SIMPLE DISTILLATION Elaine Casao, Casao, Patricia Chong, Shoula Constantino, Raymond Corpuz and Irvin De Guzman Group 3 2J Pharmacy rganic Chemistry !a"oratory !a"oratory
ABSTRACT #his e$periment aimed to separate the alcohol and %ater e$istent %ithin a certain amount o& vod'a, and to determine the amount o& (thanol in the vod'a and the percentage loss o& (thanol that has occurred during the distillation process) #here are several types o& distillation, %hich %ould "e discussed later, ho%ever, this la"oratory report %ill &ocus more on the simple distillation o& vod'a) Simple distillation involves the principle o& relative volatility and "oiling points, %hich re*uire the su"stances to have a huge di&&erence in their "oiling points to "e separated) #he su"stances that has "een separated are (thanol and %ater in the vod'a sample) #he presence o& ethanol and %ater has "een indicated through a &lame test) #he ethanol %as present at the +st distillate up to the th and last distillate, ho%ever, the &lame on the +st distillate lasted longer than the th %hich simply means that the ethanol content on the th distillate %ere decreased) #he calculations &or the percent (thanol in the vod'a is ++)33- and the percentage loss is ./-)
INTRODUCTION Distil Distillat lation ion is the proces process s o& separ separat ating ing t%o or more more li*uid li*uids s %hich %hich have have large large relati relative ve volatility "et%een the t%o su"stances and a "ig di&&erence "et%een their "oiling points) 0o%ever, the more more di&&er di&&erent ent the su"stan su"stances ces are in their their volat volatili ility ty and "oiling "oiling points points,, the easier easier it is to separate the components in the mi$ture) #here t%o phases included in this procedure, one is the li*uid phase %hich resulted &rom th e condensation part, and the gas phase %hich is usually called the vapor that resulted &rom the evaporation part o& the method due to the "oiling o& the a*ueous solution) 12 #here #here are are severa severall types types o& distil distillat lation ion,, namely, namely, simple distillation, &ractional &ractional distillation, vacuu vacuum m distil distillat lation ion and the stem stem distil distillat lation ion)) Simple distillation has the simplest setup than the the latt latter er type types s o& dist distil illa lati tion on)) #his #his invo involv lves es separation o& a volatile li*uid and a nonvolatile li*uid that have a "ig di&&erence in their "oiling points) 4ractional distillation is almost the same to the &unction o& the simple distillation, ho%ever, it has has an addi additio tion n o& a &rac &racti tion onal al dist distil illa lati tion on column, %hich contains a su"stance occupying a high sur&ace area &or a more e&&icient separation o& the t%o or more li*uids in a mi$ture) 5acuum distillation is also similar to simple distillation in term terms s o& &unc &uncti tion on,, ho%e ho%ev ver the the su"s su"sta tanc nce e involved in the mi$ture tend to decompose %hen "oiled at high temperatures, hence a vacuum is put over the li*uid to prevent prevent the decomposi decomposition tion o& the su"sta su"stance nce in the proce process ss o& separ separat ation ion)) 6hile, steam distillation, on the other hand, is also similar to simple simple distillation distillation,, ho%ever ho%ever this involves involves su"stances su"stances that are slightly slightly solu"le solu"le in %ater %ater,, that that have have a tenden tendency cy to decomp decompose ose at high higher er temp temper erat atur ures es,, and and that that have have terr terri" i"le le "ump "umpin ing g %hen %hen used used in a vacu vacuum um dist distil illa lati tion on)) Since steam lets the su"stance "oil at a lo%er
temperature, steam is used instead o& a direct &lame &rom an alcohol lamp) 1+ #o understand more deeply %hat dist distil illa lati tion on is, is, ther there e is a need need to 'no% 'no% o& the the relationship o& Raoult7s !a% and Dalton7s !a% in the process o& distillation) 5apor pressure is the pressure o& the su"stance that e$erts an e&&ort agai agains nstt the the e$te e$tern rnal al pres pressu sure re %hic %hich h is the the atmospheri atmospheric c pressure pressure)) I& there is greater greater vapor vapor pres pressu sure re,, ther there e is grea greate terr tend tenden ency cy o& the the pressure to escape) 18 Raou Raoult lt7s 7s !a% !a% stat states es that that99 :#he :#he vapo vapour ur pressure o& a solution o& a nonvolatile solute is e*ual to the vapour pressure o& the pure solvent at that that temp temper era ature ture mult multip ipli lied ed "y its its mole mole &raction); &raction); 13 #his simply says that a component7s vapor pressure inside the mi$ture contri"utes to the entire vapor pressure o& the mi$ture that is in propo roport rtio ion n to its its perc percen enttage age to the the vapor por pressure o& the pure su"stance) 1 Dalton7s !a% %hich states that :the total vapor pressure is the sum o& the partial pressures o& each each indivi individua duall compon component ent in the mi$tur mi$ture; e; supp suppor orts ts Raou Raoult lt7s 7s la% la% "y de&i de&ini ning ng %hat %hat each each vapor pressure consists o& partial pressures o& the individual components and ho% the sum o& those vapo vaporr pres pressu sure res s are are e*ua e*uall to the the tota totall vapo vaporr pressure o& the entire mi$ture) 1
