Chemistry Lab report

1

1.1

INTRODUCTION

 The  The met hods hods For For t he det ect i on of t he f unct unct i onal onal

gr oup oup

i n an or gani c compoun ounds i nvol vol ve char char act er i st i c che chemi cal cal r eact i ons.

Dur i ng t he past

avai l abl e tha that

gr oup oups.

Most

t ype ypes of of s pect r oscopy, scopy,

I R spect r oscopy, oscopy, spe sp ect r oscopy. scopy.

are sti l l

1.1.1 1.1. 1 (1) (1 )

of t hem make use of som s ome or e. g.

UV and vi si bl e spect spect r oscopy, scopy,

nucl ear ear magn agnet i c sp s pect r oscopy an and mass

Al l

t hese i nst r ument ent s ar e expen xpensi si ve and r equi r e

con consi der abl e t i me and ski ski l l che chemi cal cal

i nst r ument ent s ar e made

pr ovi de con consi der abl e i nf or mat i on rega regar di ng

many any f unct unct i onal onal ot her

f ew year s,

f or

the thei r

op oper at i on.

Ther ef or e, 1

met hods f or i dent ent i f i cat i on of t he or gani c compoun ounds popul ar .

General Gener al test for amin amines es Tetraphenyl Tetra phenyl borate test

Ami nes t hat hat have a pKa pKa of 11 or l ess may be be det ect ec t ed by t he f or mat i on of wh whi t e pr eci pi t at es wi t h t et r aphenyl bor at e sol sol ut i on.

(2) (2 )

Copper Copp er ion test

2

Wat er sol ubl ubl e l ow mol ecul ar wei ght ami nes nes s uch as ami no al cohol cohol s, sol sol ut i on.

may be det det ect ed by 10 10% w/ v cop copper per

For For mat i on of bl bl ue or bl bl ui sh sh-- gr een col col or at i on or

pr eci pi t at es wi t h t he r eagent ami ne.

sul phat phat e

i ndi cat cat es t he pr esence sence of of an

2

(3)

Fluorescein chloride test^

When ami ne sal t i s f used wi t h f l uor escei n chl or i de at 230- 260° i n pr esence of anhydr ous zi nc chl or i de, sol ubl e r ed r hodami ne dye i s f or med. some N- ar yl

(4)

ami des i nt er f er

A

Quinhydrone test ’

wat er

Hydr azo compounds and

i n t he t est .

5

Qui nhydr one has been f ound t o be an excel l ent f or t he det ect i on of cer t ai n ami nes.

r eagent

Qui nhydr one r eact s

wi t h al i phat i c and ar yl ami ne i n aqueous or i n et hanol i c medi um t o gi ve di f f er ent ami ne i . e.

pr i mar y,

col or s dependi ng upon t he nat ur e of

secondar y or t er t i ar y ami ne.

Ni t r o-

subst i t ut ed ami nes can not be det ect ed by t he r eagent .

(3)

N-Halosuccinimide test**

N- Br omosucci ni mi de and N- i odosucci ni mi de ar e good det ect i ng and di f f er ent i at i ng r eagent s f or ami nes.

Pr i mar y

and t er t i ar y ami nes r eact wi t h N- i odosucci ni mi de t o gi ve br own col or t hat does not f ade on heat i ng. pr oduce br own col or f ew mi nut es.

t hat

Hinsberg test

 Thi s t est

f ade t o yel l ow or col or l ess wi t hi n

Ter t i ar y ami nes gi ve an or ange pr eci pi t at es

wi t h N- br omosucci ni mi de.

(6)

Secondar y ami nes

)

y

i s based on t he f act t hat pr i mar y and

secondar y ami nes r eact wi t h benzenesui r ony i   nal i de to

3

f or m N- subst i t ut ed sul phonami des, wher eas t er t i ar y ami nes do not r eact wi t h t he r eagent .

Fur t her t he sul f onami des

of pr i mar y ami nes ar e sol ubl e i n al kal i ne sol ut i on and may be di f f er ent i at ed f r om t he sul f onami de of secondar y ami nes whi ch ar e i nsol ubl e i n al kal i .

(7)

Diazonium salt test

Host

of t he ar yl ami nes and phenol s under go coupl i ng

r eact i ons wi t h di azoni um sal t s to f or m col or ed azo compounds. Al kyl ami ne gi ves l ess i nt ense yel l ow col or 4- Ni t r obenzenedi azoni um f l uor obor at e

g

t han ar yl

i s t he most

ami nes.

sat i sf act or y

r eagent out of var i ous di azoni um sal t s empl oyed f or t he t est . I t does not

r eact wi t h bot h or t ho and par a posi t i ons subst i 

t ut ed ami nes.

