Chemistry Lab Report Chem. 1212K Dr.

Ray

Ashogbon, Habib

Introduction

As a chemistry student learning about everything that makes us what we are from our existence to our tiny bit of atom, understanding how to accurately analyze chemical is a favorable place to begin the acquisition of necessary knowledge to achieving success. The main objective is to acquire necessary skill and technique to perform series of chemical analyses on samples to determine the quantity of elements and compound present in that given sample. In order to accomplish this aim a few experiment must be carried out on a sample (synthesis 5) to identify the quantity of element present. The experiment contains the synthesis of a cobaltammonia-halide compound, analysis for %halide in the synthesized cobalt-ammonia-halide compound, standardization of hydrochloric acid solution, analysis for %NH3 in the synthesized compound, standardization of sodium thiosulfate solution, and analysis for %Co in the synthesized compound. These experiments are carried out with specifically different procedures that would be further elaborated later on in the report. Grasping the idea of what a compound consists of lies in the understanding of what a coordination compound really is. Coordination compounds and complexes are distinct chemical species - their properties and behavior are different from the metal atom/ion and ligands from which they are composed (BRW).

Procedure Preparation of a Cobalt Amine Bromide Product 4g of CoCO3 is dissolved in 15ml of 9M HBr, should be placed in a beaker. After effervescence, add 10ml of H2O, stir and filter the mixture. Put the filtrate to slurry of 7g NH4Br dissolved in 35ml concentrated aqueous NH3. Place the beaker containing mixture in a bowl of

crushed ice until temperature drops to 100C or below, while still in ice, carefully add 7ml of 30% H2O2 4-5 drops at a time (20sec-30sec), and stir. It shouldnt exceed 20min before the total solution. Heat the solution at 80-1000C until 2/3 of it remains, then cool to room temperature. Add 50ml of 4.5 HBr (25ml of 45% HBr to 25ml H2O) into solution. Heat the mixture at 60700C for 45-60 minutes. Cool to 100C and collect crystals using the suction filter. Wash precipitate with 10ml ethanol, and with 2 portions of 5ml acetone. Air-dry for a week, weigh product and calculate % yield. The color of the cobalt compound came out to be purple.

Analysis for % Halide in the Synthesized Cobalt Compound Prepare AgNO3 solution by dissolving 1.7-1.8g of solid AgNO3 in 50ml dH2O. Put 10 drops of concentrated HNO3 in the mixture. Weigh two separate 0.24-0.25g of CoX samples and place in separate beakers. Add 150ml of dH2O, 10 drops of HNO3, and 25ml of the AgNO3 solution into each solution. Boil solutions for 45 minutes, let it cool to room temperature, and collect each AgBr precipitate in separate gooch crucibles using suction filtration. Wash precipitates with 5ml ethanol and 6ml acetone. Dry crucibles and record mass of precipitate. Ag+(aq) + Br-(aq) AgBr(s)

Preparation and Standardization of HCl Solution Prepare a 500ml solution of approximately 0.3M HCl solution. Dissolve in 3 separate Erlenmeyer flasks about 0.8000-1.1000g of THAM in 100ml dH2O. Titrate solutions separately using the HCl solution previously prepared, adding 3-5 drops of brom-cresol-green indicator before each titration. Record the initial volume and final volume to get the volume of HCl used, and calculate the molarities for each solution. The color of the solution after titration was green. (HOCH2)3CNH2 + HCl (HOCH2)3+ + Cl-

Analysis for % NH3 using Synthesized 0.3M HCl Dissolve 2g of boric acid in 50ml dH2O placing it in an Erlenmeyer flask. This should be replicated in 3 places. Dissolve 0.3500-0.4000g of CoX in 100ml dH2O. Setup ammonia producing assembly under the hood. Rapidly add 50ml of 9M NaOH into CoX flask and cover with a rubber stopper as quickly as possible so the boric acid doesnt escape. Boil for 15 minutes, collecting escaped NH3 in the boric acid flask dipped in ice. Cool the trapped NH3 solution, add 3-5 drops of brom-cresol-green indicator, and titrate with the 0.3M HCl. A greenish-blue color is the end point which is what was derived. Record the initial volume and final volume to get the volume of HCl used, and calculate % NH3. NH3 + HCl NH4+ + Cl-

Standardization of Thiosulfate Solution Prepare 500ml of approximately 0.1M sodium thiosulfate (Na2S2O3) solution. Dissolve 0.1000-0.1200g of KIO3 in 80ml dH2O and place in an Erlenmeyer flask. Add 3.0g of KI and

