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THE EVENT
Download the rules
in pdf format here.
Teams will be provided with a specified set of testing reagents,
droppers and other necessary glassware and a flame source. Eight
unknown solutions will be provided in separate numbered vials.
The team will be given twenty minutes to identify the ion type in each vial.
The team will have 5 minutes at the end of the event to clean the glassware
Students may bring in (a) one 8.5"x 11" sheet of paper
with any notes they wish written using both sides, (b) the Rules for the event.
2. UNKNOWNS:
Unknown solutions in three categories identified as
a) anion only (3 unknowns)
b) cation only (3 unknowns)
c) both cation and anion (2 unknowns)
Teams will be given about 15 mL of each solution and the individual
tests should be run on samples of about 1 mL.
Fresh solution should be used for each new test.
1. ANION UNKNOWNS
You will be provided with about 15 mL of 3 solutions and you will
be asked to determine the anion present in each. Each of these anions
will be one of acetate, bromide, carbonate, chloride, iodide, or
phosphate as their sodium salt as shown below.
sodium acetate CH3CO2Na
sodium bromide NaBr
sodium carbonate Na2CO3
sodium chlorine NaCl
sodium iodide NaI
sodium phosphate Na3PO4
It is up to you to devise the quickest scheme to do this using
the reagents and procedures which follow :
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Cl – Br –
I –
Solution remains mildly acidic. pH approximately
4
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CH3CO2
– CO3
2– PO4
3–
Solution becomes somewhat basic, pH = 7-10
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The anions can be conveniently broken into 2 categories based upon
the pH of the solution when they dissolve. Use pH paper, not litmus
paper, if available.
Individual anions
CHLORIDE Cl –
Add a few drops of dilute nitric acid and then add about 1 mL of
silver nitrate (AgNO3) solution. A white precipitate of AgCl separates.
BROMIDE Br –
Add a few drops of dilute nitric acid and then add about 1 mL of
silver nitrate solution. A cream coloured precipitate of AgBr forms.
IODIDE I –
Add a few drops of dilute nitric acid and then add about 1 mL of
silver nitrate solution. A yellow coloured precipitate of AgI forms.
Note: The three halides (chloride, bromide and iodide) all give
precipitates with silver ions but these can be distinguished by
their colours. With a little practice you should have no trouble
telling these apart. However, to confirm your choice, you can add
an equal volume of concentrated ammonium hydroxide to each test
tube containing the precipitate. After shaking, the silver chloride
will redissolve; the silver bromide will mostly redissolve; and
the silver iodide will remain undissolved.
To further distinguish between bromide and iodide:
Add about 1 mL of paraffin oil and a few drops of chlorine water.
A red or orange colour in the paraffin oil layer indicates bromide;
a violet colour indicates iodide.
ACETATE CH3CO 2–
This solution will have a pH of about 7. Add about 1 mL of silver
nitrate solution. A white precipitate will form slowly. This precipitate
will redissolve upon the addition of about 1 mL of dilute nitric
acid. The halide's precipitate will not redissolve.
CARBONATE CO32–
Add about 1 mL of dilute nitric acid and look for the formation
of bubbles of carbon dioxide.
PHOSPHATE PO43–
To 1 mL of the phosphate solution add 1 mL of dilute nitric acid
and warm almost to boiling. Then add 1 mL of ammonium molybdate
(NH4)2MoO4 solution
and a yellow coloured precipitate will form.
2. CATION UNKNOWNS
You will be provided with about 15 mL of 3 solutions and you will
be asked to determine the cation present in each. Each of these
cations will be present as either the chloride or nitrate as listed
below.
| Aluminum chloride |
AlCl3 |
| Ammonium chloride |
NH4Cl |
| Barium nitrate |
Ba(NO3)2 |
| Copper (II) nitrate |
Cu(NO3)2 |
| Iron (III) nitrate |
Fe(NO3)3 |
| Sodium chloride |
NaCl |
| Strontium nitrate |
Sr(NO3)2 |
| Zinc chloride |
ZnCl2 |
Your task is to identify the specific cation present in each solution
as quickly as possible using the reagents and procedures which follow:
ALUMINUM Al 3+
Add about 0.5 mL of ammonia solution (ammonium hydroxide). A gelatinous
white precipitate will form.
AMMONIUM NH 4+
Add about 0.5 mL of a dilute sodium hydroxide solution. Warm the test tube in the hot water bath provided. Immediately
test the vapours emitted from the test tube with moist pH paper.
A basic pH should be observed.
BARIUM Ba 2+
Add about 0.5 mL of a sodium sulfate solution. A white precipitate
should form. Both Ba2+ and Sr2+ give this result. Barium ions can
be confirmed using a FLAME TEST (See below).
COPPER (II) Cu 2+
Add about 0.5 mL of an ammonia solution (ammonium hydroxide) and
shake. A deep blue colour indicates Cu2+ ions were present. Copper
(II) can also be confirmed by a flame test.
