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ENGINEERING CHEMISTRY LABORATORY EXPERMENTS
B.Tech I YEAR ( www.jntuworl.co! "
EXP...No. #
TITRIMETRY
AIM: Estimation of hardness of water by EDTA method
APPARATUS: - Burette, Piette, bea!ers, Standard f"as!, #oni$a" f"as! %%%et$&
#'EMI#A(S: - )&* M EDTA, Erio$hrome, B"a$!e-T, water sam"e buffer so"ution&
T'+ER:- Estimation of hardness by EDTA method is based on the fo""owin rin$i"es&
*& .irst, the indi$ator Erio$hrome B"a$!-T, whi$h is a b"ue $o"ored dye, forms an unstab"e
$om"e/ with $a"$ium or Manesium ions in hard water at H P of 0 to *)& The $om"e/
is wine red in $o"or&
1 12 Mg Ca
+ + + Erio$hrome B"a$!-T → 3M2#a4Erio$hrome b"a$!-T5
Unstab"e #om"e/ 67ine Red5
1& As this so"ution is titrated aainst EDTA, the free 1Ca + and
1 Mg +
tones in water from
stab"e meta" ion EDTA → 3M2#a-EDTA8 Stab"e #om"e/& #o"or"ess
+n$e the free meta" ions are $om"e/ed, the EDTA re"a$es #a and M ions from the
unstab"e indi$ator $om"e/ a"so, to form a stab"e $om"e/, with the resu"t, the indi$ator
is set free& Sin$e the free indi$ator is b"ue in $o"our at the abo9e mentioned P', the end
oint is the aearan$e of b"ue $o"or
3M2#a-Erio$hrome B"a$!-T8 EDTA → 3M2#a-EDTA8 Erio$hrome B"a$!-
T6B"ue5
The temorary hardness is remo9ed by boi"in and after the remo9a" of re$iitate by
fi"tration; the ermanent hardness in the fi"trate is determined by titration with EDTA as
abo9e&
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Proceure$%
* &Rinse and fi"" the burette with EDTA so"ution&
1& Piette out 1< m" of hard water into 9o"umetri$ f"as! and add 1) m" of disti""ed water and
*) m" of buffer so"ution
=& Add 1-= dros of Erio$hrome B"a$!-T indi$ator&
>& Titrate aainst )&)*M EDTA so"ution ti"" the $o"or of the so"ution $hanes from wine red to
B"ue&
<& ?ote the fina" readin and reeat to et three $on$ordant readins&
O&'er)t*on T)&le$
Sl.No
+olu!e o, the 'olut*on
t)-en *n the t*tr)t*on ,l)'-
(nl"
Burette Re)*n' +olu!e o, the
t*tr)nt u'e
1 *V V − nl
In*t*)l
Re)*n(+#nl"
/*n)l Re)*n
(+0nl"
→ @o"ume of hard water ta!en for ea$h titration 1< m"
→ @o"ume of )&)* M EDTA used 3from titration8 @* m"
#a"$u"ation: - *)) m" of * M EDTA *)) m of #a#o= * m of #a#o=
* m" of )&)*M EDTA
* *
*)) *))) *)) gm× × of #a#o= * m of #a#o=
@ m" of )&)*M EDTA I ×@ M of #a#o= / m of #a#o=
1< m" of hard water $ontains/ m of #a#o=
*))) m" of hard water $ontains /21<*)) m of #a#o= y M2(
RESU(T: The Tota" hardness of water y M2(
Pre$autions:-
*& The burette and iette, $oni$a" ."as! shou"d be rinsed with disti""ed water&
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1& The $o"or $hane near the end oint is 9ery s"ow and this shou"d be obser9ed $arefu""y&
EXPERIMENT NO.0
1ETERMINATION O/ Cu02 THRO3GH IO1OMETRIC TITRATION
AIM: Determination of #u er$entae in #oer one 6Brass5
APPARATUS: Burette, Piette, Bea!ers, Titration f"as!
