CHM142L Lab Report 3

V

Voolulumme Ne Noo. 5. 5 IIssssue ue NoNo. 3. 3 Date of Submission: N/A Date of Submission: N/A

Date of Acceptance: November 13, 215 Date of Acceptance: November 13, 215

Anal!sis an" #urification of $ompoun"s %sin& Different

Anal!sis an" #urification of $ompoun"s %sin& Different

Distillation 'et(o"s ) Simple an" Steam

Distillation 'et(o"s ) Simple an" Steam

Macatantan, Sedfrey L.

Macatantan, Sedfrey L.11_{;; Gaviño, Patricia Anne L.; Lat, Dheya O.; Manalo, Jayvee Bien D.; Dr. De Catro! Cr"#,Gaviño, Patricia Anne L.; Lat, Dheya O.; Manalo, Jayvee Bien D.; Dr. De Catro! Cr"#,}

$athlia A. $athlia A.%%

 Mapua Institute

 Mapua Institute of Tof Technologyechnology, Muralla S, Muralla Street, treet, IntramuroIntramuros, Manila, Ms, Manila, Metro Manietro Manila, Philippinela, Philippiness

A*S+A$+

A*S+A$+

&

&olaolatility i the tendency of tility i the tendency of a "'tance to va(ori#e. )t a "'tance to va(ori#e. )t i directly related to a i directly related to a "'tance* va(or (re"re. At a +iven"'tance* va(or (re"re. At a +iven te(erat"re, a "'tance -ith hi+her va(or (re"re va(ori#e ore readily than a "'tance -ith a lo-er va(or. te(erat"re, a "'tance -ith hi+her va(or (re"re va(ori#e ore readily than a "'tance -ith a lo-er va(or. actor that can affect volatility are -ei+ht and interolec"lar force of attraction. S"'tance -ith heavier -ei+ht actor that can affect volatility are -ei+ht and interolec"lar force of attraction. S"'tance -ith heavier -ei+ht and tron+er interolec"lar force of attraction tend to 'e le volatile a

and tron+er interolec"lar force of attraction tend to 'e le volatile a ore ener+y -ill 'e needed to ore ener+y -ill 'e needed to 'rea/ the'rea/ the do-n. Si(le and tea ditillation are t-o ethod "ed in thi e0(erient. Si(le ditillation i 'et "ed -hen do-n. Si(le and tea ditillation are t-o ethod "ed in thi e0(erient. Si(le ditillation i 'et "ed -hen "'tance to 'e e(arated have hi+h volatility difference. hen a co(o"nd only e0ert little va(or (re"re, "'tance to 'e e(arated have hi+h volatility difference. hen a co(o"nd only e0ert little va(or (re"re, tea ditillation i "ed, a it -o"ld re2"ire the aitance of -ater o that le (re"re -o"ld 'e in the a(le tea ditillation i "ed, a it -o"ld re2"ire the aitance of -ater o that le (re"re -o"ld 'e in the a(le container and only a lo-er te(erat"re -ill 'e re2"ired -hich can

container and only a lo-er te(erat"re -ill 'e re2"ired -hich can (revent deco(oition of (rod"ct.(revent deco(oition of (rod"ct. $ey-ord 3

1. IN+-D%$+I-N

)n or+anic cheitry, volatility of  co(o"nd i an i(ortant thin+ to 'e conidered and noted a -e are already dealin+ -ith all ort of  different co(o"nd that are 'ein+ t"died and  (roce and the idea of volatility contri'"te +reatly in the co(arion and handlin+ of the co(o"nd. irt, -e need to /no-, -hat i volatility: 8o a/e it i(le, volatility refer to the tendency of a ("re "'tance to +o into the va(or (hae. )t can alo 'e  (erceived a ho- "ch a certain "'tance -ant to  'e a +a. Different co(o"nd have different va(or   (re"re +iven a certain te(erat"re a thi tand a

a variation for the va(or (re"re. )n a anner, t-o factor ho"ld 'e conidered in dic"in+ volatility 3  the "'tance -ei+ht and interolec"lar force of  attraction <8r"'iano=. S"rely, it can 'e eaily "ndertood that if a co(o"nd ha a +reater -ei+ht, then it -ill ore li/ely tay in the li2"id (hae -hich i d"e to the hi+h ener+y that -o"ld 'e needed to convert the co(o"nd into the +a (hae. 8hi idea can 'e ot nota'le -ith hydrocar'on, e(ecially al/ane. Car'on ato are the ain fo"ndation of the tr"ct"re <a -ell a hydro+en ato= a they contri'"te to the overall olec"lar a ore. A -e can ee, a the e2"ence of ethane, ethane, (ro(ane +oe, the ore car'on ato they have, the +reater  te(erat"re it i needed to ("t "( -ith their 'oilin+  (oint. 8hi ean that a "'tance -ith +reater 

