FACULT FACULTY Y OF APPLIED SCIENCE DIPLOMA IN SCIENCE
CHM 260
ASSIGNMENT 1 QUALITATIVE QUALITATIVE ANALYSIS ANALYSIS OF BENZOIC BENZOI C ACID USING USI NG FTIR FTI R
NAME
: CHARLES ROLEND RICHARD
MATRIX NUMBER
: 2013219228
GROUP
: AS1206A2
LECTURER’S NAME
: JULENAH AG NUDDIN
DAT DATE OF SUBM UBMISS SSIION
: 8th JANUARY 2016
1.0 AIM To identi! the "#$%it$ti&e $n$%!'i' o $n #n(no)n *en+oi, $,id #'in- .o#/ie/ T/$n'o/
In/$/ed Se,t/oete/' .TIR4
2.0 INTRODUCTION
.TIR 'e,t/oet/! i' #'ed o/ the identii,$tion o ,hei,$% $nd h$/$,e#ti,$% '#*'t$n,e'4 In the /e,ent $'t the #'e o .TIR 'e,t/o',o! )ith $/o/i$te 'ot)$/e h$' *een #'ed o/ 'o%&in- die/ent /o*%e' /e%$ted to $n$%!ti,$% de&e%oent4 In $ddition5 thi' te,hni"#e i' $%'o (no)n o/ it' %o) ,o't5 'i%i,it!5 non de't/#,ti&ene'' $nd /$idit! o/ "#$%it$ti&e $n$%!'i'4 .TIR .o#/ie/ T/$n'o/ In/$/ed 'e,t/oet/! )$' de&e%oed in o/de/ to o&e/,oe the %iit$tion' en,o#nte/ed )ith di'e/'i&e in't/#ent'4 The $in dii,#%t! o thi' ethod i' the ',$nnin- /o,e'' )$' too '%o)ed4 To ,o#nte/ thi' /o*%e5 $ 'o%#tion )$' de&e%oed )hi,h e%o!ed $ &e/! 'i%e oti,$% de&i,e ,$%%ed $' inte/e/oete/4 Thi' 'o%#tion /od#,e' $ #ni"#e t!e o 'i-n$% )hi,h h$' $%% o the in/$/ed /e"#en,ie' 7en,oded into it4 A' $ /e'#%t5 the 'i-n$% ,$n *e e$'#/ed &e/! "#i,(%!5 #'#$%%! on the o/de/ o one 'e,ond o/ 'o4 Th#'5 the tie e%eent e/ '$%e i' /ed#,ed to $ $tte/ o $ e) 'e,ond' /$the/ th$n 'e&e/$% in#te'4 o't inte/e/oete/' e%o! $ *e$ '%itte/ )hi,h t$(e' the in,oin- in/$/ed *e$ $nd di&ide' it into t)o oti,$% *e$'4 One *e$ /e%e,t' o o $ %$t i//o/ )hi,h i' i:ed in %$,e4 The othe/ *e$ /e%e,t' o o $ %$t i//o/ )hi,h i' on $ e,h$ni' )hi,h $%%o)' thi' i//o/ to o&e $ &e/! 'ho/t di't$n,e t!i,$%%! $ e) i%%iet/e' $)$! /o the *e$ '%itte/4 The t)o *e$' /e%e,t o thei/ /e'e,ti&e i//o/' $nd $/e /e,o*ined )hen the! eet *$,( $t the *e$ '%itte/4 The $th th$t one *e$ t/$&e%' i' $ i:ed %en-th $nd the othe/ i' ,on't$nt%! ,h$n-in- $' it' i//o/ o&e'5 the 'i-n$% )hi,h e:it' the inte/e/oete/ i' the /e'#%t o the'e t)o *e$' inte/e/in- )ith e$,h othe/4 The /e'#%tin- 'i-n$% i' ,$%%ed $n inte/e/o-/$ )hi,h h$' the #ni"#e /oe/t! th$t e&e/! d$t$ oint )hi,h $(e' # the 'i-n$% h$' ino/$tion $*o#t e&e/! in/$/ed /e"#en,! )hi,h ,oe' /o the 'o#/,e4
