VISIBLE SPECTROSCOPY

PURDUE UNIVERSITY INSTRUMENT VAN PROJECT

SPECTROPHOTOMETRIC ANALYSIS OF ASPIRIN
(Revised: 1-20-93)
INTRODUCTION
Aspirin is certainl t!e "#st $idel %sed "edicinal a&ent ever disc#vered'
C%rrentl 30(000(000 p#%nds are s#ld in t!e United )tates eac! ear $!ic!
pr#vides "#re t!an 200 *ve &rain ta+lets ,#r ever pers#n in t!e c#%ntr' It
is e-ective as an antipretic dr%& (i'e' it red%ces ,ever) and as an anal&esic(
relievin& t!e "ild pain #, !eadac!es( ne%ral&ia and r!e%"atis"'
T!e c!e"ical na"e ,#r aspirin is acetlsaliclic acid' It is an ester derivative
#, saliclic acid and its c#""#n na"e is derived ,r#" t!e #ld .er"an
versi#n #, t!e na"e( acetlspirasae%re' Aspirin $as *rst "ar/eted
c#""erciall + t!e 0aer C#"pan in .er"an in 1199' T!e disc#ver #,
its i"p#rtant "edicinal val%e $as act%all a res%lt #, earlier st%dies #n t!e
parent c#"p#%nd( saliclic acid( $!ic! $as s!#$n t# !ave "edicinal val%e(
+%t als# s#"e side e-ects'
T!e !i&!l c#l#red c#"ple2 $!ic! ,#r"s +et$een acetlsaliclic acid
(aspirin) and ir#n(III) c!l#ride ena+les %s t# deter"ine c#l#ri"etricall t!e
speci*c a"#%nt #, acetlsaliclic acid present in a ta+let' )ince t!e intensit
#, t!e c#l#r ,#r"ed is directl related t# t!e a"#%nt #, acetlsaliclic acid
present( a series #, s#l%ti#ns( eac! $it! a di-erent c#ncentrati#n #,
acetlsaliclic acid( can +e prepared and t!e a+s#r+ance #, eac! s#l%ti#n
"eas%red' A cali+rati#n c%rve is t!en c#nstr%cted and ,r#" t!is c%rve t!e
a"#%nt #, acetlsaliclic acid in a c#""ercial aspirin pr#d%ct can +e
deter"ined'
T!e c#"ple2 i#n is ,#r"ed in t$# steps' 3irst t!e acetlsaliclic acid is
reacted $it! s#di%" !dr#2ide t# ,#r" t!e saliclate diani#n' T!en t!e
additi#n #, acidi*ed ir#n(III) i#n pr#d%ces t!e vi#let tetraa4%#saliclatr#ir#n
(III) c#"ple2'
VISIBLE SPECTROSCOPY
PURDUE UNIVERSITY INSTRUMENT VAN PROJECT
O056CTI76)
1' T# %se t!e )pectr#nic 20 ()pec 20) t# deter"ine t!e "illi&ra"s #,
acetlsaliclic acid (aspirin) in a c#""ercial aspirin pr#d%ct'
2' T# c#"pare t!e "ass and c#st #, acetlsaliclic acid in vari#%s
c#""ercial aspirin pr#d%cts'
8ROC6DUR6
A' 8reparati#n #, C#""ercial Aspirin )#l%ti#ns
1' 9ei&! #%t 0':00 & (:00 "&) #, acetlsaliclic acid and place it in a 12;
"< 6rlen"eer =as/' Add 10 "< #, 1 > NaO? s#l%ti#n and !eat t#
+#ilin&' @%antitativel trans,er t!e s#l%ti#n t# a 2;0 "l v#l%"etric
=as/ and dil%te $it! distilled $ater t# t!e 2;0 "< "ar/' T!is s#l%ti#n
$ill +e re,erred t# as t!e A)tandard Aspirin )#l%ti#n'A
2' Usin& a 1 "< &rad%ated pipette( trans,er 0'; "< #, standard aspirin
s#l%ti#n t# a 10 "< v#l%"etric =as/ #r &rad%ated clinder' Dil%te t#
t!e 10 "< "ar/ $it! +%-ered 0'02 > ir#n(III) c!l#ride s#l%ti#n' Use a
"edicine dr#pper t# &et t!e +#tt#" #, t!e "enisc%s #n t!e 10 "< line'
Trans,er t!e s#l%ti#n t# a s"all( clean( dr +ea/er ,#r "i2in& and la+el
t!is A)#l%ti#n A'A
3' 8repare A)#l%ti#n 0A in a si"ilar "anner + trans,errin& 0': "< #,
standard aspirin s#l%ti#n as in step 2 and dil%tin& t# 10 "< $it!
