example technique lab report

5/27/2018 Example Technique Lab Report

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Isolation of Eugenol from Cloves by Steam Distillation and its Identification by Infrared Spectroscopy

Eim A. ChemistCHEM 303

June 16, 2005

INTRODUCTION

Essential oils are the volatile comonents associate! "ith the aromas o# man$ lants.1%n this

e&eriment, the essential oil eu'enol (the main comonent o# oil o# cloves) "ill *e isolate! #rom 'roun!cloves usin' the techni+ue o# steam !istillation, "hich is o#ten use! to isolate li+ui! natural ro!ucts #rom

lants.2

he rincile o# steam !istillation is *ase! on the #act that t"o immisci*le li+ui!s "ill *oil at a lo"ertemerature than the *oilin' oints o# either ure comonent, *ecause the total vaor ressure o# the

hetero'eneous mi&ture is siml$ the sum o# the vaor ressures o# the in!ivi!ual comonents (i. e. - -o

A/

-o, "here -ois the vaor ressure o# the ure li+ui!s). his lea!s to a hi'her vaor ressure #or the mi&ture

than "oul! *e re!icte! #or a solution usin' aoults a" (that is - -oA4A/ -

o4, "here 4 is the mole

#raction o# the comonent in the mi&ture). he hi'her total vaor ressure lea!s to a lo"er *oilin' oint #or

the mi&ture than #or either sin'le comonent.2

urin' the isolation o# a li+ui! natural ro!uct *$ steam!istillation, "ater is one o# the comonents, an! the li+ui! natural ro!uct *ein' isolate! ("hich isimmisci*le "ith "ater) is the other comonent. he ro!uct can *e steam !istille! #rom the natural source at

a relativel$ lo" temerature (al"a$s less than 100 oC), thus avoi!in' !ecomosition o# the ro!uct.2

team !istillation can *e carrie! out in t"o "a$s7 the !irect metho! an! the live steam metho!.3%nthe !irect metho!, steam is 'enerate! *$ *oilin' a mi&ture o# the source o# the comoun! o# interest an!

"ater. he live steam metho! is carrie! out *$ assin' steam #rom an e&ternal source into the !istillation

#las8. he !irect metho! o# steam !istillation "ill *e use! in this e&eriment an! is carrie! out on a semi9

micro scale usin' the aaratus sho"n in :i'ure 1 *elo"7


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e! *$ transmission in#rare! sectrosco$ (%) as a neat samle usin' 4aCl lates5to con#irm itsstructure. his "ill *e !one in t"o "a$s7 (1) *$ loo8in' at the ma?or a*sortions in the sectrum an!

comarin' them to a correlation ta*le6an! (2) *$ comarin' the sectrum to that o# an authentic samle. he

ma?or % a*sortions are e&ecte! to *e 3200 @ 3500 cm91(H stretch), 3000 @ 3150 cm91(s2C9H stretch),1600 @ 16B0 cm91 (al8ene CC), an! 1;00 @ 1600 cm91(aromatic CC)6.

Table of C!emical Substances

ea'ent tructure=:ormula ole Mol. Dt. M ensit$

Cloves 999 ther 999 999 999 999

Meth$lene

chlori!e

CH2Cl2 olvent B;.3 9oC 3 @

;0 oC

1.32

'=m

o!ium

sul#ate

4a2; r$in'

a'ent

999 999 999 999

Eu'enol

C10H122

-ro!uct 16;.20 912to

910 oC

25; oC 1.06

'=m


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Safety Information

Compounds"

#aterial To$ic% Corrosive% Flammable% Carcinogenic%

Cloves 4o 4o 4o 4o

Meth$lene chlori!e 4o 4o 4o Fes

o!ium ul#ate 4o 4o 4o 4o

Eu'enol 4o 4o 4o 4o

Tec!ni&ues7

Dhen heatin' a reaction aaratus, *e sure that it is oen to the air so that ressure *uil! u an!su*se+uent ruture o# the aaratus !oes not occur.

Dhen heatin' li+ui!s, ma8e sure the li+ui! is stirre! (or a *oilin' chi is a!!e!) to revent*umin'.

Dhen er#ormin' an e&traction, ma8e sure to vent the centri#u'e tu*e o#ten to revent ressure *uil!9

u.