-ei+ht -o"ld re2"ire ore ener+y for the to 'e va(ori#ed. )n ter of the attraction of interolec"lar  force, it -o"ld >"t 'e a contin"ation of -hat i aid -ith the -ei+ht. 8o 'e clear, a -hat (revio"ly aid and concl"ded, if a "'tance ha tron+ interolec"lar force of attraction, then they are le li/ely to 'e volatile a -hat -ill ha((en i the force that hold the -o"ld not 'e eaily 'e 'ro/en do-n. 8hi ean that it -o"ld 'e hard for thoe "'tance to 'e va(ori#ed, ta/in+ "ch heat and ener+y to do o. <Bal"yot ? De Catro=

)t i (oi'le for co(o"nd to 'e e(arated  'ain+ it on their volatilitie. 8hi (roce of 

e(aration of co(o"nd i c alled ditillation. 8hi i

a (roce of e(aratin+ the co(onent fro a li2"id i0t"re 'y elective eva(oration and condenation. )n thi e0(erient, -e have "ed t-o ethod of  ditillation 3 i(le and tea. )n the ethod of  i(le ditillation, there i >"t a li2"id i0t"re -hich contain a volatile and nonvolatile co(o"nd. hen heat i a((lied, the volatile co(o"nd -o"ld  'e converted to va(or and the nonvolatile co(o"nd -o"ld reain a/in+ it the reid"e. Beca"e of the -ater that the already va(ori#ed volatile co(o"nd -ill "nder+o, it -o"ld a+ain 'e converted to li2"id d"e to te(erat"re difference. )n doin+ thi ethod, -e ho"ld only 'e inded that the co(o"nd to 'e e(arated "t have hi+h volatility difference o that they -o"ld not 'e 'oth t"rned into va(or. <@oder, %1=

On the other note, there i alo the tea ditillation. 8hi i "ed -henever the co(o"nd that i "ed only ha a little va(or (re"re to +ive, a thi ean that even tho"+h at hi+h te(erat"re, the co(o"nd -o"ld till not 'e converted into va(or  leadin+ to a deco(oed co(o"nd. )n tea ditillation, -ater -ill 'e "ed to add ore va(or   (re"re to the nonvolatile co(o"nd -hich i

needed to 'e t"rned into va(or -hile heat i till  'ein+ a((lied. ith thi, the co(o"nd -ill 'oil and le te(erat"re -ill 'e needed for it to 'e t"rned into va(or, hence e(aratin+ the co(o"nd. <Pahlavan, %1=

or the e0(erient, -e are to "e 'oth ethod of ditillation to (rovide analyi to +iven co(o"nd.

2. #I'N+A0 S$+I-N

'aterials %se". "ic/ fit <incl"de all a((arat" needed for i(le and tea ditillation et!"(=,  (i(ette, hot (late, 7rleneyer fla/ <or 'ea/er=

ea&ents %se". )ce, i("re car'on tetrachloride, i("re (!dichloro'en#ene, ditilled -ater 

Simple Distillation. Set!"( for i(le ditillation -ill 'e ae'led. ifteen illiliter of i("re car'on tetrachloride -ill 'e ("t to the (ear!ha(ed fla/ to erve a the a(le for the e0(erient. 4eat -ill 'e a((lied on the a(le "in+ the hot (late. Contin"o"ly, ditillate -ill coe o"t and it vol"e -ill 'e ea"red at different te(erat"re.

Steam Distillation. 8he et!"( for tea ditillation -ill 'e ae'led. One h"ndred illiliter of -ater  -o"ld 'e li+htly 'oiled, that i, for later "e. 8he (! dichloro'en#ene a(le -o"ld then 'e (laced in the  (ear!ha(ed container and it -ill 'e diolved in  L of -ater. 8he container -ith -ater -ill no- 'e heated a it i connected to the container containin+ the li2"id i0t"re. )f no i0t"re i coin+ o"t, the condener i+ht 'e clo++ed and a B"nen '"rner  ho"ld 'e "ed to clear it o"t. 8he i0t"re in the receivin+ container -ill then 'e cooled. )t -ill then  'e filtered and the reainin+ co(o"nd -ill 'e air 

dried.

3. S%0+S AND DIS$%SSI-N

)n the e0(erient, -e have (erfored the ethod of i(le and tea ditillation. Si(le ditillation -a "ed for i("re car'on tetrachloride -hile tea ditillation -a "ed for (! dichloro'en#ene. )n a anner, the volatility of thee co(o"nd -o"ld "rely affect the re"ltin+ ditillate6i0t"re that -e -ill +et.

0

5

10

15

0

10

20

30

40

50

60

70

80

90

Temperature, ⁰C

 Temperature

, ⁰C

 Figure 1. Graph of temperature vs. volume of  distillate collected during simple distillation

i+"re 1 ho- the +ra(h of the te(erat"re of the ditillate +otten v. the ao"nt of the ditillate that i collected. D"rin+ the (roce of i(le ditillation, the te(erat"re of the ditillate "ddenly dro((ed to EF

