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Chemistry Lab Manual

The document is a laboratory manual for II PUC Chemistry, detailing various experiments and procedures for students. It covers topics such as chemical kinetics, thermochemical measurements, electrochemistry, chromatography, and titrimetric analysis. The manual aims to simplify complex concepts and enhance the learning experience for both students and teachers in the field of chemistry.

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0% found this document useful (0 votes)
31 views25 pages

Chemistry Lab Manual

The document is a laboratory manual for II PUC Chemistry, detailing various experiments and procedures for students. It covers topics such as chemical kinetics, thermochemical measurements, electrochemistry, chromatography, and titrimetric analysis. The manual aims to simplify complex concepts and enhance the learning experience for both students and teachers in the field of chemistry.

Uploaded by

swamybond007
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 25

ll PUC

- JI P UC

f'agc Nu. ,
Foreword CONTENTS I

I. Chemical Kinetics
The Kamataka State PU Chemist1-y Lecturer's forum has come
· ti-vJ for the NCERT
. a labora101-y manual for II PUC Ch em1s To study the efTcct o f concentration anti tempcr~ture un the rate of
out w ith reaction between Sodi um thiosulphatc and Hydrochloric acid.
To study the effect of concentrat ion of iodide ,ons on the rare o f reaction
sy llabus.
between Kl a nd H,O, t Hydroge n peroxide)

The distinguished members of this forum with their rich 1.3 To stud y the rate of reacti on between Pu1.assium iodate (KJO, ) and Sodium
sulph ite (Na,SO, )
experience of teaching have presented this laboratory manual in a
simplified manner so that the students can understand easily and 2. Thermochemical Measurement

perform the experiments. Being a chemistry teacher for nearly four p To determine heat of so lution of potassi um nitrate or copper sul phai..:.
decades, I personally feel that this laboratory manual is simple, 12 To detennine heat of neutrali sation of strong acid [HCIJ with a stro ng ba,e
(NaOH)
excellent and unique. I am sure that this manual will be of immense 2.3 To study enthalpy change during solubility of Chloroform and Acetone.
help to students and also to the teachers. I am very much honoured
3. Electrochemistry
and privileged to thank the most distinguished experienced members
of this forum for their splendid job in bringing out this laboratory .To study the variation of cell potential of the ce ll Zn!Zn'· II Cu' "/Cu wi th
'f' change in the concentration o f electrolytes (CuSO, / Zn SO,J at room
manual. temperature.

4. Chromatography
I am confident that this laboratory manual is highly useful to
both the students and the teacher.
1 Separation of the pigments present in leaves and flowers by ascending paper
chromatography and determination of R, va lue (Retardation fa ctor)
10

4.2 Separation of the constituents of a mixture of compounds containing Pb'"and 11


Cd'' ions using ascending paper chromatography and to ca lculate the R, value.
01.03 .2024 Dr. N.Lakshmana Rao
Bangalore Retd Prof. in Chemistry 5. Titrimetric Analysis (Redox Reaction)

St. Aloysius PU College 12


-5. 1 Determination of molarity of KMnO, using 0 . 1M oxa lic ~cid by volumetric
Bangalore analysis.

13
5. 2 Determination of molarit y of KMnO, usin g 0 . 1 M Fi\S by volumetric
analysi s.
IIPUC IIPUC
Page No.
Government of Kamataka
I.\
Department of Pre University Education
I 6. Systematic qu alitatiw analysis of inorganic se lls. 18th Cross, Malleshwaram, Bangalore
I
i 7. Model procedure for the an al~·sisof a simple inorganic sail 20 II PUC CHEMISTRY
if
I .
Tests for funrrion al groups in organic compounds 3I
Ex periment
Experiments to be conducted for the Academic year 2024-25
Experiment s Hours
I 9. Preparation of ino rga nic compounds 34 No.
To detem1 in e the concentration molarity of KM nO, so lution by titrating it
I 2 Hrs
Preparation ofFerrousammonium sulphate (FAS or Mohr 's Salt ) against 0.1 M standard solution of ferrous ammonium sulphate.

II Preparation of Potas h A!urn


Preparation of Potassium Trioxa !Jtoferrate (Ill )
2.
To determ ine the concentration/molarity of potass ium pem,anganat e
solution by titrating it aga inst 0.1 M standard solut ion of o.xali c ac id 2 Hrs.
Systemati c qualitati ve analysis of simple inorgan ic salt (General procedure
., 3.
to be ex pl ai ned and recorded)
2 Hrs.
10. Preparation of organic compound s 35
4. Systemat ic qualitative analysis of simple inorganic salt I and 2 2 Hrs.
rf!- To prepare ace tanilide from ani line. 5. Systemat i, qualitative analysis of si mple inorganic salt 3 and 4 2 Hrs.
tf-2 T0 prepart' dibenza l acetone IDibenzylidinc acetone) 6. Systemati c qualitative analysis of simpl e inorganic salt 5 and 6 2 Hrs.
11ft To prepare p-nitroacetanilide from acetanilide
Itf To prepare Phenyl-azo-P-naptol (an azo-dyc)
7.
8.
Systemati c qua litat ive analys is of simp le inorganic salt 7 and 8
Systematic qua litati ve ana lysis of simple inorganic salt 9 and 10
2 Hrs.
2 Hrs.
11 .5 To prepare An11i.ne yell ow (p-amino-azo-benze ne)
9. Tests for functiona l groups in organic compounds 2 Hrs.
11. Tes ts for Cnrbohydratcs, Fats and Proteins 38 Effect of concentration on rate of reaction between sodium thiosulphate and
10. 2 Hrs.
hydroch loric acid
Tcm for Carboh ydrnt cs Effect of temperature on rate of reaction between sodium thiosulphate and
II . 2 Hrs.
Tests for Oils and Fats hydroch loric acid
Te, ts for Proteins 12. Detennination of enthalpy of soluti on of KNO, or CuSO, 2 Hrs.
I 13. Deten11ination of enthalpy of neutral ization of HCI and Na OH 2 Hrs.
1 12. Viva qu esti ons for functional groups in organic compounds 39
14. Determination of enthalpy change on mixing chl oroform and acetone 2 Hrs.
To study the va ri ation in cell potential of the cell Zn I Zn'' II Cu'· ICu wi1h
I J. Schem e of valuation in II PUC Fin al practical exa mination 42 15. change in concentration of electrolytes (CuSO, /ZnSO,) at room tcmpcrnturc 2 1lrs .
Separation of pigme111s present in leaves and !lowers by paper
14. preparation of Some Commo n Desk Reai;ent s 44 16. chromatography and detcm, ination of R, values of co mponen ts 2 li es .
Separation of constituents of a mi xture of inorgani c cnmponcni, con taining
17. two cati ons Pb'' and Cd'· using chromatographic technique 2 Hrs

18. Prepara ti on of Ferrous ammon ium sulplrntc crysta ls (Mohr's salt ) 2 fi rs .


19. Preparation of potash alum 2 llr,.
20. Preparation of dibcn zal acetone (Dibenzylidene acetone) 2 Hrs.
21. Preparation of p-nitroacetanilidc from acctanilide 2 IIr, .
22 Preparation of phenyl a7o ~-naphthol (an azo dye )
____
~ I !r,.
]
IIPUC IIPUC

I. CHEMICAL KINETICS Effect ofTrmpcraturc on rnlc of reaction :


E).¢riment No. I.I . Apparatus rc11ulrcd: Burctte, Pipette, Thermometer& Stop Clock
_,,Aim: To study the effect of concentration and temperature on the rate of reaction
between sodium thiosulphnte and hydrochloric acid solution . . Chemknl~ required : 0. 1 M Na,S,O, IM HC I
Sodium thiosulphatc reacts with hydrochloric acid giving a translucent col101dal solution of
sulphur. Procedure:
Equation: Na,S,O~.., + 2HC I,.,, - 2NaCI,.,, + H,O., + SO""+ S t 50 mL of Na,S,O., (0. 1M) is taken in a beaker havi ng •x·mark of pencil al the centre oflhe outer
The rate of precipitation of su lphur in the solution increases with increase in temperature and
increase in concentration of reactants . The increase in temperature increases the kineti c energy o f surface of the bottom is placed in a lhermoslal mai ntained al 30'C
reactant molecules and the increase in concentration increascs the number of molecular collisions per
unit vol. of solution. 5 mL of IM HCI so lution is added into the beaker containing Na,S,O, from the burcttc and the
Effect ofConcentrallon on rule ofreactlon: solution is shaken well . HCI & Na,S,O, will react together forming a yellow precipitate of
l\latc.-rials n-qulred: Burctte. Pipette, Them1omcter & Stop clock, 0 I .M Na,S,O, & IM HCI.
Procedure: sulphur. Therefore lhc solution becomes curbid and hence the 'X ' mark becomes invisible.
50 mL ofNa,S,O, (0 .1M) is taken in a 100 mL beaker having a ·x·
pencil mark at the centre of
the ouh:r , urface of the bottom . It is ·then kept in a trough containing water to allain constant A stop clock is started afier adding about 2.5ml of HCI solution and the time at which the · X ·
temperature. mark becomes invisible is recorded .
I mL HCI ( I MJ solution slowly added into the beaker containing Na,S,O, from the burctte with
constant shaking. HCI & Na,S,O, will react together giving a yellow ppt. of su lphur. Therefore The above procedure is repeated with fresh sample of Na,S,O, so lution kept in thermostat at
the solution become gradually turbid and the· X • mark become invisible. ·x• mark becomes invisible
40'C, 50'C. 60°C and 70'C temperature and the rime at which the
A stop clock is staned after adding about 0.5ml of IM HCI solution and the time at which the
'X · mark become invisible is recorded. is recorded.
The experiment is repeated with fresh sample ofO. IM Na,S,O, by adding 2ml. 4ml, 8ml &
16ml of IM HCI solution and the corresponding time at which the ·x·
mark is invisible arc Tabulation
recorded.
Tabulation
SI. No. Thermostat Temperacurc Time al which •X · mark becomes invisible
SI. No. Vol. of HCI added in mL Time 't' in second taken of ·x• mark becomes invisible
30'C
40'C
so'c
4
60'C
70'C
16
- Graph : A graph oftcmpcracure vis rime is plotted
,...Graph : A graph of volume of I-I C I V is time is plotted
y-axis
y-axis

i~

Vol.ofHC:·L~i, .5

added in mL · •.
OR
!/ Time in
Seconds
OR

....···· x-axi s
~/
~ ,c___ __ _ _ l - - - x-axis
'-----------+ x-axis
Tcmperacure in 'C
X- 11.l[ U

Time in sec.