#'EMI#A(S: #oer +ne, 'yo, CI, Br 1 So"ution, A$eti$ A$id, ?itri$ and '#", '1So>
I?DI#AT+R: Star$h so"ution
E?D P+I?T B"ue to #o"our"ess
PR+#EDURE:
Prearation of So"ution of ore
*& Ta!e about * of the fine"y round $oer ore in a bea!er and warm with *<-1) m" of $on$&
'?+= unti" the $oer asses into so"ution&
1& E9aorate to a 9o"ume of < m" and add *) m" of $on$& '#" and eua" 9o"ume of *: * '1S+>&
Aain e9aorate ti"" dense fumes of S+= aear indi$atin $om"ete remo9a" of nitroen
o/ides&
=& 'eat the mi/ture with *< m" of bromine so"ution and an eua" 9o"ume of water to $om"ete
o/idation of any As and Sb to the Penta9a"ent state&
>& Boi" off e/$ess of bromine and di"ute the resu"tin so"ution to *)) m" in a measurin f"as!&
Titration:
*& Rinse and fi"" the burette with )&* ? ?a1S1+> so"ution
1& Measure 1) m" of the ore so"ution into a $oni$a" f"as!
=& ?eutra"ie any free a$id resent by addin ?a1#+= so"ution dro by dro ti"" a faint
ermanent re$iitate remains e9en on sha!in&
>& Add di"& A$eti$ a$id dro wise unti" re$iitate Fust disso"9es<& Add * m of so"id C", $o9er the mouth of $oni$a" f"as! by fi"ter aer and a""ow the
mi/ture to stand for 1 to < minutes in the dar! the so"ution be$omes brown due to
"iberated iodine
G& Titrate the "iberated iodine with hyo so"ution added from the burette, the brown $o"our
of iodine be$omes fainter as the addition by hyo so"ution ro$eeds and when on"y a
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faint ye""ow $o"our remains add 1 m" star$h so"ution& This immediate"y form a dee
b"ue iodo-star$h $om"e/
H& ?ow add hyo so"ution further, dro by dro when on"y mi"!y white $o"our remains&
+bser9ation Tab"e:
S"&?o
@o"ume of the
so"ution ta!en in
the titration
f"as!6m"5
Burette Readins @o"ume of the
titrant used
6fina"-Initia"
readin66m"5
Initia" Readin .ina" Readin
*&
1&
=&
#a"$u"ations:
6+re So"n&5 6?a1S1+=5
?*@* ?1@1
?*1) )&*@1
?* G=&<
*))StrengthofSolution
× × 1)&*
1)
V ×
?6 1Cu + 5 1
1))
V Strenth of 1Cu + 1
1))
V G=&<2(
Per$entae of #u in ore so"ution 1
1))
V G=&<*))
StrengthofSolution× ×
RESU(T: The amount of #u resent in $oer ore so"ution is %%&
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EXPERIMENT NO.4
COLORIMETRY
ESTIMATION O/ COPPER BY COLORIMETRIC METHO1
AIM: Estimation of #oer by #o"orimetry
APPARATUS: - #o"orimeter, Test tubes, Burettes&
PRI?#IP(E: - #o"orimeter measures the oti$a" density of an absorbin substan$e where
oti$a" density 6+&D5 is defined as +&D "o *o I
I →
7here o I Intensity of in$ident "iht
I Intensity of transmitted "iht
As er beers "aw, oti$a" density of an absorbin substan$e is re"ated to the $on$entration by
the euation& & & &O D E C l =
& 6 & 5& 1O D E l C = →
7here #J is the $on$entration of the substan$e, " is the ath "enth, whi$h reresents the width
of the $e"" used and is $onstant for a i9en $e"" used, E is the mo"ar absortion $oeffi$ient and
is a $onstant for i9en substan$e& Euation 1 may be written as +&D&α # =→
Euation = reresents the uantitati9e form of BeerJs "aw & if the oti$a" density of a substan$e
is determined at 9aryin $on$entration& A "ot of +&D&9s # i9es a straiht "ine&
PR+#EDURE:- ta!e the sam"e so"ution of #uSo> and reare the fo""owin *) sam"e
so"utions in test tubes as * to *)
*& * m" )&* m #uSo> 0 m" Disti""ed water
1& 1 m" )&* m #uSo> K m" Disti""ed water
=& = m" )&* m #uSo> H m" Disti""ed water
>& > m" )&* m #uSo> G m" Disti""ed water
<& < m" )&* m #uSo> < m" Disti""ed water
G& G m" )&* m #uSo> > m" Disti""ed water
H& H m" )&* m #uSo> = m" Disti""ed water
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K& K m" )&* m #uSo> 1 m" Disti""ed water
0& 0m" )&* m #uSo> * m" Disti""ed water