F!"#$ 1: S%&$'()% *(!#(' +, FTIR
;en+oi, $,id i' $ 'o%id th$t i' ,/!'t$%%ine in $e$/$n,e5 'ii%$/ to )hite need%e'4 A n$t#/$% 'o#/,e o *en+oi, $,id i' -# *en+oin5 )hi,h ,oe' /o ,e/t$in t/ee *$/('< ho)e&e/5 *en+oi, $,id ,$n $%'o *e $de *! '!ntheti, e$n'4 The '#*'t$n,e /e,ei&ed it' n$e /o -# *en+oin5 the %$nt /o )ho'e /e'in it )$' i/'t de/i&ed Jo'eh5 20134 The ,hei,$% o/#%$ o *en+oi, $,id i' C =H6O2> it h$' 'e&en ,$/*on C $to'5 'i: h!d/o-en H $to' $nd t)o o:!-en O $to'4 Thi' ,hei,$% o/#%$ ,$n $%'o *e )/itten $' C 6H?COOH4 The ,hei,$% 't/#,t#/e o ,$/*o:!%i, $,id i' 'ho)n *e%o)4 On the %et5 it 'ho)' $%% the ,$/*on $nd h!d/o-en $to' on the *en+ene /in-5 $nd on the /i-ht5 it 'ho)' $nothe/ )$! to d/$) the *en+ene /in-5 )hi,h i' d/$)n in *%#e4 ;en+oi, $,id i' $n o/-$ni, ,oo#nd *e,$#'e it ,ont$in' ,$/*on5 $nd it i' $%'o $n $/o$ti, ,$/*o:!%i, $,id4 It i' $/o$ti, *e,$#'e it h$' $ *en+ene /in- in it' ,hei,$% 't/#,t#/e the he:$-on )ith do#*%e *ond' i%%#'t/$ted in *%#e5 )he/e the *en+ene /in- h$' $%te/n$tin- do#*%e *ond' *et)een e$,h ,$/*on4 It i' ,%$''iied $' $ ,$/*o:!%i, $,id *e,$#'e it h$' $ ,$/*o:!% -/o# in it' 't/#,t#/e5 )hi,h i' the @COOH -/o#4
F!"#$ 2: C&$'%(- S)#"%)"#$ +, B$/+% A%*
.0 REVIE OF LITERATURE 341 ;ENOIC ACID • ;en+oi, $,id o,,#/' n$t#/$%%! in &$/io#' *e//ie' not$*%! ,/$n*e//ie'5 ,inn$on5
%#'5 ,#//$nt'5 ,%o&e'5 et,4 It h$' %on- *een #'ed to inhi*it i,/o*i$% -/o)th in $n! /od#,t' in,%#din- non$%,oho%i, *e&e/$-e'5 B$' $nd e#%'iied '$#,e'4 The '$%t o *en+o$te i' o/e 't$*%e th$n the $,id o/ $nd o/e 'o%#*%e in )$te/ $(in- the *en+o$te $ $&o#/$*%e ,hoi,e o/ the 'ot d/in(' ind#'t/!4 In $ddition5 *en+oi, $,id )$' #'ed $' $ $Bo/ /e'e/&$ti&e ,oo#nd in e/ented i'h /od#,t' '#,h $' cencaluk 5 budu $nd d/ied i'h No/%id$5 20094 No/%id$ 2009 $%'o 't$te th$t thi' ,oo#nd $/e ee,ti&e to /e&ent the -/o)th o !e$'t5 o#%d $nd $ )ide /$n-e o *$,te/i$5 /o&in- th$t *en+oi, $,id i' $n io/t$nt ,oo#nd in e,onoi, ind#'t/i$% '#,h $' ood /od#,tion4 •
