Identifying Synthesized Compound

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CHEM 1212K Lab Final Report Identifying Synthesized Compound Jolly Huynh 001-93-1260 Georgia State University LeCroix

Identifying Synthesized Compound Abstract A series of experiments were performed to identify the elements and quantity in a synthesized

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compound. In this specific paper, Synthesis V will be discussed. In Synthesis V, a Cobalt Amine Halide compound is to be synthesized, distilled, and titrated to determine the percent of the specific halide, percent of ammonia, and percent of actual cobalt present in the compound to determine the overall molecule. Since Synthesis V was performed, the halide present is Bromine. The main procedures that will be discussed in detail include: % Halide in Co-Compound Analysis, % NH3 in Co-Compound Analysis, and % Co in Co-Compound Analysis. Other procedures such as preparation and standardization of an HCl Titrant will also be discussed, as two titrants are used for determining quantity. The end results are as follows: Average % of Br in synthesized sample (SS) came out to be 59.28% with a 0.27% deviation, Average % of NH3 in SS is 21.2% with a 0.47% deviation, and Average % of Co in SS is 15.94% with a 0.31% deviation. So, the final conclusion for the synthesized compound is: [Co(NH3)5Br]Br2. Keywords: synthesized, compound, cobalt, amine, halide, bromine, ammonium, titrate, distill, filter, analysis, standardization

Identifying Synthesized Compound Introduction The main problem to be addressed in these series of lab experiments is identifying the

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molecular formula for a synthesized compound. The specific synthesis procedure used in this discussion is Synthesis V; Preparing a Cobalt Amine Bromide product. Once the compound is synthesized, the sample will be put through a series of titration processes, as well as distillation to isolate the gas present in the compound. As mentioned in the lab manual, the main idea is to familiarize oneself with the process required to identify essentially an unknown, so possible errors in experimentation will also be discussed as well as deviations. Procedure(s) Synthesis Procedure V: Preparing a Cobalt Amine Halide Product Four grams of CoCO3 are to weighed out, and added in small portions to 15mL of 9M (48%) hydrobromic acid in 250mL beaker. Once the fizzing has ceased, 10mL of water is added to the mixture and stirred gently; gravity filter is used. The filtrate is then added to 7g of NH4Br (which have been dissolved in 35mL of ammonia (aq) in a separate 250mL beaker). The mixture is then placed into an ice bath to cool to 10 degrees Celsius or less. While in ice bath, 7mL of of 30% H2O2 are added slowly, 4-5 drops at a time with 20-30 seconds of stirring in between. After the desired temperature is reach and all of the H2O2 has been added, the mixture is heated on a hot plate until only 2/3 of the original volume is left; continuous stirring was done to shorten boiling time. Once the desired volume is attained, the mixture is removed from the hot plate and cooled to room temperature. While the mixture is cooled, a 4.5M of HBr is prepared; adding 25mL of 48% HBr to 25mL of water and cooling to room temperature. Once both mixtures have reached room temperature, the 50mL of HBr is cautiously added to the original mixture. It is then heated again at about 60-70 degrees Celsius for 45-60 minutes until 2/3 of the original volume is left again.

Identifying Synthesized Compound

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When done, the mixture was cooled to 10 degrees Celsius or less in an ice bath, and the crystals will be collected via suction filtration. Once all liquid have been drained, the crystals are washed with 10mL of ethyl alcohol and 10mL of acetone (in two 5mL portions). Once the filtration is done, indicated by rather dry crystals, the crystals are left to air dry for a week and weighed: 9.0173g of crystals formed. Analysis for % Halide (X-) in a Synthesized Cobalt Compound Prepared AgNO3 Precipitating Reagent Solution: 1.7267g of AgNO3 (s) weighed out, dissolved in 50mL of deionized water, about 10 drops of concentrated HNO3 were added and mixed. This will be used to precipitate the halide in each sample to be tested. Also, weight of crucibles have been clarified, and found to have an average of: 31.3284g & 30.6258g Two synthesized cobalt samples are weighed out approximately 0.24-0.25g, and transferred to separate beakers each. 125-150mL of deionized water was the added to each sample, as well as 10 drops of HNO3. 25mL of the prepared AgNO3 is then added to each sample. The samples are then gently boiled for 45 minutes and cooled to room temperature. The precipitate of each sample are then collected into separate crucibles; which have been dried and weighed The crucibles are then placed on a suction filtration flask for more filtering. Contents in the crucible are wetted via 5mL of ethyl alcohol. After the alcohol has been filtered through, 5-6mL of acetone is poured onto the precipitate. After approximately 2-3 minutes of filtration, the crucibles are placed into a beaker and dried in the oven for 30 minutes. Afterwards, the crucibles are left to cool for 25 minutes and weighed. The process is done again and reweighed until the difference is within 0.0005g. The Data and Calculations are as follows: Data Table 1: % Halide Analysis mass of Co-sample mass of precipitate % halide in Co-sample