*)& *) m" )&* m #uSo> ) m" Disti""ed water
The ten sam"e so"utions reared abo9e ha9e a 9aryin $on$ern from )&)*m to )&*m, $hoose
the fi"ter in the $o"orimeter with ma/imum absorban$e& Tabu"ate the resu"t of fi"ter and +&D
with a i9en #uSo> sam"e so"utions&
After se"e$tin fi"ter, determine the +&D& of the abo9e mentioned ten sam"e so"utions and
tabu"ate the resu"ts&
O&'er)t*on$
Tab"e-*
.i"ter ?o λ -Rane 6nm5 Pea! 6nm5+ti$a"
Density6+D5*
1
=
>
<
G
H
K
T)&le%II Selecte /*lter%%%%%%%%%%%%%%%%%%%%
S"&?o@o"ume of
>CuSo 6m"5
@o"ume of
1 H O 6m"5
#on$entration
of >CuSo
+ti$a"
Density
*
1
=
>
<
G
*)
0
K
H
G
<
)
*
1
=
>
<
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H
K
0
*)
>
=
1
*
G
H
K
0
GRAPH$ - P"ot a rah of +&D @s 3#uSo>8& A straiht "ine assin throuh oriin is
obtained the s"oe of whi$h i9es E", E is the mo"ar absortion $oeffi$ient&
S"oe1 *
1 *
y y
x x
−=
−
*
slope slope El E l
E mole cm−
= ⇒ =
= −
RESU(T: - Amount of $oer resent in i9en #uSo> so"ution is LLLLLLLLLrams
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EXP.NO.5
CON13CTOMETRY
Aim: - To determine strenth of i9en '#" So"ution #ondu$tometri$a""y
APPARATUS: - #ondu$ti9ity meter, $ondu$ti9ity $e""s, Bea!ers, Piette, Burette
#'EMI#A(S:- +/a"i$ a$id So"ution 6)&*?5, ?a+' So"ution, '#", Pheno"htha"ein Indi$ator&
Pre6)r)t*on o, St)n)r O7)l*c )c* Solut*on (o.#N"
About *&G of +/a"i$ a$id dehydrate is weiht a$$urate"y and disso"9ed in sma"" amount of
disti""ed water and made u to the mar! in 1<) m" 9o"umetri$ f"as!&
PRI?#IP(E: - The $ondu$ti9ity of '#" is 9ery hih due to mobi"ity of ' ions in it& 7hen a
so"ution of stron a"!a"i is added to the so"ution of stron a$id, the hih"y $ondu$tin ' ions
are re"a$ed by ?a
ions is $onsiderab"y sma""er than '
and hen$e addition of a"!a"i to the a$ida"ways a$$omanied by a de$rees in $ondu$ti9ity& 7hen a"" the ' are re"a$ed that is after the
end oint, further addition of ?a+' resu"ts in in$rease in $ondu$ti9ity& from the "ot of the
$ondu$ti9e @s @o"t ?a+' added, the end oint $an be $a"$u"ated
PR+#EDURE: - 1) M( +. +/a"i$ a$id is iette out into a $oni$a" f"as! and is di"uted to =)
m" with disti""ed water& To the so"ution, two dros of heno"htha"ein indi$ator is added and
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the titrated aainst sodium hydro/ide ta!en in a burette& The endoint $o"or"ess to a"e in!&
The e/eriment is re"a$ed ti"" $orre$t readin are obtained
Determination of Strenth of Ni9en '#" So"ution:-
The i9en un!nown '#" so"ution is *)) m" 9o"umetri$ f"as! is made u tot the mar! and then
*)m" of i9en un!nown '#" So"ution is ta!en in a *)) m" bea!er& To this >)m" of disti""ed
water is added, the e"e$trode of the $e"" is died in the so"ution& The $ondu$ti9ity of so"ution
is noted before addin the a"!s"i& The standardied sodium hydro/ide is added from a burette
with *m" of in$rement and by sha!in thorouh"y, the $ontents of the bea!er the $ondu$ti9ity
9a"ues are noted& The 9a"ues of obser9ed $ondu$ti9ities are "otted aainst 9o"ume of sodium
hydro/ide
The $on$entration of hydro$h"ori$ a$id is determined usin the end oint from the rah&
PRECA3TIONS$ - after 1 ea$h addition of titrant from the burette the so"ution shou"d be
thorouh"y stirred and then the readin shou"d be ta!en&
RES3LT$ - The Strenth of 'ydro$h"ori$ A$id is LLLLLLLLLL 2"it&
C)lcul)t*on$%
Standardiation of Sodium 'ydro/ide So"ution
S&?o@o"ume of +/a"i$ A$id
6@*m"5Burette Readins
@o"ume of ?a+' So"ution 6 1V
.-I5
Initia" .ina"
*
1
=
1)
1)
1)
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7E !now that * * 1 1@ ? @ ?=
@* is @o"ume of +/a"i$ A$id 1)m"
?* is ?orma"ity + +/a"i$ A$id )&*?