3ml of 6M HCl respectively. Titrate using the 0.1M Na2S2O3 already prepared until solution turns colorless. Record volume of Na2S2O3 used in each trails. Calculate molarities of the thiosulfate (Na2S2O3) solution for each trail. End point was colorless. KIO3 + 6HCl + 6Na2S2O3 3Na2S4O6 + KI + 3H2O + 6NaCl

Analysis of % Co+3 using standardized 0.1M Thiosulfate Place 0.5000-0.7000g of CoX into 35ml of dH20 with 10ml of 50% NaOH in an Erlenmeyer flask. Heat the mixture for about 20 minutes. Add enough dH 20 to get the volume in the flask to 50ml, and cool in ice. Add 2g of KI, 50ml 0f 6M HCl in 4ml increments and let it cool down to room temperature. Immediately begin titration with 0.1M thiosulfate until colorless. Repeat the entire procedure twice, and record volume of thiosulfate used in each trail and calculate % Co for each trail.
2Co(NH3)4Cl3 + 2S2032- 2Co2+ + S4062- + 8NH3 + 6Cl-

Data and Calculations Preparation and Standardization of HCl Solution Data Mass THAM (g) Initial volume (ml) Final Volume (ml) Trail 1 0.8552 10.60 35.80 Trail 2 0.8523 3.33 28.40 Trail 3 0.8585 24.00 49.55

Total Volume (ml) Color at end point Mol of THAM Mol of HCl Molarity HCl Average M HCl Deviation from avg Average Deviation % Deviation

25.20 Bluish green 0.007060 0.007060 O.2802 0.2794 0.0008 0.0014 0.50

25.07 Bluish green 0.007036 0.007036 0.2807 0.2794 0.0013 0.0014 0.50

25.55 Bluish green 0.007087 0.007087 0.2774 0.2794 0.0020 0.0014 0.50

Sample calculation: Trail 1 Molecular weight of THAM = 121.14g/mol Mols of THAM= 0.8552g / (121.14g/mol) Mols of THAM= 0.007060mol Molarity of HCl = 0.007060mol/0.02520L Molarity of HCl = 0.2802M Average Molarity of HCl = 0.2802M+0.2807M+0.2774M divided by 3 = 0.2794M Average Dev = 0.014 % Deviation = (0.014 / 0.2794) * 100

= 0.50%

Analysis for % NH3 using Synthesized 0.3M HCl Data CoX (g) Initial volume (ml) Final Volume (ml) Total volume (ml) Color at end point Mols of HCl Mols of NH3 Grams of NH3 % NH3 Average % NH3 Deviation from avg Average Deviation % Deviation Trail 1 0.3826 13.00 30.00 17.00 Greenish 0.004750 0.004750 0.08120 21.14 21.72 0.58 0.39 1.80 Trail 2 0.3829 24.00 41.95 17.95 Greenish 0.005015 0.005015 0.08540 22.30 21.72 0.58 0.39 1.80 Trail 3 0.3828 18.50 35.97 17.48 Greenish 0.004884 0.004884 0.08301 21.73 21.72 0.58 0.39 1.80

Sample Calculation: Trail 1 % NH3 = (g NH3 / g CoX) * 100 g NH3 = 0.2794M * 0.01700L = 0.004750mol

g NH3 = 0.004750mol * 17.03g/mol = 0.08120g % NH3 = (0.08120g / 0.3826g) * 100 % NH3 = 21.14% Average % NH3 = (21.14% + 22.30% + 21.73%) / 3 = 21.73% Averrage Dev = 0.39 % deviation = (0.39 / 21.72) * 100 = 1.80%

Standardization of Thiosulfate Solution Data KIO3 (g) KI(g) Initial volume (ml) Final Volume (ml) Trail 1 0.1036 3.0 4.96 32.21 Trail 2 0.1037 3.0 3.42 30.82 Trail 3 0.1035 3.0 9.22 36.32

Total volume (ml) Mols of KlO3 Mols of Na2S2O3 Molarity of Na2S2O3 Average Molarity Deviation from avg Average Deviation % Deviation

