Emerson Wang, 1 Identifying an unknown compound synthesized from copper(II) sulphate, ammonia, and ethanol, using gravimetric, volumetric,

and spectrophotometric methods. Purpose The purpose of this lab was to identify the chemical formula of a compound created from an initial mass of copper(II) sulphate pentahydrate. The compound was to be created by first creating an aqueous solution of copper(II) sulphate using distilled water, before mixing it with ammonia. The precipitate created by this process was then subject to a solution of ammonia-ethanol and filtered again to get the final compound. This compound was analyzed for the presence of copper ions, sulphate ions, and ammonia in order to come to a conclusion of its identity. Data Collection and Processing Part A Synthesis of the Compound Qualitative process The copper(II) sulphate was originally a sparkly, pure blue crystal. After adding it to water, it became a murky, indigo color. As the ammonia and ethanol were added, the solution became more and more viscous as well as emitting a noxious smell which burned the nostrils (despite the beaker holding it being held under a fume hood). The general appearance remained the same the entire time after the initial solution was created, but the smell only got more and more sharp. During the filtration process, the precipitate appears as a clay-like, indigo mass. The appearance did not change even after the second filtration. Part B Gravimetric Analysis of Sulphate Ions Table 1: Quantitative table of the raw values yielded in the Part B of the procedure, including the volumes of the unknown substance, the lead(II) nitrate, and the PbSO4 precipitate created. Sample Mass of Blue Volume of Volume of Mass of Mass of Mass of Compound the nitric lead(II) nitrate Filter Paper Filter Paper PbSO4 ( 0.01 g) acid ( 0.25 mL) ( 0.1 g) and White ( 0.11 g) ( 0.25 mL) Precipitate ( 0.01 g) A B C 0.9 0.9 1.1 10 9.95 10.05 2.5 1.5 1 0.9 0.9 0.8 1.57 1.41 1.53 0.67 0.51 0.73

Initially, the nitric acid was a clear, colorless liquid. Upon the addition of the blue compound, it became a clear, vivid light blue color. Then, after mixing this solution with lead(II) nitrate (which was also clear and colorless with slight bits of residue in it), it became a cloudy, milky blue, with a dusty precipitate in it.

Emerson Wang, 2 Average Mass of PbSO4= 0.637 0.155 g Average Mass of Blue Compound = 0.967 0.03 g PbSO4 ------> Pb + SO4 nPbSO4 = m / (MSO4 + MPb) = 0.637g / (32.065M + (4)(15.9996M) + 207.2M) = 0.0021 mol nSO4 = 0.0021 mol mSO4 = 0.0021 mol * 96.0634 = 0.202 g m%SO4 = (0.202 g/ 0.967g) * 100 = 20.86% It can be seen that out of the original samples, 0.637 g of PbSO4 was created. Then, using this mass, the moles of PbSO4 was found. Since the ratio of PbSO4 to SO4 in this equation is 1:1, the moles of SO4 must also be 0.0021 mol. Out of the original mass of the blue compound used in these samples, 0.0021 mol of it was SO4, therefore the moles of SO4 in the blue compound is thus far 0.0021 mol per 0.967 g, and SO4 has a mass percentage of 20.86% in the total compound. Part C Volumetric Analysis for Ammonia Table 2: Quantitative table containing the volumes of the unknown compound solution, methylorange, and HCl used in the titration of NH3 in the unknown compound. Sample Mass of Blue Volume of Solution Methylorange Volume of HCl Compound Created Added to Solution Before Purple ( 0.01 g) ( 0.25 mL) Color Appears ( 0.25 mL) A B C D 0.97 1.01 1 1 30.01 29.98 30.02 30.1 10 drops 10 drops 10 drops 10 drops 32 34 37.3 30.1

