CHEM202

EXPT. 2 1

CHEM202 Coordination Chemistry Laboratory Expt. 2 Synthesis of a Geometric Isomer and Application of Ionic Conductivity
Kamil Krawczyk 50411107 Oct. 14/2011 L09 Group A Method Used: B

Conductance data from method A obtained from Vinayak V.

Expt. 2 Synthesis of a Geometric Isomer and Application of Ionic Conductivity

Introduction:

There are multiple manners of chemical preparation in a lab. When producing a particular compound, one must take into account many factors brought forth by varying methods of production; for example, the availability and ease of reagents, yield and overall purity of product, and (most importantly when being prepared on a commercial level) the economics and financial aspects involved. For example, the production of sulphuric acid (chemical formula H2SO4) can be achieved by either the nitration (informally known as the Chamber/Tower) process, or the catalytic (Contact) process. Both methods produce sulphuric acid in relatively equal strengths; however, the Contact method is used to produce the majority of sulphuric acid in the world due to a far more economical nature. [1] The compound cis-potassium diaquadioxalatochromate(III) (chemical formula cis-K[Cr(C2O4)2(H2O)2]) can be prepared from either potassium dichromate (an orange solid) or potassium chromate (a yellow solid) and reacting it with oxalic acid dehydrate (an opaque white powder). The quality and purity of the manner of production will be reflected within the final product. In this experiment, cis-K[Cr(C2O4)2(H2O)2) will be produced from the two aforementioned starting materials by different groups. The products obtained through the process will be compared and analyzed in terms of their respective ionic conductance. Furthermore, molar conductivities will be calculated and compared to an authentic and pure sample. Thus, the preferred method will be evident and concluded upon, with purity in mind.

Data and Results:

Please refer to the attached results reporting form (RRF). Sample calculations are found on the RRF and the back of this report.

Discussion:

By analyzing the data formulated in the Results Reporting Form for Experiment 2, we can see that, by producing the cis-isomer via Method A, we create a more pure compound. The molar conductance, , was found to be 115 ohm-1 cm2 mol-1. Conversely, the molar conductance for the cis-isomer via Method B resulting in a molar conductance of 142 ohm-1 cm2 mol-1. The literary value provided on the sheet states that the pure cis-isomer has a molar conductance of 86 ohm-1 cm2 mol-1. Therefore, we can conclude that Method A yielded a more pure product, since the value calculated was closer to the literary value. It is interesting to note, that despite having a greater purity by utilizing method A, it seems to impact the percent yield. Comparing the data values obtained 1 Friedman, Leonard J., and Samantha J. Friedman. "The History of the Contact Sulfuric Acid Process." Acid Engineering & Consulting, Inc. (2008). Print.

CHEM202 EXPT. 2 3 to my lab partners, Method A yielded 81.92%, whereas Method B yielded 95.85%. However, this may be a cause of improper lab procedures resulting in a lower yield by the other student rather than a general ersult of the reaction in Method A. When preparing the reagents, there was no need to apply the hot spatula to the granulated powder; the reaction began spontaneously. The frothing was violent, producing a grey smoke and a black, viscous substance in the mortar. The reaction occurred similarly regardless of the method in use. However, it is notable that some students had trouble beginning their reaction; it was rather surprising to see my personal experiment begin with no need for external heat (ie. the spatula). As outlined in the lab manual, a filter paper test took place. The cis-isomer, when combined with water, did not dissolve; it formed a dark brown clump in the middle of the paper as the water spread through the sheet. However, the trans- isomer (which was provided in lab) dissolved readily with the water, forming a green/blue solution that spread across the sheet. The results lead to the conclusion that the cis-isomer of the product is poorly soluble in room-temperature water, whereas the trans-isomer is, forming a green/blue solution. The final product, regardless of method used, is a dark brown powder, bearing a resemblance to flour in consistency, although appearing to be slightly denser. An interesting observation is the measured conductivity of the substance, depending on the method: with method A, the measured conductivity was 1294S (micro-Siemens), and with method B resulting in 1594S. By further analysis, we come to the aforementioned conclusion that method A is more pure.

Questions:

1. I had not seen the product produced by Method A, but it safe to assume that both products are similar in appearance. This is because both products are the same. Regardless of the method used, cis-potassium diaquadioxalatochromate(III) is the product, and therefore should not be differentiable by appearance alone. 2. By comparison of data, it is evident that Method B yields a product with a higher conductance. This is because the product is less pure, therefore releasing more ions into solution (due to it having a lower solubility an inherent trait of low purity). Because of this, the measured conductance is greater, and therefore an indicator of lower purity. 3. The molar conductance of the products obtained by the two different methods varies. Molar conductance is a property related to purity, and this case, can be deduced with that in mind. Since method A yielded a product with a lower molar conductance (one that is more accurate to the literary value), it means that it less readily dissociates in water to form ions (less impurities, resulting in an expected and generally lower solubility). Molar conductance is also known as ionic conductance; the more moles of ion in solution, the greater the conductivity. Furthermore, since method B yielded a product with a higher molar conductance (one that is further away from the literary value), the product is less pure

Expt. 2 Synthesis of a Geometric Isomer and Application of Ionic Conductivity

(with more impurities), and thus, its solubility is hampered. Since, by comparison, a pure cis-isomer has a particular solubility, resulting in a lower conductivity, we see that method B produces something that is less pure and therefore contains a higher concentration of ions in solution, due to the solubility being affected by the impure nature of the product.

Conclusion:

In conclusion, by following the procedures outlined in the CHEM202 lab manual, the cis-isomer of potassium diaquadioxalatochromate(III) was formed via two methods (of which method B was assigned to produce personal data). Upon further analysis, it was determined that method A (involving potassium dichromate) yielded a more pure product in comparison to method B (involving potassium chromate). The overall objective of the lab to determine which method produced a purer compound was successfully completed. This was concluded by an analysis of molar conductance. It was found that method A yielded a product with a molar conductance of 115 ohm-1 cm2 mol-1 and method B yielded 142 ohm-1 cm2 mol-1; thus, it is evident that method A, with a value closer to the literary value provided in the lab notebook of 86 ohm-1 cm2 mol-1, is the production method that leads to a more pure compound. Sources of error that may have arisen during the experiment are varied. The most likely error is improper lab protocol and a lack of a thorough understanding and practice of the lab procedures. This ultimately would have lead to an even lesser pure compound and somewhat irregular molar conductance. By minimizing error from misunderstanding, the product is far more pure, far more understandable, and can be used to provide an even stronger analysis granted that purity plays a role in the experimental goal.