SHIVAJI UNIVERSITY, KOLHAPUR Schedule... · SHIVAJI UNIVERSITY, KOLHAPUR Practical Examination in Chemistry at the B. Sc. Part-II March/April, 2015 Chemistry Practical ENCLOSURES

SHIVAJI UNIVERSITY, KOLHAPURPractical Examination in Chemistry at the B. Sc. Part-II

March/April, 2015

Chemistry Practical

ENCLOSURES :

1) Distribution of Practical work amongst Examiners.

2) A copy of the circular sent to Principals for division of batches into groups A and B.

3) Distribution of Practical work amongst group A and B.

4) General instructions to the examiners.

5) Inorganic Qualitative, Gravimetric and Volumetric exercises

6) Physical exercises.

7) Organic Chemistry exercises.

8) List of requirements for examination.

9) Printed specimen slips for exercises. (one bundle containing all slips.)

SHIVAJI UNIVERSITY, KOLHAPURConfidential For Examiner

Practical Examination in Chemistry at the B. Sc. Part-II

March/April, 2015

Instructions to the Examiners in Chemistry Practicals

Dear Colleague

It gives me a great pleasure to work with you for the Practical examination in chemistry at B. Sc. Part-II

I hope that with your full co-operation the entire work will be conducted smoothly and neatly.

Please find enclosed here with the following and note the same carefully :

I) i) General instructions to examiners.

ii) Programme of practical examination at B. Sc. Part-II, March 2015, for the trio of examiners.

iii) Practical excercises to be set to the candidates, under different sections and all other relevent papers.

iv) Division of work, etc.

II) Special Instructions :

Your special attention is drawn to the following points :

i) The senior examiner in each trio - the first named person in the group, is requested to guide hiscolleagues for the smooth and efficient conduct of the examination.

ii) Before the commencement of examination, the senior examiner should kindly see that the arrangementsat the centre are properly made and the programme works according to the schedule.

iii) The division of work amongst the examiners and the experts should be mentioned to different sheetsattached herewith.

iv) The exercises under physical chemistry, need not be given by lots. Hence the experiments are to bedistributed by the concerned examiner according to his own decision.

v) Under inorganic analysis, there is option between Inorganic Volumetric, Inorganic Qualitative andInorganic Preparation. However only one experiment should be set in the group.

vi) Exercise on organic preparation need not be given to the experts. While assessing this experiment, theexaminer is requested to use his discretion.

vii) a) Journals should be collected before the commencement of the examination. b) Candidates should notbe allowed to refer the journals during examination. c) Journals must be examined and signed by theconcerned examiners, on both the days. d) If the candidate fails to submit the journal, the lost certificatemust be issued and the candidate should be given zero marks for Journal.

viii) The division of marks for practical examination giving weightage to different sections and to theexercises, as per syllabus, will be as follows.

a) Examiners are requested to enter the marks on the answer-books as well as on the marksheets, inthe order given below :

Q. 1 : Physical Chemistry Exercise 25 Marks

Q. 2 : Inorganic Chemistry Exercises 35 Marks

Q. 3 : Organic Exercises 30 Marks

Q. 4 : Journal 10 Marks

Grand Total - 100 Marks

b) For different centres, separate mark-sheets should be used. Each page should carry the name of thecentre and should be signed by all the three examiners.

ix) For each centre, all examiners are expected to remain present for Laboratory Inspection without fail.

They are further requested to see that all the necessary preparations have been carried out as perinstruction.

x) Examiners are requested to use their discretion, while assessing the results of the candidates, where theexperts results are not upto the mark.

III) Instructions to senior examiners in each trio.

A) Senior examiner is requested to collect the following material from the relevant persons and to sendthem to the concerned authorities as instructed below :

1) Kindly send the following papers to Controller of Examinations, Shivaji University, Kolhapur as soonas the examination is over.

i) Mark-list in practicals of your group in sealed packet.

ii) Attendance/Absentee report of each centre, in duplicate

iii) No relative certificate for the laboratory staff working at the examination.

iv) Certificate from Laboratory Supervisor regarding -

a) The apparatus used by all concerned with the examination are properly calibrated and

the chemicals supplied are pure.

b) The arrangement of various experiments set at exam.

v) Lost journals certificate.

vi) The joint report must be given on the performance of candidates at various centres, including

report of deficiency of serious nature regarding journals, supply of water, gas, apparatus or

chemicals etc. at your centres.

B) 1) You are also requested to write to the Principals of the colleges, where you are supposed to go forexamination, regarding i) day, Date and timing of laboratory Inspection, ii) Whether you require lodgingand boarding arrangements, etc. Further, you are requested to convey these details to your colleagues inthe examination group.

2) Submit the assessed answer-books to the Principal of respective college.

3) Examiners are reqnested to claim the T. A. & D. A. bills from their own college and remuneration fromthe respective exam, centers.

IV) If there is any typographical mistake or any mistake due to over sight, kindly bring the same to my notice,without fail, for the smooth and efficient conduct of the examination.

Yours faithfully,

Sd/-Dr. A. R. Mulik

Chairman in Chemistry,B. Sc. Part-II Examination,

March/April, 2015Chairman's Address :Dr. A. R. Mulik

Department of ChemistryKrantising Nana Patil College.Walwa, Dist - Sangli416 313.

(2)

SHIVAJI UNIVERSITY, KOLHAPURConfidential For Examiner

Practical Examination in Chemistry at the B. Sc. Part-II

March/April, 2015

Instructions to the Examiners in Chemistry Practicals

1. Principals of the various colleges where the examinations are to be held have been requested to put twonotices on the board, one showing the division of each batch of candidates, into two equal groups A & Balongwith their University Seat numbers and another showing the scheme of distribution of practical work,among these A and B groups. Examiners are requested to check up whether this is done properly or not.

2. As far as possible, all the excercises laid down should be covered, during the course of examination at thecentre.

3. Journals should be collected by the examiners before the commencement of the examination alongwith

the Lost Journal Certificates, if any. Candidates should not be allowed to reffer the journals during the

practical examination.

4. The candidates are permitted to use Practical Text-Books, Reference Books and Typed Manuscripts which donot contain data and results.

5. Candidates should not be allowed to take away their answer-books when they go out for recess.

6. Colleges have been requested to supply properly calibrated apparatus, weight boxes etc, and to supply

pure and good quality Chemicals, and to issue the certificates accordingly. The examiners are requested

to note the same on the same day of Laboratory Inspection, and see that the arrangements of the

examination at the centre are properly made.

7. If at a centre any question paper is missing or the number fails short, examiners are requested to dictate thesame from their set to the candidates or get them cyclostyled if possible, from the college authorities.

8. Examiners are requested to use their discretion in setting the experiments, in consultation with the LaboratorySupervisor, when some critical problems arise at the centre.

9. Procedures followed for certain exercises may differ from college to college. Hence the candidates may beallowed to follow the procedures which they have used in their laboratories.

10. Physical Chemistry Exercises :

a) One exercise is to be set per candidate at 11.00 a.m. and the answer-books should be collected at 2.00p.m.

b) All the exercises should be set at a centre, wherever it is possible.

c) For Physical Chemistry, only one series of kinetics experiment, should be set for the concerned numberof candidates, in a group.

11. Inorganic Chemistry Exercises :

a) Two exercises are to be set for Inorganic Chemistry,

i) Gravimetric Analysis has to be set at 11.00 a.m. and

ii) Inorganic Volumetric or Inorganic Qualitative Analysis or Inorganic preparation. may be set at 12.00noon. All the answerbooks should be collected at 5.30 p.m. If required, an additional time period ofabout half an hour may be given for gravimetric analysis.

b) Distribution : (i) Any two different quantities should be given for gravimetric analysis to two experts.

Each expert must use both the volumetric flasks, in all four crucibles are to be set and thus duplicate

results are expected. (ii) For volumetric analysis any two volumes should be given to the expert and

the results should be compared. (iii) For candidates different desired quantities of solutions, between 20to 30 ml should be distributed through 250 ml volumetric flasks for all the gravimetric and volumetricexercises, using the flasks marked 'G' and 'V' respectively.

c) For Inorganic Qualitative Analysis, at least, 12 mixtures should be prepared for a batch of 15 candidates.The same mixture should not be distributed to more than two candidates from the same group. Forevery centre, distribution of mixtures should involve the use of as many mixtures as possible, from thelist attached herewith. However prepare appropriate amount of mixtures, to avoid wastage of Chemicals.

d) While preparing the mixtures for Inorganic Semi-micro Qualitative Analysis (SMQA), as far as possible,try to avoid the costly and rare chemicals such as those of arsenic, cadmium, chromium and certainbromides, iodides, nitrates, etc.

(P. T. O.)

12. Organic Chemistry Exercises :

a) Organic Preparation/Organic Estimation : Organic perparation or organic estimation should be set at1.00 p.m. and the answer-books must be collected at 5.30 p.m. As far as possible, both kinds of exercisesmust be set with equal distribution at every centre.

b) For organic estimation, three volumes should be given to the experts, as well as to the candidates.

c) Organic Spotting : Organic spotting has to be set at 2.30 p.m. and the answer-books collected at 5.30 p.m.

d) Titre readings, weights, M. P., B. P. etc. should be initialled by the examiners.