Conclusion : Rate of reaction increases with increase in cone. of reactants.Time in sec. Conclusion : Rate of reaction increases with increase io tcmperonirc __________
lime in flee .
__,

- 1· -2-

I
j
IIPUC
IIPUC

E~ent No. 1.2 y peflment No. 1.3


.A:1m: To study the effect of concentration of iodide ions on the rate of re.action Aim: To study the rate of reaction between potassium iodate (KIOi ) and sodium
between Kl a~d H1O1 (Hydrogen peroxide) sulphite (Nal so))
Apparatus & Chemicals required : 2.5 M H,SO, , 0. IM Kl , 0.04 M Na,S,O, & 3% H,0, . Appnrnlus & Chemicals required : 2 M H,SO, . 5% starch solution, 6% KIO, & 6% Na,SO, ,.
five conical flasks (250 mL).
five conical flasks (250 mL).
Hydrogen peroxide is an oxidizing agenl which will oxidize Kl inlo I, in ac idic medium.
When potassium iodate and sodium sulphite solution arc mixed the following reaction
takes place.
2K I +H,O, + H,SO, ➔ K,SO, + 2H,O + I,
The reaction mixture is treated wilh sodiu m thiosulphale and starch solu1ion. The I, liberated in Equation: KIO, + 3Na,SO, ➔ Kl +3 Na,SO,
the solu1ion will oxidize sodi um thiosulphate into sodium tctrathionalc. When the oxidation is over
then the excess of I, present in the solution combines with s1arch fom1ing n deep blue coloured complex 5KI+KIO, +3 H,SO, ➔ 3K,SO,+3H,O+31,
compound. The lime taken to combine with fixed amount of sodium 1hiosulphatc will be known from The iodine liberated produces blue colour with the starch solution.
the lime of appearance ofbluc colour.
Procedure:
I, +2Na,S,O, ➔ 2N a l + Na,S,O, I, +starc h ➔ Deep blue solulion 25 mL of KIO, is mixed with 25 mL of 2M H,SO, and 50 mL distilled water in · A' labeled
conical flask and is then kept in a water bath to attain constant temperature.
Sodium thiosulpha1c Sodium tetrathionate.
20 mL Na,SO, + 5mL starch+ 75 ml distilled water is taken in 'B' labeled conical flask and is
then kept in a water bath to attain constant temperature.
Procedure:
15 mL Na,SO, + 5mL starch+ 80 mL distilled water is taken in 'C' labeled conical flask and is
25 mL of H,O, is m·ixed with 25 mL H,SO, & 5 mL starch solution in ·A' labeled conical flask
then kept in a water bath to attain constant temperature.
and is kept in a water bath lo attain conslanl room temperature.
IO mL Na,SO, + 5mL starch+ 85 mL distilled water is taken in 'D' labeled conical flask and is
A mixture of IO mL Na,S,O, + IO mL Kl + 80 mL distilled water is 1aken in · B' labeled conical
flask and is kepi in a waler balh 10 altain constant tcmpcralUre. then kept in a water bath to attain constant temperature.
A mixture of IO mL Na,S,O, + 20 mL Kl + 70 mL distilled waler is iakcn in 'C' lahclcd conical 5 mL Na,SO, + 5mL starch+ 90 mL distilled water is taken in 'E' labeled conical flask and is
l
flask and is then kept in a water bath to aIla in constant temperature. then kept in a water bath to attain constant temperature.
'i
l1 A mixture of 10 mL Na,S,O, + 30 mL KJ + 60 mLdistillcd water is taken in ·o· labeled conical ,25 mL of• A' & 25 mL of 'B' conical flask solutions are mixed together in a separate conical
flask and is kepi in a water ba1h to attain constant temperature. flask . A stop clock is started afier adding half of 'A' flask solution. The time taken for the
25 mL of· A' flask solution is mixed with 25 mL of 'B' flask in a separate conical flask with appearance of blue colour is recorded. The above procedure is repeated for solutions of 'C', 'D'
consl.ant shaking. After adding half of the solulion a slop clock is started and the lime taken for & 'E' flask and the time for the appearance ofblue colour to the solution is recorded.
1be appearance ofblue colour is recorded. The whole experiment is repeated twice and the average time for the appearance of blue colour
The procedure is repealed for ·c· & ·o· flask solu1ion and 1he time taken for the appearance of is found.
~lue colour 10 1he solution is recorded. The whole experiment is repealed twice and 1he average Tabulation
time ofappcarance ofblue colour is found .
Time taken for the appearance
Tabulation Composition of mixture of blue colour
0 ,, SI. No. Average time
Time taken for the appearance I II
SI. No. Composition of mixture of blue colour Average time I 25 mL ' A'+ 25 mL 'B'
I JI
I 25 mL ·A' + 25 mL ' B' flask solution 2 25 mL 'A'+ 25 mL 'C'

2 25 mL ' A'+ 25 mL 'C' flask solution 3 25 mL 'A'+ 25 mL 'D'

3 25 mL ·A' + 25 mL •D' flask solution 4 25 mL 'A'+ 25 mL 'E'

Conclusion : Rate of reaction increases as concentration of one of the reactant increases. Conclusion : The rate of reaction decreases on decreasing the concentration of one of the reactants .
. 3.
-4-
IIPUC II PUC

2. THERMOCHEMICAL MEASUREMENT Experiment No. 2.2

Experiment No. 2.1 Aim: To determine the heat of neutralization of strong acid (HCl) with a strong base
Aim: To determine the heat of solution of potassium nitrate or copper (NaOH)
sulphate Solutions required : I00 mL IN HCI & I00 mL I N NaOH
Definition : The amount of heat energy liberated or absorbed when I mole of a solute is completely
dissolved in excess of solvent such that the further dilution does not alter the heat change 1s called heat Definition : The amount of heat energy liberated or absorbed when I g equivalent mass of an acid is
of solution. completely neutralized by I g equivalent mass of a base in dilute solution is called heat of
Apparatus required: 250 mL of polythene bottle with stirrer, Thennometcr (I/I 0)'C neutralization.

Reaction : KNOJ(S) +oq ➔ KNO~,., HCI,,,, +NaOH,,,, ➔ NaCl,..,+ H,Om; L.\H,= -ve
Chemicals required: I0gKNO, (or I0gCuSO, .5H,O)
Procedure: Take a 250 mL polythene bottle fitted with a two holed cork. A thermometer and.a stirrer
Procedure: About IO g powdered KNO, crystals are taken in a clean and dry weighing bottle. It is
weighed accurately and the mass m, g of it is noted. 200 mL of distilled water is taken in a 250 mL are inserted into the bottle through the cork. This serves as calorimeter (because heat absorb; d by the
polythene bottle fitted with a thennometer and stirrer and its temperature T,K is noted. The crystals in calorimeter is neglected). 100 mLof I N HCI is taken in the polythene bottle.and its te~ perature (t,,,) is
the weighing bottle arc transferred carefully into the polytl1ene bottle and stoppered immediately. It is noted. I00 mL of I N NaOH is taken in a beaker and its tcmperatui'e (t,.,) is noted. Now pour the NaOH
stirred gently to dissolve the crystals. KNOJ dissolves by decreasing the temperature of solution. The solution into the polythene bottle, it is immediately stoppered and stirred gently. HCI & NaOH make
lowest temperature ottained (T, K) is noted. Now the empty weighing bottle is weighed and its mass
exothermic reaction liberating heat energy. Therefore the temperature of the solution will increase. The
m, g is noted.
maximum temperature attained by the solution (T ,-) is noted.
/ Observations :
I. Mass of weighing bottle + KNO,crystals=m,= .. . ..... .... g ,.,.-Observations:
2. Moss of empty weighing bottle =m,= .............g I. Temperature of HC!solution = t,=". ................... .. .. .... K
3. Mass ofKNO,crystals takcn=W=(m,- m,)= ............. g
2. Temperature of NaOH solu,tion=t_=........ .....(. ...... ) ...K
4. Temperature of distilled water =T,'G= ....... ... ,.. K t,.+t,
3. Averagetcmperature,beforemixing = T,'C = ---:;- = ......................... ..... K
5. Lowest temperature attained by the solution = T,'C= .. .. ....... .K ·, -
6. Fall in temperature = t =(T,- T,)'C " .. . .. ....... K 4. Maximum tempcrature•auained'bytl!e ll)ixture = T,°C .. ... ...... K
l
7. Mossofsolution c m= (200+W) = .... ........ g 5. Rise in tcll)perature=t='(T,-T,)'C-= .. .............. K
8. Specific heot of water = s =4.2 J K·'g"'
6. Massofsolution(IOOmLHCt .i I00mLNaOH) = m= 200g.
' .,. " 1 1
7. Specific heat of water=
~[= 4.2JK· g·
I Calculations: ( mass of)
·• · solution x fall i n )
cmperature e&lculatlons :
Heat obsorbed "' . · (m) ( (1) Heat liberated = q = (m) mass of solution x (s) specific heat x (t) rise in temperature
q= 200 X 4.2 X t

·x· =........... .
.. .. J IOI.IX X q = .............. J
l-leatubsorbedby 101. lgKNO,( I mole) - .. ....... .. ... J/mol I00 mL of I 1:-1 acid or base contuin 0.1 gram equivalent mass
w
I000 mL of acid or base contains I gram equivalent mass
Result : Heat of solution of KNO, = L.\H, =.......................kJ /mol 1
Heat liberated by the neutralization of l000 mLofl N HCI = 10 x q J = ................ .. X 10· kJ
Note : To detem1inc the the heotofsolutionof CuSO, replace KNO,
(249.5gCuSO,.5H,O = I mole =.... .. .J/mol) Result: Heat ofneutralization of HCI with NaOH = .!\H, .. ... ...... ...... . kJ

-6-
-5-
IIPUC
IIPUC

Experiment No. 2.3


3. ELECTROCHEMISTRY
Aim: To determine the enthalpy change on mixing Chloroform and Acetone.
Ex · entNo. 3.1
Principle: Acetone and chlorofonn is a real solution showing -ve deviation from Roult's law. Acetone
mixed with chloroform by forming H - bond along with release of heat energy. im: To study the variation in cell potential of the cell Zn / Zn l• II Cui•/ Cu with
change in concentration of electrolytes (CuSO,/ ZnSO,) at room temperature.
Equation: (CH,), C=O+H-CCI, ➔ (CH,), C=O.. ........H -CCI, Theory: The Daniel Cell is symbolically represented as
1
Chemicals required: Acetone, chloroform Zn.,/ Zn ·,,., 11 Cu '\,.,tC11i,1
0
Apparatus required: Polythene bottle. stirrer, thermometer If the concentration of Zn '',..,1and Cu ' ,.
1 1
is I Meach.
0
Procedure: Then the E = E\, - E',.. =+0.34-(-0.76)= I.IV
.,0

8.14 mL of chloroform (0.1 mol) is taken in a 50 ml beaker and its temperature is noted (t,°C) On changing the concentration of metal ions in solution, the• E' cell values also changes. In this
experiment keeping the concentration of Zn'' ion as constant, changing only the concentration of Cu''
7.34 mL of acetone (0.1 mo!) is taken in a I 00 mL polythene bottle and its temperature is noted ion, the emf of the cell is calculated using Nemst equation. ·
(t,'C)
2.303RT [Cu'' J 0.059 [Cu 1' ]
Chloroform is added into polythene bottle, stoppered and shaken well for uniform mixing. E., 0 = E'.. u + nF log [Zn'' ] OR E.,.= E..,u + log [Zn'' ] at298 K
Acetone mixed with chloroform liberating heat energy, increase in temperature of mixture is
noted (T,'C) Materials required : A strip of copper, a strip of zinc, a large beaker, porous pot, a plastic tube, cotton,
Calculation : 40 mL ofl M CuSO., 40 mL of I M ZnSO., , distilled water, a voltmeter with oscillator clips.
Procedure:
I. Initial temperature of chloroform: t,'C =..................
I. About I00 mL of I M CuSO, solution is taken in a porous pot. Copper metal strip is dipped
2. Initial temperature ofacetone: . t,'C = ....................

3. Averagetemperature = c•:t) =T,'C = .......... ...............°C


into it.
2. About I00 mL of 1 M ZnSO, solution is taken in a large beaker. A zinc metal strip is dipped
into it. A salt bridge of KCI is used to connect the two solutions. Thus the Daniel Cell is
4. Temperature of mixture of chloroform and Acetone= T/C = .. ....................°C formed. • ' i
I
5. Riscintempcrature t = (T,-T,) = .................... . 3. The copper plate with +ve terminal & zinc plate with the -ve terminal are connected to the
voltameter as shown in the figure.

'.
6. Waterequivalentofcalorimctcr=wg = ... ........... g
4. As soon as the circuit is completed, electric current will begin to flow & then the voltmeter
7. Densityofchloroform = l.47g/cm' reading is noted which indicates the e.m.f. of the cell. This is reading Number (I).
8. Density ofacctonc = 0.787 ~/cm' 5. The above procedure is repeated with IM ZnSO, solution and 0.2M, 0.1M, 0.05M CuSO,
9. Speci fie heat of chlorofonn = S,=0.96 J/g solution. The corresponding readings are recorded as 2, 3 and 4.
Electrodes reactions are
10. Specifichcatof acetone S, =2.l8J/g
Enthalpy ofmixturc w x sp. heat x t Atanode :Zn ➔ zn''+ 2e- (oxidation)

[(8.l4x l.47xS,)+(7.34x0.79xSJ]xt
At cathode : Cu"+ 2e- ➔ Cu (reduction)

Result : Enthalpy of mixture ofAcetone and chloroform is ~H.,,=..... ... .J


-7- -8-
IIPUC IIPUC

4. CHROM ATOGR APHY


lathe cell : Zn + eu ➔ Zn'·+ Cu (overall reaction)
1
• Experim ntNo. 4.1
ascending paper
Ai : To separate the pigments present in leaves and flowers by
E.m.f. of the cell can be calculated using Nemst equation
chromatography and determination of R, value (Retardation factor)
aphy. The R, value of
2.303 x 8.314 x T log [Cu,. i,,,] Principle : The components of the pigment are separated by paper chromatogr
E.,.= I.I + :! x 96500 each component is calculated.

