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62 viewsChemistry Practical PDF 2
Chemistry and physics practical solutions
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firepheonix5757Copyright
© © All Rights Reserved
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/ 19
Experiment No. 11
& Inorganic preparations
rf
Aim: To prepare a pure sample of Ferrous Ammonium Sulphate (Mohr’s salt)
aueeey Mohr's salt is one of the important laboratory reagent and used as a reducing agent.
Chemically Mohr’s salt is Ferrous Ammonium Sulphate (F.A.S.), an example of ‘double salt”
It is prepared by dissolving an equimolar mixture of hydrated ferrous phate (FeSO,.7H,O)
and ammonium sulphate [(NH,),SO,] in acidified water. Mohr’s salt [FeSO,.(NH,). SO,.6H,0}
crystallize as faint green coloured solid. oe
Chemical Equation: FeSO,.7H,O + (NH,),SO, ——» FeSO,.(NH,),SO,.6H,0 + H,O
(278) (132) (392) - .
Apparatus: China dish, beakers, funnel, glass rod, tripod stand, wire gauze, pair of tongs etc.
Chemicals: Ammonium sulphate, ferrous sulphate, dilute sulphuric acid, etc.
Diagram:
Evoporting
Dish
Wire guaze
a “eid stand
(6) Fittraion (©) Heating the station (©) Moneetinie
Procedure:
Weigh accurately 3.5 g ferrous sulphate and 1.5 g ammonium sulphate and transfer into
1.
100 mL beaker. Add about 2-3 mL of dilute sulphuric acid to prevent hydrolysis of ferrous
sulphate.
In another 100 mL beaker boil about 20 mL of distilled water. Now add the boiling water to
the contents of first beaker. Stir with a glass rod until the salts are completely dissolved.
3, Filter the hot solution to remove undissolved impurities and transfer the solution (filtrate)
toa china dish. Heat the solution to concentrate up to the point of crystallization and cool it
naturally to get good yield.
4. Filter the crystals to separate the mother liquor.
Wash the crystals with alcohol and dry it. The shape of Mohr’s salt crystals is monoclinic.
5.
bservations and Result:
Yield of ferrous ammonium sulphate crystals = Ca
Colour of ferrous ammonium sulphate c
Shape of ferrous ammonium
Remark and sign of teacher:
is
fe crystals = Select the correct answer for the following multiple choice type questions.
1. The mineral acid used in preparation of Mohr’s salt is.
a. dil. HCI b. cone. HCI
Veruil. H,SO, d. cone. H,SO,
2. Molar mass of Mohr’s salt is eee “
(27392 g/mol b. 278 g/mol c. 132 g/mol 9
3. The shape of ferrous ammonium sulphate crystal is. areca
a. monoclinic V% octahedral c. hexagonal voce
r’s salt. the process,
4. Concentration of filtrate leads to formation of pure crystals of Moh
involved is known as
Uerystallization b. fractional crystallization
purification d. evaporation .
5. The cooling of concentrated solution of F.A.S. is always done slowly.
4. to get good colour b. to get shining crystals
27to get good yield d. to get minimum crystals
1, Why the concentrated sojutio: stp na t be heated for along time? “Bn. mn
Ans.....L...., util. healt. OH... ie ae me .
4 abil nba i gas ji :
0] pmetrig titration Mohr’s salt is used.
HOt (bas
Experiment No. 12 a
ch alum [I (O,),-24H,
im: To prepare a pure sample of potas! ¥ HH . .
Aim: y: An equimolar mixture of potassium sulphate and hydrated a ea sulpha i
diasolves ied water, octahedral crystals of potash alum (a double salt) are obtaineg
dissolved in aci
Al(SO,),.24H,0
Chemical Reaction: .
K,SO, + Al(SO,), .18H,O + 6H,0 ——» K,SO,
Potash alum
Potassium Aluminium
sulphate sulphate
Apparatus: Beakers, funnel, China dish, glass rod, tripod stand, aie gauze, etc.
