SF04 THE DETERMINATION OF QUININE IN BEVERAGES
Discussion
Solutions of quinine fluoresce strongly when excited by
radiation at 350 nm. The relative intensity of the fluorescent peak at 450 nm
provides a sensitive methode for the determination of quinine in bverages.
Preliminary measurements are needed to define a concentration regio in which
fluorescent intensity is either linear or nearly so. The unknown is then diluted
as necessary to produce readings within this range.
Preparation of reagens
(a) Sulfuric acid, 0.05 M. Add about 17 mL of 6 M H2SO4
to 2 L of distilled water.
(b) Quinine sulfate standard, 1 ppm. Weigh (to the nearest
0.5 mg) 0.100 g of quinine sulfate into a 1-L volumetrie flask, and dilute
to the mark with 0.05 M H2SO4 (sufficiënt for 60 to
70 analyses). Transfer 10.00 mL of this solution to another 1-L volumetrie
flask, and again dilute to the mark with 0.05 M H2SO4.
This latter solution contains 1 ppm of quinine; it should be prepared daily
and stored in the dark when not in use.
Procedure
Determination of a suitable concentration range
To find a suitable working range, measure the relative
fluorescent intensity of the 1 ppm standard at 450 nm (or with a suitable filter
that transmits in this range). Use a graduated cilinder to dilute 10 mL of the 1
ppm solution with 10 mL 0f 0.05 M H2SO4; again measure the
relative fluorescence. Repaeat this dilution and measurement proces until the
ralative intensity approches that of a blank consisting of 0.05 M H2SO4.
Make a plot of the data, and select a suitable range for the analyses (that is,
a regio within wich the plot is linear).
Preparation of a calibration curve
Use volumetrie glassware to prepare three or four standards that
span the linear regio; measure the fluorescence intensity for each. Plot the
data.
Analysis
Obtain an unknown. Make suitable dilutions with 0.05 M H2SO4
to bring its fluorescence intensity within the calibration range.
Calculate the parts per million of quinine in the unknown. |