Identifying Synthesized Compound 0.2448g 0.2417g 0.3419g 0.3358g 59.44% 59.12%

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Average % Halide in Co-sample: 59.28% with 0.27% deviation Calculations 1: % Halide Analysis Sample Calculation: 0.3419gAgBr/187.77gAgBr/mol * 79.909Brg/mol = 0.1455gBr Br and AgBr 1:1 ratio, 0.1455gBr/0.2448gCo-sample = 59.44% Halide Average: (59.44+59.12)/2 = 59.28% Halide Deviation: (59.44-59.28)/59.28 * 100 = 0.27% & same for second sample (0.27+0.27)/2 = 0.27% Preparation and Standardization of HCl Solution Although this experiment does not directly provide information regarding the Co-Compound, it is still vital because the HCl made in this experiment is used to titrate with the compound to find the % NH3. Preparation of approximately 0.3M HCl solution: measure 12.5mL of HCl, dilute with deionized water to a total volume of 500mL, stir 2-3 minutes and transfer to screw cap bottle. Standardizing HCl process: approximately 0.8000-1.1000g of THAM was weighted out and put into 250mL Erlenmeyer flask and dissolved with 90-100mL deionized water. 3-5 drops of brom-cresolgreen indicator was added to flask. Contents in flask are then titrated with HCl solution to an ideal green color. Data and calculations for overall Molarity of HCl solution are as follows, with the chemical equation:

Identifying Synthesized Compound (HOCH2)3CNH2 + HCl -> (HOCH2)3CNH3+ + ClData Table 2: Molarity of HCl Solution Mass of THAM 0.8290g 0.8228g 0.8016g Vol. HCl used 23.00mL 22.85mL 22.30mL Molarity of HCl 0.2957M 0.2976M 0.2960M

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Average Molarity: 0.2964M HCl with 0.2587% deviation Calculations 2: Molarity of HCl Solution Sample Calculation: 0.8290gTHAM/121.14THAMg/mol = 0.0068molHCl (HCl & THAM 1:1 ratio) 0.0068molHCl/0.02300LHCl = 0.2957M HCl Average Molarity: (0.2957+0.2976+0.2960)/3 = 0.2964M Deviation: Sample for one value: (0.2957-0.2964)/0.2964 * 100 = 0.2362 Standard Deviation -> (0.2362+0.4049+0.1350)/3 = 0.2587% Analysis of % NH3 Using Standardized HCl The procedure for this analysis is fairly similar to the standardization of the HCl solution, but with an extra step before the titration process. Before titrating to find the % NH3 in the Co-Compound, distilling the NH3 gas from the compound is necessary. Prepared 150mL of 9M NaOH (1:1 dilution of 50% NaOH) and cooled to room temperature. Prepared 3 250mL Erlenmeyer Flasks with 2.0g of Boric Acid in 50mL of DI water; made sure to dissolve boric acid in flask before moving on. Three samples of Co-Compound were weighed out. Apparatus for

Identifying Synthesized Compound

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production of ammonia was setup; hot plate elevated on tripod, ice bath next to tripod with boric acid mixture in the ice bath, clean Erlenmeyer flask placed on hot plate, add weighed out Co-Compound into flask, rinsed all of sample into flask with DI water and continued to add DI water until 50mL reached inside flask, gentle stirring started on hot plate, quickly added 50mL of NaOH into flask with CoCompound, tight rubber seal applied to the flask on the hot plate, and the glass tube immediately placed into the flask with the boric acid. Once a steady boil was reached, the boiling continued for an extra 20-35 minutes. At the end of the boiling process, both flasks were left in place to cool off, but the rubber stopper was removed. After 4-5min, the delivering tube was raised slightly to rinse off any residue via DI water. Removing the boric acid flask with the trapped NH3, 3-5 drops of brom-cresol-green indicator was added and then titrated with the HCl solution. Data and calculations are as follows: (during distillation) (during titration) (Overall Equation) NH3 + H3BO3 -> NH4+ + H2BO3H2BO3- + HCl -> H3BO3 + ClNH3 + HCl -> NH4+ + Cl-

