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Determining the compound of a Cobalt metal sample requires several different steps and
procedures that must be completed in order to get the right results. Metals are found to react with
other molecules on the periodic table, which makes the compound change to different colors. In
this case, the Cobalt metal is used to determine the changes. The purpose of this lab is to
determine how much ammonia and halide ions such as Chlorine and Bromine will reacts with the
Cobalt metal sample. There was assigned a synthesis compound procedure to make the cobalt
sample crystals. Once the crystals are collected, more procedures will be performed so the results
can be analyzed to clarify the correct compound formula. In order to clarify the correct cobalt
sample formula, the Synthesis Procedure III was assigned, and it must be performed to make and
collect the Cobalt sample. Also, the percent halide, the standardization of a Hydrochloric Acid
solution, the percent ammonia, the preparation and standardization of 0.1 Molarity of
Thiosulfate, the percent Analysis of percent Cobalt, and the procedure for analysis of unknown
Iron (III) Salt must be determined first. These results will prove that the compound formula
selected will be accurate.
Synthesis of a cobalt-halide compound
The synthesis III procedure was assigned to make one batch of the Cobalt Amine
Bromide Product. Under the fume hood, 5 grams of cobalt carbonate and 20 milliliters of 9M
hydrobromic acid was added to a beaker. After waiting a minute for a sizzling to seize, 15
milliliters of deionized water was stirred into the solution. The solution was clear, so it did not
have to be filtered. The solution was then added to a mixture of decolorizing charcoal and 25
milliliters of aqueous ammonia in another beaker and placed in an ice bath. 6 milliliters of the
oxidizing agent hydrogen peroxide was added to the beaker, 3-4 drops at a time, and stirred. The

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solution was then heated to 60-80 degree Celsius for 20 minutes. The solution was stirred
occasionally. After 20 minute of heating, the solution was placed back into the ice bath for
cooling to 5 degree Celsius for crystallization. The solution was filtered by using a suction
filtration flask to collect the dark charcoal mixed with the product. The solid and the filter paper
was transferred to another beaker on a hotplate with 135 milliliters of boiling water and 3
milliliters of 9M Hydrobromic acid. After stirring the solution, the hot mixture was filtered once
again using a suction filtration flask. The contents of the suction flask was transferred to a beaker
to be cooled to room temperature. 10 milliliters of 9M Hydrobromic acid was stirred in the
solution, and it was placed in an ice bath to 10 degree Celsius. The solution was filtered a third
time by a suction filtration flask. The precipitate on the filter paper was washed with 10
milliliters of ethyl alcohol poured on it. Also, 10 milliliters of acetone was poured on the
precipitate to be washed. Once the orange product dried, it weighed to be 1.9 grams, and the
percent yield was 11.3%.
Analysis for % Halide in the synthesized cobalt- ammonia-halide compound
This procedure is to determine the percent halide in the cobalt sample whether it be
Chlorine of Bromine. Since Cobalt Amine Bromide was used in the previous procedure, the
percent Bromine is to be found. 1 gram of Silver Nitrate was dissolved in 50 milliliters of
deionized water, and 10 drops of Nitric acid was added to the solution. 2 samples of the cobalt
product previously made in the last procedure was weighed and recorded to be used. The
samples weighed to be .2405 grams and .2454 grams. The samples were placed into two beakers,
and 25 milliliters each of the mixed solution was poured into the 2 beakers. 10 drops of Nitric
acid and 125 milliliters of deionized water was added to the 2 beakers. 25 milliliters of Silver