342 .TIR .o#/ie/ T/$n'o/ In/$/ed Se,t/oete/' .TIR i' $ te,hni"#e th$t #'ed to o*t$in $n in/$/ed 'e,t/# o/ ei''ion o $ 'o%id5 %i"#id o/ -$'4 An .TIR 'e,t/oete/ 'i#%t$neo#'%! ,o%%e,t' hi-h 'e,t/$% /e'o%#tion d$t$ o&e/ $ )ide 'e,t/$ /$n-e4 Thi' ,on&e/'e $ 'i-nii,$nt $d&$nt$-e o&e/ $ di'e/'i&e 'e,t/oete/ )hi,h e$'#/e' inten'it! o&e/ $ n$//o) /$n-e o )$&e%en-th' $t $ tie4 In in/$/ed 'e,t/o',o!5 $n in/$/ed IR /$di$tion i' $''ed th/o#-h the '$%e4 Soe o the in/$/ed /$di$tion i' $*'o/*ed *! the '$%e $nd 'oe o it $''ed th/o#-h t/$n'itted4 A' $ /e'#%t5 the 'e,t/# /e/e'ent' the 'e,t/# /e/e'ent' the o%e,#%$/ $*'o/tion $nd t/$n'i''ion5 ,/e$tin- $ o%e,#%$/ in-e//int o $ '$%e4 .TIR $/e )ide%! #'ed *! the /e'e$/,he/' $' $ ethod to ,o%ete thei/ 't#die'4 A,,o/din- to $%e/ 201?5 .TIR h$' *een #'ed $n$%!+e the '$%e' o i,/o%$'ti,' in $"#$ti, e,o'!'te' "#$%it$ti&e%! $nd "#$ntit$ti&e%! *! ,o%%e,tin- the ino/$tion $nd $(e $n $/o/i$te $nd /e%i$*%e $n$%!ti,$% ethod' to di'tin,t%! identi! $nd $%'o to "#$nti! the'e $/ti,%e' in en&i/onent$% '$%e4 On the othe/ h$nd5 .TIR i' $%'o %$! $n io/t$nt /o%e in $ edi,$% ie%d4 N#/i$ 201 't$te' th$t .TIR h$' *een #'ed to ,o%o,$%i+e $!%oid deo'it' $nd %iid e/o:id$tion in ti''#e '%ide' /o $tient' th$t $e,ted *! A%+heie/' di'e$'e4
.0 OB3ECTIVES To /e$/e the ;/ e%%et o *en+oi, $,id • To ,$//! o#t $ "#$%it$ti&e $n$%!'i' o *en+oi, $,id #'in- .TIR •
•
To identi! IR $*'o/tion e$(' $nd the ,o//e'ondin- #n,tion$% -/o#' o $n #n(no)n 'o%id%i"#ido)de/4
4.0 CHEMICALS AND INSTRUMENTS The/e $/e 'e&e/$% io/t$nt ,hei,$% $nd in't/#ent to ,ond#,t thi' e:e/ient '#,h
$' *en+oi, $,id5 ot$''i# */oide ;/5 ;/ $%%et $$/$t#' die5 h!d/$#%i, /e''5 -/inde/5 et, $nd .TIR in't/#ent4
6.0 METHODOLOGY 6.1 T&$ 5B# M$)&+* The 'o%id '$%e *en+oi, $,id $nd the ;/ 'o%id IR -/$de )i%% *e o*t$ined
/o the de'i,,$to/4 E$,h o '$%e' )i%% *e )ei-hed $*o#t 1 -/$ $nd d/! in the o&en o/ $*o#t 23 ho#/' $t 110FC4 Thi' 'te $! *e done $he$d o tie )ith he% o the %$*o/$to/! 