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Dr.S.Alexandar,M.Pharm,Ph.D,
Associate Professor
Vinayaka Missions College of Pharmacy,
Yercaud main road,
Kondappanaickanpatty,
Salem, Tamilnadu,
Pin:636008
Non aqueous titrationNon aqueous titration
Titration in water solutions is limited by factors:
 It is impossible to titrate for a mix of acids or the bases
 It is impossible to titrate for a mix of strong and weak
acids (bases)
 It is impossible to titrate separately for a mix of acids
(bases) with near constants of dissociation
 It is impossible to define substances which are insoluble
in water.
Non-aqueous titrations have the following
advantages
 Organic acids and bases that are insoluble in water are soluble in non-
aqueous solvent.
 A non-aqueous solvent may help two are more acids in mixture. The
individual acid can give separate end point in different solvent.
 Enlargement of solubility range: many substances that are not soluble
in water can be easily titrated in water-free media (e.g. fats and oils)
 Enlargement of application range: weak bases and acids can be easily
titrated
 Substance compositions that cannot be separately determined in
aqueous media can often be titrated in non-aqueous media
 Non-aqueous solvents are useful for the titration of very weak acids or
bases that cannot be titrated in water
 Non aqueous titrations are simple and accurate, examples of non
aqueous titration are :
 Ephedrine preparations, codeine phosphate in APC, tetracycline,
teramycin, Anti- histamines and various piprazine preparations.
• Solvent which are used in non aqueous titration are called
non aqueous solvent.
• They are following types:-
1. Aprotic Solvent
2. Protogenic Solvent
3. Protophillic Solvent
4. Amphiprotic Solvent
• Aprotic solvent are most important solvent in this titration. This solvent are
chemically inert and they work as a catalyst. Like this solvent are increase
the rate of speed in reaction and also decrease the rate of speed in reaction
during the chemical process or reaction it will depend on condition.
• Neither acidic nor basic (inert solvent),
The most important examples of aprotic solvent are
• Chloroform
• Benzene
 Protogenic solvent are acidic in nature. And they
can donate the proton, and they enhance the
strength of weak bases.
Examples of Protogenic solvent are
 HCL
 H2so4
 Protophillic solvent are basic in nature. Which
possess a high affinity for proton.
Examples:-Liquid ammonia, amines and ketone.
 Amphiprotic solvent are those solvent they work
as a both mean Protogenic or Protophillic. It
means Amphiprotic solvent are acidic and basic in
nature. And they are accept the proton and donate
the proton.
For examples:- Water, Alcohols and weak organic
acids
• Visual indicator are formed to the most suitable for the detection
of end point in non-aqueous titration.
• The important indicator used for non-aqueous titration are
follow:-
1. Crystal voilet:- It is used as 0.5% solution in glacial acetic
acid, it gives voilet colour in basic medium and yellowish
green in acidic medium.
• It is most widely use for the titration of pyridine with
prechloride acid.
2. Oracet Blue B Indicator:- It is prepared o.5% glacial acetic
acid. It gives blue colour in basic medium while pink
colour in acidic medium.
Acetic acid used for titration of weak bases,
Nitrogen containing compounds
Acetonitrile / with ACOH: Metal ethanoates
Alcohols (IPA, nBA) : Soaps and salts of organic
acids,
DMF: Benzoic acid, amides etc
 Perchloric acid in acetic acid
◦ Amines, amine salts, amino acids, salts of acids
 Potassium Methoxide in Toluene-Methanol
 Quan ammonium hydroxide in Acetonitrile-
pyridine
◦ Acids, enols, imides & sulphonamides
 Acidimetry in Non-aqueous Titrations—It can
be further sub-divided into two heads, namely :
(i) Titration of primary, secondary and tertiary amines,
and
(ii) Titration of halogen acid salts of bases.
 Alkalimetry in Non-aqueous Titrations—
titration of acidic substances
Example : Primary amines
METHODOLOGY: four steps
 (i) Preparation of 0.1 N Perchloric acid,
 (ii) Standardization of 0.1 N Perchloric Acid,
 (iii) Choice of Indicators, and
 (iv) Effect of Temperature on Assays
 Materials Required : 8.5 ml of perchloric acid (70.0 to 72.0%)
; 1 Litre of glacial acetic acid ; 30ml of acetic anhydride.
 Procedure : Gradually mix 8.5 ml of perchloric acid to 900 ml
of glacial acetic acid with vigorous and continuous stirring. Now
add 30 ml acetic anhydride and make up the volume to 1 litre
with glacialacetic acid and allow to stand for 24 hours before
use.
