Copper Sulfate Analysis Using the Spectronic 20
Standard Solutions of Copper. Each pair of students
makes up one standard CuSO4 solution.
Concentrations should be 0.13M, 0.11M, 0.090M, and 0.070M (0.050M,
0.15M
are optional) as assigned by the instructor. Use 50 ml volumetric
flasks
and solid CuSO4 × 5 H2O.
Weigh the copper sulfate on the analytical balances
and record all digits. Take care to transfer all the
copper salt into
the volumetric flask. Add about 10 mls of DI water and then 20
drops
of 6 M sulfuric acid to get
the salt into solution. Then dilute to the
mark with
DI water. Dilute exactly to the mark; the bottom of the
menicus must touch the reference line. Start over (cheerfully) if
you have any doubt that you made up
the solution
correctly. Follow the same procedure for the unknown copper salt.
All groups must work together to make one solution from the unknown
copper salt using (of course) a carefully weighed amount of the
salt. The instructor
will provide copper unknown solutions A and B.
Using the Spec 20. Each pair should have a digital Spec 20. Examine the colors of light produced by the Spec 20 at 700 nm, 650 nm, 600 nm, 550 nm, 500 nm, 450 nm, and 400 nm. This can be done by placing a strip of white paper in a test tube and inserting the tube into the Spec 20. The tube opens the shutter so that the light will hit the paper. The light is dim, so the room lights should be out while the you look into the Spec 20.
Adjusting the Spec 20. Use the left knob to make the Spec 20 read 0% T with no tube present (shutter closed, no light hitting the detector). Use the right knob to adjust for 100% T with a water blank (shutter open, maximum light hitting the detector).
Finding the best wavelength. Using solution A, measure
the absorbance at different wavelengths. Every time the wavelength
is changed, the Spec 20 must be readjusted for 0% T and 100% T.
Each pair writes their results on the board. The class then picks the
best wavelength for analysis. What color is this wavelength? Why?
Alternatively (and faster!) Use an Ocean Optics
spectrometer to determine the best wavelength for analysis.
Measurements. Standard solutions are shared among the
pairs; each pair makes a calibration curve using data from just one Spec 20
(don't mix data from different spectrometers!). Each group
records data for unknowns
A and B, and the unknown copper salt solution. You should record
about four
or five absorbances for each solution
to assess the reproducibility
of the measurement. As you work with a sample, switch back and
forth between the copper sample and the water blank, making sure that
the water blank always reads 100% T. (Adjust the right knob until
it does.)
Write your
best absorbance for each known solution on the board for all to
see! Do the same for solutions A and B.
Analysis. Put all
measurements for knowns into a Excel spreadsheet with concentrations in
one column and absorbances in another. Do not average the
absorbances for a single known solution; instead, put all the
measurements into the graph. Graph the data. Try fits with
and without a y-intercept. Be sure to plot the fit line through the
data points.
Compare the fits that you get in Excel using Excel's LINEST function,
its REGRESSION function in the Data Analysis Toolpak, and the Trend
Line feature available for charts. All these methods should give
the same
equation for a line, but some methods are more helpful because the
results can be used elsewhere in the spreadsheet. The use of Trend Line alone is strongly
discouraged! In other words, don't stop fitting simply
because you have a trend line on your graph.
In the Excel spreadsheet
determine the concentrations of unknown solutions
A and B; use equation 4-15 in Harris’s textbook to estimate the error in the
concentration of the unknowns.
In the spreadsheet perform
the calculations necessary to find the % Cu in the unknown
copper
salt, and of course estimate the error or uncertainty in the % Cu. Then
each
pair should try to identify
the unknown copper salt using their value of the % Cu. The Merck Index lists many copper
salts and gives the % Cu of the salt, so the Merk Index is especially
helpful as you explore possible identities for the unknown. The
error in the % Cu is important because it will help you decide what
salts are possible and which can be ruled out by your experiment.