13. Division of work amongst the Examiners :

a) Examiner in Physical Chemistry : Physical Chemistry Exercise and Assessment of journal.

b) Examiner in Inorganic Chemistry : Inorganic Chemistry Exercises.

c) Examiner in Organic Chemistry : Organic Chemistry Exercises.

Yours faithfully,Sd/-

Dr. A. R. Mulik

Chairman in Chemistry,B. Sc. Part-II Examination,

March/April, 2015Chairman's Address :Dr. A. R. Mulik

Chairman in Chemistry,Krantising Nana Patil College.Walwa, Dist - Sangli416 313.

(2)


March/April, 2015

Instructions to the Examiners in Chemistry Practicals.

List of mixtures for Inorganic Semi-micro qualitative Analysis (SMQA)

Powder A + Powder B

1. MgCl2 + K2SO4

2. MnSO4 + NH4Cl

3. BaCl2 + KNO3

4. CaCO3 + KBr

5. ZnSO4 + Mg (NO3)26. ZnSO4 + KBr

7. MnCl2 + Ba (NO3)2

8. ZnCO3 + MgSO4

9. MgCO3 + KI

10. BaCl2 + NH4 NO3

11. Al2 (SO4)3 + Zn (NO3)212. FeCl3 + ZnCO3

13. Al (NO3)3 + MgCO3

14. CuCl2 + NiSO4

N. B. : i) Prepare the mixtures taking into consideration of the group nature of cations and anions, in thegiven mixture

ii) Prepare fresh mixtures containing Nitrate

(SCHEME OF MARKING [INORGANIC])

1) Gravimetric exercise 20 Marks

i) Weight of the residue 10 Marks

ii) Calculations 5 Marks

iii) Working 5 Marks

With analytical balance With 3 digit electronic balance

Difference in Weight in mg. ± Marks out of 10 Difference in Weight in mg± Marks out of 10

10 10 5 10

12 8 7 8

15 6 9 6

18 4 11 4

20 2 13 2

2) Volumetric exercise : Fertilizer/hardness of water. 15 Marks

Quality control/Analysis of vinegar.

(i) Titre Valae (CBR) 10 marks (ii) calculations 3 marks (iii) Working 2 marks

Difference in titre value in ml. ± Marks out of 10

Upto 0.2 ml. 10

Upto 0.3 ml. 9

Upto 0.4 ml. 8

Upto 0.5 ml. 7

Upto 0.6 ml. 4

3) Semi-micro qualitative analysis : Total Marks - 15

i) Dry tests 3 Marks

ii) Detection of +ve radicals 6 Marks (3 per radical)

iii) Detection of _

ve radicals 4 Marks (2 per radical)

iv) Working 2 Marks

4) Inorganic preparations : FAS/Tetrammine Cu (II) Sulphate. 15 Marks

i) Yield 10 Marks

ii) Systematic Work 2 Marks

iii) Appearance of the yield 3 Marks

15. CuCO3 + Ca (NO3)216. Cu (NO3)2 + K2SO4

17. CuSO4 + MgCO3

18. CdBr2 + NiCO3

19. MnCO3 + NH4 Br

20. CrCl3 + MgSO4

SHIVAJI UNIVERSITY, KOLHAPURPractical Examination in Inorganic Chemistry at the B. Sc. Part-II

March/April, 2015

(GRAVIMETRIC AND VOLUMETRIC)

1) Fe Gravimetrically :

F. A. S. 200 gm.

Pure concentrated H2SO4 5 ml.

2) Ba Gravimetrically :

BaCl2.2H2O 50 gms.

HCl concentrated 5 ml.

(INORGANIC VOLUMETRIC)

1) Fertilizer analysis :

Mix (NH4)2SO4 with Na2SO4 in different proportions to get 60%, 70%, 80% samples

[Supply 2g of well grould hougenons mixtare in container marked (V)]

2) Quality control :

Mix Na2CO3 and NaCl in different proportions to get 60%, 70%, 80% samples.

[Grind the mixture in electric mixer and distribute about 2gm sample through a container marked (V)]

3) Hardness of Water :

Stock solution of hard water should be prepared by dissolving 0.8 gm., 0.9 gm., 1.1 gm or 1.2 gm. CaCO3 in dil.HCl and diluting them to one litre each. [ supply 150 ml sample in botte marked]

4) Alkalinity of Antacid tablets.

1) Requirement : Antacid tablets, 1N HCl, 0.1 N std. NaOH Solution.phenolphtalein/methylred indicator.

Inorganic Proparations

1) Ferrous Ammonium Sulphate (Mohr'sSalt)

FeSO4.7H2O,(NH4)2 SO4, Iron nail, Conc. H2SO4

(P. T. O.)

1 litre. with dist. water

1 litre. with dist. water

}

}

2) Tetrammine Copper (11) SulphateCuSO4. 5H2O, liquor ammonia (NH3), ethanol.

SHIVAJI UNIVERSITY, KOLHAPURPractical Examination in Physical Chemistry at the B. Sc. Part-II

March/April, 2015

Instructions to the Examiners in Physical Chemistry Practicals

1) During the examination session, all the experiments (only one from kinetics) should be set.

2) Two slips one containing general instructions and other giving the procedure in brief for the experimentassigned be pasted on the answer-book of candidates.

3) Infinity reading and other data be made available to candidate well in time.

4) Examiners are requested to use discretion wherever necessary while conducting the examination.

5) In the batch of 15 candidates at least 5 instrumentation experiments should be given.

i) Polarimeter 1

ii) Conductometer 2

iii) Refractometer 1

iv) Viscometer 1

SCHEME OF MARKING

Exercises in Physical Chemistry

A) Experiments in Instrumentation

Marks

1) Polarimeter

Method of work 3

Readings 7

Graph 3

Unknown concentration 2

Calculation 3

Accuracy 3

Observation table 4

25

2) Conductometer

(a) Verification of Ostwald's law

Circuit diagram 3

Cell constant 4

Observation table 4

Readings 6

Calculations 4

Accuracy 2

Conclusions 2

25

(b) Conductometic titrations

Circuit diagram 3

Observation table and readings 4 + 8 = 12

Graph 4

Calculations of normality 3

Accuracy 3

25

(c) Verification of Onsager equation

Circuit diagram 3

Observation table 4

Readings 8

Graph 4

Conclusion 3

Accuracy 3

25

3) Refractometer

a) Technique 5

b) Density determination 4

Refractive index readings 6

Calculations of specific refractivity 6

Accuracy 4

25

4) Viscosity :

Technique 3

Readings 12

Graph 6

Accuracy (±10%) 4

25

B) Experiments in Kinetics

Marks

1) Effect of acid strength

Two sets of readings 2 x 3 = 6

Calculation of k1 & k2 2 x 4 = 8

Accuracy 4

Observation table 4

Conclusion 3

25

2) KI + K2 S2 O8 (Unequal concentrations)

Calculations of 'a' and 'b' 2

6 Titration readings 6

Calculation of K from readings OR from graph 10

Accuracy and determination of order 3

Observation table 4

25

3) Hydrolysis of methyl acetate :

Two sets of titration readings 2 x 3 = 6

Calculations of K1 and K2 2 x 3 = 6

Accuracy 3

Calculation of relative strength 4

Observation table 2 x 3 = 6

25

4) KBrO3 + KI (Equal concentrations)

Calculations of 'a' and 'b' 2

6 Titration readings 6

Calculation of K from readings 4

Graph 3

K from graph 3

Accuracy & determination of order 3

Observation table 4

25

(2)

Requirements for Exercises in Physical Chemistry

1) Polarimetry :

Polarimeter, 10% sugar solution

2) Refractomety,

Benzene, toluene, xylene, acetone, Refractometer,

3) Conductometry

Conductometer, N/10 KCl, N/50KCl, 0.1 N CH3 COOH

0.1 N HCl, 0.2 N NaOH,

Conductivity cell.

0.1 N NaCl

0.1 N KNO3

4) Viscosity :

Toluene and carbon tetra chloride, toluene and chloroform, xylene and chloro form, acetone, Viscometer

5) Kinetics

Solutions required

O.1N NaOH, 0.5N H2SO4, 0.5N HCl and Methyl acetate

0.1 N Kl, 0.1 N K2 S2 O8, 0.002N Na2 S2O3

0.1 N KBr O3, 0.1 N HCl, 0.01 N Na2S2O3, 0.25 M HCl

and at the time of examination freshly prepared starch solution must be supplied. Ice will be required for allthe experiments in kinetics in sufficient amount. All apparatus should be graduated and containers (bottles orflasks) be previously dried and kept ready. Experts are required to carry out the expriment on the day theexperiment is set and submit all results including details of calculations etc. in an answer book.

Infinity readings and other data should be informed to the candidates well in time preferably by writing onblack board every day.

Any other chemical or apparatus required in connections with the examination should be made available tothe examiners.

All the chemicals supplied must be pure and solutions prepared be sufficient for the number of candidatesbeing examined at the centre.

(3)

SCHEME OF MARKING

ORGANIC

Organic Estimation Marks - 15

1) Titration reading 10

2) Equation of the reaction involved 2

3) Calculations 3

Error in titre value ±ml.