@1 is @o"ume of Sodium 'ydro/ide- -m"
?1 is ?orma"ity of Sodium 'ydro/ide O ?
* *
1
1 V N
N V
= ∴ ?orma"ity ?a+' -------?
Determination of Strenth of '$":-
S"&?o @o"ume of ?a+' #ondu$ti9ity 6ohm-*5
*
1
=
1)
>)
@o"ume of ?a+' So"ution from rah Ph @1 -m" NRAP':
?orma"ity of ?a+' So"ution ?1 -?
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@o"ume of 'udro$h"ori$ a$id so"ution @= *)m"
?orma"ity of '#" in mi/ture ?= -----?&
1 1 = =V N V N =
1 1=
=
V N N
V =
Strenth of '#" So"ution ?orma"ity of '#" So"ution e&7t of '#" ?= =G&<
n LLLLLLLL 2(it
EXP.NO.8
POTENTIOMETRY
TITRATION O/ STRONG ACI1 +' STRONG BASE
AIM:- To Determine the $on$entration of a stron a$id by a Potentiometry titration i9en a
stron base of !nown $on$entration&
APPARATUS: - Potentiometer, Pt-e"e$trode, #a"ome" e"e$trode, Sa"t bride, *<) m" bea!ers,
Stirrer, Piette, Burette&
#'EMI#A(S: - )&*m ?a+', )&*m '#(, uinhydrone so"id, C#" So"ution&
PRI?#IP(E: - The uinhydrone e"e$trode is reared by ta!in saturated so"ution of
uinhydrone in a !nown uantity of stron a$id whose $on$entration is to be determined& This
e"e$trode is $ombined with the $a"ome" e"e$trode to ma!e the $e""& Pt, ',
'1#"16s52Saturated22'2'12Pt
In a$id medium uinhydrone e/ist in two forms&
As ?a+' is added to a so"ution of ' ions with uinhydrone the ' ions are $onsumed
steadi"y and the re"ati9e $on$entration of '1 and $hanes with the titration& At the end
oint where a"" the ions are $onsumed, '1 ets $om"ete"y $on9erted to & the e"e$trode
otentia" of the e"e$trodes is i9en as er the nearest euation&
1
)
1 1
1
)&)<0 &2 2 *)
aQ a Qh EQH Q E QH Q g
aQH
+
= −∩
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)
1
)&**K2 "o E QH Q aH
n= − 3 aQQ and 1
*8aCH =
At the endoint, whi$h aH o+
; there is a sudden fa"" in the $e"" emf1 2cell calomel aH Q E E E = +
Sin$e $a"ome" is $onstant the 9ariation of cell E is a measure of the 9ariation of 1 2aH Q
E & The
endoint is the titration is the oint where there is a ma/imum fu"" in otentia" with a sma""
addition of ?a+'&
Pro$edure: - Piettes out *) m" of the i9en '#" so"ution into a $"ean*))m" bea!er add a in$h
of uinhydrone and stir it we"" to ma!e a saturated so"ution of uinhydrone is '& di a
"atinum e"e$trode& Ta!e a se$ond bea!er with saturated C#" so"ution in it& Di the $a"ome"
e"e$trode in it& #onne$t two bea!ers with a sa"t bride; $onne$t the termina"s of the
otentiometer with the two e"e$trodes& ?ote the emf of the $e""& fi"" a burette with )&* ?a+',
add )&<m" of ?a+' into the bea!ers $ontainin a$id, stir we"" for eui"ibrium to estab"ish& ?ote
the emf of the $e"" on$e aain& The 9ariation of emf by su$$essi9e addition of )&< m" of ?a+'&Ea$h time wi"" be about *)-1)m9, as the endoint aroa$hes, the fa"" in the emf wou"d
in$rease from *)-1) m9 to >)-<) m9& At this stae add ?a+' in bat$hes of )&1 m" and note
emf after ea$h addition& At the end oint the emf fa""s sudden"y by about *))-*<) m9&
#ontinue the titration with )&1 m" of ?a+' and note <-G emf 9a"ues& ?ow the 9ariation is emf