't$4 Ne:t5 the $-$te o/t$/ $nd e't%e )i%% *e /eo&ed /o the de'i,,$to/ o/ #'e to -/ind the *en+oi, $,id $nd ;/4 Ate/ th$t5 $*o#t 1 - o *en+oi, $,id )i%% *e t$(en $nd -/indin- *! #'in- $-$te o/t$/ o/ $*o#t 1 in#te o/ o/e $nd e't%e #nti% the *en+oi, $,id *e,oe &e/! '$%% $nd 'hin!4 Hen,e5 $*o#t 80 - o ;/ )i%% *e t$(e $nd -/inded *! #'in- $-$te o/t$/ $nd e't%e #nti% it *e,oe' o)de/ed4 The *en+oi, $,id $nd o)de/ed ;/ )i%% *e i:ed in $-$te o/t$/ o/ /$tio 1>80 $nd -/ind the i:t#/e #nti% *e,oe hoo-eneo#' o/ $*o#t 30 'e,ond'4 U'in- the '$t#%$5 the i:t#/e )i%% *e ',/$ed into the idd%e $nd the i:t#/e )i%% *e -/inded $-$in $*o#t 1? 'e,ond' to i: the *en+oi, $,id tho/o#-h%! )ith the ;/4 The *en+oi, $,id $nd ;/ #'t *e ine%! -/o#nd5 o/ the i:t#/e )i%% ',$tte/ the in/$/ed /$di$tion e:,e''i&e%!4 The i:t#/e )i%% *e he$ed in the ,ente/ o the $-$te o/t$/ #'in- $ '$t#%$4
6.2 M(! )&$ 5B# P$--$) The die 'et )i%% *e /eo&ed /o the *o: o/ 'to/$-e ,ont$ine/4 Then5 the die
'et )i%% *e ,%e$ned )ith Eth$no%4 The i:t#/e o *en+oi, $,id $nd ;/ )i%% *e #t into the die 'et $nd $(e '#/e the i:t#/e i%%' the '#/$,e o the die 'et4 Ne:t5 the die 'et )i%% *e ti-hten ,%o'e%! $nd %$,ed into h!d/$#%i, /e'' -$#-e4
The H!d/$#%i, /e'' -$#-e )i%% *e /e'' #nti% the /e''#/e -oe' # to =000 'i4 Re%e$'e the $i/ $nd %et it /e't o/ 2 in#te'4 The H!d/$#%i, /e'' -$#-e )i%% *e /e''ed $-$in #nti% the /e''#/e -oe' # to 8?00 'i $nd )i%% *e /e'ted o/ 1 in#te4 Re%e$'e the /e''#/e4 The die 'et )i%% *e /eo&e '%o)%! /o the H!d/$#%i, /e'' -$#-e4 Ate/ th$t5 the die 'et $nd the ;/ e%%et )i%% *e oened4 The ,oo#nd th$t o*t$ined 'ho#%d $e$/ ,%e$/ %i(e $ ie,e o -%$'' o/ t/$n'$/ent di'(4 L$'t%!5 the ;/ e%%et )i%% *e %$,ed into $ e%%et ho%de/ o/ $n$%!'i'4 6. P#$7(#! L8"* S('7-$9 ;$() -8"*9’< "9! ( S(-) P-()$ .i/'t%!5 $ 7ne$t %i"#id '$%e )i%% *e #'ed4 Then5 'oe o the %i"#id '$%e
)i%% *e %$,ed $*o#t 12 d/o' on the %$te $nd ,o&e/ed )ith $nothe/ %$te4 The %i"#id 'ho#%d *e '/e$d o#t to ,o&e/ the enti/e %$te4 Ate/ th$t5 the '$nd)i,h )i%% *e %$,e in the IR '$%t %$te ho%de/ $nd )i%% *e ,o&e/ed )ith $ ho%ddo)n %$te4 Ne:t5 $t %e$'t 2 n#t' )i%% *e %$,ed on the o't' o the ho%de/ $nd the n#t' )i%% *e /ot$ted -ent%! to ho%d the %$te' )ith $n e&en /e''#/e4 Do not o/,e it *e,$#'e it )i%% *e ,/$,(in- the %$te'4 Ne:t5 the ho%de/ )i%% *e '%ide into the */$,(et on the in't/#ent in the '$%e *e$ $nd the 'e,t/# )i%% *e ,ond#,ted4 L$'t%!5 the '$%t %$te' )i%% *e /eo&ed $nd ,%e$ned /o the in't/#ent4 Oten $ %itt%e $,etone o%%o)ed *! d/!in- )ith i ie' )i%% do4 The '$%t %$te' )i%% *e (et in $ ,%e$n $nd d/! %$,e4