0.1 ml. 10

0.2 ml. 9

0.3 ml. 8

0.4 ml. 7

0.5 ml. 6

0.6 ml. 3

Organic Preparation Marks 15

i) Yield 8 Marks

ii) Systematic work 3 Marks

iii) Appearance of the yield 4 Marks

Organic Spotting : Marks 15

i) Preliminary tests and type 2

ii) Physical constant 2

iii) Elements 2

iv) Group test 2

v) Identification, confirmatory tests 2

vi) Reactions 2

vii) Systematic work 1

viii) Neat representation on answer paper 1

ix) Result (name and structural formula) 1

(2)


March/April, 2015

Instructions to the Examiners in Organic Chemistry Practicals

ORGANIC EXERCISES

ORGANIC ESTIMATIONS

1. Estimation of an ester

Dissolve 25 ml ethyl benzoate in one litre

absolute alcohol

Distribution - 20, 22, 24 ml, etc in round

bottom flask marked 'C'

Requirements :

1N KOH

0.1 N HCl

Phenolphthalein etc.

2. Estimation of acetone

Dissolve 5 ml freshly distilled acetone in distilled water and dilute to one lit.

Distribution - 15 to 20 ml in 100 ml

measuring flask

Requirements :

0.1 N I2

0.1 N Na2S2O3

2 N HCl

1 N KOH

Starch indicator etc.

3. Estimation of Vitamin-C

Requirements :

Vitamin-C tablet (approx. 250 mg)

0.01 N NaOH

Phenolphtnalein

ORGANIC PREPARATIONS

1) P-nitroacetanilide

Different amounts of acetanilide to be given e.g. 4, 6, 8 grams Requirements : Glacial acetic acid, conc. H2SO4,Conc. HNO3 etc.

2) Phthalimide

Different amount of phthalic anhydride to be given eg. 4, 6, 8 grams.

Requirements - Urea, ethyl alcohol etc.

3) Benzoic acid

Different amount of benzamide to be given eg. 4, 6, 8 grams

Requirements - 10% NaOH, conc. HCl etc.

4) Acetanilide

Different amount of aniline (redistilled) to be given eg. 8, 10, 12 ml.

Requirements - Glacial acetic acid, sodium acetate (fused) ethyl alcohol etc.

ORGANIC SPOTTING

Salicylic acid, phthalic acid, succinic acid, alpha naphthol, ortho and para-nitrophenols, ortho, Para and metanitroanilines, diphenyl amine, acetanilide, bromobenzene, urea, naphthalene, carbon tetrachloride, methyl acetate,aspirin, ethyl methyl ketone, nitrobenzene, acetophenone, anthracene.


Examination March/April, 2015

Distribution of Practical Work amongst groups

Each batch of the candidates is divided into 'A' and 'B' groups for the purpose of the practical examinationand will work according to the following Time-Table. The division into groups is shown in a separate notice.

Day Time Group-A Group-B

First Day 11.00 a.m. to a) Inorganic Gravimetic Physical chemistry exercise 2.00 p.m. (at 11.00 a.m.) and (to be submitted at 2.00 p.m.)

b) Inorganic semimicro qualitative a) Organic estimation/OrganicAnalysis/Inorganic volumetric / preparationInorganic preparation(at 12.00 noon)

2.30 p.m. to Both the above exercises to be b) Organic spotting5.30 p.m. continued and results to be Results to be Submitted upto 5.30 p.m

submitted at 5.30 p.m.

Second Day 11.00 a.m. to Physical chemistry exercise a) Inorganic Gravimetric 2.00 p.m. (to be submitted at 2.00 p.m.) (at 11.00 a.m.) and

a) Organic estimation b) Inorganic semi-microOr anic Preparation qualitative Analysis /(may be given at 1.00 p.m) Inorganic volumetric / and Inorganic preparation

given at 12.00 noon

2.30 p.m. to Both the above exercises to be5.30 p.m. b) Organic spotting continued and results to be

Results to be Submitted upto submitted at 5.30 p.m.5.30 P. M.

For College

(may be given at 1.00 p.m)and


March/April, 2015

Division of Batches into A and B Groups

It is hereby circulated for the information of Principals of the colleges where the practical examination inchemistry (subsidary) at the second year B. Sc. is to be held that each batch of candidates at each of the centresis to be divided into two equal groups as follows :

1) The No. of candidates in a batch should be divided into two groups 'A' and 'B' having equal number ofcandidates. The first half of each batch will form 'A' group and the remaining will form 'B' group. If thenumber is not even 'A' group will contain one candidate more than 'B' group.

2) If a batch consists of 15 or less than 15 candidates then there should be only one group 'A' and theprogramme be arranged accordingly.

3) The Principals of the colleges concerned are requested to put on the notice board well in advance thedivision of candidates into A and B groups alongwith the notice showing distribution of practical workfor these groups.

4) From the four experts appointed, the division of work shall be as follows :

a) Two experts-Inorganic Gravimetric

b) One expert - Physical Chemistry experiments

c) One expert - Organic estimation and Inorganic volumetric.

Vidyanagar, Sd/-

Kolhapur - 416 004. REGISTRAR.

For College



List of Apparatus etc required by each candidate Following apparatus should be kept ready,Burettes 50 ml at least 40.

Beakers 500 ml 2250 ml 2

Conical Flasks 250 ml 2F. B. Flasks (Wash Bottle) 500 ml 1Measuring Flasks 250 ml 1

Funnels 2" 23" 2

Crucibles Porcelain 1Crucibles Silica 1(If Silica is not available one more crucible ofprocelain to be supplied)Pipette 50 ml 1

10 ml 1Watch glasses 2Evaporating (Por) dish 1Test tube stand with 10 test tubes 1Wire gauzes with absestos 2Asbestos sheets 2Pipe clay triangles 2Pair of tongs 1Glass rods : Glass tubes 4Two rods; Glass tubes dropper,one glass rod with rubber tip blower(Driver), Blow pipe.

Pipettes 5, 10, 25 ml. at least 40

Measuring cylinders of 250 ml,100 ml, 50 ml, 10 ml atleast 4 to 6.Thermometers 3600C minimum 15Boiling point tube-enoughquantityMelting point apparatus orMelting point baths.Thermometers 0.500, 1/100 atleast 5 Feather or Camel hair brush.Glazed paperOrdinary filter papers.Retort with clamps, rings, Water baths, Sand bath, FilterPumps.Filter flasks,Kipp's apparatusWashing bottle,Weighed as filter papers.Sodium fusion tubes.M. P. capillaries.And any other apparatus required for day to daylaboratory work.

The Laboratory Supervisor at the different centres of the practical examinations are requested to communicatethe deficiencies or the defects in the apparatus supplied and/or to be supplied to the students to the examinersbefore the commencement of the practical examination.

Sd/-REGISTRAR.

Measuring cylinder : 250 ml (2)

100 ml (2)

50 ml (2)

10 ml (4)

Measuring flasks : 250 ml with numbers from 1-40 (two sets)

100 ml with numbers from 1-40 (one set),

Flat bottom flasks / R. B. flask / conical flasks with numbers 1-40 and marked 'C' .... One set.

Bottle/Flasks marked "D", "E" with number from 1-40 one set.

Filter papers, Phenolphthalein, Methyl Organge, Distillation Flasks 50 ml Water condensers, Metal cones, fordrying the ppt. Thermometers 360 degree C, Liquid paraffin, Funnel (large 6 ") (4), Spoons, Log tables and otherrequirements, thiele's tube.

(4)



Requirements of the Apparatus, Chemicals etc.

General :

1) Requirenents regarding the apparatus, chemicals etc. for normal practical work of the above mentioned class.The list of the apparatus to be given to each candidate is Supplied The chemicals used should be pure andno complaints should be received from examiners/candidates.

2) Large stock of distilled water.

3) Well Calibrated balances and weight boxes

4) Calibrated burettes, pipettes, Volumetric Flasks etc.

5) Graduated glass-wares.

6) Blank labels, gum bottle, cork opener, glass spoons, rough balances, glass Pencils, etc.

Inorganic Practicals

Pure Chemicals (For quantitative work) EthanolAmmonium chloride Eriochorome Black_TBarium chloride DiphenylamineCalcium carbonate EDTA (Disodium Salt)Potassium ferrocyanide Hydrochloric Acid (Pure) (AR)Potassium ferricyanide Nitric Acid (Pure) (AR), Sulphuric acid (pure) ARPotassium sulphate Ammonia (Liquor Pure)Zinc sulphate Copper sulphateAmmonium sulphate Ferrous sulphate

All the above mentioned chemicals must be pure and in sufficient quantities.

250 ml measuring flasks and 100 ml measuring flasks, the candidate (Two sets each with Nos. 1-40)

100 ml. pinch cock burettes - 2 for distribution of solution.

F. A. S. - FeSO4 (NH4)2 SO4, 6H2O

AR-grade H2SO4 should be used,

F. A. S. solution is to be prepared only in very pure (AR) H2SO4 (concentrated)

Other articles : Bottes for stock sotions - 2 dozens.

Gravimetric filter papers with known weight Nos. 41, 42.

Wide mouth bottles with cork stoppers (1b) - 2 Doz.Colourless glass, stoppered bottles (300 ml) 4 Doz.Capsules marked 'A' Nos. 1 to 40 for inorganic semi-microqualitative mixtures to be given to students.

