Showing posts with label Solvent Extraction. Show all posts
Showing posts with label Solvent Extraction. Show all posts

The method was discovered by Craig and Post. It is consists of 300-400 such chambers. The organic solvent and the aqueous solution is introduced to tube A and then it passes to B. It is shaken and is allowed to attain the equilibrium. Now, the apparatus is tilted so that the upper layer gets decanted through C and is collected in D. When the apparatus is again made vertical. The liquid passes through D into E in the next chamber of A and then to B. The process is repeated till the two liquids gets almost separated.

Application:

1. With the help of this method we can have accurate quantitative analysis of a single as well as the mixture of the components.

2. In this case apparatus required are very simple (separating funnel burette pipets conical flask etc.)

3. Time required for analysis is very small.

4. The method is very well used for detection of traces quantity of substance where precipitation method (Gravimetry) is not possible.

5. Fe+3 ferric ion can be easily extracted by ether from 6 molar HCl solution of the ferrous ally and iron ore.

6. The extraction can also be use in the extraction of metal as metal chelate where later has high solubility in an immiscible solvent such as chloroform and benzene.

7. In industrial and commercial field extraction by counter current extraction is frequently applied in the separation of components where the difference in the distribution coefficient are small.

8. The phenomenon is widely applied in drug analysis.

9. The solvent extraction is used in clinical laboratory.

10. Metal chelates are more soluble in non-polar solvents. Thus Ni(II) in its tetra co-ordinate complex with dimethyl glyoxime can be extracted into chloroform. In presence of citrate or tartrate the precipitation of Fe(III) and Cr(III) can be avoided.

<

Explain the Counter Current Extraction?

The method was discovered by Craig and Post. It is consists of 300-400 such chambers. The organic solvent and the aqueous solution is introduced to tube A and then it passes to B. It is shaken and is allowed to attain the equilibrium. Now, the apparatus is tilted so that the upper layer gets decanted through C and is collected in D. When the apparatus is again made vertical. The liquid passes through D into E in the next chamber of A and then to B. The process is repeated till the two liquids gets almost separated.

Application:

1. With the help of this method we can have accurate quantitative analysis of a single as well as the mixture of the components.

2. In this case apparatus required are very simple (separating funnel burette pipets conical flask etc.)

3. Time required for analysis is very small.

4. The method is very well used for detection of traces quantity of substance where precipitation method (Gravimetry) is not possible.

5. Fe+3 ferric ion can be easily extracted by ether from 6 molar HCl solution of the ferrous ally and iron ore.

6. The extraction can also be use in the extraction of metal as metal chelate where later has high solubility in an immiscible solvent such as chloroform and benzene.

7. In industrial and commercial field extraction by counter current extraction is frequently applied in the separation of components where the difference in the distribution coefficient are small.

8. The phenomenon is widely applied in drug analysis.

9. The solvent extraction is used in clinical laboratory.

10. Metal chelates are more soluble in non-polar solvents. Thus Ni(II) in its tetra co-ordinate complex with dimethyl glyoxime can be extracted into chloroform. In presence of citrate or tartrate the precipitation of Fe(III) and Cr(III) can be avoided.

<

Though the multiple extraction is more beneficial than single step extraction. For analytical chemist it is easy to find out the amount extracted in single extraction, so he follow single extraction rather than multiple extraction because it is tedious. The relation between percentage extraction (E) for single extraction can be derived as follow: We know $$ { W }_{ 1 } = \left[ \frac { { V }_{ W } }{ { V }_{ o }D + { V }_{ W } } \right] \times a \qquad ...(1) $$ where \({ W }_{ 1 }\) is the weight of solute remaining after 1st extraction.
\( { V }_{ W } \)= Volume of Aqueous Phase
\( { V }_{ o } \) = Volume of Organic Phase
\(D\) = Distribution Ratio
\(a\) = Total weight of Solute present initially.