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Nitrate was also added to each of the 2 beakers. Silver Nitrate is used as an excess for the
precipitate. The Nitric acid is used to avoid the precipitation of silver because of carbon atoms.
The solutions were boiled for 45 minutes, and then cooled to room temperature. The Silver
Bromide was collected with gooch crucibles and the aide of the suction filtration flask. The
precipitate was washed with 5 milliliters if ethyl alcohol and 5 milliliters of acetone. After
drawing air through the crucibles for 3 minutes, the crucibles were placed in two beakers to be
placed in the oven for drying for 30 minutes. After 30 minutes, the crucibles were placed in a
desiccator to be cooled to room temperature for 25 minutes. The crucibles were weighed with the
precipitate in them and placed back into the oven for another 25 minutes. After the 25 minutes,
the crucibles were cooled and reweighed a second time for accuracy. The best average weight of
the crucible was recorded. The grams of halide precipitate was obtained by subtracting the best
average weight of the crucible and precipitate from the best average weight of the empty
crucibles. The average empty crucible weights were 30.2796 grams and 29.5613 grams, and the
average crucible weight with the precipitates were 30.6167 grams and 29.9070 grams. The
percent halide could then be calculated. The percent halide was 59.81% with a 0.01% deviation.
Standardization of Hydrochloric acid solution
This procedure helped in determining the exact molarity of hydrochloric acid needed in
the next procedure. Under the fume hood, 0.3M hydrochloric acid was prepared by diluting 12M
hydrochloric acid with deionized water. The solution was stirred thoroughly, and it totaled to a
volume of 500 milliliters. In 3 Erlenmeyer flasks, 3 samples of Tris Hydroxymethyl Amino
Methane (THAM) were weighed and put into each flask. THAM is a solid base used as a
reactant with hydrochloric acid. A clean buret was set up for titration on a buret stand, and it was
filled with hydrochloric acid. Drops of Brom-cresol-green were dropped into each flask. Brom-

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cresol-green is used as a color indicator because both hydrochloric acid and THAM are colorless.
The indicator turned each of the solutions to a blue color. The initial buret reading was recorded
and subtracted from the final buret reading. Once the solution turned a greenish-yellow color, the
titration was complete. This was the final buret reading. Titration was done for the remaining
flasks also. Once the volumes were calculated, the molarity could be determined. The
hydrochloric acid was .2810 molarity with a 0.15% deviation.
(HOCH2)3CNH2 + HCL (HOCH2)3CNH3+ + BrAnalysis for % NH3 in the synthesized compound
The standardized hydrochloric acid (HCl) from the previous procedure will be used to
help determine the percent ammonia produced in the cobalt compound. Two Erlenmeyer flasks
were used in this procedure. In one of the flask, 2 grams of boric acid along with 50 milliliters of
water was added. The flask was heated to 50 degrees Celsius, so the boric acid could dissolve
thoroughly. An ammonia producing assembly was set up under the fume hood with a tripod, a
hotplate, and a connecting tube. 1 sample of the Cobalt compound was measured between .
3500-.4000 grams, and it was placed in the other flask with a stirring rod. The cobalt sample was
used as a limiting reagent. The cobalt sample was then placed onto the hot plate. Also, 1 gram of
Ethylenediaminetetraacetic acid (EDTA*4 Na) was added, and deionized water was added to
make the volume a total of 100 milliliters. With the aid of a funnel, 10 milliliters of 19M Sodium
Hydroxide was poured into the flask. The rubber stopper end of the connecting tube was placed
on top of the flask to make a tight seal. The connecting tube was placed inside the flask with
boric acid, and the flask with boric acid was placed inside a 1000 ml beaker. The heat and
stirring were turned up on the hotplate. Once the contents began boiling, the boiling continued
for 25 minutes. If the boric acid liquid started to come up the connecting tube, ice water was

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added to the beaker that the flask was in. Also, the stirring and the heat were turned up a bit more
to produce more pressure coming from the flask on the hot plate. After 25 minutes of boiling, the
flask with now purple solution was taken off the hotplate to be cooled to room temperature. The
connecting tube in the boric acid was rinsed inside the flask to get the acid off the connecting
tube, and the flask was taken out of the beaker. 3 to 4 drops of Brom-cresol-green indicator was
dropped in to the boric acid, and it was titrated with hydrochloric acid to greenish-yellow color. .
01964 Liters of hydrochloric acid was needed for titration of the flask with boric acid. The
average molarity of hydrochloric acid in the previous procedure was used to determine the
percent ammonia. The percent ammonia was 24.78%.
NH3 + H3BO3 NH4+ + H2BO3- (Distillation)
H2BO3- + HCl H3BO3 + Br- (Titration)
NH3 + HCl NH4+ + Br-

(Overall Equation)