+%-ered 0'02 > ir#n(III) c!l#ride'
8repare A)#l%ti#n CA + dil%tin& 0'3 "< #, standard aspirin s#l%ti#n t#
10 "<'
8repare A)#l%ti#n DA + dil%tin& 0'2 "< #, standard aspirin s#l%ti#n t#
10 "<'
8repare A)#l%ti#n 6A + dil%tin& 0'1 "< #, standard aspirin s#l%ti#n t#
10 "<'
VISIBLE SPECTROSCOPY
PURDUE UNIVERSITY INSTRUMENT VAN PROJECT
NOT6: I, a 1'0 "< &rad%ated pipette is n#t availa+le(
acc%ratel deter"ine t!e n%"+er #, dr#ps needed
,#r t!e deliver #, 1'0 "< and t!en %se t!e
appr#priate n%"+er #, dr#ps ,#r t!e v#l%"es needed
,#r dil%ti#n'
:' >eas%re t!e B trans"ittance #, eac! s#l%ti#n $it! a )pectr#nic 20 set
at ;30 n"' Use a c%vette *lled $it! t!e pale ell#$ ir#n(III) c!l#ride
s#l%ti#n ,#r t!e +lan/'
VISIBLE SPECTROSCOPY
PURDUE UNIVERSITY INSTRUMENT VAN PROJECT
DATA TA0<6
Solution %T Calculate A
!
A
0
C
D
6
CT!e readin&s ,#r B T are "#re precise t!an t!e readin&s ,#r t!e
a+s#r+ance' T!ere,#re t!e a+s#r+ance s!#%ld +e calc%lated rat!er t!an +e
read #- t!e instr%"ent'
A D -l#& T $!ere T D BT 100
0' 8reparati#n #, C#""ercial Aspirin )#l%ti#ns
1' 8lace #ne ta+let #, t!e c#""ercial pr#d%ct in a 12; "< 6rlen"eer
=as/' Add 10 "< #, 1 > NaO? s#l%ti#n' ?eat andE#r stir %ntil t!e
ta+let !as diss#lved' @%antativel trans,er t!e s#l%ti#n t# a 2;0 "<
v#l%"etric =as/ and dil%te $it! distilled $ater t# t!e 2;0 "< "ar/'
2' As is )tep 2 ,r#" 8art A( %se a 1 "< &rad%ated pipette t# trans,er 0';
"< #, aspirin s#l%ti#n t# a 10 "< v#l%"etric =as/ #r &rad%ated
clinder' Dil%te t# t!e 10 "< "ar/ $it! +%-ered 0'02 > ir#n(III)
c!l#ride s#l%ti#n' Use a "edicine dr#pper t# &et t!e +#tt#" #, t!e
"enisc%s #n t!e 10 "< line' Trans,er t!e s#l%ti#n t# a s"all( clean(
dr +ea/er ,#r "i2in& and la+el t!e +ea/er appr#priatel'
3' >eas%re and rec#rd t!e B trans"ittance #, t!is s#l%ti#n $it! a )pec
20 set at ;30 n"' Use a c%vette *lled $it! t!e pale ell#$ ir#n (III)
c!l#ride s#l%ti#n ,#r t!e +lan/'
:
VISIBLE SPECTROSCOPY
PURDUE UNIVERSITY INSTRUMENT VAN PROJECT
DATA TA0<6
Co""e#cial
P#ouct
%T Calculate
A$%o#$ance!
CT!e readin&s ,#r BT are "#re precise t!an t!e readin&s ,#r t!e a+s#r+ance'
T!ere,#re t!e a+s#r+ance s!#%ld +e calc%lated rat!er t!an +e read #- t!e
instr%"ent'
A D -l#& T $!ere T D BT 100
CA<CU<ATION)
C#nstr%cti#n #, t!e Cali+rati#n C%rve (A+s#r+ance vs "& AspirinETa+let)
1' Calc%late t!e c#ncentrati#n (in "&E"<) #, acetlsaliclic acid in t!e
A)tandard Aspirin )#l%ti#n'A
2' Usin& t!e relati#ns!ip ,#r dil%ti#ns:
c#ncentrati#n 2 v#l%"e D c#ncentrati#n 2 v#l%"e
calc%late t!e c#ncentrati#n (in "&E"<) #, acetlsaliclic acid ,#r eac!