Distance travelled by the substance from the reference line in cm


1
R,=
The graph is obtained by plotting cell potential on y-axis & log[Cu ' 1,., ]
on x-ax is Distance travelled by the solvent front from the reference line in cm

n
--6bsen•ation & Calculation: Study of variation of emf with respect to concentratio Procedure:
Calculated EMF of the cell Preparation of green pigment from leaves & colour pigments from flowers.
Reading Concentration of CuSO, Observed EMF of the paste into separate test
the cell (volt) from Nemst equation (volt) I . Grind the flowers and the leaves separately in a mortar and transfer
No. Solution
tubes.
I shaken well. The mixture is
2. Small amount of methanol or acetone is added to the paste and
filtered and the filtrate is collected with a test tube and corked.
2
x 17 cm is taken. A line at
A special adsorbent paper like whatman filter paper No. I of size 4 cm
end of the filter paper with a pencil is marked. Using a capillary tube drops of the
3 about 3 cm from one
of filter paper (as shown in front
prepared pigments are kept on the points a & b marked on the line
are rich with the pigments. The dry
4 cover page) and allowed to dry. This is repeated till the spots a & b
paper just dips into a solution
filter paper is hanged in a closed jar so that the bottom end of the filter
containing 19 ml of ether and I ml ofacetone or chloroform ( eluent)
Conclusion : Increase in (Cu'l increases the emf of the cell. The pigment spots also
The solvent slowly moves upwards to _reach the top due to capillary action.
Increase in [Zn • Idecreases the emf of the cell.
1

different distances along with the mobile phase when the solvent raises to about 15 cm on the
move to
is marked with a penci I. This
filt er paper, it is removed from the jar. The distance travelled by the solvent
from the reference points a and b
is called solvent front. Similarly the distances travelled by the pigment
can be calculated from using the
are also measured. The R, values for the components of the pigment
formula.

Distance travelled by the green pigment


R, value of the green pigment =
Distance travelled by the solvent front

Distance travelled by the coloured pigment


R, value of the colour pigment =
Distance travelled by the solvent front

-10-
-9-
Experinrent No. 4.2
_,/ .
-
m ounds containing Pb'" and
IIPUC
LI PUC

5. TITRJMETRIC ANA LYSIS


(REDOX REACTION)
~fm: To separate the constituents of a mi xture of co P
Experiment No. 5.1
h and to calcu late the R,
Cd 2• ions using ascending paper chromatograp Y Aim: Determination of Molarity of KMnO, usin g 0. 1 M O xalic acid by vo lu metric
analysis.
(retardation fac to r) values. Priocip~c :
. . . .. ,. . h and they are co loured using the Ac idified KM nO, will oxiJi ze oxalic ac id into CO, & H,O. Hence known vo lume of o.xa lic aci d is
Prmctple: The cauons Pb· and Cd are separated by chromatograp Y titrated aga inst KMnO, Here K.M nO,actsas ox idizi ngagenl and oxa lic acid acts as reducing agent
. th e ions on the fi lter paper their R, 60'C
developer ammonium su lphide . By measuring distances moved by es Chemica l Equation : 2K.M nO, + 3H,SO, + 5H,C,O, ➔ K,SO, + 2MnSO, + 81-1;0 T I 0CO,

, values are calculated. Ion ic Equ ation: [MnO; + Se+ 8H. ➔ Mn 1 ·+ 4H 1O·1 x 2 .. . ....... Reduc tion.
Procedure : [c,o: ➔ 2CO,+ 2clx5 .. ... ....Oxidation.
nd Procedure :
The experiment is repeated as in experiment 5.1 using the solvent mixture ethanol. cone. HNO, a
A pipette is washed with water and then ri nsed wi th the given oxa lic acid so lution. A bure ttc is
distilled water in the ratio 8: I: I (eluent) when the solvent front moves on the tilter paper carri es the ions washed with water and then ri nsed with K.M nO, solution. It is ti ll ed with KM nO, solut ion and fixed to a
stand. lnil ia l burette reading is noted 10 the upper meni scus. (coloured solution).
ab o to the d1fferem heights. When the so lvent front moves about 15 cm on the tilter paper it is removed
Exactl y 10 ml of0. 1 M oxalic acid is pipetted out.into a clean conical nask and I test tube fu ll or
dried & the spots oflhc ions are coloured by spraying ammonium sulphide (Aq . NH,+ H, S). PbS gives di!. H,SO, is added. Th e so lution is heated to 60"C.The hot solution is titrated aga inst KMnO, taken in
the burelle until a pennanenl pale pink co lour is obtained. Tbi s is 1he end po int of titration .The burellc
black spot whereas CdS gives yel low spot. The distances of these spots moved from the refe rence line readings are recorded & the tit ration is repeated for agreeing values.
Observations:
are measured . The distance travelled by the so lvent front is also measured. There by R, values of both I. Burelle: K.M nO, soluti on
2. Con ica l fl ask: 10 ml H,C,O, + I Test tube fu ll ofd il. H,SO, so lution
Pb'· and Cd' ' ions can be calculated.
3. Indicator: KMn O, is self-indicator
4. End point : Co lourless to pale pin k
Tabulation ·
Di stance rravelled by Pb'' ions in cm Tria l No.
R., va lue of Pb'· ion = Burette readings
I II Ill
Distance rravell ed by the so lvent front in cm Final read ing 2c. 0 '2'2· 0 2-2..- . '
Initial readi ng o ,oo 0 · 01) o -oo
Distance rrave llcd by Cd'· ions in cm Volume of KMnO, added in ml
R, value o f Cd'' ion = Volume of KMnO, ~v ,= ....... ml
Distance travelled by the solvent fro nt in cm Calc ulation s: I a, (M , x V,) , ., 00 . = a,(M, x V,) 11 ,,.,o, I 2-2......,
We know thal,
Where a, = No. of electrons ga ined per fo rmu la uni t o f KMnO, ~ 5
a, = No. of electrons lost per fo nnul a unit of Oxalic ac id = 2
_ 2_ X M,V, 2 X 0. 1 X I0
M,- 5 V, 5 XV,
Result : Mo larityo f KMnO, =M, = .. .... M
· 11, - 12·
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Experiment No. 5.2 6. SYSTEMATIC QUALITATIVE ANALYSIS OF


Aim: Determination of Molarity of KMnO, using 0.1 M FAS by volumetric SIMPLE INORGANIC SALTS
analysis. Analysis of salts means identification of cations and anions present in the salt. Salt is fa nned by
A'rlnciple : . . the neu1rnliza1ion reaction between an acid and a base. The No. of units of charges carried by an ion is
Acidified K.MnO, can ox idise FeSO, of FAS into Fe, (SO,),. Hence known volume of FAS ts titrated equal 10 its valency.
agai nst K.MnO, Here KMnO, acts as oxidizing agent and Ferrous sulphate acts as reducing agent.
Arid Radicals (Anion) Basic Radicals (Cation)
-Chemical Reaction:
2KMnO, + 81-1,SO, + !0FeSO, ➔ K,SO, + 2MnSO, + 81-1,O+ 5Fe,(SO, ), I) They cany-ve charge I) They carry +vc charge
2) They can be detected by using solid (0.1g) 2) They can be detected by using origi nal
..Jonie Equation : Mno; + 5e"+8 H"➔ Mn l• + 4H,O ..... Reduction .
sa il solution (2 or 3 drops)
[Fe'· ➔ Fe,. +e·]x5 ..... Oxidation. 3) They can be detected in Acidic medium with 3) They can be detected in Basic medium with
Yrocedure : P"<? P">7
A pipcne is washed with water and then rinsed with the given FAS solution. A burette is washed 4) Reaction can be seen in the fonn of 4) Reaction can't be seen instead the product
wi th water and then nnsed with K.MnO, sol ution. It is fill ed with K.MnO, solut ion and fixed to a stand . . effervescence, colour and odourof gas. wi ll be seen as precipitate.
Initial burcuereading is noted to the upper meniscus (coloutcd solution).
Exactly IOmL of 0. 1 M FAS is pipetted out into a clean conical flask and about I test tube fu ll of Analysis of a sa lt involves four steps which arc as follows:
di!. H,SO, is added. The solution of the conical fl ask is titrated against K.MnO, taken in the burclle until I. Prel iminary test 2. Detection of anion
a permanent pale pink colour is obtained. This is the end point of titration. The burcllc readings are 3. Dc1ccrionofca1ion 4. Rcpon ofsalt
recorded & repeat the titration for agreeing values. I. Preliminary Tests:
Obsen •atlons : a) State : Crystalline or Amorphous
I. Burcllc : KMnO, solution
b) Colour : White / colourless. light green (Fe ''), green (Ni"'), Blue (Cu''>. Brown (Fe"'). li ght
2. Conical fl ask: IO mL ofO. I 1\1 FAS + I test tube fu ll ~fdil. H,SO, solution pink (Mn"'). Violet (Co' ').
3. Indica tor : KMnO, is self- indicator c) Solubili ty test:
4. End point · Colourless 10 pale pink
Tabulation : Water dil.HCI dll.HNO,

Trial No. Cold Hot Cold Hot Cold Hot


Durette readings
I II Ill
Final readi ng
II. Classification of Anion (Acid Radicals).
Initial reading

Volume of KMnO, added in mL Group Group Reagent Rndlcnls present

I C•""''"'" '
We know 1hn1.
Volume of K.MnO, =V, = .. ....mL
di!. H,SO, / dil . HCI
I

co,·•
Where a, = No. ofelectrons gained per fonnu la uni t ofKMnO, ~ 5
II Cone. H,SO, Cl . Br , No, ·
a, = No. of electrons lost per fonnula unit of FAS = I

I I
M,= - X - ' -'
5
MV

v,
I x 0.1 x IO
5 x V, Ill
No reagents so;'
I '6-sufl : Molarity ofKM nO, =M, = .. . M
. IJ. -14-
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IIPUC
1
Ill De1ec1ion of I group anion
Silver Nitrate test for Chloride ion (Cr)
Obsen·ation Inference
Elperiment
Salt solution +AgNO, solution Curdy white pp!. which is Chloride ion (Cl') is confirmed
Sall + dn. H,S0/ d1I. HCI Brisk effervescence liberating I group Carbonate anio n (CO,") soluble in excess of NH,OH
(beat if neccss:iry) colourless. odourless gas which may be present
turns limcwatcrmill--y Confirmatory test for Bromide ion (Br) (Globule test).

Confirmatory test for Carbonate ion (CO,' ) {lime water lest). Experiment ,'(-..,...,..ov...
~ (JJ" 'Obsen-ation Inference
;'

upcrimeot Obsen-ation Inference Salt + Ware ~ to dissolve An orange red g lobule is Bromide ion (Br ·) is confirmed
+ Cl, water + 3 drops of CCI, , formed
Salt + Water. boi l the gas Lime wa ter docs not turns Carbonate ani o n (CO;' ) is
the mixture is shaken well
liberated is passed into the test mill--y confinned
tube contain ing lime water Silver Nitrate (AgNO, ) lest.

