DETERMINATION OF A PHOSPHATE MIXTURE

OBJECTIVE
The purpose of this experiment is to identify and determine the concentration of phosphate species in an
unknown mixture. The determination will be by acid/base titrimetry using an automatic titrator.
BACKGROUND
According to the line diagram for phosphoric acid:

H+

H3PO 4

2.15

H2PO 44.68

7.20

HPO 42-

12.15

3-

PO4

OH

9.68

each phosphate containing species can exist by itself or in compatible combination with its nearest
neighbor. Titration of an aliquot of an unknown with either standard HCl and/or NaOH will provide the
needed information to identify and determine the amount of the phosphate specie(s) in the solution.
PROCEDURE
Obtain a phosphate mixture solution and quantitatively transfer it to a 100 mL volumetric flask. Dilute to
the mark and mix well. This will be your unknown. Test a small sample of this solution with universal
indicator paper to determine if the solution is acidic or basic (use a drop or two from the solution you use to
rinse your 20 mL pipette). If the solution is not clearly acidic or basic, transfer a 20 mL aliquot to a 250
mL beaker and dilute to about 100 mL. Test this sample to determine if it is neutral by placing it on an
auto titrator and measuring the pH in the manual mode (as was done in the previous phosphate
experiment). Based upon the initial pH of the solution you will know whether you need HCl or NaOH or
both for the titration of your unknown. If the solution is acidic, titrate with standard base (Phosphate
Method). If the solution is basic, titrate with standard acid (PO4 Method). If neutral, titrate one 20 mL
aliquot with standard acid and another 20 mL aliquot with standard base. Decide what you need to do and
why. Explain your reasoning in your laboratory notebook. You have standardized the HCl and NaOH in
previous experiments use these values in your calculations.
If you keep the amount of diluted unknown used to rinse your pipette to 10-15 mL, you will have enough
of the diluted unknown for 4-20 mL trials. If you have an unknown that tests neutral, titrate two 20 mL
aliquots with acid and two with base.
NOTE 1: The automatic titrator will not detect an endpoint for the reaction of HCl with H 2PO4- or NaOH
with HPO42-.
NOTE 2: The PO43- primary standard is only 95% pure. The impurity affects the second endpoint and is
most likely HPO42-. For this unknown calculate the mmol/mL of PO43- from the first endpoint.
NOTE 3: EP1 is always the more acidic endpoint and EP2 is the more basic endpoint. The 1 and 2 do not
define the order of the endpoints.

RESULTS
Identify each phosphate species present in your unknown (NOTE: Some unknowns have only one species
others may have two). Report concentration in scientific notation with 3 decimal places as millimoles of
the phosphate containing species per milliliter in your diluted unknown. If you have more than one
phosphate containing species in your unknown, fill out a separate card for each species.

WASTE DISPOSAL
The materials used in this experiment are not hazardous. Solutions can be disposed down the drain.