List of Chemicals for semi-micro analysis

Aluminium - Sulphate, Nitrate, Chloride

Ammonium - Bromide, Chloride, Sulphate.

Barium - Nitrate, Carbonate, Chloride

Magnesium - Carbonate, Sulphate, Chloride, Nitrate, Bromide

Nickel - Chloride, Sulphate, Carbonate.

Potassium - Bromide, Iodide, Sulphate, Chloride, Nitrate.

Cadmium - Sulphide, Chloride and Bromide

(P. T. O.)

Calcium - Carbonate, Bromide, Borate, Nitrate, Chloride

Chromium - Chloride, Sulphate.

Copper - Chloride, Sulphate, Carbonate, Nitrate

Ferric - Chloride, Sulphate and Nitrate.

Sodium - Nitrite, Carbonate, Sulphate, Nitrate.

Zinc - Sulphide, Carbonate, Sulphate, Chloride, Nitrate

Lead - Carbonate, Nitrate.

Manganese - Sulphate, Carbonate, Nitrate, Chloride

Special reagents for confirming basic radicals.

ORGANIC CHEMISTRY PRACTICALS

(Solutions required for estimations)

1. Potassium hydroxide 1.0 N

2. 0.1 N Hydrochloric acid

3. 1.0 N Hydrochloric acid

4. 0.1 N Iodine solution

5. 0.1 N Na2S2O3 solution

6. 2 N HCl

7. 0.01 N NaOH

8. Vit. 'C' tablets (water soluble - 250mg)

(N. B.) : The quantities of the solution required will depend upon the number of batches to be examined at theCentre. These quantities should be available at the beginning of the practical examination.)

INORGANIC EXPERIMENTS

List of requirements - experimentwise

1) Inorganic semi-micro qualitative analysis : (SMQA)

a) Inorganic substances for analysis as per list.

b) Kipp's apparatus with wash bottles.

c) Spot test reagents

d) All other chemicals and apparatus required for day to day work.

Solutions required :

(6M HCI : 660 ml. of Conc. HCl diluted to 1000 ml. with distilled water) (0.01 M EDTA : Dissolve 3.8 gm.disodium salt of EDTA in distilled water and dilute to 1000 ml.)

(Buffer pH 10 : Dissolve 88 gm. of NH4 Cl in 600 ml. of liquor ammonia and dilute to one litre.)

(to be prepared fresh every time).

0.02 N HCl, CaCO3, 1N NaOH, 0.1 N HCl, glacial acetic acid.

Requirements : Gravimetric exercises :

BaCl2. 2H2O, very pure HCl, H2SO4, HNO3

Whatman - filter papers No 41 & 42, FeSO4 (NH4)2 SO4 6H2O, NH4 NO3 (1%)

CHEMICALS (A. R. Grade) AND APPARATUS FOR PHYSICAL CHEMISTRY EXPERIMENTS

1) Polarimetry : Polarimeter and cane sugar.

2) Conductometry : N/10 KCl, N/50 KCl, 0.1 N CH3COOH and 0.2 N NaOH 0.1 N. HCl, conductometer.

3) Kinetics: N/10 NaOH, 0.5N HCl, 0.5N H2SO4, methyl acetate, 0.25 N HCl

0.1N K2S2O8, 0.1N KI, N/500 Na2S2O3

0.1N KBrO3, 0.1N HCl, 0.01N Na2S2O3

4) Benzene, Toluene, Xylene

(2)

Freshly prepared starch solution, ice and phenolphthalein indicator.

General Instructions :

1. Any other chemical or the piece of apparatus required in connection with the examination should be madeavailable.

2. All the chemicals must be of pure quality and sufficient, according number of batches to be examined at thatcentre.

3. The apparatus, chemicals supplied to the candidates, experts and examiners should be tested, calibratedbalances well, weight boxes, burettes and pipettes etc. and should be certified as such by the Laboratorysupervisor in charge of the examination.

4. List of marked containers/capsules -

a) A 1 to 40 - For inorganic semi-micro.

b) A 1 to 40 - For organic spotting.

c) 'C' marked 250 ml flasks 1-40

d) 100 ml measuring flasks with table Nos. 1-40 D, E

e) 'B' marked capsule 1-40 for organic estimation

f) 1 to 40 bottels for organic estimation.

g) V and G - 1 to 40 volumetic flask of 250ml capacity for inorganic quantitative analysis.

Calibrated burettes 50ml and pipettes 25ml, 10ml, 5ml, Beakers 100ml and 250 ml & 500 ml for Physicalchemistry.

5. The division of work is to be brought to the notice of the experts and their names are to be communicatedto the examiners, on the day of inspection.

6. All experts are expected to be present on the day of inspection and help the examiner for arranging theexperiments.

7. In case of organic spotting, physical constants must be supplied on the day of inspection for verifying theresults of the candidates.

ORGANIC CHEMICALS

Succinic acid, Salicylic acid, Phthalic acid, Alpha naphthol, o-Nitrophencl, o-Nitro and p-Nitro aniline, m-nitroaniline, p-nitro phenol, Acetanilide, Urea, Bromo benzene, Aspirine, Diphenyl amine, Carbon tetra chloride,Anthracene, Naphthalene, Methyl acetate, Ethyl methyl ketone, Acetophenone, Nitrobenzene

For Estimation Vitamin-C tab, ethyl benzoate, acetone

10 ml Measuring Cylinders 2

25 ml Measuring Cylinders 1

500 ml Measuring Flask 1



250 ml Conical or F. B. Flasks 60

with Corks.

250 ml R. B. Flasks 20 with Corks

50 ml Burette 20

Watch glass, Small funnel etc.

For separation :

Glass marking pencil, bottles

wide mouth capsules marked 'A' Nos. 1-40

wide mouth capsules marked 'B' Nos. 1-40

Other general requirements for examiners :

(3)

(P. T. O.)

[SMQA] I-1

SHIVAJI UNIVERSITY, KOLHAPUR

B. Sc. Part-II : Practical Examination, in Chemistry March/April 2015

Time : 5 hours Semi-micro Qualitative Analysis (Inorganic) Marks - 15

complete qualitative analysis of the mixture supplied in the Capsule marked (A) bearing your table

number and give its detailed report.

N. B. :- 1. Credit will be given for neat and systematic work and intelligent interpretation of

observations.

2. Observations, as soon as made, should be entered in answerbook.

3. Dry and preliminary tests must be Performed and the examiner's signature must be

obtained before preparing the solution.

4. Positive radicals, must be confirmed by use of spot tests wherever possible.

5. Present your results in the following form.

Form for entering the results of Inorganic Qualitative Analysis.

Positive Radicals (Basic) Negative Radicals (Acidic)

1. ________________________________ 1. ___________________________________

2. ________________________________ 2. ____________________________________



Time : 5 hours FERTILIZER ANALYSIS Marks - 15

You are given a sample of nitrogeneous fertilizer in a capsule marked (V) bearing your table

number. Determine the percentage of nitrogen present in the sample.

Instructions :

1. Weigh accurately, but not exactly, 0.500 g sample of ammonium sulphate on a watch glass.

2. Transfer the weighed sample completely into a 250 ml conical flask. Add about 50 ml distilled

water and 25 ml 1N NaOH solution to the flask. Add one or two pieces of porcelain and cover

the flask with stem cut funnel.

3. Heat the flask on sand bath for about an hour.

4. When reaction is complete, cool the flask and transfer the contents to 250 ml measuring flask

along with the washings. Dilute upto the mark with distilled water, shake well and use this

solution for estimation of nitrogen by back titration.

Back Titration : Pipette out 25 ml of above diluted solution in a conical flask. Add 1-2 drops of

methyl red indicator and titrate this solution against 0.1 N HCl solution for the estimation of excess of

NaOH.

Blank Titration : Pipette out 25 ml of the given 1 N NaOH in 250 ml measuring flask. Dilute upto

the mark with distilled water, shake well.

Titrate 25 ml of this diluted NaOH solution against 0.1 N HCl using methyl red, or phenol

phthalein as an indicator.

Calculate the percentage of nitrogen in the given sample.

(P. T. O.)

I-2

Observations :

Weight of fertilizer sample = .................. W g.

Blank titration reading = .................. 'X' ml

Back titration reading = .................. 'Y' ml

Calculations :

1) Hence the amount of NaOH required to evolve ammonia from 25 ml diluted fertilizer solution in

terms of 0.1 N HCl solution = X _ Y ml

∴ Volume of 0.1 N HCl solution for W g of sample will be 10 (X _ Y) ml = A ml

2) Amount of nitrogen -

1 ml 0.1 N HCl solution = 0.0014 g nitrogen

∴ A ml 0.1 N HCl solution = 0.0014 x A

= B g nitrogen

3) Percentage of nitrogen in the given

Sample = ___ × 100 ≡ C

4) Amount of 0.1 N HCl solution Equivalent to 0.05 g sample of (NH4)2 SO

4

As W g sample ≡ A ml 0.1 N HCl solution

∴ 0.05 g sample ≡ ___ × 0.05

≡ D ml of 0.1 N HCl solution

Results

1. 25 ml dil. fertilizer solution required (X _ Y) = ............... (ml) 0.1 N HCl solution

2. Amount of nitrogen in the given sample = B = ................ g = ................. × 10-3 kg.

3. Percentage of nitrogen in the given sample = C = ................ %

4. Amount of 0.1 N HCl solution equivalent to 0.050 g (NH4)2 SO

4 = D = ........... ml 0.1 N HCl solution

N. B. : S. I. units may be used.

B

W

(2) I-2

A

W



Time : 5 hours QUALITY CONTROL Marks - 15

In a capsule marked (V) bearing your table number, you are given a sample of soda-ash (Na2 CO

3).

