University of Pittsburgh at Bradford Science In Motion Chemistry Lab

019
SPECTROPHOTOMETRIC ANALYSIS OF ASPIRIN
Introduction:
A coored com!e" is formed bet#een as!irin and the iron $III% ion& 'he intensity of the coor is
directy reated to the concentration of as!irin !resent( therefore) s!ectro!hotometric anaysis can be used&
A series of soutions #ith different as!irin concentrations #i be !re!ared and com!e"ed& 'he absorbance
of each soution #i be measured and a caibration curve #i be constructed& Using the standard curve)
the amount of as!irin in a commercia as!irin !roduct can be determined&
'he com!e" is formed by reacting the as!irin #ith sodium hydro"ide to form the saicyate dianion&
* C C+
*
C
*
*+
,
$a-% . C+ C * $a-% . /+ *$%
*
C
*
*
0
0
$s% . ,*+ $a-%
0
*
0
, /
'he addition of acidified iron $III% ion !roduces the vioet tetraa-uosaicyatroiron $III% com!e"&
*
C
*
*
0
0
. 12e$+ *% 3
/ 4
.,
*
C
*
*
.
/ 5
2e$+ *%
/ ,
.
. + * . + *
Purpose:
'he !ur!ose of this ab is to determine the amount of as!irin in a commercia as!irin !roduct& 'his ab
may aso be used to determine the !urity of the as!irin !roduced in the Microscae Synthesis of
Acetysaicyic Acid ab&
Equipment / Mteri!s:
1/6 mL erenmeyer fas7s / cuvettes
10 mL graduated cyinder 6 mL !i!et
/60 mL voumetric fas7 acetysaicyic acid
60 mL voumetric fas7 1 M 8a*+
anaytica baance $o!t&% 0&0/ M iron $III% buffer
s!ectro!hotometer distied #ater
commercia as!irin !roduct or as!irin the student has made
S"et#:
1
A#ays #ear gogges and an a!ron in the ab&
Be carefu #hie boiing the sodium hydro"ide soution& 8a*+ soutions are dangerous)
es!eciay #hen hot&
Procedure:
Prt I: M$in% Stndrds&
1& Mass 500 mg of acetysaicyic acid in a 1/6 mL 9renmeyer fas7& Add 10 mL of a 1 M 8a*+
soution to the fas7) and heat unti the contents begin to boi&
/& :uantitativey transfer the soution to a /60 mL voumetric fas7) and diute #ith disti!!ed 'ter to the
mar7&
,& Pi!et a /&6 mL sam!e of this as!irin standard soution to a 60 mL voumetric fas7& ;iute to the mar7
#ith a (&() M iron *III+ so!ution& Labe this soution <A)< and !ace it in a 1/6 mL 9renmeyer fas7&
5& Pre!are simiar soutions #ith /&0) 1&6) 1&0) and 0&6 mL !ortions of the as!irin standard& Labe these
<B) C) ;) and 9&<
Prt II: M$in% n un$no'n "rom t,!et&
1& Pace one as!irin tabet in a 1/6 mL 9renmeyer fas7& Add 10 mL of a 1 M 8a*+ soution to the
fas7) and heat unti the contents begin to boi&
/& :uantitativey transfer the soution to a /60 mL voumetric fas7) and diute #ith disti!!ed 'ter to the
mar7&
,& Pi!et a /&6 mL sam!e of this as!irin tabet soution to a 60 mL voumetric fas7& ;iute to the mar7
#ith a (&() M iron *III+ so!ution& Labe this soution <un7no#n)< and !ace it in a 1/6 mL 9renmeyer
fas7&
Prt III: M$in% n un$no'n "rom t-e product o" t-e Microsc!e S#nt-esis o" Acet#!s!ic#!ic Acid
!,&
1& Mass a of the acetysaicyic acid !roduct and record the mass in the data section& Pace it in a 1/6
mL 9renmeyer fas7& Add 10 mL of a 1 M 8a*+ soution to the fas7) and heat unti the contents
begin to boi&
/& :uantitativey transfer the soution to a /60 mL voumetric fas7) and diute #ith disti!!ed 'ter to the
mar7&
,& Pi!et 10 mL sam!e of this as!irin soution to a 60 mL voumetric fas7& ;iute to the mar7 #ith a (&()
M iron *III+ so!ution& $=hen adding 0&0/ M iron $III% soution) the coor shoud be obviousy !ur!e&
If it is not) sto! adding the 0&0/ M iron $III% soution) and aert your instructor&% Labe this soution
<un7no#n)< and !ace it in a 1/6 mL 9renmeyer fas7&
Prt I.: Testin% t-e So!utions&
1& 'urn on the s!ectro!hotometer& Press the A/T/C button on the S!ec /0 >enesys to seect absorbance&
/& Ad?ust the #aveength to /0( nm by !ressing the nm arro# u! or do#n&
,& Insert the ban7 $0!!m @ cuvet of iron buffer% into the ce hoder and cose the door& Position the ce
so that the ight !asses through cear #as& 1Aemember to #i!e off the cuvet #ith a Bim#i!e before
inserting it into the instrument&
5& Press ( A2S/3((4 T to set the ban7 to 0 absorbance&
6& Aecord the absorbance of the 0!!m soution&
/
4& *btain absorbance readings for each of the other standard soutions& Aecord the resuts on
the data sheet&
C& *btain an absorbance reading for the un7no#n sam!e$s%&
D& Ma7e a gra!h of concentration $"0a"is% vs& absorbance $y0a"is%&
9& 2rom the standard curve) determine the concentration of as!irin in the un7no#n
Sam!e$s%&
8ameEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEE
;ateEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEEE
Spectrop-otometric An!#sis o" Aspirin
Student E5!ution
,
Spectrophotometric Analysis of Aspirin Standards Data
6t:
So!ution Concentrtion *m%/L+ A,sor,nce
A
B
C
;
9
2
Spectrophotometric Analysis of Unknown Aspirin
6t:
So!ution Concentrtion *m%/L+ A,sor,nce
A
B
C
;
9
unknown
For commerci! Product:
amount of as!irin in un7no#n mg
acce!ted vaue mg
!ercent error EEEEEEEEEEEEEEEEEEEF
For microsc!e !, product:
5
mass of im!ure !roduct EEEEEEEEEEEEEEEEEEE mg
mass of as!irin in !roduct EEEEEEEEEEEEEEEEEEE mg
F !urity of !roduct EEEEEEEEEEEEEEEEEEEF
7uestions:
1& 9"!ain #hy the #aveength of 6,0 nm #as used&
/& +o# did the concentration of your as!irin soution com!are to the acce!ted vaueG
,& Is it better to buy generic or brand name as!irinG Su!!ort your concusion&
6