ets sma""er and ta!es >-< emf readins, after the endoint by addin bat$hes of *m" of ?a+'
ea$h time, tabu"ate the resu"ts&
NRAP': - P"ot a rah of em @s 9o"ume of ?a+' added and a se$ond rah of 2 E V V V @s
@o"ume of ?a+' added& ?ote the oint of ?eutra"iation from both the rah and $a"$u"ate
the $one of i9en '#" usin the $on$ern of i9en ?a+' as )&*m
RESU(T: - At the ?eutra"iation oint *) m" of i9en '#" And $on$ern of i9en
'#"LLLL
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S"&?o @o"ume of A"!a"i 6m"5 Emf 6m95Q Poly n →
E
V
∆∆
*
1
=
&
&
&
=)
#A(#U(ATI+?: -
'#" ?a+'
**)V ml =
1 LLLLL V = 6.rom Nrah5
* N =
1)&* N =
* * 1 1V N V N = ⇒ *
*
1 1V N N
V =
∴#on$entration of i9en '#" 6 * N 5 LLLL?&
EXPERIMENT 9 :
I1ENTI/ICATION O/ /3NCTIONAL GRO3PS IN ORGANIC COMP3N1S
SYSTEMATIC PROCE13RE
EXPERIMENT OBSER+ATION
IN/ERENCE
PHYSICAL CHARACTERSTICS$
)"Ph;'*c)l 't)te *" L*<u* (or" Sol*"
ii5 Amorhous 6or5
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$rysta""ine
b5 +dour i5 Pa"e ye""ow ?itro $omounds
ii5 Reddish orane ?itro amines
iii5 Brownish ye""ow Ani"ine
i95 Pa"e in! Pheno"
95 #o"our"ess #arbohydrates, a"dehydes,
!etones, $arbo/y"i$ a$ids,
esters and some sim"e
hydro$arbons&
$5 +dour i5 +dour"ess #arbohydrates, aromati$
a$ids
ii5 Bittera"ononds ?itrobenene,
bena"dehyde are absent
Aromati$ amines
iii5 .ishy sme"" A$etamide
i95 Mouse "i!e sme"" .orma"dehyde, formi$ a$id
95 Punent sme"" Esters
9i5 P"easant fruites Pheno"s
6Pheno"i$5 #arbo"i$ sme"" A$eti$ a$id
@inear "i!e #inamon "i!e #innama"dehyde
d5 Me"tin oint2 Boi"in oint
II& So"ubi"ity : Ta!e a sma"" amount of $omound in a test tube and add =-m" of so"9ent
a57ater So"ub"e in $o"d water i5 #arbohydrates, "u$ose,
.ru$tose
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ii5 Amides, urea
a$etamide
b5 < ?a+' So"ub"e in < ?a+' and May be wee! a$id "i!e
heno"s
reerated with '#"
$5 < ?a'#+= So"ub"e in < ?a'#+= and May be stron a$ids,
beno"i$,
reenerated with '#" sa"i$y"i$ a$ids&
d5 < '#" So"ub"e in < '#" reenerated May be amines "i!e
ani"ine
with ?a+'&
e5 Ether So"ub"e in ether May be nautra"
$omounds "i!e,
$h"orobenene,
A"dehydes, Cetones,
?itrobenene et$&
III. In*t*on Te't $
'eat a sma"" amount *5 Burns with non-"uminous A"ihati$ $omound
+f i9en $omounds and non-smo!y f"ame&
+n satu"a 15 Burns with (uminous Aromati$ $omound
And smo!es f"ame=5 Burns with suar sme"" #arbohydrates
1ETECTION O/ /3NCTIONAL GRO3PS
TEST /OR PHENOLS
*"=*th neutr)l /eCl> te't $ The $omound to disso"9ed @io"et 6or5 B"ue Pheno" is resent
In a"$oho" and add * 6or5 1 $o"our is obser9ed
Dros of < .e$
G < = = G <G 3 6 58 =C H OH FeCl H Fe OC H HCl + → +
**" L*e&er!)nn?' n*tro'o re)ct*on$
Ta!e the $omound in a dry A b"ue $o"our is obtained Pheno" is resent
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Test tube add sodium nitrite the so"ution turns red on
And $on$ su"huri$ a$id6*m"5 di"ution with water and b"ue
Mi/ we"" and heat ent"y on basifi$ation with di"
So" of ?a+'
Test for #arbo/y"i$ A$ids:
*&?a'#o= Test