Determine percentage purity of soda-ash in the given sample.

Instructions :

Part-A : Preparation of Soda-ash solution

Weigh accurately, but not exactly 1.325 gms. of given sample of soda-ash on a watch glass or

glazed paper. Dissolve it in a minimum quantity of distilled water in a beaker. Then transfer this

solution along with its washings in a 250 ml volumetric flask. Dilute up to the mark with distilled

water; shake well.

Part-B : Determination of % purity of soda-ash

Pipette out 25 ml of above diluted solution of Soda-ash in a conical flask. Add 2-3 drops of methyl

orange indicator; and titrate it against 0.1 N HCl. Calculate % purity of soda-ash by using the constant

burette reading. (C. B. R.) = 'X' ml.

Calculations :

1 mole of HCl = 53 gms. of Na2CO

3.

i. e. 1000 ml 1N HCl solution = 53 gms. of Na2CO

3.

1) 25 ml diluted soda-ash solution required X ml of 0.1 N HCl solution

∴ 250 ml diluted soda-ash solution = 10 × X ml.

(P. T. O.)

I-3

2) From the above relation 1000 ml 1N HCl solution = 53 gms. of Na2CO

3 (soda-ash.)

∴ 10. X X ml of 0.1 N HCl solution = A g

3) % Purily of Soda ash Sample

The quantity 'A g' is the amount of soda-ash in the 'W g' of the sample.

Now, as W g of sample = A g of Na2 CO

3

∴ 100 g of sample = = B g. of Na2CO3 (soda-ash.)

= % purity of soda-ash. (Na2CO

3)

Results :

1. 25 ml. diluted soda-ash sample solution requires = X = ................. ml of 0.1 N HCl solution

2. Amount of Na2CO3 in the given sample = A = ............... g = .................. × 10-3 kg.

3. % purity of soda-ash sample = B = .............. %.


(2) I-3

[10 × X] × 0.1 × 53

1000

100 x A

W

Calculations :

1) Standardisation of EDTA solution :

EDTA CaCl2 solution

N1V

1= N

2V

2

N1

= _____ = ________ = 'A' M of EDTA solution

2) Calculation of hardness of water.

1 ml 0.01 M EDTA solution ≡ 0.001 gm CaCO3

∴ 1 ml 'A' M EDTA solution ≡ _________ = 'B' gms CaCO3

∴ 'Y' ml 'A' M EDTA solution ≡ 'B' × 'Y' gms CaCO3

= 'C' gms CaCO3

Now, 25 ml water sample ≡ 'C' gms CaCO3

∴ 1000 ml water sample ≡ 'C' × 40 gms CaCO3

≡ 'D' gms/lit. CaCO3

≡ 'D' × 1000 mg/lit. CaCO3

≡ 'E' mgs/lit CaCO3

≡ 'E' ppm CaCO3

Results :

1. Correct molarity of given EDTA = 'A' M EDTA

2. Total hardness of water = 'E' ppm of CaCO3.

(2) I-4

0.001 × 'A'

0.01

N2V

2

V1

0.01 × 25

X


B. Sc. Part-II : Practical Examination in Chemistry March/April 2015

Time : 5 hours HARDNESS OF WATER Marks - 15

In a 250 ml. bottle marked (V) bearing your table number, you are given a sample of hard water.

Determine the total hardness of the water.

Instructions :-

Part-A : Preparation of 0.01 M CaCl2 Solution :

Weigh accurately 0.250 gms of pure CaCO3 powder by using a watch glass or glazed paper and

transfer to a 250 ml. beaker. Add pure concentrated HCl drop by drop till all the CaCO3 get dissolve

completely liberating CO2 gas. When liberation of CO

2 is stopped transfer the solution to 250 ml.

measuring flask. Wash the beaker 2-3 times with distilled water and transfer all the washings to the

same 250 ml. measuring flask. Dilute the solution up to the mark using distilled water. Shake well.

Part-B : Standardisation of EDTA Solution :

Pipette out 25ml. of 0.01 M calcium chloride (CaCl2) solution into 250 ml conical flask, dilute it

with about 25 ml. of distilled water, add 5 ml. buffer (pH = 10) and 4-6 drops of Eriochrome Black-T

indicator. Titrate with the approximate 0.01 M EDTA solution untill the colour changes from wine red

to sky blue. Take two more readings and note constant burette reading as 'X' ml.

Part-C : Determination of hardness of water :

1. Take 25 ml. sample of water in a 250 ml. conical flask.

2. Add 5 ml. buffer solution to it.

3. Add 4-6 drops of Eriochrome Black-T indicator.

4. Titrate the contents against standardised EDTA solution.

At the end point colour changes from wine red to Sky blue.

5. Take two more readings and find out the constant burette readings as 'Y' ml.

(P. T. O.)

I-4

Total amomnt to HCL in term of 0.1 N NaOH

Solution Consumed by W gm of antacid table = 10 x (Y - X) cm3 =.....................cm3

We have,

1000 ml, 1N NaOH = 40 gm of NaOH (alkali)

∴ 10(Y - X) cm3 of 0.1 NaOH=

= Z gm of NaOH

Now, W gm of antacid tablet = Z gm of NaOH (alkali content)

∴ 100 gm of antacid tablet = 100 x Z

w

= M gm of NaOH

(l.e.% of alkali Content)

Results :

1. Percentage of alkali content in the

antacid tablet = M gm =.................................g

= % of alkali contect.

(2) I-5

10(Y - X) x 0.1 x 40

1000x1



Time : 5 hours ALKALINITY OF ANTACID TABLET Marks - 15

In a capsule marked (V) bearing your table number, you are given a Antacid tablet. Delermine the

alkalinty of Antacid in the given tablet.

Instuclons

1) Weigh accurately but not exactily 0.250 gm of the tablet powder on a watch glass. Transfer it to

250cm3 conical flask by using funnel. Wash the watch glass with dist. water and transfer all the

washings in the same flask. then add 25 cm3 of 1 N HC1 to disolve the tablet, warm. cool and tranfer

all the Content of the flask to 250 cm3 volumetric flask. Dilule upto the mark with distilled water.

Back titration

Fill the burette with 0.1N NaoH solution, Titrate 25 ml of the above diluled solution against 0.1 N NaOH

Solution by using methyl red inlicator. The end point will be red to yellow OR use Phenolphthalein

indicator where colour change will be colurless to pink. Take there reading and note the constant

burette readings (C.B.R.) (say as cm3)

Blank titration :

Dillule 25cm3 of 1 N HCl solution to 250cm3 with distilled water in a Volumetric flask

Titrate 25 cm3 of this diluted solution againt 0.1N NaOH Solution from the burette using methylred

or Phenolphthalein indicator. Take two more readings and note down the CBR (Say 'Y' cm3)

Calculations

The differnce (Blank-Back) i.e. (Y-X)cm3 gives the amount of HCl in term of 0.1N NaOH consumed or

required to neutralize the alkali content of antacid tablet in 25cm3 diluted solution=.............cm3

(P. T. O.)

I-5

SHIVAJI UNIVERSITY, KOLHAPURB. Sc. Part-II : Practical Examination, in Chemistry March/April 2015

Time : 5 hours INORGANIC PREPARATION Marks - 15

Ferrous Ammonium Sulphate (Mohr's salt)

FeSO4 (NH

4)2 SO

4. 6H

2O

Instructions :

Take 10 gms of ferrous sulphate in a beaker. Add in it about 60 ml. distilled water and 5 ml. dilute

H2 SO

4. Dissolve the salt by boiling.

Then add 5 gms of ammonium sulphate. Add a bright iron nail. Boil the solution till the crystallisation

point is just reached. (avoid formation of crystal masses) Cool in ice-bath and add about 10 ml. of

ethanol.

Filter and wash the product with ethanol. Dry and weigh the product on rough balance.(w.g.)

Calculate theoretical and practical percentage yield.

Calculations :

1) Theoretical yield :-

FeSO4 . 7H

2O = FeSO

4 (NH

4)2 SO

4 . 6H

2O

i.e. 278 gms = 392 gms

10 gms = (392 x 10) / 278

= 14.1 gm Fe SO4 (NH

4)2 SO

4 . 6H

2O

2) Percentage Practical yield

∴ 14.1 gms. Product = 100% yield

∴ W gms product = (W x 100) / 14.1 = ..................... %

Results :

1. Yield of the product = W = ....................... g = ......................... × 10-3 kg.

2. Theoretical yield of the product = ............................. g = ......................... × 10-3 kg.

3. Percentage practical yield of the product = ............................. %.

I-6



Time : 5 hours INORGANIC PREPARATION Marks - 15

Tetrammine Copper (II) sulphate

[Cu (NH3)4] SO

4 . H

2O

Instructions :

Dissolve 5.0 gms of copper sulphate in about 20 ml of warm distilled water. Take about 30 ml of

liquor ammonia in another beaker. Add copper sulphate solution to liquor ammonia slowly drop by

drop with continuous stirring. Deep blue coloured solution results. (If precipitate of copper hydroxide

appears in the beaker, dissolve it by adding excess liquor ammonia). Cool in ice-bath and add about 50

ml of ethanol. Stir well.

