Engg Chemistry JWFILES

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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&



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



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 %%&



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



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

=

>

<



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



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



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)



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 -?



@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

+

= −∩



)

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



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



$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



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



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&



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&



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



#'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&



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)



@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



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



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

Engg Chemistry JWFILES

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