The amount extracted will be a $$ { W }_{ 1 } = a - a\left( \frac { { V }_{ W } }{ { V }_{ o }D + { V }_{ W } } \right) \qquad ...(2) $$ $$ = a - a\left( \frac { { V }_{ W } }{ { V }_{ o }D + { V }_{ W } } \right) $$ $$ \therefore Percentage \ extraction \ (E) = \left( \frac { a - { W }_{ 1 } }{ a } \right) \times 100 $$ Lets Substitute the values from equation (1) $$ E = \left( \frac { a - a\left( \frac { { V }_{ W } }{ { V }_{ o }D + { V }_{ W } } \right) }{ a } \right) \times 100 $$ $$ E = \left( 1 - \left( \frac { { V }_{ W } }{ { V }_{ o }D + { V }_{ W } } \right) \right) \times 100 $$ $$ E = \left( \frac { { V }_{ o }D + { V }_{ W } - { V }_{ W } }{ { V }_{ o }D + { V }_{ W } } \right) \times 100 $$ $$E = \left( \frac { { V }_{ o }D }{ { V }_{ o }D + { V }_{ W } } \right) \times 100 $$ on dividing the numerator and denominator of RHS by \({ V }_{ o }\) we get $$ E = \left( \frac { D }{ D + \frac { { V }_{ W } }{ { V }_{ o } } } \right) \times 100 $$ $$ \therefore Percentage extraction (E) = \frac { 100D }{ D + \frac { { V }_{ W } }{ { V }_{ o } } } $$ Thus % extraction (E) depends on D as well as \(\frac { { V }_{ W } }{ { V }_{ o } } \).


Derive an expression for percentage extraction?

Though the multiple extraction is more beneficial than single step extraction. For analytical chemist it is easy to find out the amount extracted in single extraction, so he follow single extraction rather than multiple extraction because it is tedious. The relation between percentage extraction (E) for single extraction can be derived as follow: We know $$ { W }_{ 1 } = \left[ \frac { { V }_{ W } }{ { V }_{ o }D + { V }_{ W } } \right] \times a \qquad ...(1) $$ where \({ W }_{ 1 }\) is the weight of solute remaining after 1st extraction.
\( { V }_{ W } \)= Volume of Aqueous Phase
\( { V }_{ o } \) = Volume of Organic Phase
\(D\) = Distribution Ratio
\(a\) = Total weight of Solute present initially.

The amount extracted will be a $$ { W }_{ 1 } = a - a\left( \frac { { V }_{ W } }{ { V }_{ o }D + { V }_{ W } } \right) \qquad ...(2) $$ $$ = a - a\left( \frac { { V }_{ W } }{ { V }_{ o }D + { V }_{ W } } \right) $$ $$ \therefore Percentage \ extraction \ (E) = \left( \frac { a - { W }_{ 1 } }{ a } \right) \times 100 $$ Lets Substitute the values from equation (1) $$ E = \left( \frac { a - a\left( \frac { { V }_{ W } }{ { V }_{ o }D + { V }_{ W } } \right) }{ a } \right) \times 100 $$ $$ E = \left( 1 - \left( \frac { { V }_{ W } }{ { V }_{ o }D + { V }_{ W } } \right) \right) \times 100 $$ $$ E = \left( \frac { { V }_{ o }D + { V }_{ W } - { V }_{ W } }{ { V }_{ o }D + { V }_{ W } } \right) \times 100 $$ $$E = \left( \frac { { V }_{ o }D }{ { V }_{ o }D + { V }_{ W } } \right) \times 100 $$ on dividing the numerator and denominator of RHS by \({ V }_{ o }\) we get $$ E = \left( \frac { D }{ D + \frac { { V }_{ W } }{ { V }_{ o } } } \right) \times 100 $$ $$ \therefore Percentage extraction (E) = \frac { 100D }{ D + \frac { { V }_{ W } }{ { V }_{ o } } } $$ Thus % extraction (E) depends on D as well as \(\frac { { V }_{ W } }{ { V }_{ o } } \).


