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Experiment 1

Date: 23 February 2014

Title Objective

: Distillation of a Mixture of Liquid. : To separate two miscible liquids based on their boiling points difference.

Chemical Equation or Structural Formula of Organic Compounds Involved:

CH3CH2-O-CH2CH3 Diethyl ether Boiling point: 34.6C Equipment

Ar-CH3 Toluene Boiling point: 110.6C

: Round bottom flask (100mL), thermometer, adapter, distillation head, clamp, water condenser, electrothermal heater, measuring cylinder (50mL) and electronic balance. : Diethyl ether (20mL), toluene (20mL), boiling chip. :

Chemicals Procedure

In this experiment, Diethyl ether (20mL) and toluene (20mL) were measured using measuring cylinder and then mixed in a 100mL round bottom flask with 2-3 pieces of boiling chips. A simple distillation apparatus which included round bottom flask, thermometer, adapter, distillation head, clamp, water condenser and electrothermal heater is set up. After that, four empty vials with caps are weighed respectively using electronic balance and labelled. The mixture in the flask is distilled using simple distillation. The fractions having boiling points (a) (32-39) C (b) (40-111) C (c) 112C are collected in four different vials. The vials with caps and products are weighed using electronic balance. The weights of the products are recorded. The products are submitted to the lecturer in a labelled vial along with jotter book. Simple distillation gave diethyl ether (0.84g) with boiling point 32-39C (ref. 34.6C) and toluene (25.85g) with boiling point 40-111C (ref. 110.6C) Observation : 32-39C 13.29g 14.13g 0.84g 40-111C 13.28g 9.20g 29.05g 19.28 15.77g 10.08 >112C 13.16g 13.51g 0.35g

Weight of empty vial Weight of empty vial + distillate Weight of distillate

Discussion

Distillation is a widely practiced physical separation process which separates two volatile liquids. There are fundamentally two different types of distillation, simple and fractional distillation. In both distillation method, a mixture of liquids is vaporized, the vapour is subsequently condensed, the condensate or distillate is later collected. Due to the vast difference in boiling points of diethyl ether and toluene, simple distillation is performed in this experiment. Since both diethyl ether and toluene are volatile liquids, an electrochemical heater is preferred over a Bunsen burner to avoid any fire accidents. The mixture of diethyl ether and toluene is heated in the distillation flask fitted with a thermometer and a water condenser using a electrochemical heater. Some boiling chips are added in the mixture prior to the heating in order to ensure a steady stream of small air bubbles is produced when the mixture is heated instead of sudden explosive boiling whereby large bubbles erupt. In the temperature range of 32-39C, the more volatile liquid (lower boiling point), in this case diethyl ether, boils first and the vapours distil over from the outlet near the top. The vapour is immediately passed through the condenser and condensed into liquid state. This condensed liquid or distillate is then collected in a labelled vial. The less volatile liquid, i.e. the one having higher boiling point, is collected in the temperature range of 40-111C. This liquid is toluene because toluene has higher boiling point compared to diethyl ether. Upon completion of the experiment, it was calculated that the mass of diethyl ether obtained is 0.84g whereas the mass of toluene were collected in two vials and the mass is 25.85g. The original weight of diethyl ether and toluene added into flask is 14.28g and 17.34g respectively. The calculation is shown below: 14.28g It has been observed that some errors occur during the experiment which leads to the disparity between the experimental result and the theoretical yield. One of the possible source of error is the parallax error when taking the reading the thermometer and measuring cylinder. Besides, few drops of distillate could have been lost during the replacement of new vial for the distillate and the distillate might have vaporized before it is weighed. To minimize the extent to which those errors affect the experimental result, it is encouraged to take several precautions. Parallax error can be reduced by taking several readings and calculate average from the readings. The new vial should be prepared earlier to replace the old vial immediately when the temperature reached to prevent the losing of distillate. Besides, the vial should be closed immediately with cap to secure the product from possible vaporization.

It is also advised to conduct the experiment in a safe manner by adopting the following measures. First, suitable amount of boiling chips (in this case 2 or 3) must be added into the mixture to avoid the occurence of bumping. Moreover, all joints should fit together without being under tension and the distillation flask should be not more than 3/4 full to avoid any potential spilling accident. Apart from that, the top of the thermometer bulb should not touch the glassware and should be even with the bottom of the distillation head side arm. The thermometer should fit tightly in the rubber holder. Furthermore, the collecting vessel (10mL grad. Cylinder) should be close to the exit from the condensing column. Lastly, it is also necessary to make sure the water vapour from the mixture can escape to the atmosphere at the end of the apparatus.

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