IRON (III) Fe 3+
Add a few drops of a dilute sodium hydroxide solution. A copious
brown precipitate should be observed.
SILVER Ag 3+
Add a few drops of dilute nitric acid and then add some drops of
a sodium chloride solution. A white precipitate should be observed.
SODIUM Na 3+
There is no simple test for sodium ions. Use a flame test.
STRONTIUM Sr 2+
Add about 0.5 mL of a sodium sulfate solution. A white precipitate
should form. Both Ba2+ and Sr2+ give this result. However, Sr2+
gives a flame test quite different than Ba2+.
ZINC Zn 2+
Add a few drops of an ammonia solution (ammonium hydroxide) and
a white precipitate should form. However, if you add about 0.5 mL
of a concentrated ammonia solution it should redissolve. Compare
this result with aluminum.
3. COMPOUND UNKNOWNS (BOTH CATION AND ANION)
You will be given about 15 mL of 2 solutions and you will be asked
to identify both the cation and the anion present in each and thus
deduce the identity of the compound that has been dissolved.
The two compounds will be composed of the cations and anions from
the previous tests. You should use the tests presented earlier for
the anions and cations separately.
4. FLAME TESTS FOR CATION IDENTIFICATION
Put the end of a splint into the solution so that some of the solution
adheres to it. Adjust the bunsen burner/butane torch so as to produce a blue
flame. Apply the unknown solution to the tip of the inner blue flame. Do not burn the splint as this will affect the
colour of the flame.
RESULTS
| Barium |
Green |
| Copper |
Green |
| Sodium |
Intense yellow/orange (colours whole flame) |
| Strontium |
Bright red |
You must try these tests with known compounds in order to become
familiar with the colours, as words cannot describe the colours
adequately.
5. A LIST OF REAGENT SOLUTIONS AND NECESSARY APPARATUS
The following is a list of reagent solutions and apparatus that
will be available on the day of the contest. You should design your
schemes with this in mind. However, it may be possible to add to
this list provided you have your requests okayed by the contest
coordinator at least one week before the event. If you have a problem
locating specific reagents, do not hesitate to contact the co-ordinator.
REAGENT SOLUTIONS
| Ammonium hydroxide |
1.0 M, Conc |
| Ammonium molybdate |
0.5 M |
| Chlorine water |
Cl2 / water |
| Nitric acid |
1.0 M |
| Silver nitrate |
0.1 M |
| Sodium chloride |
0.5 M |
| Sodium sulfate |
1.0 M |
| Sodium hydroxide |
0.1 M, 1.0 M |
| Paraffin Oil |
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APPARATUS
Test tubes and holder
Disposable pipettes
pH paper
Bunsen burner / butane torch
Wooden splints
6. PREPARATION INSTRUCTIONS FOR REAGENTS AND UNKNOWNS
After you develop a scheme and procedure for analyzing the possible
unknowns you will receive, it wouldn't hurt at all to practice.
This means that you must prepare your own unknown test solutions
and reagent solutions. The following list should prove helpful.
About 10 mL of each of these should prove more than sufficient for
any practice round.
REAGENTS
Ammonium hydroxide 1 M
Add about 1 mL of concentrated ammonium hydroxide to 10 mL of distilled
water.
Ammonium molybdate 0.5 M
Add about 1 gram of the solid to about 10 mL of distilled water.
Nitric acid 1 M
Add about 1 mL of concentrated nitric acid to 10 mL of distilled
water. Be careful with concentrated nitric acid for it can burn
you and put holes in your clothes.
Silver nitrate 0.1 M
You want about 0.2 grams in 10 mL of distilled water. If this solution
is cloudy add a few drops of dilute nitric acid. Two or three medium
sized crystals will suffice to give you 0.2 g. Don't get this solution
on your hands as they will turn black.
Sodium chloride 0.5 M
You want about 0.5 g in 10 mL of distilled water. Ten pinches of
salt is about right.
Sodium hydroxide 1 M
Three pellets of sodium hydroxide in 10 mL of distilled water is
about right. The pellets may be a little slow to dissolve but just
give them time.
Sodium sulfate 1 M
You want about 1.4 g in 10 mL of distilled water. About ten pinches
of sodium sulfate will be about right.
Unknowns
To make a solution of your unknowns use the equivalent of two or
three generous pinches of the solid in about 2.5 cm (height) of
distilled water in a test tube. The solids may be a little slow
to dissolve. A little shaking, stirring, and gentle warming will
help but so will patience.
The following compounds are recommended for making up unknowns
but other soluble salts can be used.
Aluminum chloride
Ammonium chloride
Barium nitrate
Copper (II) nitrate
Iron (III) nitrate
Silver nitrate
Sodium acetate
Sodium bromide
Sodium carbonate
Sodium chloride
Sodium iodide
Sodium phosphate
Strontium nitrate
Zinc chloride
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