The solution of the blue compound with water created a blue, opaque liquid. When the methylorange was added, the color turned a very dark blue, with a very slightly lighter blue at the bottom of the solution. As the hydrochloric acid was dripped into the solution, it gradually grew murky green, then began quite suddenly shifting to a more pinkish/purple color, with small bursts or clouds of purple appearing before the entire solution turned orange, then pink, then purple. Average Volume of HCl = 33.35 ( 0.277 mL) Average Mass of Blue Compound = 0.995 ( 0.02 g) CHCl = 0.5 M nHCl = 0.5 M*0.03335 L = 0.0167 mol nNH3 = 0.0167 mol

Emerson Wang, 3 By finding the amount of moles required for the HCl to neutralize the base in the blue compound solution, one can also find out the moles of the base in the blue compound solution. Knowing this, it can be seen that there is 0.167 mol of NH3 per 0.995 g of the blue compound, and it has a mass percentage of 30.25%. Part D Spectrophotometric Analysis of Copper Ions Table 3: Raw percent transmissions yielded from nitric acid/blue solid solutions placed into a colorometer. Sample Volume of Cu2+ Volume of Mass of Blue % Transmission Solution Used nitric acid Used Solid Used ( 0.25 mL) ( 0.25 mL) ( 0.01 g) 1 2 3 4 5 6 0 4 7 9.95 0 0 10 6 3 0 10 10 0 0 0 0 2 3 0 66.88 52.03 37.26 66.35 44.79

The solutions created were a light blue color, with each one getting slightly darker as more Cu2+ was added to the nitric acid. The nitric acid itself was a clear, colorless liquid. Table 4: Processed data showing the percent absorption for each sample, which was found using the Beer-Lambert law and the percent transmissions found using the colorometer. Sample % Absorption 1 2 3 4 5 6 Beer-Lambert Law A = ebc 0.1782 = ( 20 L mol-1 cm-1 )( 1 cm )c c = 0.1782/(20 L mol-1) = 0.00891 mol/L nCu2+ = (0.00891 mol/L) * (0.01L) = 0.0000891 mol 0 17.47 28.37 42.88 17.82 34.88

Emerson Wang, 4 m% = 28.31% As shown by the Beer-Lambert law, the colorometer was able to reveal the concentration of Cu2+ in the unknown compound, yielding a concentration (c) of 0.00891 mol/L. Using c, the moles of Cu2+ can be found by multiplying c by the liters of the solution, in this case 0.01 L of the nitric acid/unknown compound solution. This gave n of 0.0000891 mol per 0.02 g, and a mass percentage of 28.31. Chemical Formula Now that the relative moles and percent mass of each component of the unknown compound have been found, it is possible to create a ratio to each other, so that the empirical formula of the compound can be found. Table 5: Percent mass of each of the components of the unknown solid Component Molar Mass (g/mol) Percent Mass (%) SO4 NH3 Cu2+ H2O 96.0626 18.05 63.55 33.0088 20.86 30.25 28.31 20.58

Using this information we can then begin to find out how many moles each one is relative to the others, by assuming that together they make up 100g total. By doing this, each component should have a mass corresponding to their percent mass, and using that mass one can find the moles relative to each other. These values of moles correspond to the percent masses, meaning there is a direct proportionality. Table 6: Moles of each component out of 100g of unknown substance Component Mass in a 100g Unknown Moles (mol) Substance (g) SO4 NH3 Cu2+ H2O 20.86 30.25 28.31 20.58 0.2172 1.676 0.4455 0.6235

This shows the ratio of SO4 : Cu2+ : H2O : NH3 is 1:2:3:8 Therefore, the empirical formula of the unknown substance would be as follows: Cu2(NH3)8(SO4) 3H2O + 8H ---------> 2Cu2+ + 8NH4 + 1SO4 + 3H2O

