University of Pittsburgh at Bradford 019

Science In Motion

Chemistry Lab

SPECTROPHOTOMETRIC ANALYSIS OF ASPIRIN

Introduction:
A co ored com! e" is formed bet#een as!irin and the iron $III% ion& 'he intensity of the co or is direct y re ated to the concentration of as!irin !resent( therefore) s!ectro!hotometric ana ysis can be used& A series of so utions #ith different as!irin concentrations #i be !re!ared and com! e"ed& 'he absorbance of each so ution #i be measured and a ca ibration 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 sa icy ate dianion&

* * C C+ , C * *+ $s% . ,*+0 $a-% *0 C *0 * * $a-% . C+,C * 0 $a-% . /+/*$ %

'he addition of acidified iron $III% ion !roduces the vio et tetraa-uosa icy atroiron $III% com! e"&
.

*0 0 . 12e$+/*%4 3 C * *
.,

* C *

2e$+/*%5 *

. + /* . + ,*

Purpose:
'he !ur!ose of this ab is to determine the amount of as!irin in a commercia as!irin !roduct& 'his ab may a so be used to determine the !urity of the as!irin !roduced in the Microsca e Synthesis of Acety sa icy ic Acid ab&

Equipment / M teri !s:

1/6 mL er enmeyer f as7s / cuvettes 10 mL graduated cy inder 6 mL !i!et /60 mL vo umetric f as7 acety sa icy ic acid 60 mL vo umetric f as7 1 M 8a*+ ana ytica ba ance $o!t&% 0&0/ M iron $III% buffer s!ectro!hotometer disti ed #ater commercia as!irin !roduct or as!irin the student has made

S "et#:
1

A #ays #ear gogg es and an a!ron in the ab& Be carefu #hi e boi ing the sodium hydro"ide so ution& 8a*+ so utions are dangerous) es!ecia y #hen hot&

Procedure:
P rt I: M $in% St nd rds& 1& Mass 500 mg of acety sa icy ic acid in a 1/6 mL 9r enmeyer f as7& Add 10 mL of a 1 M 8a*+ so ution to the f as7) and heat unti the contents begin to boi & /& :uantitative y transfer the so ution to a /60 mL vo umetric f as7) and di ute #ith disti!!ed ' ter to the mar7& ,& Pi!et a /&6 mL sam! e of this as!irin standard so ution to a 60 mL vo umetric f as7& ;i ute to the mar7 #ith a (&() M iron *III+ so!ution& Labe this so ution <A)< and ! ace it in a 1/6 mL 9r enmeyer f as7& 5& Pre!are simi ar so utions #ith /&0) 1&6) 1&0) and 0&6 mL !ortions of the as!irin standard& Labe these <B) C) ;) and 9&< P rt II: M $in% n un$no'n "rom t ,!et& 1& P ace one as!irin tab et in a 1/6 mL 9r enmeyer f as7& Add 10 mL of a 1 M 8a*+ so ution to the f as7) and heat unti the contents begin to boi & /& :uantitative y transfer the so ution to a /60 mL vo umetric f as7) and di ute #ith disti!!ed ' ter to the mar7& ,& Pi!et a /&6 mL sam! e of this as!irin tab et so ution to a 60 mL vo umetric f as7& ;i ute to the mar7 #ith a (&() M iron *III+ so!ution& Labe this so ution <un7no#n)< and ! ace it in a 1/6 mL 9r enmeyer f as7& P rt 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 acety sa icy ic acid !roduct and record the mass in the data section& P ace it in a 1/6 mL 9r enmeyer f as7& Add 10 mL of a 1 M 8a*+ so ution to the f as7) and heat unti the contents begin to boi & /& :uantitative y transfer the so ution to a /60 mL vo umetric f as7) and di ute #ith disti!!ed ' ter to the mar7& ,& Pi!et 10 mL sam! e of this as!irin so ution to a 60 mL vo umetric f as7& ;i ute to the mar7 #ith a (&() M iron *III+ so!ution& $=hen adding 0&0/ M iron $III% so ution) the co or shou d be obvious y !ur! e& If it is not) sto! adding the 0&0/ M iron $III% so ution) and a ert your instructor&% Labe this so ution <un7no#n)< and ! ace it in a 1/6 mL 9r enmeyer f as7& P rt 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 se ect absorbance& /& Ad?ust the #ave ength to /0( nm by !ressing the nm arro# u! or do#n& ,& Insert the b an7 $0!!m @ cuvet of iron buffer% into the ce ho der and c ose the door& Position the ce so that the ight !asses through c ear #a s& 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 b an7 to 0 absorbance& 6& Aecord the absorbance of the 0!!m so ution& /

4& *btain absorbance readings for each of the other standard so utions& Aecord the resu ts 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%&

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Spectrop-otometric An !#sis o" Aspirin

Student E5 !u tion
,

Spectrophotometric Analysis of Aspirin Standards Data

6 t : So!ution A B C ; 9 2 Concentr tion *m%/L+ A,sor, nce

Spectrophotometric Analysis of Unknown Aspirin

6 t : So!ution A B C ; 9 unknown Concentr tion *m%/L+ A,sor, nce

For commerci ! Product: amount of as!irin in un7no#n acce!ted va ue !ercent error For microsc !e ! , product: 5 mg mg EEEEEEEEEEEEEEEEEEEF

mass of im!ure !roduct mass of as!irin in !roduct F !urity of !roduct

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7uestions:
1& 9"! ain #hy the #ave ength of 6,0 nm #as used&

/& ,&

+o# did the concentration of your as!irin so ution com!are to the acce!ted va ueG Is it better to buy generic or brand name as!irinG Su!!ort your conc usion&