Filter the product on Buchner funnel. Wash it with ethanol containing few drops of ammonia. Dry

the product and weigh it on a rough balance.

Calculate theoretical yield and practical percentage yield.

Calculations :

1) Theoretical yield :

CuSO4 . 5 H

2O = [Cu (NH

3)4] SO

4. H

2O

i.e. 249.69 gms = 245.74 gms.

5g CuSO4.5H

2O = (245.74 x 5) / 249.68

= 4.92 gm [Cu (NH3)4] SO

4 . H

2 O

2) Percentage practical yield :

∴ 4.92 gms product = 100% yield

∴ W gms Product = (W x 100) / 4.92 = ..................... %

Results :

1. Yield of the product = W = ....................... g = ......................... × 10-3 kg.

2. Theoretical yield of the product = ............................. g = ......................... × 10-3 kg.

3. Percentage practical yield of the product = ............................. %.

I-7

I-8



Time : 6 hours Gravimetric Estimation of Ba Marks - 20

In a 250 ml. measuring flask, bearing your table number, you are given a solution of barium

chloride & free hydrochloric acid. Determine the amount of Barium as BaSO4 gravimetrically.

Instructions :

Dilute the given solution to 250 ml. with distilled water and use 50 ml. of the diluted solution for

estimation.

Use the Gravimetric Factor : BaSO4 : Ba : BaCl2 . 2H2O = 1 : 0.5883 : 1.0467

Present your results in the following tabular form.

Results :

1. 50 ml. of the diluted solution gave ............... g. BaSO4

= ......................... × 10-3 kg BaSO4

2. Quantity of BaCl2 . 2H

2O in the given solution ................. g.

3. Quantity of Ba in the given solution ............... g.


I-9



Time : 6 hours Gravimetric Estimation of Fe Marks - 20

In a 250 ml. measuring flask, bearing your table number, you are given a solution of Ferrous

Ammonium Sulphate & free sulphuric acid. Determine the amount of Fe as Fe2O

3 gravimetrically.

Instructions :

Dilute the given solution to 250 ml. with distilled water and use 50 ml. of the diluted solution for

estimation.

( Use the Gravimetric Factor : Fe2 O3 : 2 Fe : 2 FeSO4 (NH4)2 SO4 . 6H2O = 1 : 0.6994 : 4.9111 )

Present your results in the following table.

Results :

1. 50 ml. of the diluted solution gave ............... g Fe2O

3 = ......................... × 10-3 kg Fe

2O

3

2. Quantity of FeSO4

(NH4)2

SO4 . 6H

2O in given solution ................. g = ......................... × 10-3 kg.

3. Quantity of Fe in the given solution ............... g = ......................... × 10-3 kg.


O-1



Organic Spotting

Time - 3 hours. (Along with other exercise) Marks - 15

Identify the organic compound, given in a container marked (A) bearing your table number. Give a

full report of all the tests along with reactions of postive tests you have carried out. Confirmatory test

should be done. Give the structural formula of the compound.

(M. P./B. P. of the compound should be determined before identification is started and the examiner's

signature be obtained. Wherever possible, special tests should be shown to the examiner.)

Enter your results in the following table.

Name of the Compound Structural formula M.P./B.P.




Organic Estimation

Estimation of an ester (ethyl benzoate)

(Along with other exercise) Marks - 15

In a 250 ml round bottom flask marked 'C' bearing your table number, you are given a solution of

ethyl benzoate : Determine the amount of ethyl benzoate in the given solution.

You are given following solutions.

1. Approx. 1N KOH solution in bottle marked D

2. Exact 0.1 N HCl solution in bottle marked E

Instructions :

I) Back Titration : Add exactly 25 ml given 1N KOH solution to the flask containing the ester.

Heat the reaction mixture under reflux using water condenser on a water bath for 1½ hours.

After 1½ hours cool the reaction mixture and transfer the contents to a 250 ml measuring flask and

dilute the solution upto 250 ml with distilled water. Pipette out 25 ml of the diluted solution and titrate

it against 0.1 N HCl solution for estimating the unused KOH solution. Let the C.B.R. be 'Y' ml.

II) Blank Titration : Dilute 25 ml. of the given 1N KOH solution to 250 ml. Titrate 25 ml of this

diluted solution against 0.1 N HCl solution. Let the C.B.R. be 'X' ml.

Calculations :

The amount of KOH consumed by 25 ml. of diluted ethyl benzoate solution for hydrolysis in terms

of volume of 0.1 N HCl = (X-Y) = ................ ml.

1) Therefore volume of 0.1 N HCl solution equivalent to KOH solution consumed during the hydrolysis

of ethyl benzoate in the given solution = 10 x (X-Y) = .................... ml.

O-2

(P.T.O.)

2) From reaction we get

1 gm. equivalent of KOH ≡ 1 gm. equivalent of HCl ≡ 1 mole of ester

i.e. 1000 ml 1N KOH ≡ 1 mole of ester (C6H

5 COOC

2H

5)

i.e. 1000 ml 1N HCl ≡ 150 gm of (C6H

5 COOC

2H

5)

i.e. 1ml of 0.1N HCl ≡ 0.015 gm of C6H

5 COOC

2H

5

10 x (X-Y) ml. of ≡ 10 x (X-Y) x 0.015 / 1

≡ A gm of ethyl benzoate

Enter your results in following form :

1. Volume of 0.1 N HCl solution equivalent to KOH solution consumed during the hydrolysis of

ethyl benzoate in the given solution = 10 x (X - Y) = ..................... ml.

2. Quantity of ethyl benzoate in the given solution A = ............ g = ......................... × 10-3 kg


(2) O-2



Organic Estimation

Estimation of Acetone


In a 100 ml measuring flask marked'C' bearing your table number you are given acetone solution.

Determine the amount of acetone.

You are given following solutions.

1. (Approx) 0.1 N I2 Solution in bottle marked D.

2. 0.1 N Na2S2O3 solution in bottle marked E.

3. 1 N KOH solution

4. 2 N HCl solution

Instructions :

I) Back Titration : Dilute the given acetone solution to 100 ml with distilled water. Take 10 ml of

this diluted solution in a glass stoppered bottle. To this solution, add 25 ml of 1N KOH solution and shake

well. Then add exactly 25 ml of 0.1 N I2 solution. Shake the mix. well and allow it to stand for 15 minutes.

Then acidify with 25 ml 2 N HCl solution and titrate the complete mixture immediately against 0.1 N.

Na2S

2O

3 solution using starch indicator. Let the C.B.R. be 'Y' ml.

II) Blank Titration : Titrate 25 ml. of 0.1 N. I2 solution directly against 0.1 N Na

2S

2O

3 solution using

starch as an indicator. Let the C.B.R. be 'X' ml.

Calculations :

The amount of I2 consumed by 10 ml. of diluted acetone solution in terms of 0.1N Na

2S

2O

3 Solu-

tion = (X-Y) = ................ ml.

1) Amount of I2 consumed in terms of 0.1 N Na

2S

2O

3 solution by the given acetone solution = 10 x (X-

Y) = ......................... ml.

O-3

(P. T.O.)

2) From the reaction we get

1 mole of acetone ≡ 3 moles of KI ≡ 3 moles of I2 ≡ 6 moles of Na

2S

2O

3

∴ 1 mole of acetone ≡ 3 gm equi. of I2 ≡ 6 gm equi. of Na

2S

2O

3

Thus

6000 ml. of 1N Na2S

2O

3 ≡ 1 mole of acetone ≡ 58 gm of acetone

60000 ml of 0.1 N Na2S

2O

3 ≡ 58 gm of acetone

10 x (X-Y) ml of 0.1 N Na2S

2O

3 ≡ [10 (X-Y) x 58]/ 60000 gm of acetone

≡ A gm of acetone

Enter your results in following form :

1. Amount of I2 consumed in terms of 0.1 N Na2S2O3 soln. by the given acetone

solution = 10 x (X-Y) = .................. ml.

2. Amount of acetone in given solution = A= .............. g = ......................... × 10-3 kg


(2) O-3

O-4



Organic Estimation

Estimation of Vitamin-C


In a capsule marked 'C' bearing your table number, you are given Vitamin-C tablet (appro. 250 mg).

Determine the percentage of Vitamin-C. in the given tablet.

You are given following solutions

0.01 N NaOH solution in bottle marked D

Instructions :

I) Preparation of Vitamin-C solution

Weigh accurately the given Vitamin-C tablet on watch glass. Dissolve it in a minimum quantity of

distilled water in beaker. Then transfer this solution along with its washings in a 100 ml volumetric

flask. Dilute upto mark with distilled water, shake well.

II) Determination of % of Vitamin-C.

Pipette out 10 ml of above diluted solution of Vitamin-C in a conical flask and titrate it against

0.01N NaOH solution. Calculate % of Vitamin-C in given tablet.

(P. T. O.)