Chemicals: Potassium sulphate, Aluminum sulphate, dilute sulphuric acid
Diagram:
Lez or sotsion
—_
\/ Filter paper Evoporating
+ dish
a we
guaze
Clear
filtrate
(6) Filtration (b) Heating the solution (©) Octahedrat
Procedure:
Weigh accurately 1.0 g of potassium sulphate and 4.0 g aluminum sulphate. Transfer it toger
id add to first beaker containing b
1.
into 100 mL beaker.
2. Take 20 mL distilled water in another beaker, boil it an
salts with constant stirring.
3. Add 2 mL of dilute sulphuric acid and heat the content for about five minutes.
4. If milkiness still persists filter the solution in a china dish.
5. Place the china dish on a wire gauze over the tripod stand and heat the solution with const
stirring till point of crystallisation is reached.
. Soon crystals of potash alum will separates out.
rystals if required, wash with ice cold water, dry ¢
lum crystal is octahedral.
6. Cool the hot solution naturally.
7. Decant off mother liquor. Filter the o
weigh the crystals. Shape of potash al
Observation and Result:
1. Colour of potash alum crystals
2. Shape of potash alum crystals
3. Yield of potash alum crystals
Remark and sign of teacher: >
Gx spe questions.
gelect the correct answer for the following multiple choice type 4
1, Water.of crystallization present in aluminum sulphate is/are -.
(24 b.18 c. 6
5, Shape of potash alum crystal is
“ a. moloclinic \UbSctahedral
c. cubic d. hexagonal
Potash alum is
uC double salt b, coordination complex
cc. 3D complex compound d. inorganic base
4, Dilute sulphuric acid is added during preparation of potash alum to
ce prevent hydrolysis of aluminum sulphate
b. prevent hydrolysis of potassium sulphate
¢. prevent oxidation of potassium sulphate
4: dissolve both the salts K,SO, and ALSO)». ap
‘The process occurs when crystals of potash alum is heat
a bums theerystals b. the erystal melts crystal
ye looses the water of crystallization d. no change occurs
1.Wht is potash alum?
ee Bhan lum. vo. [email protected]...
~pectgoalien...nnd... dkaminusn... ta ‘pio K
$04) 5.24.0. sevnee erent
3. Write the uses of potash alum, e Pa
< Peak tunedd...stn.. PLU ficahy@N..... ay.
f making. jaw ‘dtiiutbhin te
a3
medicxna...
3. Why does an aqueous solution of potash alum turn blue litmus red?
‘Ans. AQULOWA ludfan..o/.... peetabh...luuMn.....dwxn....blue.....
“Pirin wel oo ay kee. in nadie «
4, Differentiate complex compound and a double sal Experiment No. 13 (ac)
‘Te prepare a pure sample of the complex potassiumtrioxalatoferrate( Il).
When hydrated ferric chloride is dissolved in aqueous solution of oxalic acid containing
potassium hydroxide, green crystals of potassiumtrioxalatoferrate(III) are obtained.
involved in the formation of green crystals are as follows:.
he reactions
Chemical Reaction: FeCl, + 3KOH
Fe(OH), = 3KCI
Ferric hydroxide
2Fe(ON), + 3 H.C,O,. 2H,0 ——+ Fe. ).), + 12H,0.
Ferrous oxalate
Fe(C,O,), + 3(COOK),.H,O ——+ 2K [Fe(C,0,),J. 3H_0
Potassium oxalate potassiumtrioxalatoferrate( II)
\pparatus: Beakers.china dish, funnel, glass rod. tripod stand, wire gauze, sand bath, burner, ete
Chemicals: Ferric chloride, oxalic acid, potassium hydroxide. potassium oxalate.
Procedure:
1
Take 1.15 g of potassium hydroxide in a beaker add 15 mL water shake well to dissolve
Take | g of anhydrous ferric chloride in a another beaker add 15 mL distilled water shake well
to dissolve it.
3. Transfer KOH solution in to FeCl, solution in small portion with constant stirring, Ferric
hydroxide precipitates out. Filter the precipitates and wash it with distilled wat
4. In another beaker take 1.15 g of oxalic acid and 1.6 g of hydrated potassium oxalate and
30 mL distilled water, Warm to get clear solution.
