Instructivo para metodologia de polarografia

2.3. Measurement Procedures

(a) Pipet out 50.00 mL of the potassium ferrocyanide solution into a clean 100 mL
beaker (with a stirrer bar. Place the cell on the stirrer.
(b) Mount the three electrodes (Indicator, I; Reference, R; Counter, C) on a ring
stand using the three mini-clamps. (Be sure that the clamps are insulated
electrically from the graphite electrodes; slip plastic tubing over the electrodes in
the clamped region, if necessary.)
(c) Position the ring stand, clamps and electrodes so that the 3 electrodes
submerged to a depth of about 1/2" below the solution surface in the 100 mL
sample beaker.
(d) Connect each electrode to the Polarograph using the three individual cables
marked "I", "R", and "C".
(e) Turn the Polarograph power switch to "ON". Adjust initial settings as indicated
in section 2 above. Turn power switch to "PEN". Adjust the pen displacement knob
so that the recorder pen is on the first major chartpaper line on the left hand side.
Mark this line as "zero current". Return power switch to "ON". Turn stirrer "ON".
(f) Switch the operating mode switch from "OFF" to "AUTOSCAN"; move the meter
switch to "SCAN V." position; change the power switch to the "PEN" position;
adjust the sensitivity control to an appropriate level ( about 4 Amp full scale); turn
off the stirrer.
(g) When the recorder pen stops drifting (~30 sec.), turn the power switch to
"RECORD". This starts the recorder chart in motion. Place the pen on the paper.
When the pen crosses a major x-axis division, momentarily depress the scan
control to "START". This action begins the scan of the Indicator electrode potential
in a positive (+) direction, and a sharp vertical pen mark is made on the chart to
indicate the start of the voltage sweep.
(h) When the voltage sweep reaches the pre-set "FINAL VOLTAGE"(+1.200V.), the
Indicator electrode voltage automatically returns to the "Initial Voltage" (-.400 V.).
This event can be detected by observing the meter indicating the cell voltage; also,
a sharp change in the current level indicated by the recorder pen will accompany
the end of the voltage sweep.
(i) When the end of the voltage sweep is observed (see (h)), turn the operating
switch to "OFF"; turn the power switch to "ON". When the pen moves back, repeat
2.3.f - h, twice.



(j) Set the operating mode and power switches to "OFF"; detach and rinse the
electrodes; turn off the stirring motor, and clean the beaker.
(k) Add 50 mL of potassium chloride solution to a clean 100 mL beaker. Repeat
2.3.b - i, obtaining three background results.
(l) Repeat 2.3.j.