Data Table 3: % NH3 Analysis Mass of Co-Compound Vol. HCl in Titration 0.3568g 0.3577g 0.3573g 14.90mL 15.10mL 15.00mL % NH3 in Co-Compound 21% 21.2% 21.3%

Average % NH3: 21.2% with 0.47% deviation Calculation 3: % NH3 Analysis

Identifying Synthesized Compound Sample Calculation: 0.01490L * 0.2964M HCl * 17.024NH3 g/mol = 0.075g NH3 % NH3 = 0.075g NH3/0.3568g Co-Com * 100 = 21% Average -> (21+21.2+21.3)/3 = 21.2% Deviation -> (21-21.2)/21.2 * 100 = 0.94% (0.94+0+0.47)/3 = 0.47% Preparation and Standardization of 0.1M Na2S2O3 (Sodium Thiosulfate)

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The purpose of this experiment is the same as the HCl solution experiment, to prepare a titrant, but this time for analysis of the amount of Cobalt in the compound. Prepared 500mL of 0.1M (aq) Na2S2O3 [12.4g of S2O3 2-, the rest with DI water]; dissolved 0.3g Na2CO3 in Na2S2O3 as preservative. Standardization performed in triplicate. Weighed out 0.1000-0.1200g of KIO3, put into clean Erlenmeyer flask and added 70-80mL DI water; made sure to dissolved the KIO3. Weighed out 3.0g of KI and added to KIO3 mixture. Next, 3mL of 6M HCl was added to the mixture under the hood and swirled to dissolve. Once a brownish-red color was achieved, it was quickly titrated with the prepared Sodium Thiosulfate to the first sign of colorless. Data and calculations are as follows: (Overall Equation) IO3- + 6H+ + 6S2O3 2- -> 3S4O6 2- + I- + 3H2O

Data Table 4: Standardization of Na2S2O3 Mass of KIO3 0.1030g 0.1024g Vol. of Na2S2O3 27.60mL 27.30mL Molarity of Na2S2O3 0.1051M 0.1062M

Identifying Synthesized Compound 0.1021g 27.20mL 0.1066M

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Average Molarity of Na2S2O3: 0.1060M with 0.53% deviation Calculation 4: Standardization of Na2S2O3 KIO3 + 6HCl + 6Na2S2O3 -> 3Na2S4O6 + KI + 3H2O + 6NaCl Sample calculation: 0.1030g KIO3/214KIO3 g/mol * 6mole Na2S2O3 = 0.0029molNa2S2O3 Molarity -> 0.0029molNa2S2O3/0.0276L = 0.1051M Na2S2O3 Average -> (0.1051+0.1062+0.1066)/3 = 0.1060M Deviation -> 0.1051-0.1060 = 0.0009 (0.0009+0.0002+0.0006)/0.1060 * 100 = 0.53% Analysis of % Co3+ Using Standardized 0.1M Sodium Thiosulfate Weighed out 3 samples of 0.5000-0.7000g of Co-Compound and placed into separate, clean Erlenmeyer flask; little DI water was used to rinse all of compound into flask. Next, 35mL of DI water was added into flask along with 10mL of 50% NaOH. The mixture(s) was heated and smooth boiled under the hood for 20 minutes, afterwards cooled to room temperature in ice bath. From here, the process must be done individually. Weighed out 2.0g of Ki and added to cooled contents in flask. Contents are then swirled for 4-5 minutes. Under the hood, 40-50mL of 6M of HCl was added to mixture in small 3-4mL increments, with a bit of swirling in between addition. Once a red-brown color was reached, 5mL of Sodium Thiosulfate and 5mL of Starch indicator was quickly added. Continued on with titration process with Sodium Thiosulfate until dark color first disappears. Data and Calculations are as follows: 2Co(NH3)4Cl3 + 2S2O32- -> 2Co+2 + S4O6 2- + 8NH3 + 6Cl-