5. Add ferric hydroxide precipitate to this above solution and stir well to dissolve it.
6. Filter the solution and transfer it to china dish, heat the china dish on sand bath to reduce its
volume. Cool the concentrate to obtain fine green crystals of the potassiumtrioxalatoferrate(II1)
complex, wash the crystals with small quantity of ethyl alcohol. Dry and weigh the crystals,
7. Shape of potassiumtrioxaltoferrate({II) is octahedral
Observation and Result:
1. Colour of potassiumtrioxaltoferrate(III) is questions.
Select the correct answer for the ere io
1. Geometry of the complex K,[Fe(C,0.l « i ‘gone
a. bipyramidal ® “ —
\-©& octahedral mn
2. Complex potassiumtrioxalatoferrate(ID i§ +" agnetic alk
a. ferromagnetic PO ie ate is i
c. diamagnetic ae
3. The co-ordination number of iron in potassiumtriors
«. three . four con
4. In potassiumtrioxaltoferrate(II) complex, oxalate lige
U4. bidentate ligand id rdenate
©. tetradenate ligand é polyex is
5. The Colour of potass un trioxaltoferate(ID © compre’ £4
a. colourless b. yellow c. red
2. Why does the com
Ane Bee 1
gna potassium;
and,,atat.
3. Wri fe two examples of biden
tate ligands other than oxalate ion.
HoN
Remark and sign of teacher: No. 1
Experiment ‘ions
Organic Prepar®
hyde with acetone
Aim: To prepare dibenzalacetone. of benzald hy iy
condensation OF acrion-
Dibenzalacetone is prepared by the cia ‘en-schmidt
o
presence of sodium hydroxide. It is an example
en as:
Chemical Reaction: The chemical equation can be writte? 0
W cH=c 1XO>
9° c
Hl -H=CH- .
Benzaldehyde Acetone
rit, ice
etc
Apparatus: Conical flask, beaker, test tube, funnel. filter POPE °°"
ethanol/rectified SP"
jenzaldehyde, acetone, 10% NaOH.
pirit in a small conical flak
Chemicals:
Procedure:
1. Take 0.5 mL benzaldehyde, 0.2 mL acetone and 5 mL methylated s
Cork the conical flask and shake well. ;
flask with constant shaking:
2. Add | mL of 10% NaOH drop wise to the conical
3. Cork the conical flask and shake vigorously for about 10 minutes.
ressure developed.
4. Intermittently remove the cork of the flask to release the p
. ein ter.
5. Keep it for 20 minutes to complete the seaction and then cool it in ice cold wa
6. Filter the yellow coloured solid and wash it with water.
7. During recrystallization dissolve the solid in hot rectified spirit, cool, filter and dry the crystals,
(Do not heat directly with burner, use hot water bath)
9
Result: 1. Yield of dibenzalacetone =
2. Colour of dibenzalacetone crystal
Remark and sign of teacher: rect answer for the following multiple choice type
Select the
‘The colour of dibenzalacetone crystal is. yellow
1
“Gellow
dred
sah ondinpad On
white b. green
used in the formation of dibenzalacetor
b, addition
d, double decomposition
Awe benzyl suliays
Ustwo benzyl rings
d. two ketonic groups
. oxidation
4a. wo phenyl groups
¢. one benzene ring
4, Claisen-Schmidt reaction takes place between
\a@liphatic ketone and aromatic aldehyde
b. aliphatic ketone and aliphatic aldehyde
¢. aromatic ketone and aromatic aldehyde
d. aromatic ketone and aliphatic aldehyde
5. Recrystalisation of dibenzalacetone is carried out by using ethanal
a.NaOH — Lbthanol c. water d. acetone
Short answer questions
1. Write the molecular formula of dibenzalacetone.
Ans...... :
ation of benzaldehyde and acetone?
dA -PsuUaNnee....@f,.
Ans....,
4. Is it necessary to recrystallize the dibenzalacetone obtained from the reaction? Explain
ans Nh. ft... NOCLONALY fp, sucauetalize afinnyglacon..
ara CMe caste
hat will be the product obtaine alent of benzaldehyde reacts with one
equivalent of acetone?