OBJECTIVES #he o"
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METHODOLOGY #he #he e$pe e$peri rime ment nt re*u re*uir ired ed a *uic *uic' '&it &it appa appara ratu tus, s, vod' vod'a, a, alco alcoho holl lamp lamp,, and and "oil "oilin ing g ston stones es)) Simp Simple le dist distil illa lati tion on %as the the 'ind 'ind o& distil distillat lation ion ass assign igned ed to the group) group) #his #his &orm &orm o& dist distil illa lati tion on sepa separa rate tes s comp compon onen ents ts thro throug ugh h a simple process o& evaporation and condensation) Simple Simple distil distillat lation ion is possi" possi"le le due to di&&er di&&erent ent "oilin "oiling g point point o& compon component ents s in a mi$tur mi$ture) e) #he #he &irst step in this e$periment re*uires preparation o& materials) #his involves la"eling and cali"rating test tu"es to /)m! that %ill "e used to receive the distillate) Simultaneously, 3 mem"ers o& the group care&ully prepared the setup) #his setup is prepared %ith the use o& t%o iron stands, one supports the condenser, and one holds the *uic' &it distil distillin ling g &las') &las') =nder =nder the *uic' *uic'& &it it distil distillin ling g &las' is the alcohol lamp, a"ove the &las' is a ther thermo mome mete terr and and on its its dist distal al port portio ion n is the the attachment o& the condenser) n the end o& the condenser most pro$imate to the distilling &las' is the the %ate %aterr outl outlet et,, %hil %hile e the the pro< pro&te >&terr the the prep prepar arat atio ion n o& the the set setup up,3 ,3 piec pieces es o& "oil "oilin ing g stones are introduced into the &las' that contains 3/ m! o& vod'a) #hen an alcohol lamp %as lit up and placed directly "elo% the distilling &las') #he lamp lamp re*uir re*uires es rotati rotation on in order order to contro controll the dist distri ri"u "uti tion on o& heat heat to the the set setup up)) It is also also important to record the temperature o& the &irst drop and so as every distillate received "y the /) m! cali"rated test tu"es)
#he content o& the +st test tu"e and the last test tu"e %as tested &or their &lamma"ility) oth o th prod produc uced ed &ire &ire,, mean meanin ing g the the dist distil illa late te collected &rom the &irst test tu"e and the last test tu"e contains ethanol) Figue &" T'e Si()le Dis#illa#ion Se#*U)
COMPUTATIONS 4or percent ethanol9 distillate
- ethanol
3.4
- ethanol Su"se*uent to the e$periment per&ormed) #est &or &lamma &lamma"il "ility ity %as %as e$ecut e$ecuted) ed) #his #his test test re*u e*uires ires a %atch atch gla glass, a sou source rce o& &la &lame ?match@, and the +stand last distillate) Placing 3 drops o& distillate &rom the +st test tu"e on a %atch %atch glass and the applica applicatio tion n o& &lame &lame to it &rom a lightened match did this procedure) #he previo previous us proces process s %as %as repeat repeated ed to the last last test test tu"e) #he presence o& &lame pertains that there is ethanol in the distillate)
RESULTS AND DISCUSSION 4ive distillate distillates s %ere collected collected throughou throughoutt the the e$pe e$peri rime ment nt)) 4igu 4igure re no)+ no)+ sho% sho%s s the the data data collected)
distillant
30
x 100
x 100
++)334or percent loss9
- loss
Vs −( Vf + +Vi ) x 100 Vs 30
- loss
−( 3.4 + 21 ) 30
x 100
+A)B.#he percentage loss sho%s the amount o&
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contr ontro ol, read eading ing o& tempe emperratur ture &rom rom the the thermomet thermometer er,, the attachment attachment or tuning tuning o& the instruments used that could have allo%ed proper removal o& vapor &rom the instrument) >llin all, the process o& distillation is an e&&ective %ay o& separating andEor puri&ies li*uid mi$ture)
REFERENCES 1+ Fu"ric', J) 6) ?+.@) Chapter Chapter 20:Distill 20:Distillation ation For Dummies Dummies (fromThe (fromThe Organic Chem Lab SurvivalManual !th "#$% Retrieved &rom https9EE%%%)ero%id)orgE https9EE%%%)ero%id)orgEarchiveErhod archiveErhodiumEchemist iumEchemist ryEe*uipmentEdistillation8dummies)html 12 Hu
13 http9EE%%%)chemguide)co) http9EE%%%)chemguide)co)u'EphysicalEp u'EphysicalEphasee*iaE hasee*iaE raoultnonvol)html
[4] Distillation ?n)d)@) Retrieved &rom http9EE%%%)umsl)eduEor http9EE%%%)umsl)eduEorgla"EdocumentsEdis gla"EdocumentsEdistilla tilla tionEdist)htm
[5] "'plain the #ifference in the usage of aoult)s La* an# Dalton) s La* SH Pusat andar andar Puchong Puchong + 4orm 4orm B ?n)d)@) Retrieved &rom http9EEsm'p"p+&ormB)%ordpress)comE2/+/E/3E+ .Ee$plainthedi&&erenceintheusage .Ee$plainthedi&&eren ceintheusageo&raou o&raoult lt -(2-A/-sla%anddal -(2-A/-sla%anddalton-(2-A/-s ton-(2-A/-s la%E