E'(ERI#ENT)*

he aaratus sho"n in :i'ure 1 "as assem*le! usin' a 259m roun! *ottom #las8 as the !istillation

ot. he !istillation ot "as char'e! "ith 1.032 ' o# 'roun! cloves an! 15 m o# !istille! "ater. he cloves

"ere allo"e! to soa8 in the "ater until thorou'hl$ "ette! (a*out 15 min), then the mi&ture "as !istille!, the!istillate *ein' collecte! at the rate o# a*out one !ro ever$ 2 @ 3 secon!s. A#ter a*out 6 m o# !istillate

"ere collecte!, the !istillate "as e&tracte! "ith 2.0 m o# CH2Cl2(a8a CM), then a'ain "ith (2 & 1.0 m)

o# CM. he CM e&tracts "ere com*ine!, !rie! over 4a2;, an! evaorate! to 'ive the ro!uct eu'enol


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%n a!!ition, the % o# the ro!uct #rom the steam !istillation o# cloves closel$ correson!s "ith that o#

an authentic samle o# eu'enol sho"n in the la* te&t.Bhere#ore, it can *e conclu!e! that the oil "hich "as

isolate! #rom cloves is in #act, eu'enol.0.00 ' o# eu'enol "as recovere! #rom 1.032 ' o# cloves. his correson!s to a ercent recover$ o#

.;6G7

Amt. Eu'enol isolate! 0.00 'G ecover$ 999999999999999999999999999999 99999999999999 & 100 .;6G

Amt. Cloves use! 1.032 '

Althou'h the G recover$ seems ver$ lo", the e&eriment rocee!e! as lanne!. here "ere no sills

or other a*normal h$sical losses. %t is ossi*le that the ratio o# the si>e o# the 'lass"are to the theoreticalamount o# eu'enol "hich can *e o*taine! #rom cloves in this e&eriment is lar'e, lea!in' to a!herence o# a

lar'e ercenta'e o# the ro!uct on the si!es o# the 'lass aaratus. %# this is so, then steam !istillation o# alar'er samle o# cloves shoul! 'ive an imrove! recover$. ther"ise, it can *e conclu!e! that cloves

contain aro&imatel$ .5G eu'enol.

SU##)R, )ND CONC*USIONS

%n this e&eriment, it "as sho"n that a*out .5G o# an oil coul! *e recovere! #rom cloves *$ steam!istillation. his oil "as i!enti#ie! as eu'enol *$ comarison o# its in#rare! sectrum "ith an authenticsamle.

REFERENCES

1. -avia, . . amman, ,


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)NS-ERS TO .UESTIONS

1. Dh$ is eu'enol steam9!istille! rather than uri#ie! *$ simle !istillation

Eu'enol has a hi'h *oilin' oint (25; oC), an! man$ or'anic comoun!s !ecomose at such

hi'h temeratures. team !istillation allo"s eu'enol to *e !istille! at a much lo"er *oilin'oint (K 100 oC), thus minimi>in' the otential #or !ecomosition.

2. %n a steam !istillation, the amount o# "ater actuall$ !istille! is usuall$ 'reater than the amount calculate!,assumin' that *oth "ater an! or'anic su*stance e&ert the same vaor ressure "hen the$ are mi&e! than

the$ e&ert "hen each is ure. Dh$ !oes one recover more "ater in the steam !istillation than "ascalculate! (Hint7 Are the or'anic comoun! an! "ater trul$ immisci*le)

%n most cases, or'anic su*stances have some solu*ilit$ in "ater. %# this is true, then the

amount o# "ater "hich is re+uire! to steam !istill the su*stance in its entiret$ is the calculate!

amount lus an amount nee!e! to !istill over the amount o# su*stance !issolve! in "ater.


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ero!uce! #rom the ectral ata*ase #or r'anic Comoun!s (). """.aist.'o.?=%==c'i9*in=creLin!e&.c'i(accesse! Ma$, 2006)
http://www.aist.go.jp/RIODB/SDBS/cgi-bin/cre_index.cgihttp://www.aist.go.jp/RIODB/SDBS/cgi-bin/cre_index.cgihttp://www.aist.go.jp/RIODB/SDBS/cgi-bin/cre_index.cgi

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