#, t!e standard )#l%ti#ns A( 0( C( D and 6'
3' Deter"ine t!e c#ncentrati#n ("&E"<) rati#s #, t!e ,#ll#$in& s#l%ti#ns'
c#nc 0Ec#nc A c#nc CEc#nc A c#nc DEc#nc A c#nc 6Ec#nc A
:' :00 "& #, acetlsaliclic acid $as diss#lved and dil%ted t# "a/e
)#l%ti#n A' )ince all #, t!e aspirin s#l%ti#ns $ere diss#lved and dil%ted
e2actl t!e sa"e $a as )#l%ti#n A( $e can c#ncl%de t!at i, t!e
aspirin s#l%ti#n !as t!e sa"e a+s#r+ance as )#l%ti#n A( t!en t!e
aspirin ta+let "%st !ave c#ntained :00 "& #, acetlsaliclic acid'
3%rt!er"#re( since )#l%ti#n 0 !as less acetlsaliclic acid t!an
)#l%ti#n A + t!e ,racti#n c#nc 0Ec#nc A( $e can c#ncl%de t!at t!is
s#l%ti#n c#%ld !ave +een "ade + diss#lvin&:
;
VISIBLE SPECTROSCOPY
PURDUE UNIVERSITY INSTRUMENT VAN PROJECT
and dil%tin& it as $e did ,#r )#l%ti#n A' 9e $ill call t!is ,racti#n t!e
A"& #, acetlsaliclic acid in )#l%ti#n 0A +eca%se( i, an aspirin s#l%ti#n
!as t!e sa"e a+s#r+ance as )#l%ti#n 0 $e can c#ncl%de t!at t!e
ta+let c#ntained t!is "an "& #, acetlsaliclic acid'
Calc%late t!e A"& #, acetlsaliclic acidA ,#r eac! #, t!e standard
s#l%ti#ns'
;' On a &rap! $it! appr#priate precisi#n( pl#t a+s#r+ance vs' A"& #,
acetlsaliclic acid'A A+s#r+ance s!#%ld +e #n t!e vertical a2is and
A"& #, acetlsaliclic acidA s!#%ld +e #n t!e vertical a2is'
Deter"inati#n #, t!e "& #, Acetlsaliclic Acid 8er Ta+let
1' Usin& #%r data( and t!e data ,r#" #t!er st%dents deter"ine t!e "&
#, acetlsaliclic acid per ta+let ,r#" t!e cali+rati#n c%rve' .et t!e
#t!er data needed t# *ll in t!e ta+le ,r#" t!e appr#priate aspirin
+#ttle'
A%&i#in
P#ouct
Calculate
A$%o#$anc
e
E'&e#i"ent
al
"( ) ta$let
Acce&te
"( ) ta$let
Co%t Pe#
Ta$let
Ta$let
acid cylic acetylsali of mg 400 x
A Conc
B Conc
= B Solution in acid cylic acetylsali of mg
F
VISIBLE SPECTROSCOPY
PURDUE UNIVERSITY INSTRUMENT VAN PROJECT
RESULTS AND CONCLUSIONS
*+ ,-ic- ta$let &#o.ie% t-e -i(-e%t nu"$e# o/ "( o/ a%&i#in &e#
olla#0 E'&lain+
1+ P#ouct% %uc- a% Anacin
2
a#e la$ele 3e't#a %t#en(t-+3 Ho4
"an5 "( o/ a%&i#in o t-e%e 3e't#a %t#en(t-3 &#ouct%
contain0
6+ On a co%t &e# "( $a%i%7 a#e 3e't#a %t#en(t-3 &#ouct% a 3(oo
$u503
8+ E'&lain -o4 t-e S&ec 19 4a% u%e to #elate t-e a$%o#$ance to
t-e concent#ation o/ t-e a%&i#in+
G
VISIBLE SPECTROSCOPY
PURDUE UNIVERSITY INSTRUMENT VAN PROJECT