Detection of 11 group anions. Salt solution +AgNO,solution Pale yellow ppt. which is Bromideion(Br ')is confirmed
sparingly soluble in NH,OH
a. Salt + conc.H,SO, is taken a. A colourless pungent smell II group ch loride ion (Cr) may
in a dry test rube. gas which gives dense while be present Confirmatory test for Nitrate ion (NO, ·) (Brown ring lest).
fumes with glass rod dipped
in NH,OH is ex posed to the Salt solution + equal volume of A brown ring is formed at the Nitrate ion (NO,') is confirmed
mouth oflhe test tube freshly prepared FeSO, solution junction of two liquids
+ few drops of cone. H, SO, are
b) White fumes followed by
Reddi sh brown pun gent Bromide ion (Br') may be added slowly along the sides of
present the test tube.
fumes
Detection of Ill group anion
b. lfno reac tion in cold a piece Reddi sh brown fum es are Nitrate anion (NO; ) may be
Test for sulphate ion (SO, .,).
of Cu / Paper ball iJ added to evolved present
Experiment Obsen-ation Inference
the test lube and heated

Sall solution + BaCI, solution A thick white ppt. is ob~ined Ill group Sulphate ion (SO;' ) is
Confirmatory tes t for Chloride ion (Cl) (Chromyl chloride test).
Above ppt. + excess ofdi!. HCI Precipitate is insoluble present and confirmed
Sa ll + K,Cr,O, crystnl s in a dry O range red vapo urs arc evolved
tes t tube + conc.H,SO,. Detection of Cations ffiasic radicals)·
The detection of basic radicals of salt is based on the precipitation react ion in solution. Hence it
The above va pours are passed
Yellow solutioni s obtained is necessary to prepare the solution of salt or original solution (O.S)
into a rest tube con taining
NoOH so lution Preparation of original solution (OS): The salt may be soluble in H,O or dil.H CI or dil.HNO, . The
choice oflhe solvent to prepare original solution is known from solubility test under preliminary test.
To the above yello w solution ~ Bright ye llow prccipi tntc Chloride anion (Cl') is Preparation : About½ test tube of solvent is taken and the salt is added little by little with constant
acetic ac id + lead acetat e
confirn1ed shaking until a saturated cl ear, homogeneous solution is obtained.
solutions are added
Nole: Always use 2 or 3 drops oforiginal solution forthc detection ofbasic radicals.

-15- - 16-
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II PUC
CLASSIFICATION OF C ATIONS(BASIC RADICALS) Conflrmutory tcsl for Aluminium Ion (Al'')
Group rcui:cnt Nalurc of prccipllutc
Group No. C11lons pmenl a) OS + di!. NaOH, first small A white gelatinous ppl. soluble
quantity, followed by excess in excess of NaOH giving a
0 NH: No rcngcnl c;lcar solulion Aluminium ion (Al ' ') is
dil.llCI Above clear solu1io11 + solid White gelatinous ppl. reappears confinncd
NH,CI, boil & cool under lap
-- dil.llCI t 11,S g~s -- wutcr Aluminium ion (Al ' ') is
NH,Cl,,. + excess Nll,011 Hydroxide prcci pirntc b) OS + blue litmus solution + A blue floaling mass is fom1cd confinncd
Ai"' drops ofNH, OH
NH, Cl,,,+ excess Sulphide prccipiratc 1
zn· . Mn ·
1 1 Annlysls of IV group cut Ions (Zn · , Mn'').
NH,011 + 11,S gas
OS + one spaluln of solid A white or flesh coloured IV group calions ( Zn ''or Mn '')
NII, Cl,,, • excess Carbonntc preci pitnle NH,CI + excess of NH,O1-1
Ba'' , Sr·•& Ca·• precipitnle is fonncd . may be pn:scnl
NH,011 + (Nli,),CO, solution + l-1 1S
Mg·• No rengcnt -- Confirmntory ll'st fo r Zinc ion (Zn'').

Dcrrction or •zero' group cation. Ammonium Ion (NH, · ), I. OS + dil. NuO l-1 A while ppl. soluble in excess of Zinc ion (Zn'') is con finn ed
NnOH is fonncd
Eiprrlmtnt Obscnullon lnkrcncc A bluish White prccipitale is Zinc ion (Zn'') is con finned
2. OS + K,[Fc(CN), ]
fonned
Salt + di 1. NaOHsolution Pungent -smell or NH, gus is Ammonium ion (NH,') mny be Conflrmutory test for Mnngnnous Ion (M n'').
heat evolved lvhich gives dcnsl' prcscnl
I. OS +dil. N11Ol-1 While ppl. is oblaincd which Mongnnou s ion (Mn'') is
wl11tc ltimcs with gloss roJ
slowly rums inlo brown Oil conlinncd
dipped in Cono. IICIsolu1ion L'Xposure 10 nir
2. Pcr11111ngnnlc ncid test
ConflrmAtory trsl for Ammonium Ion (N II ,'). Ncsslcr's rcngcnt test (I-IMnO,) :
Few urops of OS + Pinoh of A pink supernatant solulion is Mnngnno us ion (Mn " ) is
OS + Nc~~lcr 's reagent ·t NaOll Brown prccipilulc is fonncd Ammonium ion (NII.") is PbO, ·t· I mL Cone, HN01 ohluincd confim1 cd
(slight cxrcss) cunfinned boil the mixture cool, di lute
& clecnnl the solu1io~
Analysis or I group c111io11s .

OS I dil.llCI No rrcci pitart· I group c ut ions llrl' 11bse111 Anulys ls ofV gro1111 cntlons (Do '', Sr'' , Cu'')

AnRlysls or II group cu1lons OS + solid Nll,CI + excess of While prccipilntc is fonncd V group ca ti ons may be
NI l,Ol-1 solullon + (Nll,),CO, prcscnl
F.1prrlmcnt Ohscn·n1ion lnl'crcncc solution ·
Confirmatory test for Rurlum Ion (llu '').
OS ~d,I.I I C l ➔ 11,S No preci pilntc II group cm ions nre nbSL'lll
I. OS + Pot.chrnmnic (K,CrO,) A yellow precipi1111c is fonncd Barium Ion (Bo '') is con!1nncu
Anal,\·lil~ of Ill i:roup rnllOO! (Al"') sulu1ion
2. Flume lcsl : A pustc of lhc
E11wl'lmrnt Ob1crv11lon lnfrrcnrc given salt is prcpurcd wilh u
Apple srccn colour is Imparted Barium ion(Bo' 1)isco111inncd
few drops of.one. HCIund ii
Oli • o , pa1ulo ofi,oliJ Nl-1,rl , A gc la1inous wh ile prc,i piu11c lll i;roup Aluminium iun\Ar' i 1u1he !lame
is cxposcu 10 1hc c11 lo11rlcss
C\f.'l"\~ 11f Nll,O1-t ~11l11t ion. is fu m1ed mny be prc.,cn1 flnmc lhruugh Pl 111in11m
wire
.p .
I .
IIPUC II PUC
7. MODEL PROCEDURE FOR THE ANALYSIS OF SIMPLE INORGANIC SALT
Coofirm111ory test for Strontium ion (Sr'')
SIMPLE INORGANIC SALT- I
I. OS + (NHJ,SO, , beat and A white precipiwte is fom1cd Strontium ion (Sr ' ') is
scratch the sides of test tube con finned Preliminary Test: c) Solubi lity test:
a) State : Crystalline solid
with a glass rod
2. Flame Test; b) Colour : White Water dil. HCI dil. HNO,
A paste of the given salt is Crimson red colour is imparted Strontium ion (S r"') is Cold Hot Cold Hot Cold Hor
[Original solution (0.S) : Salt + Cold water] i-:....:.::.._j..._ _-1-----1---+---+-- - l
prepared with few drops of to the name continned
cone. HCI .and it is exposed II Dclcclion of onions
to the colourless name Detection of l group anion
through Pt wire
1 Experiment Obser\'alion Inference
Confirmatory test for C11lcium ion (C11' )
I. OS + Ammonium oxalate A white precipitate is fonncd Calcium ion (Ca ' ' ) is Salt +dil.HCI No brisk effervescence takes I group anion is absent
((NH,),C,O,) confinned place
2. Flame Test Detection of II gro up anions
A pasle of the given salt is Brick red colour is imparted to Calcium ion (Ca '' ) is
prepared with few drops of the name confim1ed Salt+Conc. 1-1,SO, is takenina Reddish brown vapours are II group Bromide ion (Br") may
cone. HCI and it is exposed dry test rube evolved be present
10 the colourless flame
through Pt wire Confirmatory lest for Bromide ion (Br· ). (a) AgNO, test
Analysis of VI group basic radica l l\lagncslum Ion (Mg''). Salt solution + di!. HNO, + A pale yellow precipitate is Bromide ion (Br) is con finned
,\ OS + solid Nl-1,CI + excess of White crystall ine precipitalc is Magnesium ion (Mg'') is silvcrnitratc(AgNO, )solution formed which is sparingly
NH,01-1 + Na,H PO, or fonned soluble in NH,OH.
ii (NH.),HPO, , scratch the inner
confinned .
(b) Orange globule lest (Chlo rine water lest)
walls of test tube with a glass
\ rod Salt solution + equal volume of Orange red globule is fom1ed Bromide ion (Br") is confirmed
I
I
NOTE: FLAME TEST Cl, water + CCI, shake and
allow to settle
• Metal chlorides are volarilc and impart characteristic colour 10 the name. Hence name test is always
done by using cone. HCI solurion. Ill Detection of cat ions
Detection of zero group cation Ammonium ion (NH;-)
A paste of the salt is prepared Apple Green Ba''
in cone. HCI on a watch glass. li Salt + NaOH solution, heat Gives a pungent smelling NH,_ Zero group cation NH; is
is heated on a cl.:aned pt."loop in Brick Red Ca'' gas which gives dense white present
non luminous· Bunsen name.
'I The colour give,i out by the salt
in 1he flame is observed
Crimson Red Sr'' fumes with a glass rod dipped in
cone. Hydrochloric acid
Green Cu''
Preparation of Nessler s reagent : Confirmatory test for Ammonium ion (NH,) (Nessler's reagent test)

Alka line potassium mercuric iodide solution is called Ncsslcr's reagent It is prepared from Original solution + Nessler's A brown precipitate is fonned NH; is confirmed
1-fgCI,& Kl solurion. · · reagent + excess of NaOH
_ ~hen drops ofKJ arc added to 1-lgCI,, n scarlet red ppt. is fom1ed which dissolves in excess of Kl Report:
g,vmg a _clear soluuon. To the clear solution an equal volume of NaOl-1 is added Th I·
~oluuon 1s colled Nessler 's reagent. · e resu ting Acid radical Bromide ion Br·

1-lgCl,+ 2KJ ➔ 1-lgl,·r 2KCI Hgl,+ 2KJ ➔ K,1-lgl, Basic radical Ammonium ion NH;
K, Hgl, + NaOH ➔ Nessler 's reagent. Potassium mercuric iodide Sall Ammonium Bromide NH,Br

- 19- -20-
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IIPUC
-- - - ··- -- - -- - -
SIMPLE INORGAN IC SA LT-2 Drll'ction of V ~roup basic radical
I Prcli mhuir) te~, : Solubilit y tnhk
Original ~o lution +NH,C I (solid) A while ppl. i~ obtained V Group basic radical5 Ba'',
!l) StaieAmorphous ,1,lid , Nll,011 (excess) 1 {N ll,),CO,
Wat r r dil, HCI tlil . II NO, Ca'' or sr'· may be prc'.cnl.
bl Colour-\\'lute
Cold Hot Co ld Hot Cold llot
c) Solubtlll\ Snluhk tn cold dil Hl'I
Connrmntory test for Br'' Sr'' & Co''
[ Ongmal , ol uuon (0 S) Salt , cold dtl I IC I]
II Dei-rrllon of add radicals Ori gin al ,o lu tion I K,CrO, No ye llow ppt. is obta ined Ba'' ,~ absent
~olu1 ion
E1pcri m cnt OhSl'r\ Olion Inference
Ori ginul solution f (N ll.),SO, No white ppr. i, obtained Sr' 1 i, absent
5ah -. d1I l lC: I (it\'C ~ brn k cffcn c•~ccncc IgrPup nc1 J 1adico l i, prc~cnl s<ilutil111
A colou rl c~s gn, wh1cl1 !um, May he CO, ' Origina l s11lu1ion 1 /N ll,)011 I wh ite ppt. iq obtai ned Cn '' ion ,s confi rmed
lime "liter 1nitky ammonium oxa late {N I l,J 1C,O,
Flume test: Bm:k re<l colour i~ imparted ra'' ion 1q wn rtrm ed
C'onlirmntof) ll'st for CO,' Sn ll t-wn . I ICI make pn~lc. igni te
on plat inu, n wire lo the 110 11 ·
Sult ~ "':lier. hcnt , trnngl>. r,a ~, I itn c wnlct doc, not tum, milk y l'I ), ' ion i, conlirmcd luminous llun,cn name.
the g;" th n•uµh lune \\Oler

