EXPERIMENT 6

DISTILLATION & CHROMATOGRAPHY

NAME:JOSHUA HARRIPERSAD DATE:20/11/2021 Lab Day: MONDAY

DEMONSTRATOR; DONNA HITLAL

PRE-LAB EXERCISES [Pre Lab Total 28 Marks]

1. Draw SIMPLIFIED flow charts of your experimental procedures A - D to be performed.

[4 x 5 marks]

Part A Simple Distillation of a Mixture

Part B Fractional Distillation of a Mixture
Part C TLC Analysis of Spinach and Carrot Extract
Part D COLUMN CHROMATOGRAPHY OF BEET
2. State ALL the different stationary phases that could be used in TLC or column chromatography. [ 3
marks]

1. Silica gel
2. Alumina
3. Cellulose

3. What other type of distillation technique is available for use in the laboratory? What is it used for?[5
marks]

Steam distillation is used in the laboratory to separate easily volatile substances from mixtures
containing

non-volatile substances.
DATA ANALYSIS [Total 47 Marks] Parts A and B Simple and Fractional Distillation of
a Mixture

1. (a) Mass of distillate 1 from SIMPLE distillation: 28.6g [1 mark]

Mass of distillate 2 from SIMPLE distillation: 42.16g [1 mark]

Mass of distillate 1 from FRACTIONAL distillation: 17.46g [2 marks]

Mass of distillate 2 from FRACTIONAL distillation: 45.72g [2 marks]

(b) Boiling point of distillate 1 from SIMPLE distillation: 59.oC [1 mark]

Boiling point of distillate 2 from SIMPLE distillation:100.oC [1 mark]

Boiling point of distillate 1 from FRACTIONAL distillation: 80oC [2 marks]

Boiling point of distillate 2 from FRACTIONAL distillation: 100oC [2 marks]

Part C TLC Analysis of Spinach and Carrot Extract

2. Rf value for each spot observed on your TLC chromatogram:

(i) Spinach [5 marks]
SPOT # Distance moved by spot / cm Distance moved by solvent front / cm Rf value

1 2.7 7.3 4.6

2 3.2 7.3 4.1

3 3.5 7.3 3.8

4 6.8 7.3 0.5

5 2.7 7.3 4.6

6 3.2 7.3 4.1

7 3.5 7.3 3.8

8 6.8 7.3 0.5

6
CHEM 1070 Experiment 6

(ii) Carrot [5 marks]

SPOT # Distance moved by spot / cm Distance moved by solvent front / cm Rf value

1 6.8 7.3 0.5

2 6.8 7.3 0.5

3. Draw a properly labelled, annotated diagram of each of your TLC sheets: [2 x 5 marks]

(i) Spinach

(ii) Carrot
Part D Column Chromatography of Beet Extract

4. Volumes and colours of your fractions from your column chromatography experiment:

[5 marks]
FRACTION # VOLUME / mL COLOUR

1 4.9 Purple

2 2.8 Red

3 3.0 Red

4 3.6 Orange

5 5.6 Pale Pink

6 4.0 Colourless
5. Properly labelled diagram OF YOUR COLUMN, showing very clearly your column results: [5
marks]
OVERALL CONCLUSIONS/ANY OTHER COMMENTS [5 marks]

● The boiling points that varied in the simple distillation setup were 59℃ for distillate 1
and 100℃ for distillate 2. The fractional distillation values were 80℃ for its first
distillate and 100℃ for the second.
● An important fact to note is that the simple distillation procedure worked effectively for
temperature variations of 41℃ while fractional distillation separated substances of a
more precise temperature difference of 20℃ in this experiment.
● For Thin Layer Chromatography, the spinach extract presented more separations of
components or more spots on the TLC plate than the carrot extract.
● The Retention Factor (Rf) values for the spinach extract were 4.6cm, 4.1cm, 3.8cm,
0.5cm, 4.6cm, 4.1cm, 3.8cm and 0.5cm for spots numbered 1 to 8 respectively for two
sample spots that were presented on the x’s of the TLC plate after subjection to the
mobile phase. The Retention Factor (Rf) values of the carrot extract were both 0.5 cm for
the two sample spots that were presented on the x’s of the TLC plate after subjection to
the mobile phase.
● In the Gravity Column Chromatography of the beet extract, the distilled colours
observed after distillation from the column into 6 different measuring cylinders were:
purple, red, red, orange, pale pink and colourless. These 6 colours respectively
corresponded to volumes of 4.9ml, 2.8ml, 3.0ml, 3.6ml, 5.6 and 4.0ml.