 The acetic anhydride reacts with the water (approx. 30%) in
perchloric acid and some traces in glacialacetic acid thereby
making the resulting mixture practically anhydrous. Thus, we
have :
H2O + (CH3CO)2O → 2CH3COOH
Acetic anhydride Acetic acid
 Weigh accurately about 0.5 g of potassium hydrogen
phthalate in a 100 ml conical flask.
 Add 25 ml of glacial acetic acid and attach a reflux
condenser fitted with a silica-gel drying tube. Warm until
the salt gets dissolved completely. Cool and titrate with
0.1 N perchloric acid by making use of either of
the following two indicators :
 (a) acetous crystal violet-2 drops, end point Blue to
Blue-Green (0.5% w/v)
 (b) acetous oracet blue B-2 drops, end point Blue to
Pink.
S.No. Name of Indicator Colorchange
Basic
Observed
Neutral
Acidic
1
2
3
4
Crystal violet (0.5% w/v
in glacial acetic acid)
Oracet Blue B(0.5% in
glacial acetic acid)
α-Naphtholbenzein
(0.2% in glacial acetic
acid
Quinalidine Red
(0.1% in methanol
Violet
Blue
Blue
Magenta
Bluish
green
Purple
Orange
—
Yellowish
green
Pink
Dark-
green
Almost
colourless
(a) Perchloric acid is usually available as a 70 to 72% mixture with
water .It usually undergoes a spontaneous explosive decomposition
and, therefore, it is available always in the form of a solution.
(b) Conversion of acetic anhydride to acetic acid requires 40-45
minutes for its completion. It being an exothermic reaction, the solution
must be allowed to cool to room temperature before adding glacial
acetic acid to volume,
(c) Avoid adding an excess of acetic anhydride especially when
primary and secondary amines are to be assayed, because these may
be converted rapidly to their corresponding acetylated non-basic
products :
R—NH2 + (CH3CO)2O → R.NH.(CH3CO) + CH3COOH
Primary amine Acetylated product
(d) Perchloric acid is not only a powerful oxidising agent but also a
strong acid. Hence, it must be handled very carefully.
S.No. Name of Substance Indicator Employed
1
2
3
4
5
Amantadine
hydrochloride
Chlorpromazine
hydrochloride
Clonidine hydrochloride
Cyproheptadiene.HCl
Ephedrinehydrochloride
Crystal violet
Methyl orange
α -Naphthol benzein
Crystal violet
-do-
Preparation of 0.1 N Potassium Methoxide in Toluene-Methanol
Materials Required: Absolute methanol : 40 ml ; dry toluene : 50 ml ; potassium
metal : 4 g.
Procedure: Add into a dry flask, a mixture of methanol (40 ml) and dry toluene
(50 ml) and cover it loosely. Carefully add freshly cut pieces of potassium
metal to the above mixture gradually with constant shaking. After complete
dissolution of potassium metal, add enough absolute methanol to yield a clear
solution. Toluene 50 ml is added with constant shaking until the mixture turns hazy
in appearance. The process is repeated by the alternate addition of methanol and
benzene until 1 litre of solution is obtained, taking care to add a minimum volume of
methanol to give a visible clear solution.
Preparation of 0.1 N Sodiun Methoxide
It is prepared exactly in a similar manner as for 0.1 N Potassium Methoxide, using 2.3 g of freshly-cut sodium in
place of potassium.
Preparation of 0.1 N Lithium Methoxide
It is prepared as for 0.1 N Potassium Methoxide, but using 0.7 g of lithium in place of potassium.
Standardization of 0.1 N Methoxide Solution
Materials Required: Dimethylformamide (DMF) : 10 ml ; Thymol blue (0.3% in MeOH) ; 0.1 N lithium
methoxide in toluene methanol ; benzoic acid : 0.6 g.
Procedure : Transfer 10 ml of DMF in a conical flask and add to it 3 to 4 drops of thymol blue and first
neutralize the acidic impurities present in DMF by titrating with 0.1 N lithium Methoxide in toluene-methanol.
Quickly introduce 0.06 g of benzoic acid and titrate immediately with Methoxide in toluene methanol.
Caution: Care must be taken to avoid contamination of neutralized liquid with atmospheric carbon
dioxide.