To a saturated so"ution Bris! effer9es$en$e #arbo/y"i$ a$id is resent+f sodium bi$arbonate is obser9ed
in water 6*m"5 add the
i9en $omound
= 1 1 COOH NaHCO COONa H O CO− + → + + ↑
ii5 Ester Test:
'eat the mi/ture .ruity sme"" is obser9ed #arbo/y"i$ a$id is resent
+f the a$id, ethano" 6*m"5And $on$entrated su"huri$ a$id
in a dry test-tube in a water bath&
Pour the rea$tion mi/ture $arefu""y into a
Bea!er $ontainin ?a1#o= So"ution&
1 >&* *
1
Conc H SO
Heat COOH OH COO H O− + → +
iii5 .e #"= Test:
?eutra"ise)&< m of the i5 A buff 6or5 brownish $o"oured Aromati$ a$ids
A$id with e/$ess of ammonia t is obtained
In a boi"in test tube& Boi" the ii5 An intense ye""ow $o"our is α -'ydro/y a$ids
So"ution to remo9e e/$ess obtained
+f ammonia, $oo" and add a few iii5 A 9io"et 6or5 f"eshy $o"our is β -substituted aromati$
Dros of neutra" ferri$ $h"oride obtained hydro/y a$id
So"ution&
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Test for #arbony" #omounds:
I5 Rea$tion with 1,> D?P*
Disso"9e the $arbony" $omound a ye""ow or orane $o"our may be a
6*)) m 6or5 *-1 dros5 in ethano" 61-=m"5 t is formed $arbony" $omound
To this add an a"$oho"i$ so"ution of
1,> O di nitro-heny" hydraine 61 m"5
and Sha!e the mi/ture we""&
ii5 To""enJs Test:
To the to""enJs reaent 6*m"5 a rey b"a$! t6or5 si"9er May be a"dehyde is
Add a so"ution of the a"dehyde mirror deosits on the inner resent61 dros 6)*5 <) m5 disso"9ed wa""s of a test tubeIn a"dehyda free a"$oho"
6-1-= m"5 and warm the so"ution
in a hot water bath&
iii5 .eh"in Test:
Add .eh"in so"ution 61-= m" Red re$iitate of may be a"dehyde is
By mi/in eua" amounts of $urous o/ide is formed resent
.eh"in A .eh"in B) to the
+rani$ $omound &and warm the mi/ture
1 1 11 6 5 1CHO Cu OH COOH Cu O H O− + → + ↓ +
1 1 11 6 5 1CHO Cu OH COOH Cu O H O− + → + ↓ +
.eh"in So"ution Red
i95 S$hiffJs Test
To a so"ution orani$ @io"et 6or5 ur"e $o"our 6in!5 may be a"dehyde is
#omound add S$hiffJs is obser9ed resent
Reaent 61-= dros5 and
Sha!e the $ontents
95 Iodo form test:Disso"9e the i9en $omound A ye""ow t "odo form may be !etone61-= m" 6or5 *)) m5 in water is obser9ed
61-=m"5 in a test tube and add
1-=m" ?a+' 6*)5& To this addA saturated so"utaion of iodine-in C"
with stirrin unti" the dar! $o"our of
iodine ersists& 'eat the so"ution in a boi"in water bath for *-1 minutes&
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1
= = =
I NaOH NaOH CH CO Cl CO CHl COONa+ → → + Iodo form ye""ow so"id
Te't ,or C)r&oh;r)te'$
*".Mol*'ch?' Te't$Add an a"$oho"i$ so"ution of A 9io"et rin is obser9ed at the may be$arbohydrateα
-?aPhtho" 6*)5 to an aueous Fun$tion of two "ayersSo"ution of substan$e& Then add
#on$ 1 > H So 6*m"5 $arefu""y a"on
the sides of the test tube a""ow to stand
for 1 minutes&
ii5&Barfoed Test:'eat the aueous so"ution i5 red $o"our re$iitate of #u1+ $arbohydrate is resentof the $omound 6im"5 with is formed resent
barfoed reaent 6*m"5 in
boi"in water bath for *-1 minutes