IV l{csull :
Ill l>N t-c tlon of ll:,~k ru dk!tls
Dcl<'<'tl on of Z,no uro up IJ aslc rn di rn l (N H.") Acid ru<licul Ca rbonate ion co,'
l est for ,11. :
------------- -------~----- --------, Ba,il: rudica l Ca lci um inn Ca 1•
Sall-+ Na< )11,nlu1111n. heat No pun11en1 , 111rtling Nit , g:is /,c rn group bn,ic rad1 cul, NII ."
iun is ah~r nl Sall Cukiu m Cu rhonutc CaC'O,

Octe1:1lon ot I ~ro up b:i~le n 11llc al


Orig ,n:11 ,l1lutu ,11 • Jtl. I ICI No wh ite prcc 1p1 tntc I ( lniu p husic rud ,cul~ arc nhscnl

DelC<'llo n of II J!l'O ilJl li:i ,l c ntdk11 I


r o11g11m l , .. ~.,-;; t ; II CI ' 11,s Nu" htlc· fH CCl[ltl Hll' II <,n,up hustc , :idtCu l, 11 re I
[J~'- -- - -- - - - --- (I ~ - l
I
OcH•c lion of 11 1 i,: ro uJl hu,(c ru dirn l

-111 nrnup
I
I
Ong1nr1I ~:i1111 11,11 ➔ NIVI (•<•I~ lNo prcc1p11n~ - hu,,c 1:idi~11 I, arc
[ ~ 11 ~0 11 (cx,c,, ) _ _ _ ____ _ nb~ tt _ I
01'1 <'«:11011 of IV grou p hu,lr rndlcH I
,,,1i;,;1r1 ,Nii",c1 {~1111111 lNop,:c1p11u1c
Or1 g1nul
f , Nl l,llfl <r~"·,, ) , 11,s ,•.1~ _ ~----·-- j IV U111up huNtc 111Ji~ ~ u-,,-. - -
,1h, c11I

l l JI --
UPUC
llPUC
\ Sl l\1 PLE INORG AN IC SALT- 3
Detection of II group basic radical
I Prelimi nan · test: Solubility table:
\ a) State: Cry; talline solid Origi nal solution + dil. HCI + H,S No precipitate II group basic radicals are absent
b)Colour-Whitc I Wa ter dll.HCI dll. HNO, I
\ c) Solubiljty: Soluble m cold water I Cold I Hot Cold I Hot Cold I Hot I Detection of Ill group basic radical
11:.Origin:il solution (0. S) Salt + cold,, :iter] I + I I I I I
Ori gi nal solut ion + NH,CI (solid) white gelatinous pp! Ill group basic radical Al.. is
+ NH,OH (excess) present
Drtrction of I group acid radical

Expe riment Obsen ·ation Inference


Confirmatory lest for Al'' ion
Salt - dil. lKI No brisk ctTcrvcsccncc I group acid radical is absent
Orig in al solut io n + NaO H A white gelatinous ppt is formed. Al,_ ion is confirmed
I Dettttlo n of II group acid radical solution which is soluble in excess NaOH
Salt ~ Cone. H,SO, in a dry test No reaction takes place in cold 11 group acid radicals er or Br" Clear solution+ NH,Clis, to form clear solut ion.
arc absent heat &cool Gelatinous white ppt reappears
and no gas is e\'ol\'ed
Add Cu turn ings or paper b:ill and No reddish brown fumes No,· is absent
beat strongly e, olved. Result :
II group ac id radicals are absent
Acid radical Sulphate ion so:-
Basic radical Aluminium ion Al,.
Detection of Ill group acid radical
'. Test fo r SO.' :
Salt Aluminium Sulphate Al,(SO,),

Sall solution · BaCI, solution. add A white preci pitate is formed SO/ radical is present and
excessof diL HCI which is insoluble in excess of confirmed
dilute hydroch loric acid

1 Ill Drtectlon of Bask ra dica ls


I Detectio n of Zero gro up bllik radica l (/'li ll,')
Tcu for N H; :

Salt .,. NoOH M>lution. bent No pungent smell ing NH, gas Zero gro up basic radical, NH;
ion is ab, cnt

Detect-Jon of I gro up basic ra dical


Origi nal so luti on ➔ d1LHCI No white preci pitate I Group basic radica ls are absent
i ,◄

--- -
,, . 2).
-24-
UPUC IIPUC
[ Detection of II i:ro up basic radical

I Pn>liminal') tt'5t:
SI\IPLE l~ORG,\..~ IC SALT- 4
Solubili ty !3bk : Original solution + dil.HCI + H,S No precipitate
gas
II group basic radicals are ~ 1 I
a) St:llle_Cryst3lline solid dil.HCI dil. H:-iO_,
Wutrr
h) Co.lour. colour!~
ColdI Hot Cold I Hot Cold I Hot Detection of Ill group basic ra dica l
dSotubili t)~ Solublcmcc_,ld " -:it.er
( :. Origin:il solution (0 . S) ~t ~ cold water] I J I Original solution + NH,CI (solid) No white gelatinous white ppl. is
+ NH,OH (excess) fonncd
Ill group bas ic radicals arc
absent I
Tl Dt'trction or Acid ludkab Detection of I group add radical Detection of IV group basic radica l I

Drttttion of I group acid radical


Expe.riment Obst"rntion Inference
Original solution + NH,CI (solid) No prccipiwrc is fonn ed
+ NH,OH (excess) + H,S gas
IV group basic radical$ arc
abscnl j
I group aci d radical is absent I
53.11-di.l. HCI :--o bri sk effm ·esc-ence
Detection of V group basic radica l I
~trction of II group ac-id nadkal
S3lt - Cone. ll ,SO, m a dry test No rc:iction takes place in rold II group :Kid rJdicals Cr or Br"
Original solution + NH,CI (solid) No ppt. is obtained
+ NH,01-1 (excess) + Nl-1,),CO,
V group ba~ic rndicals are
absent j
and no gas is cvoh ed an: absent

.-\dd Cu tummgs or paper ball is No n."ddish bro\,11 fumes NO; ion is absent Detection of V I group basic radical I
I
11.dded lllld he:i.1 strongly t'.\ Oh ed.
Confirmatory test for Mg'"
I
Original solu1ion + Nl-1,C I A whi le ppt. is fonned Mg'· is confinncd
(solid) + NH,OH + Disodium
Drtttlion of UI group acid nadical
! hydrogen phospha1c (Na,HPO,)
Test for SO.' : or diammonium hydrogen
phosphate (NH,),HPO,
S3h solution -.- BJCl, solution. add A \\ hite pn:cipimte is fo m1ed Ill group SO.'° ion is prescnl and Scratch the inner sides of the
exc=ofJ il HCI which i.s insoluble in excc,s of confinncd test tube wi1h glass rod.
dilute hydrochloric acid

Res ul t:
, Ill DetN.·tion of Bil.sir radkals
DrtMtion of Zero group basic radical (1'\H,) Acid rndical Sulphalc ion so:·
Basic radirnl Magnesium ion Mg'"
S-lh - NaOH solution. ~ 1 No pungent smdling NH, g.is Z.:ro group bask radi.:al. NI1;
,on is absent Salt Magnesium Sulphate MgSO,

\
Drtection of I group basic radical
/ Origin:il sol ution~ d1I. HCI INo whi1c:- pr..-cipiuue / t Group basic r:idicn ls arc obsrn1

.25. -26-
• IIPUC 11ruc
- -- --- ---- - - - - - --- ---
SIMPL E INO RGAN IC SALT - 5 Detection of If group basic radical
Solu bi lity tnbic: II group bas ic radiC:J ls are absent
I Prelim inary test:n) Stote: Crystall ine solid Original solution + dil.HCI + H1S No precipi tate
gas
b) Colour. White
I Wn ter dil. II CI I dil. II NO, I I
•I c) Solubiliry: Soluble in cold wa ter
r Cold I lfot Cold I Hot I Cold I 1101 I
I:. Origi nah olution(O. S) ~Salt +cold water] Detection or Ill group basic radical I
I + I I I I I
IU group basic radicals an:
Original solut ion + NH,CI (solid ) No precipita te
Detection of I group acid radical absent
+ NH,OH (excess)
Inference
Experi ment Obsen •ation
II
Salt +dil.HCI No brisk cffcrvcsccncc I group acid radica l is absent De tection of IV group basic radical I

TV gro up basic radicals are


Detection or II group acid radical Origi nal solut ion + NH,Cl (solid) No precipi ta te
absent
+ NH,Ol-1 (excess)+ H,S gas
Salt + Cone. H,SO, in a dry test Reaction takes place in cold II group acid radical is present
rube giving a colourless fuming gas er or Br·may be present
which gives dense white fumes De tec tion of V group basic radical .
wi th a glass rod dipped in V group basic radicals are
ammonium hydroxide_ e r ion may be present Original solution + NH,Cf (solid) A white pp!. is obtained
+ Nf-f,01-1 (excess) + NH,),CO, present
solution Ba'', ea•· or Sr'- may be present
Con0rmatory test for chloride
1
a) Cbromyl chloride tes t :
1 1
Confirmato ry test for Ba ·, C a • or Sr'~ .
Sa lt + Potass ium dichromate Reddish brown vapours of Cr ion is confinm:d
cryst.ils (K,Cr,O, ) + conc.1-1,SO, chromyl chloride ore evolved Original solution + K,CrO, Yellowppt. is obtai ned Ba1• ion is confirmed
heat Pass the vapour into the Yellow solution is obtained solution
NaOH solution
Yellow precipitate is obtai ned
Yellow solution + di lute acetic
acid + lead aceta te solurion Flame test : Apple green colour is impaned Ba'· ion is confirmed
Salt + cone. 1-fCI make paste,

S,h ~ ,"';•~ • ilil.HNO, • , iim


mtrn tc soluuon
I
b) S liver ni trate tes t for Br radical

A ' "''' wh;,e p« , ;p;w,e ;,


fo rmed which is soluble in
excess NH,01-1
I '°" ;,
er ,.,n~,,
ignite on a platinum wire to the
non-luminous bun.sen fl ame.

Res ult:
111 Detection of 81ul.c radicals
Detection of Zero group basic r11dlc11I (N H,) Acid radical Chloride ion er
Teu for NII." : Basic radical Borium ion Ba'·

Sult + NuOl-1 solution, heat I No pungent smelling NI-I, gas I Zero gro up bas ic radica l NI-I; is
absent
Snit Dnrium Chloride BnC L.

Detection of I group basic radical


Original so l uti o n ➔- d1l. llCI / No white precipitate / ' Group basic radicals an: absent
:
I
...... - l
.z7.
IIPUC
- - - - - 111•uc
- - -- -- - --------- --- -- ---- - -
r .- - - - SI M;L[ ll"iOHGAN IC SALT· 6
1 Soluh1hty mbk . Detection o f 111 ~ro up tunic radical
I Prclimlna~ 1r,1 :a) Stale . ( ry,talhnc ~C'hJ
\ b)Culour. Palepmk
I Walrr dll. II CI I dll. II NO, I Origi nal so lut ion ~ NI l,C I (solid) No prcc1 pitn1e Ill group 1n.~,c radi ca ls a rc
c) Solutnhf) . Soluhk m rold " arcr
I Cold I Hol Cold I ll ol I Cold I ll ol I ➔ NII 0 11 (excess) ab<ienl
1·. 0ng muh o lut1on (O S) c $.a h t c0 ld\\ Ulcr]
I

I + I I I I I
II Dr tl"C'tio n or Acid Radicals
Dclccflo n or IV g roup bas ic radical
Dr ll"C'tlon of I group aci d radlc:a l
Ei-prrimrnt Obsrn·ation Inference Origi nal so luti on -~ NI 1,C I (so lid ) Preci pitate is fo rmed IV group bas ic rad icals are
+ Nll,O H (cx ce~s) ➔ 11,S gaq prese nt
Snh + J1 l l-1Cl No bri\k cffen·cscencc I group acid radic al is abse nt
A buff colo ured precipitate is Mn'' ,on may be present
DrlttJion o f 11 g roup ar id ra dica l obtai ned
Salt + Cone. H,SO, m a dr)· tcsl No Rcacuun takes place in co ld II group aci d radical s li ke er &
rube and no gas is evolved Br·1m: absenl
Confirmato ry tesl for Mn' ' Ion
Add Cu tum mgs or paper ball and No reddi sh brown fum es No,· ion is absent
he:it strongly e, olvcd. Origi nal solut ion + NaOl-1 A white prec ipita te is fo rmed Mn'' ion is con fi rmed
so lution which turns brown on exposure to
II gro up acid radica ls are absent ai r