Na + CH3
OH → CH3
ONa + H ↑
Interaction between sodium metal and methanol is an exothermic reaction and hence, special care must be taken
while adding the metal into the dry solvent in small lots at intervals with adequate cooling so as to keep the
reaction well under control.
H2
O + CH3
ONa → CH3
OH + NaoH
H2
CO3
+ 2CH3
ONa → 2CH3
OH + Na2
CO3
Preparation of 0.1 N Tetrabutylammonium Hydroxide in Toluene-Methanol
Materials Required: Tetrabutylammonium iodide : 40 g ; absolute methanol : 90 ml ; silver oxide : 25
g ; dry toluene : 150 ml.
Procedure: Carefully dissolve 40 g of tetrabutylammonium iodide (Bu4NI) in 90 ml of absolute
methanol, add to it 20 g of finely powdered purified silver oxide and finally shake the mixture
thoroughly for 1 hour. Centrifuge about 2-3 ml of the resultant mixture and test for iodide in the
supernatant liquid. In case, it gives a positive test, add about 2 g more of silver oxide and shake for an
additional period of 30 minutes. The said method may be repeated until the supernatant liquid obtained
is completely free from iodide. The mixture thus obtained is filtered through a fine sintered glass filter
and finally rinse the container with 3 portions, each of 50 ml of dry toluene. These washings may be
added to the filtrate and the final volume is made up to 1 litre with dry toluene. The clear solution may
be flushed with CO2-free nitrogen for at least five minutes and duly protected from both CO2 and
moisture during storage.
2Bu4
NI + Ag2
O + H2
O → 2Bu4
NOH + 2AgI
Tetrabutyl- Tetrabutyl ammonium
ammonium bromide hydroxide
Standardization of 0.1 N Tetrabutylammonium Hydroxide
Materials Required : Benzoic acid : 60 mg ; dimethylbromide : 10 ml ;
thymol blue solution (0.3% w/v in methanol) ; 0.1 N tetrabutylammonium
hydroxide.
Procedure: Accurately weigh about 60 mg of benzoic acid into 10 ml of
previously neutralized Dimethyl formamide to the blue colour of thymol blue
(3 drops) by titration against 0.1 N tetrabutylammonium hydroxide. Allow
the benzoic acid to dissolve gradually and completely and titrate with 0.1 N
tetrabutylammonium hydroxide.
0.01221 g C7H6O2 ≡ 1 ml of 0.1 N

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Non Aqueous Titration

  • 1. Dr.S.Alexandar,M.Pharm,Ph.D, Associate Professor Vinayaka Missions College of Pharmacy, Yercaud main road, Kondappanaickanpatty, Salem, Tamilnadu, Pin:636008 Non aqueous titrationNon aqueous titration
  • 2. Titration in water solutions is limited by factors:  It is impossible to titrate for a mix of acids or the bases  It is impossible to titrate for a mix of strong and weak acids (bases)  It is impossible to titrate separately for a mix of acids (bases) with near constants of dissociation  It is impossible to define substances which are insoluble in water.
  • 3. Non-aqueous titrations have the following advantages  Organic acids and bases that are insoluble in water are soluble in non- aqueous solvent.  A non-aqueous solvent may help two are more acids in mixture. The individual acid can give separate end point in different solvent.  Enlargement of solubility range: many substances that are not soluble in water can be easily titrated in water-free media (e.g. fats and oils)  Enlargement of application range: weak bases and acids can be easily titrated  Substance compositions that cannot be separately determined in aqueous media can often be titrated in non-aqueous media  Non-aqueous solvents are useful for the titration of very weak acids or bases that cannot be titrated in water  Non aqueous titrations are simple and accurate, examples of non aqueous titration are :  Ephedrine preparations, codeine phosphate in APC, tetracycline, teramycin, Anti- histamines and various piprazine preparations.
  • 4. • Solvent which are used in non aqueous titration are called non aqueous solvent. • They are following types:- 1. Aprotic Solvent 2. Protogenic Solvent 3. Protophillic Solvent 4. Amphiprotic Solvent
  • 5. • Aprotic solvent are most important solvent in this titration. This solvent are chemically inert and they work as a catalyst. Like this solvent are increase the rate of speed in reaction and also decrease the rate of speed in reaction during the chemical process or reaction it will depend on condition. • Neither acidic nor basic (inert solvent), The most important examples of aprotic solvent are • Chloroform • Benzene
  • 6.  Protogenic solvent are acidic in nature. And they can donate the proton, and they enhance the strength of weak bases. Examples of Protogenic solvent are  HCL  H2so4
  • 7.  Protophillic solvent are basic in nature. Which possess a high affinity for proton. Examples:-Liquid ammonia, amines and ketone.
