Question
Hi,
I'm writing a lab simple distillation report for my organic chemistry class but i'm unsure how to determine the characterize the ester with my data.
Are literature values the same as reference value?
Thanks!
ated time for the experiment: 2.0 h. Estimate Ph Compound Ethyl acetate trars ave cal Properties of Components MW Amount mp(C) 88.12 1.0 mL. bp("C) d nD 1.2-Dibenzoylethylene 236.27 77 0.90 1.3723 50 mg nts and Equipment. Transfer 1 mL of the yellow stock solution el Reax-1,2-dibenzoylethylene/ethyl acetate, 50 mg/mL) to a 3-mL conical vial matic delivery pipet (remember to place the vial in a small beaker to t tipping during the transfer). Place a boiling stone (or a magnetic spin desirable) into the vial and assemble the Hickman still head. The still by auto ne if va is mounted in a sand bath on a hot plate (see Fig, 6.2). mental Conditions. The temperature of the bath is raised to 90-100 °C at a rate of 5 °C/min. CAUTION: Do not let the temperature of the still rise too rapidly Once boiling commences, the rate of heating should be lowered to the point where the temperature increases at 2-3 °C/min. A slow distillation rate is very important in establishing equilibrium between the vapor and liquid com- ponents in the mixture. Follow the course of the distillation by the rise of con- densate on the sides of the Hickman column. When the condensate reaches the trap, adjust the bath temperature so that liquid is removed from the col- umn slowly (100 L/3 min). A smooth, slow distillation will provide a cleaner Clamp Thermometer Clamp 14/103 Hickman still head Clamp O-ring Thermometer 90-100 °C 14/101 and threaded compression cap Crystallizing dish 3-mL conical vial Sand Boiling stone mnmmnnhnn Hot plate Magnetic stirrer Heat control Stir control Figure 6.2 Hickman still
Explanation / Answer
yes, maximum time litrature value is same as reference value. but it depend on the how much crystal is pure. if your crystal is pure (checking from nmr, there is no signal for impurity) then you can get accurate value of melting point. You can take maximum litrature value as a reference but before taking you can check pure nmr of product.
