime juice carry out the reaction in microwave for 45 secs. Cool the mixture to obtain

product. Filter the solid,wash with water, recrystallise the crude product from about from

absolute alcohol. Dry weigh and determine the melting point of the product.

Reaction:

Observation:

1) Weight of the product = ________ g

2) Theoretical yield =_________g

Result:

1. M.P of the product =_________ g

2. Percentage yield (using microwave) =_________ g

3. Percentage yield (using conventional method) = _________g

Inference:



Project: 14

SYNTHESIS OF ZINC OXIDE NANOPARTICLES BY PRECIPITATION METHOD

Aim:

To synthesize zinc oxide nano particles by the alkaline precipitation method.

Chemicals Required:

Zinc acetate dihydrate, sodium hydroxide, triethanolamine, ethanol.

Apparatus required: 250 ml Round bottom flask, 50 ml measuring cylinder, magnetic stirrer with

temperature control.

Theory:

The unique properties of nanomaterials have motivated the researchers to develop a simpler,

rapid and an inexpensive technique to produce nanostructures of technologically important

materials. Nano-structure zinc oxide, an n-type II-VI compound semiconductor has widerange

applications ZnO nanoparticles can be prepared on a large scale at low cost by simple alkali

precipitation. .This study is aimed at the synthesis of ZnO nanoparticles from zinc acetate dihydrate

and sodiumhydroxide in the ethanol rich phase using triethanolamine (TEA) as surface acting

agent..

Procedure:

1. Prepare zinc acetate solution by dissolving 0.001 mole of Zn(CH3COO)2.2H20 in 50

ml of water.

2. Prepare the alkaline mixture solution by dissolving NaOH (0.002 mole) and TEA

(0.003 mole) in 100 ml of absolute ethanol.

3. Stir the mixture until a homogeneous solution is obtained

4. Add the zinc salt solution into the alkaline mixture solution and subject it to magnetic



stirring at 60-70°C for 2 hours.

5. After 2 hrs, allow the product to cool naturally at room temperature.

6. Wash the resulting product with ethanol to remove the organic agent TEA and hydroxide

ions and filter and dry in oven at 60°Cfor 3 hours.

Result:


Documents

Submission of Proposal under Star College · Web viewA method involving systematic study of performance of a process is called scientific method. Various types of experiments of routine