If a solution contains two or more solutes say A and B, it is observed that when A is extracted, some amount of B is also extracted. The extent of the seperation can be expressed in terms of one factor called Seperation Factor \(\beta\) . This is related to the distribution ratio of A and B. $$ \boxed { \beta = \frac { D_{ A } }{ { D }_{ B } } = \frac { { { C }_{ o(A) } }/{ { C }_{ a(A) } } }{ { { C }_{ o(B) } }/{ { C }_{ a(B) } } } } $$ It is ratio therefore no unit and no dimension.

The larger value is always placed in the numerator. \beta must be made as large as possible by choice of extractant and by adjusting the volume ratio.

When \(D_{ A }\) = 10 and \(D_{ B } \)= 0.1. The \(\beta = \frac { 10 }{ 0.1 } = 100%\)

single extraction in case will remove 91% of A and 9% of B. It can be obtained for A, $$ E = \left[ \frac { 100{ D }_{ A } }{ { D }_{ A } + { { V }_{ W } }/{ { V }_{ o } } } \right] $$ for $${ V }_{ W } = { V }_{ o }\qquad \qquad \therefore { { V }_{ W } }/{ { V }_{ o } } = 1 $$ $$ \therefore E = \left[ \frac { 100 \times 10 }{ 10 + 1 } \right] = \left[ \frac { 1000 }{ 11 } \right] = 90.9% $$ $$ Similarly \ for \ B, \ E = \left[ \frac { 100{ D }_{ B } }{ { D }_{ B } + { { V }_{ W } }/{ { V }_{ o } } } \right] $$ $$ for \ { V }_{ W } = { V }_{ o }\qquad \qquad \therefore { { V }_{ W } }/{ { V }_{ o } } = 1 $$ $$ \therefore E = \left[ \frac { 100 \times 0.1 }{ 0.1 + 1 } \right] = \left[ \frac { 10 }{ 1.1 } \right] = 9.1% $$ The seperation of A is almost complete from B if the seperation factor B is high. It can be only in the case when \({ D }_{ A }\) is large and \({ D }_{ B }\) is small. For a given value of \({ D }_{ A }\) and \({ D }_{ B }\), the seperation effect can be increased by adjusting the volume ratio given by Nush Densen Equation which says. $$ \boxed { \frac { { V }_{ o } }{ { V }_{ W } } = \frac { 1 }{ { \left( { D }_{ A }{ D }_{ B } \right) }^{ { 1 }/{ 2 } } } } $$


Explain the separation factor?

If a solution contains two or more solutes say A and B, it is observed that when A is extracted, some amount of B is also extracted. The extent of the seperation can be expressed in terms of one factor called Seperation Factor \(\beta\) . This is related to the distribution ratio of A and B. $$ \boxed { \beta = \frac { D_{ A } }{ { D }_{ B } } = \frac { { { C }_{ o(A) } }/{ { C }_{ a(A) } } }{ { { C }_{ o(B) } }/{ { C }_{ a(B) } } } } $$ It is ratio therefore no unit and no dimension.

The larger value is always placed in the numerator. \beta must be made as large as possible by choice of extractant and by adjusting the volume ratio.

When \(D_{ A }\) = 10 and \(D_{ B } \)= 0.1. The \(\beta = \frac { 10 }{ 0.1 } = 100%\)

single extraction in case will remove 91% of A and 9% of B. It can be obtained for A, $$ E = \left[ \frac { 100{ D }_{ A } }{ { D }_{ A } + { { V }_{ W } }/{ { V }_{ o } } } \right] $$ for $${ V }_{ W } = { V }_{ o }\qquad \qquad \therefore { { V }_{ W } }/{ { V }_{ o } } = 1 $$ $$ \therefore E = \left[ \frac { 100 \times 10 }{ 10 + 1 } \right] = \left[ \frac { 1000 }{ 11 } \right] = 90.9% $$ $$ Similarly \ for \ B, \ E = \left[ \frac { 100{ D }_{ B } }{ { D }_{ B } + { { V }_{ W } }/{ { V }_{ o } } } \right] $$ $$ for \ { V }_{ W } = { V }_{ o }\qquad \qquad \therefore { { V }_{ W } }/{ { V }_{ o } } = 1 $$ $$ \therefore E = \left[ \frac { 100 \times 0.1 }{ 0.1 + 1 } \right] = \left[ \frac { 10 }{ 1.1 } \right] = 9.1% $$ The seperation of A is almost complete from B if the seperation factor B is high. It can be only in the case when \({ D }_{ A }\) is large and \({ D }_{ B }\) is small. For a given value of \({ D }_{ A }\) and \({ D }_{ B }\), the seperation effect can be increased by adjusting the volume ratio given by Nush Densen Equation which says. $$ \boxed { \frac { { V }_{ o } }{ { V }_{ W } } = \frac { 1 }{ { \left( { D }_{ A }{ D }_{ B } \right) }^{ { 1 }/{ 2 } } } } $$