Standardization of Sodium Thiosulfate solution

This procedure helped in determining the molarity of sodium thiosulfate (S2O32-) needed
in the next procedure. 12.4 grams of thiosulfate and .3 grams of sodium carbonate was added 500
milliliters of water in a beaker. Sodium Carbonate was used so that thiosulfate will carbonate to
prevent acid from being present in the solution. The solution was stirred to make 500 milliliters
of 0.1 molarity aqueous sodium thiosulfate. Three 0.1000-0.1200 grams of potassium iodate
(KIO3) were each placed in an Erlenmeyer flask. 70-80 milliliters of deionized water were added
to each to dissolve the solutions. 3 grams of potassium iodide (KI) was added to the potassium
iodate solution. Also, under the hood, 3 milliliters of 6 molarity hydrochloric acid was diluted
(5:5) and added to the solutions. The hydrochloric acid made the solutions turn a reddish-brown

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color. Once the solutions were swirled and mixed, the solutions were immediately titrated until
the solution turned light yellow and finally clear. The volumes were recorded, and the molarity of
sodium thiosulfate could be determined. The sodium thiosulfate was .09901 molarity with a
0.01% deviation.
IO3- + 6 H+ + 5 I- 3 I2 + 3 H2O
6 S2O32- + 3 I2 3 S4O62- + 6 IIO3- + 6 H+ + 6 S2O32- 3 S4O62- + I- + 3 H2O (Overall Equation)
Analysis for % Co in the synthesized compound
The standardized thiosulfate (Na2S2O3) from the previous procedure will be used to help
determine the percent cobalt produced in the cobalt compound. 3 samples of cobalt compound
were weighed between 0.5000-0.7000 grams and each placed in 3 Erlenmeyer flasks. 35
milliliters on deionized water and 10 milliliters of 50% Sodium Hydroxide (NaOH) were added
to each flask. All 3 flasks were heated to a smooth boil on a hotplate for 20 minutes. After
boiling for 20 minutes, the flasks were taken off the hotplate to be cooled to room temperature
and deionized water was added to each flask for a total of 50 milliliters. 2 grams of potassium
iodide was added to one flask and swirled for 4-5 minutes, and 40-50 milliliters of hydrochloric
acid was also added 3-4 milliliters at a time and swirled. Once the solution turned a clear red
wine color, it was ready for titration. 5 milliliters of thiosulfate was immediately added to the
flask from the buret, and 5 milliliters of starch indicator was added afterwards to make the
solution turn to a dark blue due to the presence of I3-. Titration was continued until the solution in
the flask turned to a pinkish color. This was repeated for the remaining 2 flasks. The percent
cobalt could now be determined. The percent cobalt was 14.44% with a 1.9% deviation.

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2 Co(NH3)4Br3 + 6 OH- 2 Co(OH)3 + 6 Cl- + 8 NH3

6 H+ + 2 Co(OH)3 2 Co+3 + 6 H2O
2 Co+3 + 2 I- 2 Co++ + I2
2 S2O32- + I2 S4O62- + 2 I2 Co(NH3)4Br3 + 2 S2O32- 2 Co+2 + S4O62- + 8 NH3 + 6 Br- (Overall Equation)
After all of the necessary calculations were done for all of the procedures, the formula
could be determined. The percentages of the halide, the ammonia, and the cobalt were all divided
by the molar mass of each one to get the moles of each one. Once the moles were calculated,
each one was divided by moles of cobalt to get the mole ratio of each one. The compound
formula was found to be [Co(NH3)6]Br3.

% Halide

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Standardization of HCl
Mass of THAM
Final Volume
Initial Volume

.9767 g
28.80 mL
0.00 mL
28.80 mL

.9810 g
32.21 mL
8.35 mL
28.86 mL

.9803 g
45.81 mL
17.05 mL
28.76 mL

% NH3
Mass of Co-Compound
Final volume
Initial Volume

.3785 g
25.67 mL
6.03 mL
19.64 mL

Standardization of Na2S2O3
Grams of KIO3
Final Volume

.1109 g
31.43 mL

.1083 g
33.15 mL

.1106 g
34.53 mL

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Initial Volume

0.10 mL
31.33 mL

2.69 mL
30.46 mL

2.93 mL
31.60 mL

.5017 g
20.40 mL
7.83 mL
12.57 mL

.5163 g
33.40 mL
20.40 mL
13.00 mL

.5020 g
32.55 mL
20.50 mL
12.05 mL

% Cobalt
Mass of Co- Sample
Final Volume
Initial Volume