LAB ,RITTEN BY: JOHN CHAMBERS7 PRU PHILLIPS7 AND ;ATHY
,HITFIELD
1
TEACHERS< =UIDE
SPECTROPHOTOMETRIC ANALYSIS OF ASPIRIN
C<A))ROO> U)A.6
T!is e2peri"ent $ill $#r/ $ell i, st%dents !ave t!e necessar 4%antitative
s/ills' T!ere,#re it is ,elt t!at t!is e2peri"ent s!#%ld +e ,#r sec#nd se"ester
*rst ear st%dents #r sec#nd ear st%dents' T!is s!#%ld n#t +e t!e
intr#d%ct#r e2peri"ent ,#r t!e )pec 20'
T!is e2peri"ent $as envisi#ned as an entire class activit s# t!at "an
aspirin sa"ples c#%ld +e analHed and c#"pared' One #r t$# &r#%ps #,
st%dents $#%ld +e resp#nsi+le ,#r "a/in& s#l%ti#ns ,#r t!e cali+rati#n c%rve
and #t!er &r#%ps #, st%dents $#%ld +e resp#nsi+le ,#r dil%tin& aspirin
sa"ples'
)TUD6NT TI>6
1 class peri#d ,#r s#l%ti#n preparati#n and 1 class peri#d ,#r data c#llectin&'
>AT6RIA<)
acetlsaliclic acid( rea&ent &rade: eac! cali+rati#n c%rve needs 0':00 &
I, acetlsaliclic acid is n#t availa+le( an Anacin
I
ta+let "a +e %sed
,#r t!e standards' T!e la+el states t!at t!is +rand c#ntains :00 "& #r
0':00 & #, aspirin'
NaO? )#l%ti#n( 1'0 >: eac! dil%ti#n needs 10 "<
Ir#n(III) C!l#ride s#l%ti#n +%-ered t# a p? #, 1'F $it! ?Cl-JCl +%-er' T!e
cali+rati#n c%rve re4%ires ;0 "<K eac! aspirin dil%ti#n re4%ires 10 "<' T#
"a/e 100 "< #, t!is s#l%ti#n( place 39'; "< #, 0'20 > ?Cl int# F0'; "< #,
0'20 > JCl' T!en add :'1; & #, 3eCl
3
F?
2
O
(#r 3'2: & an!dr#%s 3eCl
3
)'
Re,erence ,#r +%-er: CRC ?and+##/
Distilled $ater
Co""e#cial A%&i#in P#ouct%
0aer Aspirin
I
.eneric Aspirin 0a+ Aspirin
Al/a-)eltHer
I
Anacin
I
0%-erin
I
62cederin
I
>id#l
I
62tra )tren&t! Aspirin
6@UI8>6NT
)pectr#nic 20 $it! c%vettes
2;0 "< v#l%"etric =as/s
1'0 "< &rad%ated pipette
10 "< v#l%"etric =as/s #r &rad%ated clinders
"edicine dr#ppers #r dr#ppin& pipettes
s"all +ea/ers (;0 "<)
+alance and $ei&!in& paper
)A36TL AND DI)8O)A< )tandard <a+#rat#r )a,et 8r#ced%res
)A>8<6 )TUD6NT DATA

Solutio
n
%T Calculate
A
A 11'2 0'G:0
0 2:'F 0'F10
C 3;': 0':;2
D ;1'2 0'290
6 G0'F 0'1;1
)A>8<6 CA<CU<ATION)
1' Calc%late t!e c#ncentrati#n (in "&E"<) #, acetlsaliclic acid in t!e
Astandard aspirin s#l%ti#n'A
2' Usin& t!e relati#ns!ip ,#r dil%ti#ns:
mL
mg 1.6
=
mL 250
aspiin mg 400
c#ncentrati#n 2 v#l%"e D c#ncentrati#n 2 v#l%"e
calc%late t!e c#ncentrati#n (in "&E"<) #, acetlsaliclic acid ,#r eac!