In choosing a proper solvent for solvent extractions, the following factors must be taken into consideration.

1. The solvent selected should be such that, the solubility of the solute to be extracted is more. This means seperation factor (B) must be large.

2. The two phases used must be totally immiscible.

3. The solvent must not react chemically with the solute present in aqueous solution.

4. The solvent must be recoverable without much expenditure.

5. The density of the solvent must be different than aqueous phase it will help in quick settling of the two phases.

6. The solvent should not be toxic.

7. The solvent should be cheap.

8. The solvent should possess low inflammability.

9. The solvent should have low viscosity, low vapour pressure and low freezing point.

10. The solvent should be readily available.


Choice of solvent is very important in solvent extraction process, Explain.

In choosing a proper solvent for solvent extractions, the following factors must be taken into consideration.

1. The solvent selected should be such that, the solubility of the solute to be extracted is more. This means seperation factor (B) must be large.

2. The two phases used must be totally immiscible.

3. The solvent must not react chemically with the solute present in aqueous solution.

4. The solvent must be recoverable without much expenditure.

5. The density of the solvent must be different than aqueous phase it will help in quick settling of the two phases.

6. The solvent should not be toxic.

7. The solvent should be cheap.

8. The solvent should possess low inflammability.

9. The solvent should have low viscosity, low vapour pressure and low freezing point.

10. The solvent should be readily available.


In general, organic solute (covalent solute) are more soluble in non polar (organic) solvents than water and hydrated salts are more soluble in water (polar) solvent. The inorganic salts in the solution are in the form of ions. In solvent extraction, we must see that solubility of inorganic salts in water should be less and solubility in organic solvent must be increased. The solubility of the metal ions in water is due to the association of water molecules with charged metal ions. in other words due to the hydration. Therefore, if the charged on the metal ions is neutralised, the solubility of the metal ions in the watt will be decreased. The charge on the metal ion is neutralised by reaction of metal ions with the appropriate complexing agent to form the metal-chellate complex. The bulkier the complex and if it is more hydrophobic in nature better will be extraction. .. Each ion will have to be treated differently. Thus, aluminium ions in the solution are usually converted into hydroxy aluminium quinolate by the addition of 8-hydroxy quinolene. The chellate thus formed can be extracted by using benzene or chloroform. It is possible to extract aluminium at pH 5:18, 3 in the presence of iron Nickel and Vanadium. The other complexing agents are dimethyl - glyoxime, acetyl acetone cupferron, \(\alpha\) - nitroso \(\beta\) - naphthol dithizone etc.


Explain the Role of complexing Agent in Solvent Extraction?

In general, organic solute (covalent solute) are more soluble in non polar (organic) solvents than water and hydrated salts are more soluble in water (polar) solvent. The inorganic salts in the solution are in the form of ions. In solvent extraction, we must see that solubility of inorganic salts in water should be less and solubility in organic solvent must be increased. The solubility of the metal ions in water is due to the association of water molecules with charged metal ions. in other words due to the hydration. Therefore, if the charged on the metal ions is neutralised, the solubility of the metal ions in the watt will be decreased. The charge on the metal ion is neutralised by reaction of metal ions with the appropriate complexing agent to form the metal-chellate complex. The bulkier the complex and if it is more hydrophobic in nature better will be extraction. .. Each ion will have to be treated differently. Thus, aluminium ions in the solution are usually converted into hydroxy aluminium quinolate by the addition of 8-hydroxy quinolene. The chellate thus formed can be extracted by using benzene or chloroform. It is possible to extract aluminium at pH 5:18, 3 in the presence of iron Nickel and Vanadium. The other complexing agents are dimethyl - glyoxime, acetyl acetone cupferron, \(\alpha\) - nitroso \(\beta\) - naphthol dithizone etc.


