METHODS OF PURIFICATION OF ORG ANIC CoMPOUNDS

APPLICATIDNS
ME THOD PRINCIPlE

Oystalltzatirn given oc CTuslalliynlion oy suqr (Nacl

aitevent soluubilies D} aagiven
a
impity ) is achicved by shakKing
nd it impuyitics in same solvent.
the impume solit with bot
ethanol at 34 8k
Sigon - solucble
Impuzity- iMoluuse
Iodire Pom Na CI
2 Stblimation Some solid suubstanes ehenqe from’ Camphor, naphthale, unthracer
oithout
Solid to vapDui state
Sublmabde benzoi c acid,et ne
pasig thpyh liqut state.
compouurds qet seperated from þuonitied
non- sublimahle impuitics.
31tistillntion Tt is Used to seprte ’ Hexanc (bp342K) , Toulene
volatle liquids fom non- volatile Cbp. 384k)
impuni ties -’ Chloro 7orm(bp. 334K) nd
tiquid hauing sujbicient aniline Cbp. s 57K)
di7bovence in their boiling poinl
II the iffevence in boiling -’ (rde oil in petroleum ënustr
iutillation point is 40k ’ methanol (65°C) and
Acetone (56°)
’ Fthanol+ H,o can't be
Scp<rated due to soimtion D7
azeotropic mixtre.

i Stem This method is ued to sepe vate ’ Anilinc is seperated from

distillalion Substances uhich ane anilix-oatex mixtre
) stem volattle ’Essential cik, tipentine ois,
t) /mmiseible ith water -nitiophenol, bromobenzene
i) poses vapoipre ssre O nitrobenzene etC., Can b
Io-15 mm Ok H poribied.
 20VAIOS03-3AA 10MOTIAJRISUS
METHO) PRINCIPLE APPLICATIONS.

iv Vaccum dulilation Liquid which deomposes at Glycenol decomposes at iu B

(o1) Unde-Yeduced it boilig poiot 0.e,2q0oc at bmm Dt Hq
Pvesstne distillatiorn

Oifevcotial By shaking n aq soln oy an oc Benzolc acid cUn be extra

exhacier
toith oqanic solvnt in ohi ch oc tiom its t0ater solution
soluble thmn oater. The
Wsirg benzene.
Nganic solvent , the aq soln should
be Ùnmi scble toith each other
o that they carn 7orm too
distinct lauers tuhich can be
Sepevtted by using sepertng
tunnel.
Chaomatoaphy itfeential movement o itdivictual Widely tsed tor sepration,
componenk oy a mixtve throgh puijcation, identiicatin
stationany phue nder the chavetty isation oy component
ingluence D7 a mobie phese Ck a mi xtuve ,whe ther
ccloLvred or colbuwless.

J Adsowplion ykential adsonption o vanios

Chvomad oq1aphy comporents D a mixtwe on a
SuLitable adsorbent such s
silita qel or alumina
a) Colwmn Th mixture s pruse over ’ Mixtune oj naphtthalene and
chrtoq1aphy atorbent packed in qlus tuhe benzophenone

The mixtire s pased Ovex ’ Amino acids Can be detected

b) Jhin lauer
adsorbent on a this gus plate by sprayung the plate with
chcmntogagny
ninhytiin sDlution.
 MITHOD PRINCIPLE APPLICATIONS.

biperenlial pvititioning ot
chvematogaphy Component ot a mixture
be tuocen Stationan and mcbile
phases
a: papen
chomttoqaphy A Special qualily paper ’Fo sepenaton D7 sugns
chromntogaphy and mino acics.
contauns

tnttr thapped in it ,ohich acts

stationany phse

TyPES OF CHROM ATOGRA PHY MDBILE|STATIONARY PHIASE

Column chromaloqinphy Liquid | solid
:,Thin laue1 chomatoqaphylTL) Liquid | solid
5. High pa homance liquid Liquid |solid
chromatogiaphy(tHPLC)
Gas lquid chiomttogaphy
Ponlition(en paper chrcmatoqvaphy Liqud |Liqud.

1) Reten licn fator (R!) Dstane thaeled b compoud tom hae line
Dstance trawelled by solvent from bue line
to be teuted jor purily
Afkr puoni7icaton,an cnic Ccmpamd eds
A plue tiqanic compound posesses charactv tic phyical propesties
Such as ref1ctue intex, speci7ic qiwily , boiling pont, crystalline shructune
and mtirg -point.
 lilw:nlory ony mlng point (fom tolldu) ei boiling tod
(io liquida) ae ued au ritria o, Dunity.
(for
The thucture deteminmtion and characterisction ol an oc ivolves the
tollacing steps:
I Detection of ckeni (aualitative Omlysu)
2 Estintion o elemne nt (Quantilaltur nalys)
3. Dotenuvton molkculai mass
Calclation o empixical and molkclar formulae.
Qualitative Analysis

DETECTION CONFIRMATORY TEST REACTIDNS

ETEMNI

(opper cxide test CO, qas turns lime Co,+ Ca(OH),-’ CacO,t Hy0
Canbon
tuatu milks Lin milky
unter

thydroqen
on coolex pant of White Bluue
iqnition tube ard
tuxrs anhyrow
Cusoy blue

Lassaigne's extract (LE) LE+ Fesoy +NaOH, FesOy t 2NAOH’ Fe(o), t Na,s
Nihogen
Na+(4 N NacN boil &cool t Fea, t Fe (DH), t NaCN Na, [FecN)
(LE) Conc. H t) Nao
Na s used in L¼ Gives blut or qreen Hl

Nais Reactve metas colouY

Na[Fe(cNJ+ Fedls
8NacI +Na Fe[Fe (cr
(or) (Prssian bluc
3Na4[Fe ((N)G]+ 4Felly
FeylFe (CN), 1,+12N
(prusian blt1e )
AME NI CONE IRMA1ORy TEST REACTIONS.