Calculations :

10 ml diluted Vitamin-C solution required = X ml of 0.01N NaOH solution

∴ 100 ml diluted Vitamin-C solution ≡ 10 x X = Y ml of 0.01N NaOH solution

∴ 1 mole of NaOH ≡ 176 g of Vitamin-C

: 1000 ml 1N NaOH ≡ 176 g of Vitamin-C

1000 ml 0.01N NaOH ≡ 1.76 g of Vitamin-C

'Y' ml 0.01 N NaOH = ______ g of Vitamin-C

= Z g of Vitamin-C

W g of Vitamin-C tablet = Z g of Vitamin-C

∴ 100 g of Vitamin-C tablet = ________ g of Vitamin-C

= % of Vitamin-C

Enter your results in the following form :

1. Volume of 0.01 N NaOH required for the Vitamin-C present in the given tablet = 10 x X = Y =

............... ml.

2. Quantity of Vitamin-C in the tablet (z) = .......................... g = ......................... × 10-3 kg

3. % of Vitamin-C in the tablet = .........................


1.76 x Y

1000

100 x Z

W

(2) O-4

∴

O-5


B. Sc. Part-II : Chemistry Practical Examination, March/April, 2015

Organic Preparation

Preparation of p-nitroacetanilide


Preparation of p-nitroacetanilide from acetanilide.

You are supplied with acetanilide, glacial acetic acid, conc. H2SO

4 , Conc. HNO

3, etc.

Procedure :

Transfer the given amount of acetanilide to a dry conical flask and add 10 ml glacial acetic acid. Keep

the flask in ice-salt bath and add 10 ml conc. H2SO

4 gradually with constant stirring.

Take 5ml of conc. HNO3 and 3 ml conc. H

2SO

4 in a test tube and cool. Then add this nitrating mixture

drpowise to the reaction mixture placed in ice bath with constant stirring. After complete addition

remove the conical flask from ice bath and keep at room temperature for one hour. Then pour the

reaction mixture in 100 ml ice-cold water. p-nitroacetanilide precipitates out. Filter, wash, dry and weigh

the crude product. Recrystallise from alcohol.

Results : Weight of the crude product = .................. g = ......................... × 10-3 kg

N. B. : 1) Submit your product for inspection to the examiner.

2) S. I. units may be used.

O-6



Organic Preparation

Preparation of Phthalimide


Preparation of phthalimide from phthalic anhydride.

You are supplied with phthalic anhydride, urea etc.

Procedure :

Transfer the given amount of phthalic anhydride to a clean and dry conical flask. Add 3 g urea and

heat the flask on sand bath at 130-135 0C.

The reaction begins with frothing of the mass at temperature about 1600C. When frothing sub-

sides, stop heating. After cooling add cold water to spongy solid. Separate the phthalimide by filtration

with suction. Wash with water, dry and weigh the crude product.

Results :

1. Weight of the crude product = .................. g = ......................... × 10-3 kg



O-7



Organic Preparation

Preparation of Benzoic acid


Preparation of benzoic acid from benzamide :

You are supplied with benzamide, 10% NaOH solution, conc HCl etc.

Procedure :

Transfer the given amount of benzamide to a clean and dry conical flask and add 50 ml 10% NaOH

solution. Heat the flask on sand bath for about 30 minutes to expell the ammonia completely. (test with

turmeric paper.)

Cool the flask and add conc. HCl dropwise with stirring till complete precipitation of benzoic acid.

Filter, wash, dry and weigh the crude product.

Results :




O-8



Organic Preparation

Preparation of Acetanilide


Preparation of acetanilide from aniline :

You are supplied with aniline (redistilled), glacial acetic acid, sodium acetate (fused) etc.

Procedure :

Transfer the given amount of aniline to a clean and dry conical flask. Add 10 ml glacial acetic acid

and 5 gms Sodium acetate. Fit air condenser and heat the flask on sand bath for 30 minutes. Then

pour the reaction mixture in 100 ml ice-cold water. Acetanilide precipitates out. Filter wash dry and

weigh the crude product.

Results :




P-General



(PHYSICAL)

1. Write your examination seat number and also table number on the answer book.

2. Get your volumes and other readings initialled by the examiner concerned.

3. Marks are assigned for technique, method of work, calculations, presentation and accuracy

of results.

4. Graphs are to be drawn wherever necessary.

5. Get the electrical or other connections checked by examiner before starting with your

work.

6. S. I. units may be used.

SHIVAJI UNIVERSITY, KOLHAPUR P-1

B. Sc. Part-II, Practical Examination, in Chemistry, March/April, 2015

Time : 3 hours] PHYSICAL [Marks : 25

Conductometry

To verify Ostwald's dilution law. Given-N/10 KCl or N/50 KCl solution, N/10 CH3COOH solution.

Note :- Show all the connections to the examiner.

Procedure - A) Determine the Cell Constant of the given conductivity cell by using N/10 or N/50

KCl solution. Ask for the specific conductivity (Ko) of N/10 or N/50 KCl solution.

B) Prepare following solutions (100 ml each) viz. N/20, N/40, N/80 by using conductivity water

from the given N/10 weak acid (CH3COOH) solution.

Take approx. 60 ml. of the given N/10 CH3COOH in a 100 ml beaker. Measure the Conductance of

the solution.

Similarly measure the Conductance of each of the solutioins prepared.


Observation Table

A) Determination of cell constant

1) Sp. conductivity (Ko) for N/10 KCl = .................

2) Sp. conductivity (Ko) for N/50 KCl = .................

Solution usedConductance

observed (Co) ohm-1

Cell constant

A =

N/10

or

N/50

KCl

B) Determination of conductance of acetic acid solutions of different concentrations.

Ko

Co

Sr.

No.conductance

observed (C)

Ohm-1

k= cell constant x C

oh m-1 cm-1

1 N/10

2 N/20

3 N/40

4 N/80

λv

λ∞concs.

N

Eq. cond.

λv =

ohm-1 cm2 eq-1

1000 X k

N

α =(Disso-

ciation

const.)

1. Given - λ∞ = 390.8mohm-1

2. Show all details of calculations in your answer book.

3. Draw circuit diagram of Wheatstone's bridge.

4. Use of digital conductometer is allowed.

Result : 1) Cell Constant = .............................cm-1

2) mean k =..............................

3) conclusion =..........................

cm-1

K=α2N

Sp.cond.

PHYSICAL - P-1




Conductometry

To determine the normality of the given strong acid by titrating it against a strong alkali

conductometrically.

Given : 0.1N (approx) acid solution, 0.2 N strong alkali solution.

Note :- Show circuit diagram and all the connections to the examiner.

Procedure : Place 10 ml. of the approx 0.1 N acid solution by a pipette in a 100 ml. beaker. Add

50 ml. of conductivity water to dip the electrodes of the conductivity cell properly. Stir well.

Determine the conductance of the solution (C). Add exactly 0.5 ml. of 0.2N strong alkali solution

from the burette. Stir well and determine the conductance. Similarly take the readings after every

addition of 0.5 ml. upto 10ml. of alkali.

Plot a graph of the Conductivity (C) of the solution against volume of the strong alkali added.

From the graph find out the equivalence point.

Calculate the normality of the given strong acid.

Present your results in the following tabular form :

10 ml. of strong acid +50 ml. of conductivity water in beaker.

Sr. No. volume of alkali added in ml Conductivity - (C) ohm_1

Results :

1) Equivalence point from the graph = ............................. ml.

2) Normality of the given acid = ....................... N.

SHIVAJI UNIVERSITY, KOLHAPURP-3



Conductometry

To determine the equivalent conductance at infinite dilution of strong electrolyte at five different

dilutions by conductometric method and to verify onsager equation.

Given : 0.1 N KCl/NaCl/KNO3/HCl Solution

Note : Show all the connections to the examiner.

Procedure : Prepare 100 ml each 0.08 N, 0.06 N, 0.04 N, 0.02 N Solutions from the given 0.1 N

electrolytic solution by using conductivity water.

Take approx 50 ml of the given 0.1 N electrolytic solution in a 100 ml beaker measure its

condnctance and similarly measure the conductance of each of the solutions prepared.


Ask for cell constant of given conductivity cell.

Cell constant = ...................... cm-1

Determination of equivalent conductance

Sr.

No.

Conc. of

Solution

CN

Observed

conductance

Ohm-1

Specific Conductance

(k) = Cell constant x

observed conductance

ohm-1 cm-1

Equivalent conductance

λv = ________

ohm-1 cm2 eq-1

1 0.1

2 0.08

3 0.06

4 0.04

5 0.02

Plot a graph of λv against √C and find the value of equivalent conductance at infinite dilution.

Results :

i. λ∞ for given electrolytic solution = ........................

ii. Conclusion.

√C1000 × k

C




Polarimetry

To determine the angle of rotation and hence specific rotation of the given substance and to

determine the concentration of unknown solution.

Given : 10% aqueous solution of an optically active substance and a solution of an unknown

concentration of the same substance.

Prepare five solutions of different concentrations as per instructions from the examiner.

Determine the angle of rotation θ, for each of these five solutions.

Calculate the specific rotation [α] of the substance.

Present your results in a neat tabular form. Show all details of calculations in the answer book.

obs.