Permanganlc acid test


I Drtttt.io n o f Ill g roup acid radical Salt+ PbO, Powder + co ne. Pink coloured supernatant liq uid Mn' ' ion is co nfirmed
I Tesl for SO.' r:idica l HNO, + waler. heat and cool is formed

Sall solulion + BaCI, solution. add A white precipirntc is formed so:· ion is present and
excess of dil. HCI which is insoluble in excess of confi rm ed
dil ute hydroch loric acid Result:

I Ill Deltction of Bas ic radicals Acid rad ical Sulphate ion SO/
Dc-lection of Zero group bask radical (NH ,') Mn' '
Basic radical Manganese ion
Test for NH; :
Sall + NaOH solut ion, heat I No pungent smell ing gas Zero group basic radical, NH; is
absent
Salt Manganous Sulphate MnSO,

I
Detection of I group basic radical
Original solution+ dil.HC I INo whi te precipi tate 11Group basic rad icals are absenl

1
Drteclfo n of Sl'cond group basic radical

gas
I
Original so lu1 ion + dil.HC I + H,S No preci pitate 111 group basic radica ls arc absent

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UNCTIONAL GROUPS IN oRGANicCOMP OUNDS. c) Benedict's/ Fchllng's reagent lest.
. TEST FOR F .
compounds. t • organic Organic compound+ Benedict's A brick red precipitate is Aldehyde group is present
Aim: To identify the functional groups prcscn m
l I. TEST FOR UNSATU RATION. a)DrommcwalerlcSt
Inference
rcagcnl / Fchling's solution & obtained
heated
Tcsr Obscn·alion
d) Schiff's reagent test.
bromine is lndica re s the pre se nce of
Organic compound is dissolved Orang•' colourof1he
~ d ompound Organic compound + Schitf's A pink colour isobiaincd Aldehyde group is present
in CCI, ~ few drops of bromine Jisch:irgcd. unsaturate c · reagent
water with continuolb ~haking. Test for Ketones (-CO-) a) m-dlnltro benzene test
b) Baeycr's test. Test Observation lnfrrence
Organic compound dissolvcd in Pink colour of 1J1e KMnO, is Indicate s th e presence Organic compound + a small A violet colour is obtained. Ketonic group is present.
nd5 ·
acetone + few drops of alkaline discharged. unsaturated compou amount of powdered m-
KMnO, solution. dinitrobenzene + NaOH
solution, shaken well
II. TEST FOR ALCOHOLIC GROUP (R-OH). a) Ceric ammonium nitrate ICSI.
(b) Sodium nitroprusside test:
Tttt Obsen·ation Inference
Organic compound + Sodium A red colour is obtained. Ketonic group is present
Organic compound + few drops Red colour appears Indicate s the presence of
nitroprusside + NaOH solution
of Ceric ammonium nitrate alcoholic group
solution shaken well Test for carboxyl group (-COOH) a) Litmus paper test
Test Observation Inference
(b) Lucas rngcnr test:
Organic compound+ blue litmus paper Blue litmus paper turns red The carboxylic group is present .
Organic compound T Lucas Layers separate immediately 3° alcohol
reagent (mixture of anhydrous Layers separate within 2° alcohol (b) Sodium bicarbonate test:
ZnCI, & Cone. HCI ) shaken minutes
I O alcohol Organic compound+ NaHCO, solution Brisk effervescence is obtained. The carboxylic group is present
well. Layers do not separate
Ill. TEST FOR PHEl'iOLIC GROUP(AR-OH). a) Neutral Ferric chloride test. c) Esterification test
Test Obscn·ation Inference Organic compound + few drops A fruity smell is obtained The carboxylic group is present
A violet colour is obtained. Indicates the presen ce of of alcohol + 2-3 drops of cone.
Organic compound + few drops
ofneutral FeCI, solution phenolic group. H,so• ., heat, cool & pour the
mixture into Na,CO, solution
(b) Phthalein d~•e test or Phthalein fusion test (It is used to detect Phenol)
Organic compound + a pinch of A pink colour is obtained. The Indicates the presence of VI. TEST FOR PRIMARY AMINES (NHJ. a) Litmus paper test.
phthalic anhydride + Cone. colour di sappears on addition phenolic group. (Ar-OH)
H,SO, . heat the mixture. cool & of excess ofNaOH solution Test Observation Inference
pour into dilute NaOH solution Organic compound+ red litmus Redlitmuspapertumsblue Primary amine is present
paper
IV. TEST FOR ALDEHYDES AND KETONES GROUP
a) 2,4-DNP test.(lt is a general rest for aldehydes & ketones) b) Carbylamine test:
Test Observation Inference Organic compound + CHCI, + Offensive I bad smell is Primary amine is present
alcoholic KOH, heat obtained (aliphatic/aromatic).
O~ic compound + 2,4-DNP Crystallineorangeprecipit ateis Confirms the presence of
(din1trophenyl hydrazine obtained. carbonyl group. (aldehyde or
ketone) c) Diazotisation or Azo dye test (Test for aromatic primary amine)
solution)
Test for aldehldes (-CHO) (b) ToUen 's reagent test or Silver mirror test: rganic compound dissolved in A red or orange dye is obtained Primary aromatic amine is
il.HCI and cooled in ice + ice present
Organic compound + Tollen's Silver mirror or black Aldehydegroupis present ooled NaNO, solution + ice
::r:::;•c:e:t~:1.00 a water bath, precipitate is obtained ooled solution of P-naphthol in
aOH
-3 1- -32-
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TEST FOR FUNCTIONAL GROUPS IN ORGANIC COMPOUNDS. 9. PREPARATION OF INORGANIC COMPOUNDS


Observation Experiment No. 10.1
Organic compound Name of the test
Aim: Preparation of ferrous ammonium s~lphate (FAS or Mohr's Salt)
I. Ccric ammonium nitrate test Red colour
Alcohol Apparatus & Chemicals Required: Two 25 mL beakers, a glass rod, china dish, funnel, stand, wire
(-OH) gauze, tripod stand & filter paper
2. Lucas reagent test ( I' ) N O Layers are fanned
(2°) Layers separate within 14gofFeSO,,6.5gof {NH,),SO, & 2mldil.H,SO,
few minutes An equimolar FeSO, & {NH,),SO, solution upon concentration & cooling gives pale green crystals of
(3') Layers separate FAS (Mohr's salt) are formed.
immediately heat
FeSO,+ {NH,),SO, + 6H,O ➔ FeSO,(NH,),SO, .6H,O
Reaction:
Ferrous Ammonium FAS
sulphate sulphate
Procedure:
I. Violet colour

OOH
Phenol I. Neutral FeCl1 test
I. 14gof FeSO, are treated with 2ml ofdil. H,SO, in a 100 ml beaker.About6.5 g (NH,)1SO, crystals
2. Phthalein dye test 2. Pink solution
are added into it.
2. Dissolve the contents of beaker in 50 ml of distilled water. The solution is then boiled & cooled to get
thecrystals of FAS.
3. The crystals are separated by filtration & purified by recrystallisation from hof water.
Aldebydes I. 2,4 DNP I. Orange yellow ppt. Result: The yield of FAS = ..................g
(-CHO) 2. Toll en's reagent test 2. Silver mirror
Fehling's reagenttest 3. Brickredppt. 10.2 Preparation of potash alum (K2s0. A1 2 (S0 4 )3 24H2 0).
3.
4. Benedict's / Schiff's reagent 4. Pink colour Chemicals required: 6.6gAJ,(SO, )1 ,2.4gK,SO, and dil.H,SO,
test Procedure:
I. 6.6 g Al,(SO, )1 and 0.5 mL dil.R,SO, are dissolved in IO rnL of hot water & about 2.4 g of K,SO,
crystals are added into it. ,,
Ketones I. m-dinitro benzene I. Violet colour
(-CO-) 2. The mixture is heated with constant stirring until K,SO, dissolves completely.
2. Sodium nitro prusside test 2. Red colour
3. The solution is cooled to get white crystals of potash alum. The crystals are finally separated by
filtration.and dried between folds of filter paper.
K,SO, + Ali(SO,) 3 + 24H,O ➔ K,SO, . Al,(SO,)1 . 24HP
Carboxvl.ic arid I. Sodium bicarbonate test I. Effervescence
(-COOH) Result: Yield of potash alum = ................. g.
2. Esterification test 2. Fruity smell
10.3 Preparation of potassium trioxalatoferrate (lln
Chemicals required : 3g of oxalic acid, 3 .8 g ofKOH, 2.5 g of FeCI,
Amines I. Carby I amine test I. Foul smell Procedure:
(-NHJ 2. Diazotisation test 2. Yellowppt. ,I. 3g oxalic acid is dissolved in 15 rnL of hot distilled water and 3.8 g KOH are dissolved in a beaker
with constant stirring.
2. 2.5 g FeCl 3 are ·a dded into the above solution with constant stirring. The solution is then boiled &
cooled to get white crystals of potassium trioxalatoferrate (Ill). The crystals are separated by
filtration and dried between the folds offilter paper.
heat
FeCI, + 6KOH + 3 H,C, O, ➔ K,[Fe(C,O, ),] + 3KCI + 6H,O

Result : Yield of potassium trioxalatoferrate (Ill) = ..................g .


. 33.
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. , ., '.
UPUC IIPUC

10. PREPARATION OF ORGANIC COMPOUNDS Experiment No. 10.3

Experiment No. IO.I Aim : Preparatfon of p-nitro acetanilide from acetanilide


Apparatus and Chemicals Required:
Aim: To prepare acetanilide from aniline. . . .
.. • h d ·d, (5 ml) Glacial acetic acid /\cctanilidc (2g), Glacial acetic acid (2 mL), Cone. HNOi( lml) &Conc.H,SO,(5 mL), beaker
Apparatus and Chemicals Required: Amhne (S ml), Acetic an Y n t: •
{S mL), Ethanol, funnel, RB flask ( I00mL), beaker(250mL). ( I 00 mL), funnel, glass rod, ice bath .
It c.m be prepared by heating aniline with acetic anhydride. Preparation :It can be prepared by the nitration ofacctanilide.

0~
• 5 mLofaniline is dissolved in 5 mLacetic anhydride and 5 mL glacial acetic acid and wi th conS tant
NHCOCH,


shaking in a round bottomed flask.
The mixture is refluxed on a sand bath for about 15 minutes. Aniline reacts with acetic anhydride
Cone. H,SO, ()°OCH,+ H,O
giving acetanilide.
✓,;:; + Conc.HNO, - - -c-a- -
11 1

• The reaction mixture is poured into a beaker containing l00 ml of i~e water.Ac~tanilide NO,
precipitates from the solution as white solid. It is separated by filtrat10n and punfied by
Acctanilidc p - Nitroac~tanilide

'
recrystallization from hot water containing little alcohol.
NH Glacial acetic acid ONH-CO-CH,
~

0
Procedure:
+ (CH,CO),O -----➔ + CH,COOH
# # • 2g acetanilide is dissolved in 2 mL glacial acetic acid taken in a beaker. 4mL of cone. H,so. arc
Acctanilidc Acetic acid added slowly with constant shaking until a clear solution is obtained, The mixture is cooled in ice
Aniline Acetic anhydride
cold water bath for some time.

• I ml cone. HNO, and 1ml cone. H,SO. (Nitrating mixturc)is carefully added in to the above
Experiment No. 10.2 solution with constant shaking and allowed for 30 minutes to complete the reaction. Acetanilidc
Aim : To prepare dibenzal acetone (Dibenzylidine acetone). reacts with nitrating mixture forming p-nitroace~ilide.
Apparatus and Chemicals Required: Benzaldehyde (3.2 mL), Ethanol (25 mL), Acetone (2.3 ml), • The reaction mixture poured into I 0OmL ice water taken in a beaker. A yellow solid of p-nitro
NaOH solution, Conical flask(250 mL), beakcr(250 ml), funnel. acetanilide is obtained . It is separated by filtration and purified by recrystallisation from- ethyl
Preparation :It can be prepar~ by the treatment ofbenzaldehyde with acetone in the presence of dil. alcohol. White solid is obtained.
NaOH / di!. KOH solution. The reaction is called Claisen - Schmidt reaction.