(8)

Lignin test

Webst er

9

has pr oposed a ver y si mpl e t est

and secondar y ar yl ami nes. l i gni n i n newspr i nt appl i ed on newspr i nt aci d.

paper . paper

The t est

f or pr i mar y

depends on t he act i on of

Et hanol i c sol ut i on of

ami nes

and t r eat ed wi t h 6N hydr ochl or i c

Pr i mar y and secondar y ar yl ami ne pr oduce i mmedi at el y

yel l ow or or ange col or ,

whi l e al kyl

and al i cyl i c ami nes

r equi r e heat i ng of t he sol ut i on f or col or

devel opment .

4

(9)

Miscellaneous

Primary to

produce 10

 b e n z e n e

a nd

secondary

bl ue , test

red

is

or

ary lamines

brown

also

used

of

primary

 W a t e r

aliphatic,

soluble

P r i ma r y

isocya nide s o d iu m

test

and

other

S e c o n d ar y  A c o n i t i c

f or

aroma tic

Hantzsc h

and

for

is

detected

the

reac tion

with

13 14

amines.

the

detection

a m i ne s .

by

Rimini

test.

’

citric

dia zot ization, glutaconi c

alde hyde

rev eals

Therefor e, th e

wi t h

nic kledithiocarbamate.

acid-acetic

anhydride

1B

that

primary it

was

detec tion

there

is

no

ali phati c desirable of

the

spe cif ic as

to

well fi n d

 g on

1

’

, the

acetylace tone-fo rmaldeh yde

pri ma ry

r e a g e nt

to

as out

prim ary

amino

amin es

react

produce

1  f\ 

tests

compounds.

r e a c t i o n,

12

15

amines.

of

2

, 5-nitr oso-B-h ydroxyq uinolin e ,

detected

and

chloranil

of

heteroc yclic

by

tertia ry

for

employed

detected

detecti on

reagen t

containing

In w i th

th e

17

is

surve y

a mi n e s .

general

group

for

Lit era tu re

reagent

a

by

detection

are

reagents.

a m i ne

anhydride

perf orme d

,

amines , or

is

with

2 , 4 - D m i t r o f l u o r o-

the

alkylamine

pentacyano aquofer rate

furfural

are

2

for

aromatic

primary

a r o ma t i c

c ol o r .

11

 p - D i m e t h y l a m i n o b e n z a l d e h y d e

react

yellow

c ol or ed N- s ubs t i t ut ed- 3, 5- di ac et y1- 1, 4- di hydr ol ut i di ne i n

,

5

a qu eo us

s o l ut i o n.

a pp l i c a t i o n of

T he r e f o r e ,

wa s

t h e r e ac t i o n t o d e t e c t

I n t he p r e s e nt

wo r k ,

t he

r e a c t i o n a r e mo d i f i e d s u i t a b l y d e t e c t i o n of

it

t h ou gh t

t o e x t e nd t h e

a mi n e s .

r e a c t i o n c o n di t i o ns t o e s t a bl i s h

t h e p r i ma r y a mi n e i n a q u e o u s

a t es t

me d i u m.

of

Ha n t z s c h

f or

t he

6

1. 2

EXPERI MENTAL

2. 3. 2

Appar at us

1.

Corni ng

volum etri c

2.

Corning

3.

Borosil

4.

Sy str oni c

5.

Double

25,50

gradua ted

pipette

2,5

measuri ng

cylinder

pH

beam

 m a t c h e d 6.

flask

and

25,50

100ml 10ml

and

capacity.

capacity.

100ml

capacity.

meter. Backman

cell

Constant

and

of

Model-25

1cm

light

tempera ture

spec trophotom eter

having

path.

water

bath

(Townson

and

Mercer

L t d. ,

En gl an d).

1. 2. 2

Reagent

andMat er i al s

Sulphanilanide hydrochloride

B .P . ,

 M o n o e t h a n o l a m i n e ( SD 's ) ,

Thiamine

p-Aminobenzoic

p-Toludine

I.P.,

Isomazid

hydrochloride

I .P .,

Sodium

I .P .,

( S D' s ),

I .P .,

hydrochloride

Ethylenediamine

I .P .,

Cyst inehydroc hloride ( SD 's ), ( Su n

Glutamic

Pharma),

I. P. ,

acid

Sodium

acetate

(anhydrous

double

d isti lled

water

U . S .P . ,

Aminophylline sulphate

L-Asparagine ( SD ' s) ,

( B DH ) , used

(BDH),

Nor-Valine acid 

Formal deh yde

Acetic

acid

in

st u d y.

the

I .P .,

( M e r ck ) ,

5 -Aminosalicylic

(SD's),

were

L-Lysine

Calcium pentothanete

L-Leucine

Acet yla cet one

I .P .,

( S D' s ),

I . P. ,

I .P .,

a c i d 

Glycine

(SD's),

( S D 's ) ,

Procaine

Anthranilic

sulphate

( S D' s ),

Dihyd ralazine

l-Alanin

I .P .,

«