Experiment 2 Lab Report

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ADAMSON UNIVERSITY

College of Engineering

Chemical Engineering Department

M a n i l a M a n i l a

Experiment no. 2 Experiment no. 2

STEAM

STEAM DISTILLATDISTILLATIONION

S!mitte" !#$ S!mitte" !#$

Lavilles, Francis Dominic Lavilles, Francis Dominic

Lee Gee Hyun Lee Gee Hyun Lojica, Kathlyn Joyce M. Lojica, Kathlyn Joyce M.

Date performe"$

Date performe"$ July 18, 201 July 18, 201

Date %!mitte"$

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A&STRACT$

Steam distillation is an important method of separating immiscible liquids. This experiment aims to observe a steam distillation process. In order to observe the steam distillation process, toluene-water system was used in the study. A simple steam distillation set up was used in the experiment. The distillation was made and the temperature was recorded when the total volume of the distillate in the receiver has reached certain corresponding amounts. The results showed that as the temperature increases, the pressure also increases for toluene, water and mixture. The value of the pressure for the mixture was between the values of the pressure of toluene and water. The pressure versus temperature or toluene water and the mixture was plotted. ear accurate

results of the temperature at each volume of the distillate was obtained. The steam distillation process was observed comprehensively in this experiment.

INTRODUCTION$

"mmisci#le li$ui%s are li$ui%s that %o not mi& to 'ive a sin'le (hase. )hen t*o immisci#le li$ui%s are #oile%, they *ill #oil at tem(erature lo*er than the #oilin' (oint o+ either o+ the (ure li$ui%s. team %istillation is a use+ul (rocess o+ se(aratin' immisci#le li$ui%s. "n this (rocess, a li$ui% *hich is immisci#le *ith *ater is %istille% usin' steam.

team %istillation *or-s on the (rinci(le that in a mi&ture, there is a (oint *here t*o li$ui%s #ecome immisci#le. "n this mi&ture system, the total va(or (ressure %eviates +rom aoult/s La* (re%iction. %%in' the va(or (ressure o+ t*o li$ui%s com(risin' the #inary mi&ture system *ill result to va(or (ressure o+ the system. he mole +raction o+

each li$ui% in the #inary system *ill not a++ect the va(or (ressure. lso at the #oilin' (oint o+ the mi&ture, %ivi%in' the (artial (ressures o+ the com(oun% in the va(or *ill

result to the ratio o+ the va(or (ressures o+ the (ure li$ui%s. "n this e&(eriment, steam %istillation o+ the toluene  *ater system *as %one. he stu%y aims to e&amine the steam %istillation (rocess o+ the toluene  *ater system.

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pA ° pB ° ' pA pB ' NAP NBP ' NA NB ' nA nB ' wAMB wBMA 33 wA wB ' MApA ° MBpB°

REVIE( O) RELATED LITERATURE$

u#stances *ith %i++erent volatilities can #e se(arate% #y %istillation. he (rocess o+ %istillation *as +irst %evelo(e% #y Ja#ir i#n Hayyan. "n mo%ern times, %istillations are *i%ely a((lie% in la#ortory scale, in%ustial %istillaton, %istillation o+ her#s +or (er+umery an% me%icinals, an% +oo% (rocessin'. team %istillation is use% +or com(oun%s that are heat sensitive. team is #u##le% throu'h a heate% mi&ture o+ the ra* material. he va(ori4ation o+ the tar'et su#stance can #e %escri#e% #y usin' aoult/s La*.

team %istillation has many a((lications. "n a recent stu%y, steam %istillation is use% to o#tain laurel e&tract 56e-ovic, et. al.7. "n another stu%y, the steam %istillation o+ essential oils +rom Lemon Grass *as e&amine% 5mena'ha*on, 2017. team %istillation o+ essential oils *as also investi'ate% in other stu%ies 5Mulvaney, et. al.7. nother stu%y (ro#e the e&traction o+ essential oil +rom 9innamon 59innamomum 4eylanicum7. he

in+luence on the $uality o+ essential lemon oil #y %istillation (rocess is %etermine% #y a recent stu%y 5Gamarra, et. al.7

here are also a%vance *ays o+ (er+ormin' the %istillation o+ mi&tures li-e #en4ene an% toluene.5:hiyanalinmat, 2017. ome a%vance metho%s use al'orithms to

%etermine the o(timum re+lu& ratio 5#ol(our an% Mohe##i, 2017

"n mi&tures that involve more than t*o com(onents, more com(licate% (rocesses are nee%e% in %etection an% se(aration o+ su#stances.  com(le& sam(le o+ #en4ene, toluene, ethyl#en4ene an% &ylene re$uires a hy#ri% se(aration an% %etection %evice +or analysis as e&amine% in recent researches 5"'lesias et. al. , 200;7. )hen #en4ene an% toulene mi& *ith other como(un% li-e &ylene, the concentrations are %termine% usin' a%vance (rocess such as Hi'h :er+ormance Li$ui% 9hromato'ra(hy<= %etection 5H:L9<=7 5>ahrami, et. al.7