Sutph Na +s Na,s ) LE + Sodulm nitro )NO,S 4 Na,[Fe( CN;NO]

(LE) pvusside (Sodium niho prusiae)
Na,[Fe. cCN)5NDSJ2
Deep voilet
)LE + CH,COOH |t0 Na,s + (CHy (oo), Pb 1
+(CH,co0), Pb |CHg t0OH
pbst 2 CH, C0ONa
(Black ppt)
Nthcgen é; Na4CNNtS Blbod red colouation NasCN+ FeCly’[Fe (scN)JCI,
(Blood redcolbur)
Sulphuur NasCN(LE)| Confirs presene D&
t NacL
Soditun thiocyarnate N 5 both

Na, O Soluution is boiled wolth Na,P0t 3HNO,’ H;POs 3NaNo

hesphoariy P. boil A hitic aid é, then H,POy t 12 (NH) MoOy t 21HNO,
treated with
ammonium molubdat.
Amronium phosphomolybdate
Fomation o llo
ppt. indicates presene 2| NHåNO, t I) H0
D} phosphors
Na+ - Na(l LE HNO, tAgND, Nax + AqNOs Aq x
Haloqcn (LE) i) tuhite DDt solble in
HNO,
(Ppt)
The functioy of Bofl?
aq Ny tongirms CL
befoe tastghalogP ydlouo ppt pcutially tohite Soluble
ita destOyCN AS TonS (olublk in aq NHy ppt
NaCN +HNO;NagTtonsisBY Feansot be tectad bys
Nast HNONaNO,Tulelloo nnt inoluble.ugne test because

(n ONganic Compound can be detected indire luy

bu ksting thk Comppund contiining functicnal gyop guch
tuch sas - OH,
 Quantitaive Analysiu i
) VarioUs clement
belemination cy the onclalwe popontiors (au ) O
DNqanic compound is alled quantitative amysis.

EIEME NT METHHOD

Coibon and Liebiq's Combus tion Mettod

A knoun mass O n C s bnt in the presence ok
Hytogen
Cx Hy t
+Cao)
- CO, evolved is absorbed by conc.solh o KOH (o) ascante (NaOH
nhy. Cacl, (0) MCI O4))
H,0 produced is absovbed by
TIncease in mauies o these absorbing
compOLIds gi ves the
protuced
masses of co, ad H,O
mass o; Co, kormed
44 mass o compoLund
7 o H- 2 x mass O H,o Bor med
mass os compoun
i) Jumas methodi
Nihoqen Nihogen contauning organic compound is heated with Cuo in co, atmohad

N, evolved get colkected over conc. KOH soln which absorbs al qases.
N = 28 X
vol· ok N, at sTP x lDo | Vol·N, at $TP DV, *273
22400 msso (ompoL 160 xT|
P= tm ples -a
ii) Kjeldahlk method : 2NaoH,
tension
(NHu), SOy Na,soyt 2NH, t2 H,0
(Conc)
 METHIDD
kLEME NI
O)= ass Of Organic
(onlinuaticn: coup

I:4x molaoits o acid x vol: of acid sed xhasicity opacid

%o N:
mss D} Compoud taken
·4X nomalit o acid x Vol- O, atid sed (morohasic)
o} N
mass of compoud taken

Caniu Methodr
Haloqens
Haloqen in Dc is ppted as Silvenhalde by boiling toith
(onc. HNO, an then adding AqNO,
X Agx L
AgNOs
35.5 mass ob Aqcl 7oImed
I43.5 mass o} compound

kormed
80 x mas D AgBY * 100
168 mas O7 tompound

/% o} I mawso} AqI jormed

235 ms o compound

Canius Method i
Sulyhur Sulphn in 0c converted into H, sOu by boiling oth
Na, 0, o1) conc.HND u pptd as Basoy by adding
(xcess O7 BaCl, coln in t0at
i) HNO, A
Basoy
i) Bal tohite ppt
32 x MUS Of Ba O4 7ormned n 100.
233 mass D} compound
 LMENT METHOD

hosphous Jonitcn Metodi

HNO3
P
heat

H,Poy + Mq Ny() Mg NHy POy t HCI

nagne sium ammbnium
phosphate (white.ppt )

Mg, P, O1 4 2NH H,0

2Mq NHyPOy ’
aqnesium pyrophocphate.
6) mass o Mg, P, D? jomed x 100.
)22
mass Dt compod tken

Iodine Method
Orqanic tormpoxurd + Dther qaseos protucts
| 2C +0,
| I,05 + 5 ( 0 I ,+50, ]*2

10(@ + 50, + 2I, O5

mmis o (0, 7ormcd

88
mass of (ompound
taken

oo 5 l6 mass o I, 7ormed 100

mass oy compound
taken