No.Concentration of the

solution (C)

Reading

for Solution (A)

Reading for

distilled water

(B)

Angle of

rotation

θ = (A - B)

Specific rotation

[α] =100 X θ

l X C

1

2

3

4

5

6 unknown

Length of the Polarimeter tube in decimeter (l) = ........................... dm

Plot the graph of angle of rotation θ, against the concentration of the Solution.

From the graph, determine the concentration of the given unknown Solution.

Results :

1. Mean [α] = .............................. .

2. Concentration of unknown solution = ...................... %

from graph.




Refractometry

To determine the specific and molar refractivities of liquids A, B & C and hence to determine the

refractivity of _ CH2 group.

[Ask for molecular weights of liquids A, B, C]

Record the observations in the following tabular form.

Observation Table

Calculate specific and molar refractivities.

1. Specific refractivity (RS) = ______ x ___

2. Molar refractivity (RM

) = _________ x ___

3. ∆RM1

= RM(B)

- RM(A)

and ∆RM2

= RM (C)

- RM(B)

Result :

Mean Refractivity of -CH2 group = .......................

LiquidsMol. wt.

(M)

Refractive

Index

(n)

Density

gm/cm3

(d)

Specific

Refractivity

(Rs)

Molar Refractivity

Mx Rs

(Rm

)

Refractivity of

-CH2 group

∆Rm

A

B

C

Determine the densities of all liquids by using specific gravity bottle.

Given - Density of water dw = 1 gm /ml.

Liquids

A

B

C

Dist. water

wt. of empty sp.

gr. bottle 'x'

wt. of sp gr. bottle

+ liquid 'y'

wt. of liquid

(y - x)

Density =

d = __________ x dwwt. of liquid

wt. of water

n2 - 1

n2 + 2

1

dn2 - 1

n2 + 2

M

d




Viscosity Experiment

Determine the percentage composition of unknown mixture by using viscometer

Given : Pure liquid A and B, mixtures C, D, E and F.

Procedure : Find the time of flow 't' in seconds for A, B, C, D, E and F by using viscometer.

Record the observations in the following tabular form.

Observation Table

Liquids

A 100 0

B 0 100

C

D

E

F Unknown Unknown

% of A % of B Time of flow 't' Density 'd' (d x t)

Plot the graph of (d x t) against the percentage composition of A and find percentage composition

of F.

Note : Ask for densities of A, B, C, D, E and F.

Results : Percentage composition of F from graph

% of A = ............................ %

% of B = ............................ %




Chemical Kinetics

Determination of relative strength of acids from hydrolysis of methyl acetate.

Given - Methyl acetate, 0.5 N HCl solution, 0.5N H2SO4 solution, 0.1N NaOH solution.

Procedure - Perform two sets of experiments as follows.

Set I - Bottle No. 1 : 5 ml. of methyl acetate

Bottle No. 2 : 100 ml. of 0.5 N HCl solution.

Set II - Bottle No. 1 : 5 ml. of methyl acetate

Bottle No. 2 : 100 ml. of 0.5 N H2SO4 solution.

Take given quantities of methyl acetate & acids in different stoppered bottles. Keep the

stoppered bottles in water bath for some time, to attain the same temp. Transfer acid to methyl

acetate, shake well & take the readings immediately. Note this reading as '0' (zero) reading. Take 5

readings including '0' reading. Use 5 ml of the reaction mixture for titration. Ask for infinity

readings.

T∞ for Set I - ...................................... ml.

T∞ for Set II - ..................................... ml.

Present your results in the following tabular form

Observation Table

Set I (0.5N HCl)

a = T∞ _ T0 = .................ml

Set II (0.5N H2SO

4)

a = T∞ - T0 = ................. ml

Time

in min

(t)

Titrationreading

(Tt) ml

x =

(Tt-T

0)

log

a

(a-x)

(a-x)k

1

min-1

Timein

min(t)

Titrationreading

(Tt) ml

x =

(Tt-T

0)

log

a

(a-x)(a-x)

k2

min-1

0 0

10 10

20 20

30 30

40 40

Mean k1 =......................min-1 Mean k

2 =...................min-1

Hence Calculate Relative Strength of acids.

Relative Strength of acids =

Write all details of calculations in your answer book.

Result : 1) mean k1= ......................min-1

2) mean k2 =.......................min-1

3) Relative strength of aeids = .................

Mean k2

Mean k1

2.303

t

a

a-xK = _____ log ___




Chemical Kinetics

To study the effect of acid strength (0.5 M and 0.25 M HCl solution) on hydrolysis of an ester

Procedure : Perform two sets of experiments as follows.

Set I : Bottle No. 1 : 5 ml of methyl acetate

Bottle No. 2 : 100 ml of 0.5 M HCl solution

Set II : Bottle No. 1 : 5 ml of methyl acetate

Bottle No. 2 : 100 ml of 0.25 M HCl solution

Keep these bottles in water bath for about 10 minutes to attain the same temp.

Transfer the acid soln. from bottle No. 2 to bottle No. 1

Note the mixing time as zero time. Pipette out 5 ml of reaction mixture for titration. Take five

readings including zero reading. Now repeat the same procedure for Set II. Ask for infinite readings

for both sets.

T∞ for Set I = ......................... ml

T∞ for Set II = ........................ ml

Present your results in the following tabular form :

Observation Table

Time in

min

(t)

0

10

20

30

40

Titration

reading

(Tt) ml

x = Tt - To a - x log ____ = Velocity

constant

(min-1)

Prepare simler observation table for the velocity constant - K2 for set II. Calculate the velocity

constant k1 and k2 by using the equation

k = _____ log _____

Result : 1) mean k1 =.............................min-1

2) mean k2 =.............................min-1

3) conclusian =

a = T∞ - To = ------------- ml.

a

a - x

2.303

t

a

a - x

K1




Chemical Kinetics

To investigate the reaction between potassium persulphate and potassium iodide in solution

with unequal concentrations of the reactants.

Given :- 0.1 N K2S

2O

8 , 0.1 N KI ; 0.002 N Na

2 S

2 O

3 . 5H

2O solutions.

Procedure : Perform the experiment as follows

Bottle 1. Place 10 ml. 0.1 N K2 S

2 O

8 solution + 30 ml. H

2O

Bottle 2. Place 20 ml. 0.1 N KI solution + 20 ml. H2O

Keep the two stoppered bottles in a water bath at room temperature to attain the same

temperature.

Transfer contents of bottle no. 2 to bottle no. 1 and shake well. Titrate 10 ml. of the reaction

mixture at the inervals of 10, 15, 20, 25, 30, 40 minutes from the start of the reaction against

0.002 N Na2S

2O

3 solution using starch as an indicator.

Enter your results in a tabular form given below.

a =....................... ml. Na2S

2O

3 ; b = ................... ml. Na

2S

2O

3

Sr.

No.Time in

minutes

(t)

Titration

Reading = x

ml. 0.002 N

Na2S

2O

3

(a - x)(a-x)

(b-x)

dm3 mole-1 min-1

2.303

t (a-b)

1 10

2 15

3 20

4 25

5 30

6 40

Calculate the values of a and b

Calculate the values of K by using above formula

Plot the graph of log against time (t) and from the graph calculate the value of k using

the formula, k =

Give all the details of your calculations.

Results : 1. Mean k (by calculation) = .................. dm3 mole-1 min-1.

ORk from graph = ............... dm3 mole-1 min-1.

(b - x)(a-x)

(b-x)log log

b (a-x)

a (b-x)

K =

(a-x)

(b-x)2.303 × slope

(a - b)

OR




Chemical Kinetics

Determine the order of the reaction between HBrO3 and HI.

Given :- 0.1N KBrO3, 0.1N HCl, 0.1N KI and 0.01N Na

2S

2O

3 solutions.

Procedure - Perform the set of experiment as follows.

Bottle 1. 25 ml. 0.1N KBrO3 solution

Bottle 2. 25 ml. 0.1N KI + 100 ml. 0.1N HCl + 100 ml. distilled water.

Keep the two stoppered bottles in water bath for about 10 minutes. Transfer the contents of

bottle 2 to bottle 1.

Titrate 25 ml. of the reaction mixture at the intervals of 5, 10, 15, 20, 25 and 30 minutes from the

start of the reaction against 0.01N Na2 S2O3 soln.

Enter your results in a tabular form given below.

a = .................. ml. Na2S

2O

3 ; b = .............. ml Na

2S

2O

3

Sr.

No.Time in

minutes

(t)

Titration

Reading = x

ml. of 0.01 N

Na2S2O3

(a - x)1

(a - x)

1 5

2 10

3 15

4 20

5 25

6 30

Calculate the values of a and b.

Calculate the value of k by using above formula.

Plot the graph of against t.

Calculate value of k from the graph by using the formula, k = slope

Give all the details of your calculations & Show that order of reaction is 2.

Results : 1. Mean k (by calculation) = .................. dm3 mole-1 min-1.

2. k from graph = ............... dm3 mole-1 min-1.

3. Conalusion -

1

(a-x)

k = = -

dm3 mole-1 min-1

1

a.tx

a-x

1

t [ ]1

a-x

1

a( )

Documents

SHIVAJI UNIVERSITY, KOLHAPUR Schedule... · SHIVAJI UNIVERSITY, KOLHAPUR Practical Examination in Chemistry at the B. Sc. Part-II March/April, 2015 Chemistry Practical ENCLOSURES