Emerson Wang, 5 Conclusion and Evaluation Conclusion Initially, the compound was synthesized by mixing a copper(II) sulphate solution alternately with ammonia and ethanol. After the initial solution was created, a second was then made using another ammonia-ethanol solution mixed with the precipitate of the first solution. This precipitate was to be identified by isolating and analyzing certain components of it. First, it was established through the use of gravimetric analysis that the unknown compound contained SO4 with a percent mass of 20.86%. This was done by using lead(II) nitrate and nitric acid to create a precipitate, PbSO4, isolating the sulphate component of the mystery compound. Using this, the percent mass off sulphate in the unknown compound was found. Next, a titration was performed in order to isolate the concentration of ammonia in the unknown compound. This was done by first making the unknown compound into an aqueous solution using distilled water. Then, hydrochloric acid was used in conjunction with methylorange indicator in order to observe what volume of the hydrochloric acid was required for the methylorange indicator to turn a purplish color, indicating that he ammonia in the unknown compound had been neutralized. By calculating the moles of the 0.5M hydrochloric acid which was required to neutralize the ammonia, it was possible to then find out how much ammonia there was to be neutralized. The ammonia was found to have a percent mass of 30.25%. A colorometer was used to find the percent transmission of solutions containing various concentrations of Cu2+. Using the percent transmission, one can also find the percent absorption using A = log(1/T). Once the percent absorption was found for a 10 mL nitric acid solution containing 0.2 g of the unknown solid, the Beer-Lambert Law of A = ebc was used to find out the concentration of Cu2+ in that particular solution. Once that was found, the moles of the Cu2+ was easily found, and the percent mass out of 0.2 g was found to be 28.31%. With the rest of the percent masses already found, it was simple to subtract them from 100% and find that the amount of H2O in the compound was 20.58%. To find the formula of the compound, the percent masses of the four components had to be utilized to find out the ratio of each component to the others. This could be done by finding out, based on the percent mass that each component had, how many moles each component would have relative to the others. By doing this, a ratio was found of SO4 : Cu2+ : H2O : NH3 . In order to find this ratio, each component was assumed to be part of an unknown substance of 100g. This meant that, according to each of their percent masses, they would have a proportional mass. Using these proportional masses, the moles of each component were found, these moles being relative to their percent masses. Then, using the lowest amount of moles as a starting point, a ratio of moles to moles was made. This ratio ended up being 1:2:3:8. Now that the ratio was found, it was a simple matter to find out how molecules of each component were in the formula, because the molecules had the same ratio as the percent masses and the moles. The formula was found to be as follows:

Emerson Wang, 6 Cu2(NH3)8(SO4) 3H2O + 8H ---------> 2Cu2+ + 8NH4 + 1SO4 + 3H2O Evaluation This lab contained several points of error, the first of which being that it was done over several days. This meant that different sets of equipment were frequently switched around, and the conditions of the lab area were different at several points in the experiment. This could possibly affect the yield of the synthesis, because different temperatures, pressures, and humidity could affect the reactions, and different measurements taken with different instruments could lead to skewed measurements and slightly incorrect volumes and masses being used. Enough of these small errors undoubtedly led to an inaccurate percent yield. It would be better if the entire lab could be done in a shorter amount of time, such as two days rather than three (as doing it in one day would be outside of classroom limits, but perhaps a special event could be held for this lab). The titration process was also slightly inaccurate due to the ambiguity of using a visual indicator such as the methylorange. Because of the nature of the indicator, it is hard to tell exactly when the ammonia was properly neutralized. First of all, it isn't certain exactly which color means that the ammonia is neutralized (the procedure stated colors from orange, to salmon pink, to purplish). Second of all, it isn't possible to tell exactly what a color is, so human eyes aren't the most reliable way to track a neutralization. This again could add to the overall error. It would be better if even the colors being indicated were more definitive and less ambiguous. Rather than stating that it might be a few colors, give a specific color to watch out for, and maybe even use a different indicator to make this easier (an indicator which is more obvious and definitive when titrating). The filitration process was the last part which may have caused any significant error outside of random and human errors. The precipitate could not always be completely filtrated, because residue could always remain on the precipitate, mainly because they had to be left to dry overnight, meaning there is a chance of residue getting into the precipitate and perhaps changing the results of each analysis even slightly. Again, having less time and perhaps more security during the drying of the precipitate might be better, such as using the acetone to increase the drying speed, or even something as simple as covering the precipitate (this would increase the time required to dry the precipitate, meaning a drying agent would be even better). Reducing the errors in the filtration process would help to reduce the overall errors which were present in this lab.