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:rocess simulation has #een a((lie% in a recent stu%y to %esi'n the #en4enetoluene %istillation 5:hiyanalinmat, 2017. nother stu%y (resente% mo%elin' an% simulation o+ a #en4ene recovery (rocess #y e&tractive %istillation 5>ron%ani, et. al., 2017

MET*ODOLO+Y$

 steam %istillation setu( *as (re(are%. ?i'hty milliliters o+ toluene *as (lace% in the roun% #ottom +las- an% *ater *as +ille% in the %istillin' +las- u( to hal+ o+ the +las-. he %istillin' +las- *as heate% until the *ater #oile%. )hen it starte% to #oil, the +lame has #een lo*ere% just enou'h to continue the #oilin'. he +irst %istillate 52@mL7 *as %is(ose%. he tem(erature *as recor%e% an% the receiver *as (lace% #ac- un%er the a%a(ter. he %istillation an% recor%in' o+ tem(erature *as continue% until the %istillate in the receiver *as 2.ml, ml, !.ml, 10ml, 12.ml, 1ml, 1!.ml, 20ml, 22.ml, 2ml. Distillation *as sto((e% *hen the collecte% %istillate ha% reache% 2ml. he %istillates *ere coole% an% *ere le+t to se(arate +ully. ?ach o+ the %istillate *ere trans+erre% in the 'ra%uate% cylin%er to measure the volume o+ *ater an% toluene. he %ata +or va(or (ressure o+ toluene an% *ater in %i++erent tem(eratures 50c,0c,A0c,!0c,80c,;0c7 *as

o#taine% +rom the han%#oo-. he va(or (ressures o+ the mi&ture at those tem(eratures are com(ute%. he va(or (ressures o+ toluene*ater an% the mi&ture *as (lotte%. he theoretical #oilin' (oint o+ the mi&ture *as %etermine% +rom the (lot. he theoretical com(osition o+ the %istillate *as also o#taine% +rom the (lot.

RESULTS AND DISCUSSION$

he (ressure v.s tem(erature 'ra(h o+ toluene an% *ater mi&ture *as ma%e a+ter a((lyin' aoult/s La* to the mi&ture. s the tem(erature increases, the (ressure also increases +or toluene, *ater an% mi&ture. he values o+ the (ressure +or the mi&ture *ere #et*een the values o+ the (ressure o+ toluene an% *ater.

he use o+ steam %istillation in e&tractin' inor'anic li$ui%s has many a%vanta'es. "n the steam %istillation (rocess, the *ater va(or trans+er small amounts o+ the va(ori4e%

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su#stance to the con%ensation +las- *here the se(aration o+ con%ense% li$ui%s occurs. his allo*s easy collection. Bormal %istillation o+ inor'anic li$ui%s *ill re$uire hi'h tem(erature. ome o+ these molecules *ill #e #ro-en u( #y heatin' at hi'h tem(erature. <sin' steam %istillation avoi%s this #ecause the re$uire% tem(erature is lo*.

"t is not (ossi#le to carry out steam %istillation at 100 c #ecause the #oilin' (oint o+ the *ater is 100 %e'ree celcius so the *ater *ill #oil i+ the tem(erature e&cee%s 100 %e'ree celcius. "n steam %istillation, the (ressure o+ the t*o com(onents must a%% u( to 1atm.

a#le 1C em(erature an% va(our (ressure o+ *ater, toluene, an% the mi&ture. em(erature 5 ℃ 7 =a(or :ressure o+

oluene

=a(or :ressure o+ :ressure

=a(or :ressure o+ Mi&ture 0 ;.1A .@@ .8; 0 ;2.11 ;2.8 ;2.1 A0 1@8.;A 1;. 1!.;2 !0 20@.! 2@@.8; 22;.1 80 2;1.22 @.!8 @A.0 ;0 0A.! 2!.2 0;.8;

a#le 2C =olume an% #oilin' (oint o+ Distillate

=olume 5ml7 2.  !. 10 12. 1 1!. 20 22. 2

em(erature 5 ℃ 7

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a#le @C =olume, mole +raction an% volume (ercent o+ the mi&ture =olume o+ Mi&ture =olume o+ *ater =olume o+ oluene Mole o+ H2 Mole o+ toluene 2. 0.2 2.8 0.011 0.001;  0.8 .2 0.0 0.00!A !. 1. A 0.08@ 0.01 10 1.8 8.2 0.1 0.01! 12. @.8 11.2 0.21 0.0@A 1 .A ;. 0.@1 0.0@ 1!. 10 !. 0.A 0.0; 20 1!. 2.A 0.;! 0.1A 22. 22. 0 1.2 0.2 2     =olume o+ Mi&ture Mole +raction o+ H2 Mole +raction o+ oluene =olume E + H2 =olume E + oluene 2. 0.8 0.1 8 ;2  0.8 0.1 1A 8 !. 0.8 0.1 20 80 10 0.8 0.1 18 82 12. 0.8 0.1 2.@@ !.A! 1 0.8 0.1 @!.@@ A2.A! 1!. 0.8 0.1 !.1 2.8A 20 0.8 0.1 8! 1@ 22. 0.8 0.1 100 0 2    