I...
Remark and sign of teacher: Experiment No. 15
ndergc tion reaction with nitrous acid (HNO,) at low temperature to form benzene
diazonium cholride. It further undergo coupling with 2-naphthol to produce 2-napthol aniline
dye. 2-naphthol aniline dye (Benezene-azo-2-naphthol) is a scarlet red azo dye
HNO, + NaCl
A HNO. Diazotization
° 2 (NaNO, + HCI) low temp.
N,"CI°
O OF sin OH,
iii. oa ul.Nat
273K
Benzene
diazonium — 2-naphthol (Orange red dye)
chloride
Apparatus: Beaker, conical flask, glass rod, ice bath, buchner funnel, ete.
Chemicals: Aniline, sodium nitrite, conc. HCI, fs naphthol, 10% NaOH.
Procedure:
1. Take 1 mL aniline in 2.5 mL of concentrated HCl, in a 100 ml conical flask add 5 mL distilled
water and cool the flask in a ice bath.
2. Take 1 g of NaNO,, in another beaker add S mL_ distilled water to dissolve it. Cool this beaker
in a ice bath.
3. Add ice cooled solution of NaNO, slowly to the cold solution of aniline and HCI with continuous
shaking, to prepare benzene diazonium chloride.
4, Add 2 g of 2-napthol in 15 mL of 10 % NaOH in test tube and dissolve it.
5, Now add benzene diazonium chloride solution to 2-napthol in NaOH with constant stirring with
glass rod.
6. Orange red dye crystals of 2-napthol aniline dye is formed. Filter it in a buchner funnel. Wash
this dye with water.
7. Dry it and find weight of crystals.
Observation and Result:
i. Yield of 2-naphthol aniline dye crystals
ii. Colour of 2-naphthol aniline dye "!
Note: Azo-dye synthesis is nearly quantitative, so
equations. Any excess of certain reactants may cause
‘one should use amount of reactants as per the
decomposition of unused material and
may produce ‘tar’.
Remark and sign of teacher: ing mull
Select the correct answer for the follow’ a rand!
1 The colour of pure anitine is.{(EOk ger ello
a. blue b. red Fain api HK ould BE
2. The colour of naphthol aniline dye #2 inet
Corange b. yellow c. ne above expe
3. The temperature maintained tug he msi action.
4, more than 25°C b. . Fe
oles than 5°C
4. Addition of NaNO, to the cold solution of Ml
f. exothermic b. Sea
5. Formation of benzenediazonium chloride is.
nitine on
jon
sactio’
: ae ing Fe
a. coupling reaction b. di azo-coupling
ve diazotization d. combination
‘ions
Short answer quest!
1. Write die
zotization reaction of ethylamine.
eae Bellis
5%
vo svvitencade ization of aniline
2. What is diazotization? write the reaction i)
erat acid. can
ag th aml. pce Ziunnd apa jonny lua ae
Of. ee idl <-NHa NaNO LH py or N= Ne.
WI we do you understand by coupling reaction?
Ans fie qb. -aeactan, fn... cabich van
4h li Fen ite “fg amped, ; cortéalning.
4. Which of the ci i a on diazotisation followed by coupling with 2 naphth
will form an azo-dye? (i. p-toluidine ii, benzylamine iii, N-methylamine?)
Ans. Omino...,. doo... wa op ALOR MATS OL
Fede isp rath ale lly |
C NOTES /CALCULATIONS /ROUGH WORK. =)
: ~ CALWATO ay yfeld a} B—nagtha aniline
Malu mn aig Gf Aniline." 93-19 eg :
Malai. man) af B- reg npthaleviLine. = 248.289
Bo. avin
aa a B= pdpthel = artline.
; end AO. a ,iline bY CH,-Co.
. F Sty,
ofa [ chloride is 62"
. ride. up ot cel Seay
Aim: To prepare acetanilide from acetyl chlori¢ ‘4 with a Ti
‘Theory: The replacement of one hydrogen HO",
in the presence of glacial acetic acid gives acet!
out in the presence of glacial acetic acid. -
rH
Chemicals Reactior
H 1
