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Fluoride Deter PDF
Fluoride Deter PDF
Purpose: determine the amount of fluoride ion in samples of toothpaste, mouthwash, and
tap water using standard addition and serial dilution (calibration) methods.
Background Reading:
Background
One type of an ion selective electrode (ISE) with which you have experience already is
the pH meter, which selectively measures the amount of H3O+ in solution. There are
several other types of ion selective electrodes, including the one used in this experiment
which measures for fluoride ion.
Fluoride ion is a necessary evil, good at a low concentrations but detrimental at higher
ones. At 1 ppm ( 1ppm = 1 mg/L) it prevents tooth decay, which is why it is added to
water and dental products, but in the 2- 13.7 ppm range, staining, cracking, mottling, and
pitting of the teeth can result. At higher concentrations, it is a known cause of bone
cancer.
Water is generally fluoridated to 1 ppm but in some areas, such as the southwestern
United States, where fluoride exceeds 4 ppm, it is reduced to acceptable levels. You can
go online to www.epa.gov and follow the link for the Office of Water to obtain water
quality report for a particular area.
This experiment requires the use of an ion selective electrode (ISE), to detect fluoride.
Refer to p. 672 of your text for a detailed description of the fluoride electrode.
Briefly, the electrode contains a crystal of lanthanum fluoride as the membrane, through
which fluoride ions are mobile. The crystal is doped with europium fluoride to increase
conductivity. When immersed in a solution containing fluoride ions, a potential develops
across the membrane measured against a constant reference potential with a standard
pH/mV meter. The Nernst equation describes the measured potential as a function of the
activity of fluoride ions in solution.
E = Eo - EJ + (RT/ZF) ln a
Where
The activity, a, represents the effective concentration while the total fluoride ion
concentration may include some bound ions as well. The electrode responds only to free
ions so it is important to avoid the formation of complexes that are meant to be measured.
In this case, complexation would lower the activity and therefore the electrode response.
The addition of a high concentration of non-interfering ions in the buffer help maintain a
constant total ionic strength and prevents a fluctuation in the activity coefficient of the
ion being measured.
pH and ionic strength
Potential is a function of activity rather than concentration, but if the ionic strength is
kept constant, then the activity will then be proportional to the concentration.
The ionic strength is defined as
I= ½ Σ cizi2
i
ai= γi ci
where γ is the activity coefficient. Making substitutions into the Nernst equation
E = Eo - EJ + (RT/ZF) ln a
Note that the terms in the argument of the log are separated and ln is converted to log in
the last term. Also, if we consider that
pF = -log CF
E = (59.16) pF + constant
The significance of this equation is that it shows when one changes the concentration of
the fluoride sample by a factor of ten, the potential changes by 59 mV. This is a good
way to check if the electrode is functioning properly and that you are observing
“Nernstian” behavior.
PROCEDURAL INFORMATION
Buffer
Prepare 500.00 ml of pH 5.25 acetic acid/sodium acetate buffer. Before class calculate
the mass of sodium acetate and volume of 1.0 M acetic acid to make a buffer with a pH
of 5.25. The total acetate (HA and A-) must equal 0.5 M. Test the pH of your buffer with
a pH strip and add dropwise 6M NaOH if necessary. Addition of base may also help in
dissolving the sodium acetate. STORE IN A PLASTIC BOTTLE.
Use a volumetric pipet to transfer 25.00 mL of your standard to a beaker and add
25.00 mL of buffer. Swirl solution gently before taking readings of you sample.
Before discarding the stock solution of 0.020M sodium fluoride, measure the potential of
the unbuffered solution to discover what effect the buffer has on the solution.
Use 25.00 mL of the excess 0.02 M sodium fluoride solution to make a 0.002M dilution
with DI water. As was done with the stock solution, add an equal amount of buffer to the
diluted solution to prepare the sample for a reading. Use the plastic beakers when taking
measurements. Continue to make serial dilutions until you have a total of five
measurements. Note that the electrode should be rinsed with DI water and blotted dry in
between measurements of each of the solutions you have made.
Now prepare four samples for analysis using four 100-mL volumetric flasks.
In each flask add 50 mL of buffer and 5 mL of tap water.
One sample will have no standard added to it and can simply be diluted to 100-mL with
water.
Before diluting the other three samples, add 10 mL of standard to one , 20 mL to another,
and 30 mL to the last one.
.
Make sure all solutions are mixed well before taking measurements.
Constant stirring is vital but avoid stirring vigorously enough to generate heat that will
affect the measurements. If the stirrer seems to produce heat, use a Styrofoam sheet or
wire gauze in between the stirrer and the beaker.
Rinse the electrodes with distilled water and blot dry in between .
Improper storage of the electrode can cause irreparable damage. Make sure at the end of
the day that the electrode is immersed in 10 ppm F- and that the electrode has filling
solution (4M KCl) up to the level of the filling hole.
STORAGE
When you are done for the day, the fluoride electrode must be stored in 10ppm
fluoride solution with an equal volume of buffer added. Make sure that the
electrode remains filled with the 4M KCl filling solution. The electrode should never
be stored in water as it will disrupt the behavior of the electrode itself.
NAME___________________ Kit #________
Partner___________________ Balance #________
Date___________________ Fluoride Ion Electrode #________
REPORT SHEET
Using the standard addition curve, what is the concentration of fluoride ion in your
water sample? How does this compare to results from the calibration curve?
Discuss the difference in potential between the stock solution of 0.020 M NaF with and
without buffer.
Suppose you have a contaminant, such as an organic solvent, in the sample. Which
method- the calibration curve method or standard addition method would be more
advantageous in terms of data analysis. Which method works better? Why do you think
this is more advantageous?