6. S('7-$ 7#$7(#()+ ,+# FT=IR R$,-$%)(%$< The 'o%id '$%e' )i%% *e -/o#nded ine%! *eo/e #'e4 Ne:t5 the 'e,t/# o
*en+oi, $,id )i%% *e ,ond#,ted #'in- the Re%e,t$n,e ethod4 L$'t%!5 $n #n(no)n )i%% *e o*t$ined /o the %$* in't/#,to/ $nd the 'e,t/# )i%% *e ,ond#,ted4 >.0 EXPECTED OUTCOME
F!"#$ : I,#(#$* S7$%)#( +, B$/+% A%*
(?$"'@$# %' =1< 9001100 1300 16801=?0 2?003300
T7$ +, @+* ;en+ene OH CO OH
F"%)+(- G#+"7 A/o$ti, H!d/o:!% C$/*o:!%i, $,id H!d/o:!%
T(@-$ 1: T(@"-()+ D()( +, I,#(#$* S7$%)#( +, B$/+% A%*
.0 CLOSING REMAR5S
.TIR i' /ee//ed o&e/ di'e/'i&e o/ i%te/ ethod' o in/$/ed 'e,t/$% $n$%!'i'4 Thi' i' *e,$#'e thi' ethod h$' $n! $d&$nt$-e'4 Seed i' one o the $in /e$'on'4 A%% o the /e"#en,ie' th$t $/e e$'#/ed5 o't e$'#/eent' *! .TIR $/e $de in $ e) 'e,ond'4 Othe/ th$n th$t5 it /o&ide' e:,e%%ent 'en'iti&it!4 The dete,to/' $/e #,h o/e 'en'iti&e5 the oti,$% th/o#-h#t i' #,h hi-he/4 .TIR $%'o inte/n$%%! ,$%i*/$ted5 thi' in't/#ent' #'e $ HeNe %$'e/ $' $n inte/n$% )$&e%en-th ,$%i*/$tion 't$nd$/d4 Thi' HeNe %$'e/ $/e 'e%,$%i*/$tin-4 The'e $d&$nt$-e' $(e e$'#/eent' $de *! .TIR e:t/ee%! $,,#/$te4 Th#'5 it i' $ /e%i$*%e te,hni"#e o/ o'iti&e identii,$tion o
&i/t#$%%! $n! '$%e4 The 'en'iti&it! *eneit' en$*%e identii,$tion o e&en the '$%%e't o ,ont$in$nt'4 Thi' $(e' .TIR $ &e/! -ood too% o/ "#$%it! ,ont/o% .
.0 REFERENCE
Jo'eh5 45 in-'%e!5 ; 20134 So%#*i%it! o ;en+oi, A,id in #/e So%&ent' $nd ;in$/! i:t#/e'4 Journal of Chemical & Engineering Data, ??115 =13
No/%id$5 ;45 20094 Dete/in$tion o ;en+oi, A,id in .e/ ented .i'h /od#,t' #'inHLC4 QD Chemistry5 16=5 1=6 $%e/5 A45 ind/i,h5 .45 ./$n(5 L45 $%$nin5 45 %$#'Jo,hen5 K4 201?4 Identii,$tion o i,/o%$'ti,' *! .TIR $nd R$$n i,/o',o!4 Analytical and Bioanalytical Chemistry5 0=225 6=91 ;en'en!C$'e'5 N45 N#/i$5 45 O:$n$5 C45 $/ine5 .45 C%$de/$5 J4 2014 An$%!ti,$% Chei't/!4 American Chemical Society5 8625 12012
