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In this experiment, the amounts of Co(II) and Ni(II) in a mixture will be determined by two
different approaches. First of all, the Co(II) and Ni(II) will be isolated by ion exchange and
the separated components assayed. After that Co2+ will be complexometrically titrated using
replacement method and Ni2+ will be determined by gravimetric analysis.
II. Introduction
And the Ni(II) passes through the resin. The R group is often -CH3. In 4 M HCl the CoCl42-
ion breaks down into cationic forms of cobalt(II) and all the cobalt(II) passes through the
resin.
Determinations of the separated components (and of the ions in the mixture) will employ
volumetric and gvarimetric method. For the determination of Cobalt or Nickel, the EDTA
with substitution titration (PAN as an indicator) will be applied and dimethylglyoxime uses as
precipitant for the determination of nickel.
Adding tartarate or citrate ions before the precipitation of the red nickel complex prevents
interference from Cr, Fe and other metals. These anions selectively form tightly bound soluble
complexes with the metals and prevent the formation of insoluble metal hydroxides in the
buffered solution.
An alcoholic solution of dimethyglyoxime (DMG) is used as the precipitating reagent during
the experiment because DMG is only slightly soluble in water (0.063 g in 100 mL at 25°C). It
is therefore crucial to avoid the addition of too large an excess of the reagent because it may
crystallize out with the chelate. It is also important to know that the complex itself is slightly
soluble
III. to some extent in alcoholic solutions. By keeping the volume added of the chelating
Reagents
reagent small, the errors from these sources are minimized. The amount of the reagent added
Provided:
is also governed by
Prepare an ion exchange
the presence column
of other metals as demonstrated
such by the
as cobalt, which formteaching
solublestaff. Use
a glass wool
complexes plugreagent.
with the in the bottom then
If a high add a of
quantity slurry ofions
these resinis(Dowex-1X8, 20-50
present, a greater mesh),ofuntil
amount
DMG themust
height
beof the resin column is 15 cm. Never allow the liquid to drop below the resin
added.
level.
Next, add another glass wool plug to the top of the level of glass wool column. Keep
about 5 cm of liquid above the resin column initially, and keep the liquid just above the
glass wool at all other times. Don't let any air into the resin.
Sample Unknown.
WARNING - Glassware used for this experiment must be scrupulously clean! The various
dilutions are tricky to keep track of, and are a common cause of error.
After the column is made up, it should be "charged" by passing 9 M HCl through the
column. See the following figure for details, and follow the directions there very carefully.
With a pipette, add 5.00
mL of the unknown onto
the column.1Allow the level
of the liquid to fall to just
the top of the glass wool
before adding the HCl
eluent.
• Elute the cobalt with 4 M HCl using the portions and flow rates as indicated in the figure. As
the HCl is diluted on the column, the blue CoCl42- complex will break down to form a pink
color as Cl- is replaced by water in the complex.
• After all the cobalt is eluted,3 stop the flow and transfer the collected solution to a 100 mL
volumetric flask. Dilute to volume with deionized water (sample B).
• Rinse the column with 75 mL of DI H2O in 15 mL portions. Remove the glass wool, and
dump the resin in the container provided.
The following dilutions should be made during this lab period in preparation for the second
week of this experiment. (Use pipettes and volumetric flasks for all dilutions.)
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B.Volumetric determination of Cobalt[AS1]
2. Heat the solution to approximately 950 C using the hot plate/stirrer (DO NOT BOIL!).
3. Add 5 drops of xylenol orange indicator (0.2 g/100 mL, 50% alcohol) and a stirring bar
to the solution, and titrate immediately with EDTA solution. Maintain the solution
temperature in the range of 85-950 C. The endpoint is a sudden color change from violet
to yellow-pink.
1. Add 10 mL of sodium acetate- acetic acid buffer pH=5 to each 10.00 mL of unknown
Co2+ solution (B solution)
2. Heat solution to the boiling using the hot plate/stirrer (DO NOT BOIL!) Add 3 dropps
of copper sulfate-EDTA solution and 8 drops of PAN indicator solution. Titrate to a
green-yellow color with standard solution.
Pipetting 10.00 mL of (A) sample to 250 mL beaker. Add 10 ml. 20% ammonium
chloride solution, add 20 ml. 10% tartaric acid, dilute to 200 ml., heat to nearly boiling,
cautiously add ammonium hydroxide (1:1) from a buret until the solution is slightly
alkaline. Take back to feebly acid by addition of a few ml. HCl. The reason the
precipitation is from acid solution is that a more easily filterable precipitate will result.
The changes in color will indicate the acidity to alkalinity of the solution, but this should
be checked against a sensitive indicator paper (not litmus). If iron hydroxide appears when
the solution is made alkaline, insufficient tartaric acid is present.
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NOTES:
1. Once you load the sample on the resin, the elution must be completed within the same lab
period.
2. Use dimethylglyoxime test solution with l drop of eluent to test for completion of Ni2+
elution. Add a couple of drops of NH4OH to the test solution. Look for red Ni(DMG)2. In a
separate test, you may also use a drop of the yellow ligand solution (which you will use more
of in week 2). Ni2+ is indicated by a color change from yellow, to pink or red.
3. Use thiocyanate test solution with 10 drops of ethanol and l drop of eluent to test for
completion of Co2+ elution. A blue color signifies Co2+ is present. In a separate test, you may
also use a drop of the yellow ligand solution (which you will use more of in week 2). Co2+ is
indicated by a color change from yellow, to pink or red.
4. Use a burette to deliver the buffer solution, a volumetric pipette to deliver the complexing
agent, and the graduated (Mohr) pipette for the metals and unknown (columns 2, 3, and 4, of
all three tables).
What are some of the advantages of method A and B used in this experiment? Which would
you expect to be more precise?
Could KCl be used instead of HCl (as a source of chloride ion) for elution? How about LiCl?
Explain.
What is the difference between ion- exchange chromatography and ion chromatography? Try
to figure out the principle of ion chromatography for determination of Cobalt and nickel in a
mixture.
Suggest alternative methods for the determination of nickel in steel. Explain in detail the
principle of ONE alternative method.