Surname and Name : Mhlonyane Vuyelwa

Student Number : 202250216

Title : SEPERATION OF THREE COMPONENT MIXTURE BY EXTRACTION
Course Code : PAC213 Experiment 1
Due Date : 30 March 2023
THEORY

"Extraction" refers to transference of compound(s) from a solid or liquid into a different solvent
or phase. It is also possible to partition the components of a mixture between two immiscible
liquids. This process is called liquid- liquid extraction. There two types of liquid- liquid extraction
namely, organic solvent extraction and acid- base extraction. Organic solvent extraction in
which an organic solvent with high affinity for the desired compound is used to extract the
compound from another solution. An acid-base extraction, in which an organic acid or base is
extracted from an organic solvent by using an aqueous solution of an inorganic base or acid
respectively. A neutralization occurs which converts the compound into an ion, water- soluble
salt, causing it to transfer from the organic phase to the aqueous phase.

Method

A 3.0 g sample of three component mixture was dissolved in 25 ml ether. The solution was
transferred into a separating funnel.

A solution of 3ml concentrated HCl was added into 25ml water and shook thoroughly to extract
the basic component (p- toluidine), the technique of using a separating funnel was followed as
described above. The lower aqueous layer was drawn off into a 100ml water conical flask and
the extraction was repeated two more times. Then finally the excess HCl that may be dissolved
in the ether layer was extracted with 100ml of water. The three acid extracts were combined
with the water extract and set aside.

To separate the acidic component (2- naphthol) from the mixture, the remaining ether solution
was extracted 3 times with 25ml of aqueous sodium hydroxide (NaOH) and once with 10ml
water. The three alkaline extracts were combined with the water extract in an Erlenmeyer flask
and set aside.

The remaining ether solution which should contain only neutral component (p-dichlorobenzene)
was poured out through the top of the separating funnel into a conical flask. Enough anhydrous
calcium chloride (anhydrous CaCl2) was added to cover the bottom of the conical flask and the
mixture was swirled occasionally for 15 minutes. Then the ether was decanted into a small
beaker of known weight and placed in the hood to allow the ether to evaporate. The residue was
weighed, and its melting point was determined.

The combined acidic extracts were neutralized by adding 10% aqueous sodium hydroxide
(NaOH) until the solution is alkaline to litmus paper. The alkaline solution was extracted twice
with 25ml portions of ether, separating the first 25ml ether and combining it later with the second
25ml extract. Anhydrous calcium chloride was added and swirled as described above. Then the
ether was decanted into a small beaker of known weight and placed in the hood to allow the
ether to evaporate. The residue was weighed, and its melting point was determined.

The combined alkaline extracts were neutralized by adding conc. HCl drop by drop until the
solution is acidic to litmus paper. The solution was cooled in ice. The product was filtered off
under vacuum. The product was weighed, and its melting point was determined.
Results and Calculations

Compound Mass of a beaker Mass of a beaker

and product
Acidic 91,56 120,39
Nuetral 39,55 78,23
Basic 125,39 139,15

DISCUSSION

After the 3.0g sample of the three-component mixture was dissolved in 25ml ether and
transferred into a separating funnel then a solution of HCl and water was also added into the
separating funnel, two layers were visible in the separating funnel. The upper was brown in
colour and the lower layer was colourless. The lower layer became light pink when extracted
from the separating funnel into a conical flask. Another 100ml water was added to remove
excess HCl that may be dissolved in the ether layer.

From the mixture that’s in the separating funnel a solution NaOH was added to separate the
acidic component (2- naphthol), there were two layers visible the upper layer was brown in
colour and the lower layer became light brown. Then the lower aqueous layer was extracted.

The remaining ether solution which contained only the neutral component (p- dichlorobenzene)
poured out from the separating funnel to a conical flask then enough anhydrous CaCl2 was
added to cover the bottom of the conical flask and the mixture was swirled for 15 minutes. After
the ether was decanted into a small beaker the anhydrous calcium chloride became light pink.
The beaker is placed in the hood to allow the ether to evaporate. After it completely evaporated
the residue was weighed and its melting point was between the range of 50-60 degrees Celsius.

After adding the sodium hydroxide to the combined acidic extracts to check the alkalinity of the
solution, the litmus paper became blue indicating that the solution was alkaline. The alkaline
solution (25ml) was extracted twice with portions of ether (25ml). After the extraction, the
solution was goldish then the anhydrous calcium chloride was added to cover the bottom of the
beaker and swirled occasionally for 15 minutes.
The ether was decanted into a small beaker and placed into a hood to allow the ether to
evaporate having a melting point with a range of 40-50 degrees Celsius. The alkaline extract
was neutralized by adding concentrated HCl drop by drop then the solution became milky after
adding 24.8ml of concentrated HCl. When the litmus paper was inserted the colour became pink
while at first the litmus paper was blue. The milky product was cooled in ice then filtered off
under vacuum. The filtered product became clear and its mass was greater than 110.

CONCLUSION

The purpose of this experiment was to separate a sample of p-toluidine, 2- naphthol,

and p-dichlorobenzene of unknown proportions. The data supports that the separation
of all three compounds was successful. The melting point ranges and colours of the
products correspond to the physical properties of p-toluidine, 2-naphthol, and p-
dichlorobenzene.

ANSWERS
1. Advantages

(a) Ether is a good solvent for many organic compound

(b) It is immiscibility with water offers a fine separation if extracting from a water
solution.
(c) (c) Its low BP and it makes it easy to remove from the product.

Disadvantages

(a) Ether is very flammable

 (b) Under certain conditions it can oxidize into an explosive.

(c) It is anaesthetic

1. Kd= concentration of ether layer ÷concentration of ether in water

= (0.6g/100ml) ÷ (0.12g/100ml)
=5
Kd = 5= X/100ml ÷ (0.6- X)/100ml
5(0.6-X) =X
X= 0.5g

Kd = 5= X/50ml ÷ (0.6- X)/100ml

5(0.6-X) = 2X
X = 0.43g

Total extracted= 0.5g +0.43g = 0.93g

%A =0.4g/ 0.93 ×100
= 46.24 %

References

https://pressbooks.bccampus.ca/chem1114langaracollege/chapter/1-3-laboratory-
techniques-for-separation-of-mixtures/

https://chem.libretexts.org/Ancillary_Materials/Demos_Techniques_and_Experiments/
General_Lab_Techniques/Acid-Base_Extraction
https://pressbooks.bccampus.ca/chem1114langaracollege/chapter/1-3-laboratory-
techniques-for-separation-of-mixtures/