27.25 0.0004841 0.002905 0.1066 0.1066 0.0 0.0003 0.28

27.40 0.0004846 0.002907 0.1061 0.1066 0.0005 0.0003 0.28

27.10 0.0004836 0.002902 0.1071 0.1066 0.0005 0.0003 0.28

Sample Calculation: Trail 1 Molecular weight for KIO3 = 214.0g/mol Mol KIO3 = 0.1036g / 214.0g/mol = 0.0004841mol Mol Na2S2O3 = 0.0004841mol * 6 = 0.002905mol Molarity Na2S2O3 = 0.002905mol / 0.02725 = 0.1066 M Average Molarity Na2S2O3 = 0.1066 Average deviation = 0.0003 % Deviation = (0.003 / 0.1066) * 100 = 0.28%

Analysis of % Co+3 using standardized 0.1M Thiosulfate

Data CoX (g) Initial vol Na2S2O3 Final Vol Na2S2O3 Total vol Na2S2O3 Average M Na2S2O3 Color at end point Mols of Na2S2O3 Mols of Co Grams of Co % Co Average % Co Deviation from avg Average Deviation % Deviation

Trail 1 0.5094 3.00 16.10 13.10 0.1066 Clear 0.001396 0.001396 0.08227 16.15 16.12 0.03 0.07 0.4

Trail 2 0.5060 4.00 16.90 12.90 0.1066 Clear 0.001375 0.001375 0.08103 16.01 16.12 0.11 0.07 0.4

Trail 3 0.5045 10.00 23.00 13.00 0.1066 Clear 0.001386 0.001386 0.08168 16.19 16.12 0.07 0.07 0.4

Sample calculation: Trail 1 Mols of Cobalt = Mols of Na2S2O3 Mols of Na2S2O3 = 0.1066M * 0.01310L = 0.001396 % Co = (gCo / g CoX) * 100

gCo = 58.93g/mol * 0.001396 Mol = 0.08227g % Co = (0.08227 / 0.5094) * 100 = 16.15 % Average % Co = 16.12 % Average deviation = 0.07 % Deviation = (0.07 / 16.12) * 100 % Deviation = 0.4%

Result/ Analysis Preparation of a Cobalt Amine Bromide Product The experiment was properly carried out because everything came out as planned. No sign of visible error or mathematical error. I was able to retrieve 8.02 grams of Cobalt compound out of a possible 11 grams of compound (4g of CoCO3 and 7.00g of NH4Br) , and that can be attributed to evaporation and splattering when boiling. The compound color came out to be purple which was expected of my synthesis number (5). Analysis for % Halide in the Synthesized Cobalt Compound The % deviation in this experiment was 0.545% which is not significantly high, but there appear to be a little shortage of the average %halide in the Co-sample. After the necessary calculation, it was determined that the average % halide present is 59.67%. It appeared that this error may have occurred during transferring of the compound from the weigh bowl or an inaccurate reading from using the analytical balance. It is also possible that some compound may have splattered when

boiling. Putting all those in consideration, it is safe to tag this experiment as a success because the % deviation is not far off. Preparation and Standardization of HCl Solution This experiment ended with a 0.50% deviation. It is well within a reasonable frame of error. The numbers of all 3 trials were pretty close. Errors made in this experiment are attributed to inconsistency of the analytical balance. Titration might be a factor, but I didnt over titrate because I achieved the color at endpoint, and all 3 trails are consistently within 25.00ml.

Analysis for % NH3 using Synthesized 0.3M HCl It is nothing of a surprise that the % deviation for this experiment is 1.80%. There are so many places where something might have gone wrong. An obvious margin for error couldve been when adding 50ml of 9M NaOH. The boric acid must have escaped during that process before the stopper was placed back. Another visible margin for error, it could possibly have been water finding its way into the solution from the pipe. Also, the analytical couldve played a part in the error acquisition. It is also possible that when titrating, the solution wasnt in the desired temperature. Everything couldve played a major role in the outcome of the result. The numbers from all 3 trails are somewhat consistent.

References Chemistry Faculty, Georgia State University. Chem 1212K Lab Manual and Notebook. Atlanta: 2012. Print. Hanan, Garry S. et al. Coordination Arrays: Tetranuclear Cobalt (II) complexes with [2x2]-Grid Structure. Angew. Chem. Int. Ed. Engl. 36.17 (1997): 1842-1844. NicDhuinnshleibhe, Siobhan. A Brief History of Dyestuffs and Dyeing. Runestone Collegium. Heather McCloy (2000). Natarajan, P. et al. Photoprocesses of Coordination Compounds and Dyes in solutions And nanoporous materials: Evolution from milliseconds to femtoseconds. J. Chem. Sci. 123.5 (2011): 531-553.