***".Test with Benedi$t so"ution:Add Benedi$t so"ution 61m"5 to the
Aueous so"ution of orani$ substan$e Red t is obser9ed #arbohydrate is resent6redu$in suuar5
I+". TEST /OR) ) )3* ,1 ,= 8 AMINES$
*& #arby"amine test:
To the $omound add few m" a fou" sme"" is obser9ed may be )* amine
+f $h"oro form and then add 1 m"
of a"$oho"i$ C+'; mi/ we"" and ent"y warmed&1 = 1 1
= = = Heat NH !OH CHCl NC !C" H O− + + → + +1& Aodye Test:
Ta!e 1 m" of $omound, add 1 m" orane red dye is formed resen$e of )*
amine
+f '#", $o"" in i$e, and then add1 m" of i$e $o"d *) A ?a?o1
so"ution& Add to it $o"d so"ution of )&> ms
of 1-?ahtho" in > m" of < ?a+' so"ution is added&
EXPERMENT NO.#@
Pre6)r)t*on o, A'6*r*n
AIM : To Preare Asirin from sa"i$y"i$ A$id
APPARATUS: #oni$a" f"as!, 7ater bath, bea!ers, "ass rod
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#'EMI#A(S: Sa"i$y"i$ a$id, a$eti$ anhydride, su"huri$ a$id, a"$oho"
PR+#EDURE:
*& Ta!e < m of sa"i$y"i$ a$id in a *)) m" $oni$a" f"as!& To this add about *) m" of a$eti$-
anhydride and *-1 m" of $on&'1So>&
1& 1Sha!e the $ontents to K))#, be$ause of e/othermi$ rea$tion& Maintain the tem at G)-
H)) for about *< minutes, !eein on a water bath&
=& A""ow the so"ution to $ome to room temerature and the our it in *)) m" $o"d water
ta!en in a <)) m" bea!er with stirrin 6water is added to destroy the e/$ess a$eti$
anhydride whi$h ets $on9erted to a$eti$ a$id&
>& To indu$e $rysta""iation s$rat$hes the sides of the f"as! with "ass rod&
<& .i"ter the so"id and wash it with $o"d water& Press it in between the fo"ds of fi"ter aer&
G& Sread the so"id on the fi"ter aer to dry
H& To obtain $o"or"ess $rysta"s, re$rysta""iation $an be done usin eua" 9o"umes of
ethano" and water so"9ent system&
RESU(T: - ie"d
Pre$autions:-* Ta!e a$eti$ anhydride in e/$ess as if a$ts as a$ety"atin aent as we"" as
So"9ent&
1& Ma!e sure that a"" the sa"i$y"i$ a$id is disso"9ed&
#'EMI#A( EUATI+?:
E76er*!ent No.##
INETICS$
To determine the rate $onstant of hydro"ysis of methy" a$etate $ata"ysed by an a$id a"so
the a$ti9ation enery&
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of a"!a"i reuired for titration is noted and is ta!en as @+& Simi"ar"y *) m" of rea$tion mi/ture
is ta!en out in su$$essi9e inter9a"s of time *), 1), =), >), <) minutes& To obtain $omute
hydro"ysis the rea$tion mi/ture !et in a water bath maintained at for about ha"f an hour&
After the hydro"ysis $om"eted and it is $oo"ed at room temerature and titrated the *) m" of
rea$tion mi/ture with ?a+' so"ution and is ta!en as @ ∞ &
Metho o, C)lcul)t*on$%
The initia" 9o"ume of titrate; ?a+' is @+ at T)) # is roorsona" to the amount of '#" resent
in the rea$tion mi/ture at ero time& 7hen there is an a$eti$ a$id resent as the hydro"ysis
ro$eeds )V V
∞ − dire$t"y roortiona" to initia" $on$entration of ester 6a5, at su$$essi9e
inter9a"s of time t V V ∞ − is roortiona" the $on$entration of esters at timetJ6a-/5&
*
1&K)=
*) O
t
V V
! g t V V
∞
∞
−= ÷−
*
K)C −
Same ro$edure and $a"$u"ation is reeated for 1? '#" so"ution&
Rel)t*e 'trenth o, two )c*' *' *en &;1
*
!