  • 8.  Amphiprotic solvent are those solvent they work as a both mean Protogenic or Protophillic. It means Amphiprotic solvent are acidic and basic in nature. And they are accept the proton and donate the proton. For examples:- Water, Alcohols and weak organic acids
  • 9. • Visual indicator are formed to the most suitable for the detection of end point in non-aqueous titration. • The important indicator used for non-aqueous titration are follow:- 1. Crystal voilet:- It is used as 0.5% solution in glacial acetic acid, it gives voilet colour in basic medium and yellowish green in acidic medium. • It is most widely use for the titration of pyridine with prechloride acid. 2. Oracet Blue B Indicator:- It is prepared o.5% glacial acetic acid. It gives blue colour in basic medium while pink colour in acidic medium.
  • 10. Acetic acid used for titration of weak bases, Nitrogen containing compounds Acetonitrile / with ACOH: Metal ethanoates Alcohols (IPA, nBA) : Soaps and salts of organic acids, DMF: Benzoic acid, amides etc
  • 11.  Perchloric acid in acetic acid ◦ Amines, amine salts, amino acids, salts of acids  Potassium Methoxide in Toluene-Methanol  Quan ammonium hydroxide in Acetonitrile- pyridine ◦ Acids, enols, imides & sulphonamides
  • 12.  Acidimetry in Non-aqueous Titrations—It can be further sub-divided into two heads, namely : (i) Titration of primary, secondary and tertiary amines, and (ii) Titration of halogen acid salts of bases.  Alkalimetry in Non-aqueous Titrations— titration of acidic substances
  • 13. Example : Primary amines METHODOLOGY: four steps  (i) Preparation of 0.1 N Perchloric acid,  (ii) Standardization of 0.1 N Perchloric Acid,  (iii) Choice of Indicators, and  (iv) Effect of Temperature on Assays
  • 14.  Materials Required : 8.5 ml of perchloric acid (70.0 to 72.0%) ; 1 Litre of glacial acetic acid ; 30ml of acetic anhydride.  Procedure : Gradually mix 8.5 ml of perchloric acid to 900 ml of glacial acetic acid with vigorous and continuous stirring. Now add 30 ml acetic anhydride and make up the volume to 1 litre with glacialacetic acid and allow to stand for 24 hours before use.  The acetic anhydride reacts with the water (approx. 30%) in perchloric acid and some traces in glacialacetic acid thereby making the resulting mixture practically anhydrous. Thus, we have : H2O + (CH3CO)2O → 2CH3COOH Acetic anhydride Acetic acid
  • 15.  Weigh accurately about 0.5 g of potassium hydrogen phthalate in a 100 ml conical flask.  Add 25 ml of glacial acetic acid and attach a reflux condenser fitted with a silica-gel drying tube. Warm until the salt gets dissolved completely. Cool and titrate with 0.1 N perchloric acid by making use of either of the following two indicators :  (a) acetous crystal violet-2 drops, end point Blue to Blue-Green (0.5% w/v)  (b) acetous oracet blue B-2 drops, end point Blue to Pink.
  • 16. S.No. Name of Indicator Colorchange Basic Observed Neutral Acidic 1 2 3 4 Crystal violet (0.5% w/v in glacial acetic acid) Oracet Blue B(0.5% in glacial acetic acid) α-Naphtholbenzein (0.2% in glacial acetic acid Quinalidine Red (0.1% in methanol Violet Blue Blue Magenta Bluish green Purple Orange — Yellowish green Pink Dark- green Almost colourless
  • 17. (a) Perchloric acid is usually available as a 70 to 72% mixture with water .It usually undergoes a spontaneous explosive decomposition and, therefore, it is available always in the form of a solution. (b) Conversion of acetic anhydride to acetic acid requires 40-45 minutes for its completion. It being an exothermic reaction, the solution must be allowed to cool to room temperature before adding glacial acetic acid to volume, (c) Avoid adding an excess of acetic anhydride especially when primary and secondary amines are to be assayed, because these may be converted rapidly to their corresponding acetylated non-basic products : R—NH2 + (CH3CO)2O → R.NH.(CH3CO) + CH3COOH Primary amine Acetylated product (d) Perchloric acid is not only a powerful oxidising agent but also a strong acid. Hence, it must be handled very carefully.
