Aya Rahav CHEM351L (0108) 02-16-09 Post-lab Questions - TLC Q 1. Why is it important to co-spot when identifying an unknown? A 1. It is important to co-spot when identifying the unknown to make sure that after the TLC is done, there is only one dot and not two close together. Q 2. A TLC plate showed two spots with Rf values of 0.25 and 0.26. The plate was removed from the developing chamber, the residual solvent was evaporated from the plate, and the plate was returned to the developing chamber. What would you expect to see after the second development was complete? A 2. After the second development was completed, there should be a more distanced distance between the spots. The spots moved about a quarter o the page, so on the second time, they should move about the same (almost to the middle). In addition, as said before, the distance between them should be about twice as it was. Q 3. Why might it be very difficult to visualize the separation of cis- and trans- 2-butene by TLC? A 3. Cis and trans 2-butene have many chemical and physical properties. Although they have double bonds between the carbon atoms, it is possible to break them and make new bonds (i.e. temp), and for that reason, cis 2-butene can become trans 2-butene and vise versa. Since polarity is used in TLC, it would be hard to see the difference in them. Aya Rahav CHEM351L (0108) 02-16-09 Pre-lab questions – Melting Points and Recrystalliztion Q 1. Two test tubes, labeled A and B, contain substances with approximately the same melting points. How could you prove that the test tubes contain two different compounds? A 1. In order to determine whether the two substances are different, s mixing of both substances and checking the mixture’s boiling point will help determine if the test tubes contain two different compounds. If the melting point of the mixture remains the same (as previously recorded) then the two substances are the same, but if the melting point range increases and lowers in temperature, then the two substances are different. Q 2. If 25 g of phthalic acid is dissolved in boiling water and then recrystallized by cooling the solution to 14oC, a. How many grams of phthalic acid will recrystallize out? b. How much of the phthalic acid is unrecoverable by virtue of its insolubility at 14oC? A 2. a. Phthalic acid is very soluble in boiling water (18g/100mL) and it is very insoluble in 14oC (0.54g/100mL). Therefore, 139g of water are needed to dissolve all phthalic acid. Now, calculating how many grams will recrystallize out: 18-.54=17.46 17.46*139/100=24.27 Therefore, 24.27g will recrystallize out. b. If starting with 25g of phthalic acid and 24.27g recrystallize, 0.73g will not be recoverable. Q 3. The goal of recrystallization is to obtain purified material with a maximum recovery. Explain how using an unnecessarily large volume of solvent to dissolve the crude material will impact this goal. A 3. The yield when performing recrystallization is never 100% because while the cooling solvent will release some crystals, some will remain dissolved in the cold solvent. So, by using an unnecessarily large volume of solvent, more of the sample will remain in the solvent after cooling.