⁰

C -hen the hot (late i at %E

⁰

C. At the 'e+innin+, the rate of dro( -a  dro( (er  in"te, '"t a the te(erat"re increae, the rate ha finally 'ecoe 55 dro( (er in"te. )n here, an i("re car'on tetrachloride ha 'een "ed a a co(o"nd a(le. ro the co(o"nd itelf 'ein+ i("reH, it ean that it ha a -ea/ interolec"lar  force of attraction -hich i -hy it i 'etter "ited -ith i(le ditillation d"e to the te(erat"re of the volatile and nonvolatile co(onent. 8he rate of the ditillate that i coin+ o"t ha increaed a the te(erat"re increaed. )t i 'eca"e at a hi+her  te(erat"re, the co(o"nd -ill 'e ac2"irin+ ore ener+y, hence 'rea/in+ the interolec"lar force of  attraction 'indin+ it and t"rnin+ it into va(or 2"ic/er  than -hen only a lo- te(erat"re i a((lied. hen the ori+inal a(le i a((lied -ith heat, it i t"rned into va(or, '"t 'eca"e of the (ath that it -ill "nder+o -hich i "rro"nded -ith -ater, a difference in te(erat"re -o"ld 'e noted -hich i -hy -hen it

coe o"t a a ditillate, it -ill 'e in a for of a li2"id a+ain.

Table 1. ata regarding the analysis of the impure carbon tetrachloride

Boilin+ (oint of the a(le EI

⁰

C 8otal vol"e collected 1%.1 L

Percenta+e ecovery F.KE

8a'le 1 i(ly ho- the data that i +athered fro the i("re car'on tetrachloride that -e have. Seventy!nine de+ree Celi" a a 'oilin+  (oint i 2"ite reaona'le +iven that it i an i("re one. or the vol"e of the ditillate collected, fro the ori+inal 1 L, it ean that there had 'een a lar+e ao"nt of ("re "'tance fro the ori+inal a(le and a (ercenta+e recovery of F.KE a/e it reaona'le.

Table !. ata regarding the analysis of p" dichloroben#ene

Meltin+ (oint of cr"de a(le %.5E

⁰

C Meltin+ (oint of ("rified a(le 5.E

⁰

C

ei+ht of cr"de a(le % + ei+ht of ("rified a(le 1.F +

Percenta+e ecovery I

8a'le % ho- the data -e +athered re+ardin+ the (!dichloro'en#ene -herein tea ditillation i "ed. 8he -ater hel(ed the a(le 'oil -hich then (rod"ced a tea. 8he tea +ot crytalli#ed a it clo++ed, o heat i a((lied and the a it t"rn into li2"id, it +ot crytalli#ed a+ain a -hile after receivin+ container. Stea ditillation ha 'een "ed in thi co(o"nd (ro'a'ly 'eca"e it only e0ert very little va(or (re"re even if it i "'>ected in a hi+h te(erat"re, and alo to avoid deco(oition of the co(o"nd. ith thi, -ater i "ed o that va(or (re"re -o"ld 'e added -hich -ill a/e the i0t"re achieve ato(heric (re"re even at a lo- te(erat"re. ater i then heated o that to+ether, -ith the i0t"re, they -ill 'e ditilled off. 8he re"ltin+ container i in an ice 'ath o the re"ltin+ i0t"re +ot crytalli#ed. After crytal are fored, it i no- filtered o that only the ("re

co(onent -o"ld really 'e left. 8he re"ltin+  ("rified a(le -ei+hed 1.F + -hich i ean that the ori+inal a(le oeho- contain a 'i+ ao"nt of the ("re one, and -ith that, -e +ot I a the  (ercenta+e recovery.

ro the t-o (rocee, it can 'e een that altho"+h 'oth can -or/ really -ell, tea ditillation i 2"it a (refera'le one. )t i 'eca"e a 'oth deal -ith te(erat"re, it can 'e een that tea ditillation tend to lo-er the te(erat"re that -ill 'e re2"ired  'y lo-erin+ the (re"re that there i in the fla/. 8herefore, it (revent the co(o"nd to 'e deco(oed.

. $-N$0%SI-N

)n the e0(erient, -e have dealt -ith the analyi and ("rification of car'on tetrachloride and  (!dichloro'en#ene, "in+ i(le and tea ditillation, re(ectively. )t can 'e een that i(le ditillation -or/ -ell -hen the "'tance to 'e e(arated have a lar+e difference in volatility. Alo, in here, increaed te(erat"re -o"ld a/e the rate of  ditillate dro((in+ to 'e fater a there -o"ld 'e ore ener+y a((lied in the a(le, t"rnin+ it into va(or fater.

or tea ditillation, it can 'e een that oe co(o"nd -o"ld only e0ert very little va(or   (re"re. ith that, one thin+ to do i find a -ay to

-herein there -o"ld 'e ore va(or (re"re, and it i  'y addin+ -ater a a o"rce. 8hi -ill then leen the needed te(erat"re 'y a/in+ the (re"re inide the fla/ le.

)n a ore (ractical anner, in 'oth ethod of  ditillation, it ho"ld 'e noted that the condener  ho"ld al-ay 'e filled -ith -ater o that ri+ht -hen the ditillate reache the re"ltin+ container, it -ill 'e in the for of a li2"id, d"e to te(erat"re difference.

5.

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 Figure !. Simple istillation Set"up

 Figure $. Steam istillation Set"up