  • 18. S.No. Name of Substance Indicator Employed 1 2 3 4 5 Amantadine hydrochloride Chlorpromazine hydrochloride Clonidine hydrochloride Cyproheptadiene.HCl Ephedrinehydrochloride Crystal violet Methyl orange α -Naphthol benzein Crystal violet -do-
  • 19. Preparation of 0.1 N Potassium Methoxide in Toluene-Methanol Materials Required: Absolute methanol : 40 ml ; dry toluene : 50 ml ; potassium metal : 4 g. Procedure: Add into a dry flask, a mixture of methanol (40 ml) and dry toluene (50 ml) and cover it loosely. Carefully add freshly cut pieces of potassium metal to the above mixture gradually with constant shaking. After complete dissolution of potassium metal, add enough absolute methanol to yield a clear solution. Toluene 50 ml is added with constant shaking until the mixture turns hazy in appearance. The process is repeated by the alternate addition of methanol and benzene until 1 litre of solution is obtained, taking care to add a minimum volume of methanol to give a visible clear solution.
  • 20. Preparation of 0.1 N Sodiun Methoxide It is prepared exactly in a similar manner as for 0.1 N Potassium Methoxide, using 2.3 g of freshly-cut sodium in place of potassium. Preparation of 0.1 N Lithium Methoxide It is prepared as for 0.1 N Potassium Methoxide, but using 0.7 g of lithium in place of potassium. Standardization of 0.1 N Methoxide Solution Materials Required: Dimethylformamide (DMF) : 10 ml ; Thymol blue (0.3% in MeOH) ; 0.1 N lithium methoxide in toluene methanol ; benzoic acid : 0.6 g. Procedure : Transfer 10 ml of DMF in a conical flask and add to it 3 to 4 drops of thymol blue and first neutralize the acidic impurities present in DMF by titrating with 0.1 N lithium Methoxide in toluene-methanol. Quickly introduce 0.06 g of benzoic acid and titrate immediately with Methoxide in toluene methanol. Caution: Care must be taken to avoid contamination of neutralized liquid with atmospheric carbon dioxide. Na + CH3 OH → CH3 ONa + H ↑ Interaction between sodium metal and methanol is an exothermic reaction and hence, special care must be taken while adding the metal into the dry solvent in small lots at intervals with adequate cooling so as to keep the reaction well under control. H2 O + CH3 ONa → CH3 OH + NaoH H2 CO3 + 2CH3 ONa → 2CH3 OH + Na2 CO3
  • 21. Preparation of 0.1 N Tetrabutylammonium Hydroxide in Toluene-Methanol Materials Required: Tetrabutylammonium iodide : 40 g ; absolute methanol : 90 ml ; silver oxide : 25 g ; dry toluene : 150 ml. Procedure: Carefully dissolve 40 g of tetrabutylammonium iodide (Bu4NI) in 90 ml of absolute methanol, add to it 20 g of finely powdered purified silver oxide and finally shake the mixture thoroughly for 1 hour. Centrifuge about 2-3 ml of the resultant mixture and test for iodide in the supernatant liquid. In case, it gives a positive test, add about 2 g more of silver oxide and shake for an additional period of 30 minutes. The said method may be repeated until the supernatant liquid obtained is completely free from iodide. The mixture thus obtained is filtered through a fine sintered glass filter and finally rinse the container with 3 portions, each of 50 ml of dry toluene. These washings may be added to the filtrate and the final volume is made up to 1 litre with dry toluene. The clear solution may be flushed with CO2-free nitrogen for at least five minutes and duly protected from both CO2 and moisture during storage. 2Bu4 NI + Ag2 O + H2 O → 2Bu4 NOH + 2AgI Tetrabutyl- Tetrabutyl ammonium ammonium bromide hydroxide
  • 22. Standardization of 0.1 N Tetrabutylammonium Hydroxide Materials Required : Benzoic acid : 60 mg ; dimethylbromide : 10 ml ; thymol blue solution (0.3% w/v in methanol) ; 0.1 N tetrabutylammonium hydroxide. Procedure: Accurately weigh about 60 mg of benzoic acid into 10 ml of previously neutralized Dimethyl formamide to the blue colour of thymol blue (3 drops) by titration against 0.1 N tetrabutylammonium hydroxide. Allow the benzoic acid to dissolve gradually and completely and titrate with 0.1 N tetrabutylammonium hydroxide. 0.01221 g C7H6O2 ≡ 1 ml of 0.1 N