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UEMK2023
INSTRUMENTAL ANALYSIS
Lab Report
Objectives
Introduction
Aspirin (acetylsalicylic acid) is a salicylate drug which important to be used for its analgesic,
antipyretic and anti-inflammatory properties. Aspirin is a white, crystalline, weakly acidic substance
which melts at 135C. It is one of the most widely used medications as a pain reliever.
Direct calibration curve method can be applied for analyzing unknown sample only when standard
solutions and unknown solution are prepared and measured under exactly the same conditions.
However, substances other than analyte will affect absorbance reading of sample solution at
wavelength chosen for analysis, known as matrix effects. This can be avoid by conducting the standard
addition method so that the matrix present in the sample can affect the absorbance readings for both
the analyte in the standard and the sample. Therefore, it is possible to analyze the analyte accurately
even in the presence of matrix.
Method of standard additions can be used to improve the result in certain circumstances the matrix,
which contributes significantly to the absorbance of a sample and is also highly variable. The basic
idea is to add standard to analyte sample so that the standard is subjected to the same matrix effects as
analyte, this method assumes that the system obeys the Beers Law. Aspirin (acetylsalicylic acid)
amount in commercial analgesics can be determined when it has been hydrolyzed to salicylic acid and
diluted to a concentration where the law is obeyed.
Reagents and Apparatus
Standard Solution
1.2
y = 0.0242x + 0.0655
1 R = 0.9912
Absorbance
0.8
0.6 Absorbance
0.2
0
0 10 20 30 40 50 60
Concentration(mg/L)
Sample Calculations
For M1,
1000mg
0.1g(1g )
M1 =
0.1L
100cm3 ( )
100cm3
M1 = 1000mg/L
M1 V1 = M2 V2
M1 V1
M2 =
V2
0.1L
(1000mg/L)(1.00cm3 )( )
M2 = 100cm3
0.1L
100cm3 ( )
100cm3
M2 = 10mg/L
Aspirin Solution
Sample Calculations
At volume of 10cm3,
y = 0.0242x + 0.0655
When y = 0.114,
0.114 0.0655
x=
0.0242
x = 2.00mg/L
2.004mg 0.1L
Weight = ( ) (250cm3 )( )
L 100cm3
Weight = 0.5mg
Percentage Difference
|5mg5.035mg|
= 100%
5mg
= 0.7%
Discussion
The purpose of this lab was to determine the actual amount of acetylsalicylic acid in the actual
aspirin tablets. Aspirin, is a widely known drug for its analgesic, antipyretic, and anti-inflammatory
properties, is a compound derived from two acids namely acetic acid and salicylic acid. To analyse the
composition of an aspirin sample or the amount of acetylsalicylic acid, the hydrolysis of the sample
by alkali into neutrality is required. By using the Double Beam Ultraviolet Absorption
Spectrophotometry, we were able to measure the absorbance of various dilutions to find the
relationship between the absorbance and the concentration of acetylsalicylic acid in the solution.
First, a stock solution was prepared by weighing 0.1g of pure salicylic acid and quantitatively
transfer to a 100cm3 volumetric flask. The substance was then mixed and diluted with 0.1 mol/L NaOH
solution to form the stock solution. The series of standard solution were then prepared by transferring
the stock solution into a 100cm3 volumetric flask. The concentration of the series standard solution
were 10mg/L, 20mg/L, 30mg/L and 40mg/L respectively.
The graph peaks are labelled and they shows the absorbance of each standard solution. The
graph result is chosen after the 250nm wavelength because the graph form before 250nm is considered
as noise due to the presence of impurities. From the graph, we find that it is a linear relationship and
we are able to calculate the amount of acetylsalicylic acid in the tablets after determining the
absorbance of solution. The amount of acetylsalicylic acid we found in the table was 0.035g more than
the amount stated 0.5g. We found the value is 0.7% more than the stated amount as shown in the
calculation part.
There are some precautions to be taken in order to get a more precise result. The cuvette that
used to contain the standard solutions needs to be wiped cleanly after each test. During the experiment,
we carefully discarded the cuvette and cleaned it every time before we filled it with another standard
solution with different concentration to prevent changes in concentration of the solution. Furthermore,
the way when we inserted the cuvette into the Varian Cary 100 UV-Vis double-beam scanning
spectrophotometer must be taken precisely. The clear and smooth surface of the cuvette must face the
light source and allows the light to pass through. While conducting the experiment, we accidentally
inserted the cuvette with rough surface facing the light source. Therefore, a mistake of curve, attached
in the appendix, which is very different with the other curves, was recorded in our result. Besides, the
original stock acetylsalicylic solution might have some impurities that lead to a secondary reaction that
produced particles that absorb the UV light and affected the experimental result.
Besides the method of Double Beam Ultraviolet Absorption Spectrophotometry, the
experiment can be conducted by using back titration method, diazotization by using 2,4-
dichloroaniline and HPLC method.
Q1.
In this experiment, salicylic acid stock solution prepared by using 0.1 mol/dm3 sodium
hydroxide (NaOH) because NaOH can hydrolyse the salicylic acid into sodium salicylate. This
reaction assures that the aspirin is 100% hydrolysed into salicylic acid. Then, the salicylic acid will be
diluted by NaOH and reach a certain concentration.
After stock solution has been done, it will obey Beers law and its concentration can be
calculated. The reaction of salicylic acid hydrolysed by NaOH is as below:
If the salicylic acid is not 100% hydrolysed, it cannot detect the accurate wavelength of salicylic
acid in the experiment because the other compound will affect the wavelength of the solution.
Q2.
From this experiment, the wavelength we obtained is 296nm and 297nm. In reality, the
wavelength of salicylic acid approaches 297 nm so this result can be accepted.
The absorbance of the abfive standard solutions have different values which are 0.278, 0.553,
0.831, 1.064 and 1.233 due to the different concentration of stock solution.
By using Beers Law, the absorbance (A) is equal to molar absorptivity () of solution times
the path length (b) and times the concentration of the solutions(c). In these cases, the path length and
molar absorptivity are constant because of same wavelength which is around 296nm and 297nm.
Therefore, we can generally conclude that the absorbance is proportional to the concentration of
solution.
The absorbance of the solution with ratio of 1:10 is the same with standard solution 2. Thus,
we can confirm that the concentration of the unknown solution is the same with standard solution 2
which is 20mol/L.
Conclusion
A. M. Helmenstine. (2017). Dilutions from Stock Solutions. Retrieved, 15 June 2017, from
http://chemistry.about.com/od/chemistryquickreview/a/dilutionmath.htm
D. A. Skoog, D. M. West, F.J. Holler, S.R. Crouch. (2014). Fundamentals of Analytical Chemistry,
California: Brooks/Cole- Thomson Learning.,
J. Clark. (2006). A Double Beam Uv-visible Absorption Spectrometer. Retrieved, 15 June 2017, from
http://www.chemguide.co.uk/analysis/uvvisible/spectrometer.html
W. Reusch. (2013). Visible and Ultraviolet Spectroscopy. Retrieved, 16 June 2017, from
http://www2.chemistry.msu.edu/faculty/reusch/VirtTxtJml/Spectrpy/UV-Vis/spectrum.htm