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Objectives
I. To use ultraviolet (UV) to visible light as a stimulus to ibuprofen complexed with
cobalt and measure the extent of its absorption by the analyte.
II. To estimate the concentration of ibuprofen from commercially available samples
using the Beer-Lambert Law.
Motivation
A. Theoretical Background
UV-Vis spectrophotometry is widely used for the quantitative determination
of a large number of inorganic, organic, and biological species (2). All organic
compounds are capable of absorbing electromagnetic radiation, because all contain
valence electrons that can be excited to higher energy levels. In this case, ibuprofen
will be the compound subjected to the UV to visible light.
Transmittance, the ratio between transmitted radiant power and incident
radiant power, and absorbance, the common logarithm of the reciprocal of
transmittance, is not normally determined inside the laboratory, but instead inside a
transparent container or a cell. After the spectrophotometer has found the absorbance
of a certain concentration of the sample, one could make use of a linear equation
relating concentration and absorbance which is rooted upon the Beer-Lambert Law:
A = εlc (Equation 1)
such that A refers to absorbance, ε is the molar absorptivity which is a measure of
how well a chemical species absorbs a given wavelength of light, l is the path length
of the cell holder which is usually 1 cm, and c is the concentration of the sample (2).
Despite this, the Beer-Lambert Law is limited in the sense that it can only
describe the absorption behavior of dilute solutions, because of solute-solvent,
solute-solute interactions or hydrogen bonding can affect the absorptivity of the
analyte (2). One case in which this occurs is when a particle affects the charge
distribution of its neighboring particles which changes the analyte’s ability to absorb
at a given wavelength.
B. Basic Instrumentation
Reagents
Reagents Physical and Chemical Safety Precautions
Properties
Methodology (9)
I. Calibration Curve
A. Make 100 mL 0.2 M stock cobalt chloride solution.
B. For standard solutions, dissolve 10 mg pure ibuprofen in 100 mL water
(pH=8.5) as stock.
C. Prepare five standard solutions by mixing 10 mL pure ibuprofen stock in 10
ml varying concentrations of cobalt chloride (0.01, 0.02, 0.04, 0.08, 0.1).
D. Shake standard solutions for approximately 5 minutes at room temperature.
E. Make 100 ml stock solution of benzene and cyclohexane in 2:3 ratio. Extract
each by 4 mL organic phase mixture from 2:3 benzene-cyclohexane mixture.
Place the mixture in a separatory funnel, shaken and vent frequently. The top
layer or the organic layer is then separated out of the mixture.
F. Measure in UV-Vis at 603 nm.
II. Sample Preparation and Analysis
A. Crush 10 ibuprofen tablets using a mortar and pestle.
B. Dissolve a quantity of this equal to one tablet in water (pH=8.5) and add one
drop NH4OH solution.
C. Transfer in 100 mL volumetric flask and fill to mark with water.
D. Make 5 10mL aliquots and add 0.01, 0.02, 0.04, 0.08, 0.1M of cobalt chloride
by standard addition.
E. Extract each by 4 mL organic phase mixture from 2:3 benzene-cyclohexane
mixture.
F. Measure in UV-Vis at 603 nm and compare to calibration curve.
III. Waste Disposal
A. Dispose used organic solvents in Non-Halogenated Waste container.
B. Dispose all other waste accordingly.
References
(1) Ogbru O. Ibuprofen [Internet]. [Place Unknown]: MedicineNet.com; [Date Unknown]
[updated 2017 Nov 1; cited 2018 Jun 10]. Available from:
https://www.medicinenet.com/ibuprofen/article.htm#what_is_ibuprofen_how_does_it
_work_mechanism_of_action.
(2) Skoog DA, Holler FJ, Crouch SR. Principles of Instrumental Analysis. 6th Ed.
Boston, MA, USA: Cengage Learning; 2007.
(3) Ibuprofen MSDS [Internet]. US: Sciencelab.com; 2005 Oct 9 [updated 2013 May 21;
cited 2018 Jun 9]. Available from:
http://www.sciencelab.com/msds.php?msdsId=9924344
(4) Water MSDS [Internet]. US: Sciencelab.com; 2005 Oct 10 [updated 2013 May 21;
cited 2018 Jun 9]. Available from:
http://www.sciencelab.com/msds.php?msdsId=9927321
(5) Benzene MSDS [Internet]. US: Sciencelab.com; 2005 Oct 10 [updated 2013 May 21;
cited 2018 Jun 11]. Available from: www.sciencelab.com/msds.php?msdsId=9927339
(6) Cyclohexane MSDS [Internet]. US: Sciencelab.com; 2005 Oct 10 [updated 2013 May
21; cited 2018 Jun 11]. Available from:
http://www.sciencelab.com/msds.php?msdsId=9927145
(7) Cobalt Chloride MSDS [Internet]. US: Sciencelab.com; 2005 Oct 9 [updated 2013
May 21; cited 2018 Jun 11]. Available from:
http://www.sciencelab.com/msds.php?msdsId=9923522
(8) Ammonium hydroxide MSDS [Internet]. US: Sciencelab.com; 2005 Oct 9 [updated
2013 May 21; cited 2018 Jun 11]. Available
from:http://www.sciencelab.com/msds.php?msdsId=9922918
(9) Jasim HH, Abed NK. Determination of Ibuprpfen in Aqueaus Solutions and
Pharmacetical Preparations by UV-VIS Spectrophotometric. Journal of Al-Nahrain
University; 2015 Jun. 18 (2):1-9. Available from:
http://jnus.org/pdf/1/2015/1/1093.pdf
Signature 6/11/2018