#, t!e standard )#l%ti#ns A( 0( C( D and 6'
)#l%ti#n A: (0'; "<)(1'F "&E"<) D M(10 "<) M D 0'010 "&E"<
)#l%ti#n 0: (0': "<)(1'F "&E"<) D M(10 "<) M D 0'0F: "&E"<
)#l%ti#n C: (0'3 "<)(1'F "&E"<) D M(10 "<) M D 0'0:1 "&E"<
)#l%ti#n D: (0'2 "<)(1'F "&E"<) D M(10 "<) M D 0'032 "&E"<
)#l%ti#n 6: (0'1 "<)(1'F "&E"<) D M(10 "<) M D 0'01F "&E"<
3' Deter"ine t!e c#ncentrati#n ("&E"<) rati#s #, t!e ,#ll#$in& s#l%ti#ns'
c#nc 0Ec#nc A: 0'0F:E0'010 D '10
c#nc CEc#nc A: 0'0:1E0'010 D 'F0
c#nc DEc#nc A: 0'032E0'010 D ':0
c#nc 6Ec#nc A: 0'01FE0'010 D '20
NOT6: All s#l%ti#ns are c#"pared t# )#l%ti#n A +eca%se all #, t!e
aspirin s#l%ti#ns $ill +e dil%ted as )#l%ti#n A $as dil%ted' (T!e
aspirin ta+let $as diss#lved and dil%ted t# 2;0 "<' A 0'; "<
sa"ple #, t!is s#l%ti#n $as t!en dil%ted t# 10'0 "<')
I, #% $ant a "#re c#ncentrated s#l%ti#n( sa 0'F "< #, t!e st#c/ s#l%ti#n
dil%ted t# 10'0 "<( and called t!is )#l%ti#n 3( t!e c#ncentrati#n #, t!is
s#l%ti#n $#%ld +e:
)#l%ti#n 3: (0'F "<)(1'F "&E"<) D M(10 "<) M D 0'09F0 "&E"<
and t!e rati# s#l%ti#n 3Es#l%ti#n A D 0'09FE0'010 D 1'2
:' :00 "& #, acetlsaliclic acid $as diss#lved and dil%ted t# "a/e
)#l%ti#n A' )ince all #, t!e aspirin s#l%ti#ns $ere diss#lved and dil%ted
e2actl t!e sa"e $a as )#l%ti#n A( $e can c#ncl%de t!at i, t!e
aspirin s#l%ti#n !as t!e sa"e a+s#r+ance as )#l%ti#n A( t!en t!e
aspirin ta+let "%st !ave c#ntained :00 "& #, acetlsaliclic acid'
3%rt!er"#re( since )#l%ti#n 0 !as less acetlsaliclic acid t!an
)#l%ti#n A + t!e ,racti#n c#nc 0Ec#nc A( $e can c#ncl%de t!at t!is
s#l%ti#n c#%ld !ave +een "ade + diss#lvin&:
and dil%tin& it as $e did ,#r )#l%ti#n A' 9e $ill call t!is ,racti#n t!e
A"& #, acetlsaliclic acid in )#l%ti#n 0A +eca%se( i, an aspirin s#l%ti#n
!as t!e sa"e
a+s#r+ance as )#l%ti#n 0( $e can c#ncl%de t!at t!e ta+let
c#ntained t!is "an "&
#, acetlsaliclic acid'
Calc%late t!e A"& #, acetlsaliclic acidA ,#r eac! #, t!e standard
s#l%ti#ns'
)#l%ti#n 0: 0'10(:00 "&) D 320 "&
)#l%ti#n C: 0'F0(:00 "&) D 2:0 "&
)#l%ti#n D: 0':0(:00 "&) D 1F0 "&
)#l%ti#n 6: 0'20(:00 "&) D 10 "&
;' On a &rap! $it! appr#priate precisi#n( pl#t a+s#r+ance vs' A"& #,
acetlsaliclic acid'A A+s#r+ance s!#%ld +e #n t!e vertical a2is and
A"& #, acetlsaliclic acidA s!#%ld +e #n t!e vertical a2is'

Co""e#cial
P#ouct
%T Calculate
A$%o#$ance
Osc# Dr%& 23': 'F31
A%&i#in
P#ouct

Calculate
A$%o#$anc

E'&e#i"ent
al

Acce&te
"()ta$let
co%t &e#
ta$let
acid cylis acetylsali of mg 400 x
A Conc
B Conc
= B Solution in acid cylic acetylsali of mg
e "()ta$let
Al/a-)eltHer
I
';1 30F 32:
Osc# Dr%& 'F31 330 32;
A))6))>6NT
1' .ive st%dents an %n/n#$n s#l%ti#n and as/ t!e" t# deter"ine t!e "&
#, aspirin t!at
it represents %sin& t!e standard c%rve'
2' Usin& t!e A)tandard Aspirin )#l%ti#nA( "a/e a s#l%ti#n $!ic! $#%ld +e
e4%al t# 2;0
"& #, aspirin' 7eri, t!is $it! t!e data ,r#" t!e )pec 20'
R636R6NC6
Central 8ennslvania Ass#ciati#n #, C!e"istr Teac!ers in C##perati#n $it!
N)3( 5%niata C#lle&e( and 8rivate Ind%str' (1990)' )t%dent <a+#rat#r
>an%al ,#r 62cellence'