!
#a"$u"ation of A$ti9ation Enery:-
1 1 *
* 1
"o1&=)=
! % % Ea
! %
−= ×
× &
1 1
* 1 *
*) 1&=&= ! %
Ea g ! % %
= × × ×−
Resu"t:-Rate #onstant for hydro"ysis of methy" a$etate by *? '#" are 1 ! ------, 1
! = ----
A$ti9ation Enery Ea = -------------------
+bser9ation Tab"e:-
Tab"e-* Standardiation of ?a+':-
S"&?o@o" of +/a"i$ a$id
6@*M*5
Burette Readins @o" of ?a+' 6@15
@1 .-IInitia" .ina"
* 1)
1 1)
= 1)
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@o" of +/a"i$ a$id So"ution @* 1) m"
?orma"ity of +/a"i$ A$id ?* )&1 ?
@o" of ?a+' So"ution @1 ---- M*
?orma"ity of ?a+' ?1 -----?
?*@*?1@1 ⇒ * *
1
1 N V
N
V
= →
∴ ?orma"ity of ?a+' ?1 ----------------?
#a"$u"ations for determine rate $onstants
.or *? '$"
S"&?o Time 6t5
Minutes
@o" of
?a+'
6@t5
t V V α − )
t
V V
V V
α
α
−
−
)*)
t
V V g
V V
α
α
−
−
)
*
1&=)="o
t
V V !
t V V
α
α
−=
−
*
1
=
>
<
G
H
K
0
)
*)
1)
=)
>)
<)
G)
V α
A9erae C *
)V ml = − − NRAP':
V α = −− −
)V V ml α − = − − − −
.rom Nrah
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1 * LLLLLLLLLL
1 *
*
1&=)=
* 1&=)=
y ySlope
x x
! Slope
! Slope
−= =
−
=
⇒ = ×
.or 1? '#":
S"&?o Time 6t5
Minutes
@o" of
?a+'
6@t5
t V V α − )
t
V V
V V
α
α
−−
)*)t
V V g
V V
α
α
−−
)
1
1&=)="o
t
V V !
t V V
α
α
−=
−
*
1
=
><
G
H
K
0
)
*)
1)
=)>)
<)
G)
V α
A9erae C 1
)V ml = − − NRAP':
V α = −− −
)V V ml α − = − − − −
.rom Nrah 1
1
1 * LLLLLLLLLL
1 *
1&=)=
1&=)=
y ySlope
x x
! Slope
! Slope
−= =
−
=
⇒ = ×
EXPERIMENT %#0
AIM$ % Prearation of Thio!o" Rubber
O6er)tor': - Bea!ers, N"ass Rod, .unne", .i"ter Paer
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Che!*c)l'$ - Ethy"ene Di$h"oride, ?a1 S1 6Sodium P"oy Su"hide5
Proceure$ -
*& P"a$e about *) m"& of Ethy"ene di$h"oride so"ution in *)) m5& bea!er
1& Add about < r& of sodium o"ysu"hide and 'eated to form o"y su"hide rubber
6so"id5
=& 7ash the abo9e so"id with water and dry it in the fo"ds of fi"ter aer
>& #a"$u"ate the yie"d of the rodu$t
Re'ult:
The yie"d of Thio!o" Rubber is LLLLLLL r&
#'EMI#A( EUATI+?:
n#"-#'1-#'1-#" ?a1S1 Q Poly n → ----------3#'1 O #'1-S-S-8n
6Ethy"ene #h"oride5 6Sodium Po"y Su"hide5 6Po"y Su"hide Rubber 6or5 Thio!o"5