2
O
,
CHO
+' CH,COCH,
dil. NaOH

0
CHaCH-CO.CH• CH O + ,H,O
ExperimentNo.10.4
Aim: To prepare phenyl- azo,- P- naphthol (azo dye)
Chemicals Required : Aniline (2 mL), concentrated HCI (6.5 mL), Glacial acetic acid ( 12 mL),
Benzaldchyde Acetone Dibcnzal acetone Sodium hydroxide (2g), Sodium nitrite ( 1.6g) and P-naphthol (3 .2g)
Preparation :When aniline is treated with ice cold sodium nitrite ( NaNO,) solution and cone.
Procedure: Hydrochloric acid solution benzene diazonium chloride is formed (Diazotization reaction), which on
• 3.15 g ofNaOH is dissolved in a mixture of25 mL ethanol and 30 mL distilled water taken in a 250 treatment with alkaline P-naphthol solution gives an orange red dye [phcnyl-azo-P-naphthol]

o--:: N
=NB'
ml conical flask. Cool the mixture in an ice bath. OH

• Benzaldehyde is mixed with acetone in a beaker. The mixture is then added into a conical flask NH, NaNO,+Conc. HCI oN=N-CI P-naphthol + Dil. NaOH
containing above NaOH solution with constant shaking for about 30 minutes. (0-5°C) /4' .,,.;r
O
• Benzaldehyde and acetone react giving a yellow solid of dibenzal acetone which is separated by
filtration and purified by recrystallisation from Ethyl alcohol. \ #
Aniline Benzene diazonium chloride phenyl-azo-P-naphthol
(orange red dye)
.35. -36-
llPUC
nruc

Procedure : o
11. TESTS FOR CARBOHYDRATES, FATS AND PROTEINS

. . • • k
Cone. HCI and NaN0, arc dissolwd m water m separatv bc;;.a ers a
nd the so lution is cooled to 0 C I Experiment I Observation I Inference I
I) Molisch test ( General test for Carbohydrates)
in ice, Similarly P-Naphthol is dissolved in I 0% di!. Na0H in a beaker.
• • • dd . d to it w ith constant stirring . Aqueous solution of the compound + A deep violet ring is formed Carbohydrate is present
• Toe HCI and NaN0, solution are mixed together and an11me 1s 3 c . . a lcoholic solution of a-naphthol + at the junction of the two
nd
Aniline makes diazotization reaction giving yellow solution of benzene diazomum chlo e . Cone. H,S0, is added carefully along layers
• The solution of all..11line P-naphthol is added into the above solution with conSlant shaki~g. An the sides of the test tube
. b • d ·- eparat ·d from the so lution by General test for reducing sugars :
orange red precipitate ofphenyl-azo-P-naphthol 1s o tame . 1t 1~ s 1:

fi.ltrntion and purified by recrystall isation from glacial acetic acid. 2) Benedict's reagent test : Solution A red precipitate is form ed Carbohydrate is reduci ng
of the compound + Benedi ct's reagent. sugar
Experiment No. 10.5 The test tube is heated on a water bath.

Aim: To prepare aniline ~·ellow ( p-amino-azo-benzene). 3) Fehling's solution test : Solution A red precipitate is formed Carbohydrate · is reducing
of the compound + Fehling's solution. sugar \
Apparatus and Cbemitals Required : Aniline (7 ml). Aniline hydrochloride ( 1.5 g). G lacia l acetic The test tube is heated on a water bath.
acid (7 mL). Carbontetrachloride (9 mL ). Diazo aminobenzene (3 g). conical fl ask ( 100 m L).
4) Tollen 's reagent test : Solution of A black precipitate of si lver Carbohydrate is reducing
thermometer. funnel. water bath. the compound + To lien's reagent. The or a shining silver mirror is sugar
test tube is heated on a water bath. obtained
Preparation :It can be prepared by the reaction of diazo aminobenzene with ani line hydrochloride in
presence of aniline solvent. Distinguish test between monosaccharide and dlsaccharide

o N =N J D ~ o N=N-Cl + H,N - 0

Benzene diazonium
5) Barfoed's test : Solution of the Orange red precipitate
compound + Barfoed 's reagent. The
test tube is heated on a water bath. ~!l Orange red precipitate
Distinguish test between Ketose and Aldose
Carbohydrate is a monosaccharide
Carbohydrate is a disaccharide

Diazo :uninobenzene Carbohydrate is ketohexoses

o
chloride. Aniline 6) Seliwanoff's test: Solution of the Red colour or precipitate
compound + Seliwanoff's reagent. Blue green colour Carbohydrate is ketopeatose

0 N=N-C l + O NH, N=N O NH, + HC I


The test tube is heated on a water bath. _No colour or precipitate
Test for polysaccharides (starch)
7) Iodine test : Starch solution + few A blue colour is obtained
Carbohydrate is aldose

Starch is confirmed
Benzene diazonium Aniline yellow drops ofiodine solution
Ani line
chloride.
(P-amino-az~-benzenc) B. Test for oils and fats
8) Acrolein test: 3 drops of the oil or A pungent smell is obtained oil or fa t is present
Prottdu~ : melted fat + few crystals of potassium due to the form ation of
hydrogen sulphate. The m ixture is acrolein.
• 3g of diazo aminobenzene is dissolved in 7 mL of aniline in a conical fl ask. Add 1.5 g powdered heated gently
anili ne hydrochloride into it C. Test for Proteins
• The reaction mixture is wa nned o n a hot water bath fo r about 1 hour. 9) Biuret test (For peptide bonds): A violet colour is obtained Protei n is present
Protein solution (egg albumin)+ 2mL
• Remove the fl ask from hot water bath & allow to stand at room temperature fo r 30 minutes. of 10% NaOH + few drops of CuS0,
solution, warm the mixture.
• Add 9 m l of I : I aqueous acetic acid 10 the above mixture & shake thoroughly 10 remove excess of
aniline. 10) Ninbydrin test : Protein solution A blue colour is obtained Protein is present
+ Ninhydrin solution, heated & cooled
• Anil.ine yellow precipitate is fom1ed which is separated by fil tration and puri fi ed by II) Xanthoproteic test : Protein Yellow colour is obtained Protein is present (Test for
rec.rystallisation from CCI,. It is fin all y dried between the fo lds of fi ller paper. solution + few drops of cone. HN0~ which.turns to orange red on proteins containing benzene
wanned the mixture adding Na OH solution ring)
-37-
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IJPUC UPUC
.--------------=---:-:--:::::--::-.;~ ~T~IOrliN~VIVA QUESTIONS 7. Name the organic compound formed in phthalein dye test for phenol.
12. U YEAR PUC PRACTICAL EXAMINORGA ANIC COMPOUNDS Ans. phenolphthalein. •
FOR FUNCTIONAL GROUPS IN
8. What is neutral ferric chloride solution?
ALCOHOLS Ans. Aqueous solution of Neutral ferric chloride is acidic due to hydrolys is. It is made neutral by
I. Which is the functional group of alcohol ? adding NH,OH
Ans. -OH (Alcoholic group)
9. Write the formula of phenol.
2. Name a test for alcohols Ans. C,H,OH
Ans . Ceric ammonium nitrate test.
10. Why phenol should not touch with bear hands ?
3. Explain Ceric ammonium nitrate test. . . •nk d colour appears. Ans.
\Vhen an alcohol is shaken with Ceric ammonium nitrate solullon, P1 or re It is highly corrosive.
Ans .
4. Which type of alcohol reacts slowly with Lucas reagent? ALDEHYDES AND KETONES
Ans. Primary alcohols.
I. What is the common functional group found in aldehydes and ketones?
5. Which type of alcohol reacts instantaneously with Lucas reagent? Ans. Carbonyl group (>C=O)
Ans. Tertiary alcohols. 2. What is the functional group of aldehydes?
6. Name the chemical reagent used to distinguish primary alcohol. secondary a lcohol a nd tertiary Ans. -CHO (aldehydic group)
alcohol ? 3. What is the functional group ofketones?
Ans. Lucas reagent. Ans. >CO (ketonic group)
7. Whal is Lucas reagent? 4. Name the common test for aldehydes and ketones
Ans. A mixture ofanhydrous Zn Cl, and Cone. HCI is called Lucas reagent. Ans. 2, 4 - DNP hydrazine test
8. What is the meaning of2' alcohol? 5. Expand 2,4 - DNP hydrazine
Ans. The alcohol in which-OH group is attached to secondary carbon atom. Ans. 2,4- Dinitro phenyl hydrazine

9. What is the general formula of primary alcohol? 6. Which coloured precipitate. is obtained when an aldehyde or ketone is treated with 2,4 - DNP
Ans. R-CH,-OH hydrazine ?
Ans. Orange coloured precipitate.
10. What is the general formula of secondary alcohol? 7. Name the orange coloured product formed when benzaldehyde is treated with 2,4-DNP
Ans. R-CH-R' hydrazine.
I
OH Ans. Benzaldehyde 2,4 - DNP hydrazone.
PHENOLS 8. What is To lien's reagent?
I. What is phenolic - OH group? Ans. Ammonical silver nitrate solution is called To lien 's reagent.
Ans. -OH group which is directl y bonded to Benzene ring.
9. Explain Toll en's reagent test.
2. Phenol does not displace CO, from NaHCO, solution (Sodium hydrogen carbonate) Why? Ans. When an aldehyde is heated with Toll en's reagent, a black ppt. (silver) is formed.
Ans. Since phenol is less acidic than carbonic acid . 10. N ame a test forketones.
3. Write any two tests for phenols. Ans. m-dinitrobenzene test or Sodium nitroprusside test.
Ans. i) Neutral Ferric Chloride test
ii ) Phthalein dye test CARBOXYLIC ACIDS
I. What is the functional group ofCaboxylic acids?
4. Ex pl ain Neutra l ferric chloride tes t for phenol. Ans. -COOH (Carboxyl group)
Ans. When phenol is treated with Neutral ferric chloride, a violet colour is obtained.
2. Explain litmus test forcarboxylic acids.
5. Explain phthalein dye test for phenol. Ans. When a blue litmus paper or blue litmus solution is treated with a carboxylic acid, it tums to red.
Ans. Pheno l is mixed with phthalic anhydride and Cone. H,SO, . The mixture is heated, cooled and
3. Explain Sodium bicarbonate test forcaboxylic acids.
poured into a dilute sodium hydroxid e. A pink coloured solution is formed. Ans. When a carboxylic acid is treated with sodium bicarbonate solution, effervescence occurs due
f 6. Why pink colo ur is formed in phthalcin dye test ? to the liberation of CO, gas.
Ans. II is du e to fo rm ation of phenolphthalein.

