By Yellow Group

Week One: Coordination Complex Synthesis Week Two: Cobalt Analysis Week Three: Ammonia Analysis Week Four: Chloride Analysis
Techniques used include: Titration, qualitative transfer, crystallization, vacuum filtration, and gravimetric analysis.

Tria l 1 2 3

Mass of Cobalt Complex (g) 0.02 0.02 0.02

Initial EDTA (ml) 25.0 25.0 25.0

EDTA Used (ml) 8.4 8.1 6.7

Calculated Amount Cobalt (g) 4.95e-3 4.8e-3 3.95e-3

% Mass Cobalt

24.8% 24.0% 19.75%

avg

0.02

25.0

7.7

4.56e-3

22.85%

Determining % Mass Cobalt Amount EDTA used x M EDTA x Cobalt:EDTA molar ratio x Cobalt molar mass = g Cobalt g Cobalt / mass of Cobalt complex sample x 100% = % mass Cobalt 7.7 mL EDTA 1L
x

Ratio Co to EDTA= 1:1

1 L x 0.0100 mol EDTA 1000 mL L

1 mol Co 1 EDTA

58.93 g Co = 4.56 x 10-3 g Co 1 mol Co

4.56 x 10-3 g Co x 100 % = 22.85% 0.020 g Co complex

Trial 1

Mass Co Complex (g) 0.050

Initial 0.104 M HCl (ml) 17.0

0.104 M HCl Added (ml) 11.0

Mass NH3 (g) 0.021

% Mass NH3 41.3

2
avg

0.050
0.050

17.0
17.0

10.8
10.9

0.020
0.021

40.5
40.9

Determining % Mass Ammonia Amount HCl Used x M HCl x HCl:Ammonia Borate molar ratio x Ammonia:Ammonia Borate molar ratio x Ammonia molar mass = g Ammonia g Ammonia / mass of Co complex sample x 100% = % mass Co 10.9 mL HCl x 1 L 1 1000 mL -2 g ammonia = 2.1 x 10
x

0.104 mol HCl L

1 mol Ammonia borate x 1 mol NH3 1 mol HCl 1 mol ammonia borate

18.04 g NH3 1 mol NH3

(2.1 x 10-2 g NH3) / (0.05 g Co Complex) x 100 % = 40.9%

Material Initial Mass Cobalt Complex Watch Glass + Filter Paper Watch Glass + Filter Paper + Precipitate Mass of Precipitate Percent Mass ClDetermining % Mass Chloride Mass of watch glass + filter paper + precipitate - Mass of watch glass + filter paper = Mass of precipitate (AgCl)

Mass (g) 0.301 43.324 43.782 0.458 37.7

Mass of AgCl (g) x Molar mass AgCl (g/mol) x 1:1 molar ratio Cl:AgCl x Molar mass Chloride (g/mol) = g Chloride g Chloride / mass of Co complex sample x 100% = % mass Cl 0.458 g AgCl x 1 mol AgCl 1 143.32 g AgCl
x

1 mol Cl 1 mol AgCl

35.45 g Cl = 0.113 g Cl 1 mol Cl

0.113 g Cl x 100 % = 37.7% Cl 0.301 g Co complex

Co Percent Mass 22.85

NH3 40.9

Cl37.7

Determining Emirical Formula After determining the mass percent of each component, it is assumed that 100 g of each are present and are converted to moles. The smallest value is divided by itself and by the other values to determine the ratio. Our empirical calculations are as follows: (37.7 g Cl)/(35.5 g/mol Cl) = (1.062 mol Cl) / (0.388 mol Co) = 2.5 approx 3 (40.9 g NH3) / (17 g/mol NH3) = (2.406 mol NH3) / (0.388 mol Co)= 5.7 approx 6 (22.85 g Co) / (58.93 g/mol Co)= (0.388 mol Co) / (0.388 mol Co) = 1

Cl:Co3+ ratio = 3:1 NH3:Co3+ ratio = 6:1

[Co(NH3)6]Cl3

 Inner Ligands: 6NH3 (Neutral Charge) Outer Ligands: 3Cl(-3 charge total) Central Atom: Co3+ (+3 charge total) Complex: [Co(NH3)6]Cl3

[Co(NH3)6]Cl3
Complex Cation: [Co(NH3)6]3+ Counter Ions: (Cl)3 with a charge of -3 Overall complex has all charges balanced 3D Molecular Structure

Synthesis of Complex decomposition of hydrogen peroxide (not kept cold enough or added to quickly), loss due to transfer, inconsistent boiling temperature and rigor, accumulation of smaller errors from individual groups, these errors are carried forward to all analysis experiments Cobalt Analysis loss due to transfer, insufficient or excessive heating to liberate cobalt ions, insufficient and uneven cooling
Ammonia Analysis escape of gas (failure to cover the flask immediately or insufficient cooling of catch flask), uneven heating, loss due to transfer, improper cleaning of glassware (too basic or acidic) Chloride Analysis excessively evaporation of 3M NaOH and complex solution, reduction of silver ion to silver metal (light reaction), loss due to transfer, improper cleaning of glassware, insufficient drying of precipitate

The ammonia analysis was the least reliable while the chloride analysis was the most reliable. Ammonia analysis had the most potential sources of error such as escape of ammonia gas, unclean glassware due to tainted basicity/acidity, loss of product during transfer from weigh boat to flask Chloride analysis was the most reliable because there was not as much room for loss of product; reduced chloride could have resulted from loss of sliver or loss of product during transfer from filter flask to weigh boat. Cobalt was more reliable than ammonia but still somewhat unreliable because when Co3+ was reduced to Co3+ by heating, it may not have been heated long enough and we would have reduced product.

CoCl3(NH3)6(aq) +OH-(aq) Co3O4(s) + O2(g) + 6NH3(aq) + H2O(l) + 3Cl-(aq)

The solution turns brown due to the formation of Co3O4(s), a solid. The ammonia is a gas, and although it is water soluble, we must make it more stable for analysis. We did this by reacting the ammonia gas with boric acid to form ammonium borate. NH3(aq) + H3BO3(aq) NH4+H2BO3-(aq)

The boric acid would be drawn into the tygon tubing by a negative pressure differential. This differential would pull the solution up the tubing. That is why when the pull was too strong, we opened the stopper to equalize the pressure.

Boric acid acts as a bronsted base. Donates a proton.

NH3(aq) + H3BO3(aq) NH4+H2BO3-(aq)

4 H3BO3 (aq) + 2NaOH(aq) Na2B4O7(aq) + 7H2O(l) Acid Base Conj. Base Conj. Acid

Reaction between boric acid and sodium hydroxide

Acid base reaction. If it occurs, it would raise the pH, so fewer HCl would be added in the titration, resulting in a lower percent ammonia.