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30 40 50 60 70 80 90 100 0 100 200 300 400 500 600

P vs T graph

toluene water mixture Temperature pressure

Fi'.1 :ressure v.s. em(erature o+ oluene, )ater an% Mi&ture

CONCLUSIONS AND RECOMMENDATION$

"n the con%uct o+ e&(eriment, the (rocess o+ steam %istillation *as o#serve%. he steam %istillation o+ the #inary system o+ toluene an% *ater *as e&amine%.  (lot o+ (ressure versus tem(erature +or toluene, *ater an% the mi&ture *as ma%e an% *as

stu%ie%.

he researchers recommen%e% that care+ul measures must #e ta-en so that there *ill #e no lea-a'e %urin' the %istillation (rocess. his must #e %one in or%er to 'et #etter

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RE)ERENCES$

1. 6e-ovic 6.:., Le(ojevic 6.D., Mujic ".., 200;, Laurel ?&tracts #taine% #y team Distillation, u(ercritical Flui% an% olvent ?&traction. Journal o+ Batural :ro%ucts. =ol. 2, (( 1010;

2. mena'ha*on B.., -huelei'#e K.?., '#ei%e .?., an% -ieimen 9.. 201. Mo%ellin' the Kinetics o+ team Distillation o+ ?ssential ils +rom Lemon Grass 59ym#o(o'on ((.7"nternational Journal o+ ((lie% cience an% ?n'ineerin' 201. 12,2C (( 10!11

@. "'lesias .., so*F ., )an' ., For4ani ?.., ao B,. 200; Hy#ri% e(aration an% Detection Device +or nalysis o+ >en4ene, oluene, ?thyl#en4ene, an% ylenes in 9om(le& am(les. Journal o+ nalytical 9hemistry, 200;, 81 5217, (( 8;@08;@

. #ol(our >., Mohe##i ,. 201. (timi4ation o+ the re+lu& ratio o+ #en4enetoluene sta'e %istillation columns #y the 9uc-oo al'orithm. :etroleum cience, 201, =ol. 11, "ssue @, (( A@

. Mulvaney J., 2012. ?ssential ils an% team Distillation. Journal o+ the Be* 6ealan% ssociation o+ Me%ical Her#alists 2012

A. )on' .9., hma%Mu%4a$$ir M.., an% )annur%iyana ).., 201. ?&traction o+ ?ssential il +rom 9innamon 59innamon 4eylanicum7. riental Journal o+ 9hemistry, 201, =ol. @0, Bo. 1

!. Gamarra F.M.9, a-ana-a L.., am#our'i ?.>., 9a#ral F.., 200A. "n+luence on the Iuality o+ ?ssential Lemon 59itrus auranti+olia7 oil #y Distillation :rocess. >ra4ilian Journal o+ 9hemical ?n'ineerin', 200A, =ol @2, Bo. 01, (( 28@2;1

8. >ahrami ., Mahju# H., a%e'hian M., Gol#a#aei F., 2011. Determination o+ >en4ene, oluene an% ylene 5>7 9oncentrations in ir <sin' H:L9 Develo(e% Metho% 9om(are% to Gas 9hromato'ra(hy."nternational Journal o+ ccu(ational Hy'iene 2011 ;. :hiyanalinmat ., 201. Desi'n o+ >en4eneoluene Distillation +or the Minimum ?ner'y 9onsum(tion #y 9hemical :rocess imulation. De(artment o+ "nustrial

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9hemistry, Faculty o+ cience, hailan%. 1!th e'ional ym(osium on chemical ?n'ieerin'.

10. >ron%ani L.>., Flores G.>., oares .:., 201. Mo%elin' an% imulation o+ a >en4ene ecovery :rocess #y ?&tractive Distillation. >ra4ilian Journal o+ 9hemical ?n'ineerin', 201, =ol. @2, Bo. 01, ((. 28@  2;1

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=a(or :ressure +or oluene log₁₀

(

P_mmHg

)

=6.95464− 1344.8

40℃₊_219.482

P_mmHg

=

59.16 mmHg

=a(or :ressure +or )ater

log₁₀

(

P_mmHg

)

=

6.95464

−

1750.286 40℃

+

₂₃₅

P_mmHg

=

59.16 mmHg

=a(or :ressure +or Mi&ture

0.8547

(

55.33 mmHg

)+

0.1453

(

59.16 mmHg

)=

55.89mmHg Mole o+ )ater 0.2_ml

(

1 g ml

)

18 g mol

=

0.011_mole Mole o+ oluene 0.2ml

(

0.87 g ml

)

92.14 g mol

=

0.0019mole

Mole +raction o+ *ater 0.011mole

0.011mole

+

0.0019 mole

=

0.85

Mole +raction o+ oluene 0.0019 mole

0.011mole

+

0.0019 mole

=

0.15 =olume :ercenta'e o+ )ater

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0.2

+

2.3 x 100

=

8.00

=olume :ercenta'e o+ oluene 2.3