Identifying Synthesized Compound Data Table 5: % Co Analysis Mass of Co-Sample 0.5018g 0.5072g 0.5047g Vol. of Na2S2O3 12.80mL 13.00mL 12.85mL % Co 15.9% 16.01% 15.9%

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Average % Co: 15.94% with a 0.31% deviation Calculation 5: % Co Analysis Sample calculation: 0.01280L Na2S2O3 * 0.1060M Na2S2O3 * 58.93Co g/mol = 0.0800g Co % Co = (0.0800g Co/0.5018g Co) * 100 = 15.9% Average -> (15.9+16.01+15.9)/3 = 15.94% Deviation -> 15.9-15.94 = 0.04 Standard Deviation = (0.04+0.07+0.04)/3 = 0.05 -> 0.05/15.94 *100 = 0.31% Discussion Although the proper tools were provided for the experiments to identify the Co-Compound, it still isnt safe to say that every piece of information found was correct. Various factors come into play when working with the tools; the two main factors that could have possibly thrown the data off is time and being human. Being a human, mistakes are bound to happen when handling equipment of any kind, such as measurements or transferring materials that are close to one another; for example, transferring more ice into an ice bath with a flask inside.

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With that being said, although the Standard Deviations were quite low on each calculation, certain data could be inaccurate. With these series of experiments, what was found to be the greatest obstacle was time. For the most part, the bulk of the experimentation was spent on waiting. Either waiting for the contents to finish heating and drying, or boiling. Due to the fact that there was only a limited amount of time allowed in the lab, some parts of the experiment had to be rushed. Also, a confusion about certain instructions were also a problem. This became a big problem when performing the distillation experiment. There was confusion as to how long to keep the contents at a steady boil so as to trap the NH3 gas in the boric acid. For the first two trials, the boil was kept at a steady 35 minutes. However, instructions were changed by the time the third trial came around, and that trial was only kept for 20 minutes. Heat is energy essentially, so the longer the contents boiled, the more should have transferred, unless there was only a set amount of NH3 to be distilled trapped. Other than those reasons being a possible factor in data miscalculation, it is believed that the set of experiments done was successful in identifying the correct Co-Compound formula. Each and every procedure done in these series of lab experiments were vital in identifying a synthesized compound. Once a compound has been synthesized, it is difficult to know exactly what is in the sample because a lot of external factors can come into play; such as any possible impurities, or equipment that havent been properly cleaned. Every step, especially the standardization experiments, were vital. If the titrants are prepared correctly, the chemical equation wouldve been offset and the calculations mightve looked a lot different. So in order to determine the percent amount of each substance in the sample, practice in titration are necessary since it is being done by a human. Results and Conclusion After having conducted the various experiments to determine the percent amount of each substance in the Co-Compound sample synthesized, the following data was reached: An average of

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59.28% of the halide, in this case Bromine, with a deviation of 0.27%, an average of 21.2% of Ammonia with a deviation of 0.47%, and an average of 15.94% with a 0.31% deviation. These values were found as best as humanly possible. Once these values were gathered, a comparison was done with the chart provided in the lab manual and two conclusions were reached. The Co-Compound could either be identified as [Co(NH3)6]Br3 or [Co(NH3)5Br]Br2. The data points for formulas were relatively close, however the data for [Co(NH3)5Br]Br2 came to be much closer to the data found in the experiments. Although the % Halide for [Co(NH3)6]Br3 was much closer to the data found, the % Ammonia and % Co for the chosen option matched up more with the experimentally found data. Why choose the latter even though the % Halide for the former was closer? Simply because the % Halide Analysis was done much sooner than the other experiments, and the other data was found via titration. Titration processes provide more accurate information about a compound because it reveals the pKa of the sample, the reactivity of the sample, and it [titration process] was also done to find one of the harder to identify substance in the compound, the ammonia gas. Distillation is a difficult process, if done wrong, the amount of gas trapped could be gone in an instant. To put it simply, [Co(NH3)5Br]Br2 is more accurate because of the three necessary data sets that were needed to be found, two were a very close match-up. In this case, it might be bad to say, but majority rules. With two data sets out three matching up to the experimentally found data, there is a much higher chance for accuracy with more match-ups. To conclude, Synthesis V, the production of a Cobalt Amine Halide complex, is [Co(NH3)5Br]Br2.