It is the simplest and most widely used method. The method is to be applied when the distribution D is high.

Requirement: Simple glass separating flask beaker, funnel etc.

Experiment: In this technique the aqueous phase containing the solute to be extracted is brought in contact with the immiscible organic solvent in a simple separating funnel. The two phases are shaken vigorously at least for 10-15 minutes. Then are allowed to attain the equilibrium. After the layers become clear, the denser liquid is withdrawn by opening the stop cock of the funnel. Once the denser liquid is separated, then lighter layer is separated.


Describe the batch extraction in the solvent extraction method?

It is the simplest and most widely used method. The method is to be applied when the distribution D is high.

Requirement: Simple glass separating flask beaker, funnel etc.

Experiment: In this technique the aqueous phase containing the solute to be extracted is brought in contact with the immiscible organic solvent in a simple separating funnel. The two phases are shaken vigorously at least for 10-15 minutes. Then are allowed to attain the equilibrium. After the layers become clear, the denser liquid is withdrawn by opening the stop cock of the funnel. Once the denser liquid is separated, then lighter layer is separated.


When the distribution is small, we have to carry out the multiple extractions. But multiple extraction brings no. of the complications and is very tedious. Kutcher and Steudel devised a continuous extractions to avoid the multiple extractions.

1. When the extracting solvent is heavier than water (aqueous). It is consist of tube and reservoir. The reservoir contain the same organic solvent. The tube is fitted with the condenser. The solvent in reservoir is heated slowly which is converted into vapours, Which move up and are condensed and the organic solvent is converted into liquid which is heavy and descend while moving through aqueous, the solute gets transferred from aqueous to organic and at the bottom we get solution of solute in organic. so the level increases and corresponding solution will fall in reservoir. This continue till maximum amount of solute is transferred from aqueous to organic. Then by opening the stopper at the bottom, we can separate organic and aqueous layer, then solute can be extracted from organic.

2. When organic solvent is lighter than aqueous. In that case reservoir contain organic, which on warming is converted into to the vapours, which ascends and is condensed in condenser which descends through bubbler type of funnel. This liquids goes to bottom but as it is light so it ascends, and passes through solution and here the solute gets transferred from aqueous solution. So the level of of the solution increases and the corresponding gets transferred to reservoir.


How is continuous extraction carried out.

When the distribution is small, we have to carry out the multiple extractions. But multiple extraction brings no. of the complications and is very tedious. Kutcher and Steudel devised a continuous extractions to avoid the multiple extractions.

1. When the extracting solvent is heavier than water (aqueous). It is consist of tube and reservoir. The reservoir contain the same organic solvent. The tube is fitted with the condenser. The solvent in reservoir is heated slowly which is converted into vapours, Which move up and are condensed and the organic solvent is converted into liquid which is heavy and descend while moving through aqueous, the solute gets transferred from aqueous to organic and at the bottom we get solution of solute in organic. so the level increases and corresponding solution will fall in reservoir. This continue till maximum amount of solute is transferred from aqueous to organic. Then by opening the stopper at the bottom, we can separate organic and aqueous layer, then solute can be extracted from organic.

2. When organic solvent is lighter than aqueous. In that case reservoir contain organic, which on warming is converted into to the vapours, which ascends and is condensed in condenser which descends through bubbler type of funnel. This liquids goes to bottom but as it is light so it ascends, and passes through solution and here the solute gets transferred from aqueous solution. So the level of of the solution increases and the corresponding gets transferred to reservoir.