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II PUC
JIPUC
. -· bicarbonate test for carboxylic 13. Government of Karnataka
4. How can you confirm the liberation of CO~ gas dunng sodium
Pre-University Education
acids?
Ans. By p:issing CO, gas into lime water which tums milk-y. II PUC EXPERIMENTS FOR CHEMISTRY PRACTICAL EXAMINATION
5. Whal is lime water?
Ans. A solution of calcium hydroxide. Time: 2 Hrs. Total Marks: 30
6. ExplainEst~rifi~at!ont~stf or~arboxylicacids. c H, SO, . The mixture is
A carboxyhc acid 1s mixed with an alcohol and a few drops of Co~ · · Salt analysis
Ans.
healed and pour inlo sodium carbonate solution, fruity odour is obtained. Q-1 Analyse the given simple inorganic salt systematically and report one acid I0Mark.s
7. Name the ester formed when acetic acid is heated with ethyl alcohol in presence of Cone. radical and one basic radical.
H,SO, .
Ans. Ethyl acetate. Titration (Volumetric Analysis)
Q-II Estimate the Molarity of KMnO, solution using given standard (0. 1 M) FAS I0Mark.s
8. Other I.ban carboxylic acid which acid is used in esterification test?
Ans. Conc. H,SO, . solution. (procedure of the titration should be given).
..
9. What is the role of Cone. H,SO, in esterification? Q-111 Viva on tests for functional groups in organic compounds. 4Mark.s
Ans. Dehydrating agent.
Q-rv Submission of the duly completed and certified record 6Mark.s
I 0. Name the 1ests for carboxylic acids.
Ans. I. Li onus paper 1es1 3. Esterification test 30 Marks
2. Sodium bicarbonate test TOTAL

AMINES
I. What is the general formula of I', 2' and 3' amines? Time: 2 Hrs.
SCHEME OF VALUATION Total Marks: 30
Ans. )'amines : R-NH, 2'anunes: R-NH-R' 3'amines : R-N-R'

2. Nan1e the confirmatory test for primary amines. k"


. Q-1 Salt analysis (IO Marks)
Ans. Carbylamine test which is answered by both aliphatic and aromatic primary amines. I) Preliminary tests (any two correct) I mark
ii) Detection ofAcid radical (4 Marks)
3. How do you distinguish between aliphatic and aromatic primary amines?
Group detection
Ans. By azo-dye test which is answered only by aromatic primary amines.
(Correct group identification - I mark
4. Which is the functional group of primary amines? Correct radical identification - I Mark) 2marks
Ans. -NH,(aminogroup) Confirmatory test 2marks
iii) Detection ofBasic radical (4..Marks) 10 Marks
5. Which type of an1ines answers carbylamine test?
Group detection ·
Ans. All primary amines.
(Correct group identification - I mark
6. What type of odour is observed in carbylamine test? Correct radical ide(!lification - I Mark) 2marks
Ans. Offensive or bad odour is observed. Confirmatory test 2 marks
I. 7. Explain azodye test for primary amine. For writing systematic procedure with absence of previous groups I mark
Ans. An aromatic primary amine is dissolved in dil.HCI and mixed with ice cold sodium nitrite
solution, to this P-naphtbol solution in NaOH is added, a red dye is formed . Q-II Titration ( 10-Marks)
I) For performing the experiment 3 marks
8. Explai n carbylami ne test for primary amines.
For recording the readings in the tabular column I mark
Ans. When a primary amine is hea ted with chloroform and alcoholic potash (KOH), a bad smell of
ii)_For accuracy of the Titre value 3marks
carbylamine is obtained.
Upto K 0.3 mL error 3marks
9. Why bad smell is obtained in carbylami ne test? K0.4mLerror 2marks
Ans. Due to liberati on of carbylamine. K 0.5 mL error I mark
I 0. Whal is alcoho lic potash'? K 0.6 mL& above Omark IO Marks
Ans. A solu1ion of KOH dissolved in alcohol. iii) Calculations of Molarity (2 Marks)
a. Formula I mark
b. Substitution and answer ( I + I) 2marks

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II PUC
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4 p repuatlon of Sorne C - - - - - - - - - - - - - - -- -
-
I\
1 L------ -....:..:.~ ~
O
• rn mon Desk Reagenu
Q-1 11 , ,a on fo nr-rton sl group in organic rompou nd (2 marks) 4 MJrks J. Hydrochloric acid (2 N) :
four ;iue,11..»1'. 1" ,, each on an, i"I' v fun rt1011JI gNup, ( I ' 4 l
Add 170 mL ofconc. HCl to 800mLofw , _ .
. Nitric acid (2N): atc r w,th st 'mng and make up to I I,tre.
R('('Ord : Suhm1,,ion of the Jul) ,-omplctcd and certi ti~d n:corJ 6 Marks 2
Q-1\
Add 128 mLofconc. l-fNO t
• • '
0 5
oo ml of water with dilu1 e to I litre
TOTAL .10 Marks 3. Sulphunc acid (2 N) : ·
Add IOO mLofconc. H SO 1
I •• of e,pmmen1> pcrfonned and Maximum marks to be . . ' • 0 800 ml of water carefullyand dilute to I litre.
I SI. ;-;o Acehc acid (2N):
recorded awarded 4.
>90°0 6 Di lute I 14mL ofG lacial acetic acidto I litre ofwater
I :'
I

bl•, to 90 °, 5
5.
6.
Sodium ~ydroxide (iN) : 80 g ofNaOH is dissolve~ in I litre of water.
Ammon'.um Hydroxide(iN): Dilute 133 mL ofN H, to I litreofwat er.
71 ' , ro80 'o 4 7. Ammonmm carbonate(2N)
96 g of Ammonium carbonate is dissolved in liquor ammonia
j
41 • • to 70 °, 3 and di luted to I litre with water.
8. Barium Chloride (0. 5 N) : Di ssolve 30.5g in 500 mLofdi stilled water.
5 40 °, 0
9. L~ad ~cetate (Od.5N) : Dissolve 47.5g of the solid in a mixture of 250 ml water and IO ml of
g ac,a acetic ac, and di lute to 500mL with water.

~ore: I ):'\o nttd ro enter scheme of valuation and vin Questions gh•en in the Laboratory 10. Potassium chromate (0.2N): Di ssolve 9.7 g in 500 mL of disti lled water.
:\fo uua.l in the Practical Record.
[!reparation of Some Special Reagents \
2) Vin questions are to be asked from the laboratory manual only.
a) The follO\•~ng saii,- are suggested to be given fo r analvsis for practical examina1ion : NH,Br,,.
J. Ammonium acetate (2M): Dissolve 154g of the salt in distilled water and dilute to I litre.
1'"H,Cl.' (Al,(SO, ), . :\1n SO., ZnSO, I ZoCO, . 'C~CO, , BaCI, / Ba(NO,), , Sr(NO,), ,
/ MgSO, / MgCO .. 2. Ammonium chloride(SM): Dissolves 267.5gofthe sal t in dist illed water and dilute to I litre.
bJ Fon iva: 3. Ammonium molybdate:
Dissolve I00 _g of the sa_lt in a mixture of I00 mL of liquor ammonia so lution and add 250 g of
Functional grou p Tests ammomum nitrate and dilute it to I litre with distilled water.
Alcohol Ceric ammonium nitrate test and Lucas tes1 4. Ammonium oxalate (0.5 M): Dissolve 71 g of the salt in distilled water and dilute to I litre.
5. Ammonium Sulphate (IM) : Dissolve 132 gofthe salt in di stilled water and dilute to I litre.
Phenol Neutral ferri c chl oride. Phthalein dye lest
6. Bromine Water (approx.saturated) :
Aldehydcs and Ke1ooes 2.4 - DNP and Tollen·s reagent test. Fehling's reagent test Add 2 ml of bromine in 100 mL of di stilled water shake the mixture well. Keep it in a dark bottle.
7. Chlorine water: Prepare chlorine gas by treating solid KMnO, wi th cone. HCI. Saturate one
Carboxylic acid Litmus test, sodium bicarbonate test and esterification test litre of distilled water with chlorine gas and keep solution in a dark co loured bonle.
Primary amine Carbylamine tes1, azo dye test (coupling reaction) 8. Dimethylglyoxime (I) : Dissolve 1.0 go fthe solid in I00 ml of ethyl alcohol.
9. Dipbenylamine (0.5%) :
c) Inorganic sails and test for organic compounds other than the mentioned above but given in Dissolve 0.5g of the solid in 85 ml of cone. sulphuric ac id and dilute it with care with di still ed
the prescnbed manua l can be given to students in regu lar practical class for practice. waterto 100 ml
d) AII experiments as men tioned io the II PUC practical manual are to be conducted and recorded. I 0. Disodium hydrogen phosphate Na,HPO, I 2H,O (0.3 M) :
Dissolve 120 g of the sa lt in distilled water and make up the volume to 1 litre.
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-44-
lll'U'--

! 11. Fl'rrk rhlorldl' (FeCl,.6H,O) (0.3 M):


. . . . .
k
L f nc . MCI and ma e up
the vol um
e
6. Ceric ammonium nitrate solution :
Dissolve 40 g ofreagcnt in I00 mLof 2N nitric acid.
Dissolve 90 g of the salt 111 d1s11lled water contammg IO m O co
to I litre. 7. 2,4-dlnitrophenylhydrazlne reagent:
i. For water soluble compounds
12. Iodine solution: . . . . in minimum amount of water
Dissolve I g of iodine crystals in a solution of2g potassium iodide Add 0.5 g of solid in a mixture of 42 mL cone. HCI and 54 ml water and dissolve by boiling on
and dilute the solution to I00 mL. water bath. Add water to make up the volume to 250 ml.
13. Lime water (Ca(OH),) (0.021\1): . ii. For compounds not soluble in ~ater
. lilt the solution afler sometime
Shake 2-3 g of Calcium Hydroxide with I litre distilled water, I e_r d . to rotect the reagent Di~s_olve lg of reagent in 7.5 ml cone. H1SO, . Add this solution gradually to 7.5 mL rectified
and keep it in a reagent bottle. Bottle should be securely stoppered Ill or er P spmt. Make up the volume to 250 ml by adding water.
from CO, of atmosphere. 8. Fehling'ssolutlonA: Dissolve69.28gofCuSO, crystals in I litreofwatcr.
14. Ncssler's l'l'&gents:
9. Fehling's solution B:
Dissolve 350 g ofRochellc's salt and I 00 g ofNaOH in I litre water.
Dissolve 23 g of Mercuric iodide and 16 g of Potassium iodide in distilled water a nd make up th e
volume to I00 mL. Add I 50 ml of 4 M NaOH solution. Allow it to stand for 24 hrs all d decant the I 0. Hydroxylomlnc hydrochloride : Dissolve 69.5 g ofdry solid in I litre of methyl alcohol.
solution . Solution should be stored in dark coloured bottle. 11. Molisch'sreogcnt:
IS. Potassium ferrocyunlde(0.15 M): Dissolve IO g of cx-nophthol in 90 mLofrcctificd spirit.
Dissolve46 gofthc salt in distilled water and dilute to I litre. 12. Nlnhydrln reagent:
16. Potassium ferrlcyunide(0.2 M): Prepare 0.25% aqueous solution.
Dissolve 55 g oflhc salt in distilled water and dilute to I litre. 13. Schiff's reogent:
17. Potassium iodide (0.S M): Dissolve I g of rosaniline in 50 mL water with gentle wanning. Cool, saturate with sulphur dioxide
Dissolve 83 g of the salt in distilled watcrand make up thevolumc to I litre. gas. Dilute the solution upto I litre with water. If pink colour reappears on standing add few drops
of saturated aqueous solution of S01 with stirring until the colour just disappears.
18. Potassium thlocynnute(0.5 M):
14. Seliwonoff's reagent:
Dissolve49 gofthe salt in distilled waterand dilute to I litre.
19. Phenolphthnleln Indicator : Dissol ve I g oft he solid in I 00 mL of ethyl alcohol.. Dissolve I g ofrcsorcinol in I 00 ml of20 % HCI acid.
20. Sodium nitroprusslde: Dissolve 4 gofthe solid in 100 ml of distilled water. 15. Sotlium hydrochlorite (21\1):

21. Starch: Prepare apasteofabout Ig of soluble starch in cold water and pour it to gradually in 100 Dissolve 100 g ofNaOH in 200 ml of water in a large beaker. Cool the solution and add about
mLofboilingwater\\ith constant stirring. Boil it for 10 min. and cool it. 500 g of crushed ice. Weigh the beaker on a rough balance and pass chlorine gas until the weight
increases by 72 g. Dilute the solution to I litre with water. The solution must be kept in a cool dark
place. Even then it slowly decomposes .
Special Reagents Used In Organic Analysis
16. Tolleo's reagent:
I. Alcohol ( 1: I): Mix equal volume of rec ti tied spirit with disti lied water. To I mL of2% solution of silver nitrate add I ml of 10% sodium hydroxide till the precipitate just
2. Alcoholic Pota~ium Hydroxide Solution appears. Add solution of ammonium hydroxide with stirring till the solution becomes clear.
Ammonium hydroxide should not be added in excess.
Dissolve 11 .2 g of potassium hydroxide in I00 mL ethanol by boiling for 30 mins.
(Always use fresh Tollen'sreagent).
J. Alkalinr P-naphtbol:
Dissolve IO g of P-naphthol in I00 ml of I0% sodium hydroxide solution.
4. Barfoed reagrnt : Dissolve 13g copper acetate in 200 mL of I % acetic acid.
5. ~nedlcr'11 solution:
~i~ h e I 7.3 g of crystalline copper sulphat~ in I00 ml of water. Separately dissolve 173 g of
l sodJ~m Clll"Jte and 100 S of anhydrous sodmm carbonate in 800 ml of water. Mix both the
L.-- w luuons and make up the volume to I litre.
. 45. -46-

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