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Module 3-Acidimetry Method of Analysis

The document covers titrimetric analysis focusing on neutralization reactions, detailing objectives such as understanding acidimetric titration and calculating the purity of acidic drugs. It includes methods for direct and residual titration, examples of drugs analyzed, and formulas for calculating the percentage of analytes. Additionally, it provides practice problems and references for further study in pharmaceutical analysis.

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Bryan Yu
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26 views

Module 3-Acidimetry Method of Analysis

The document covers titrimetric analysis focusing on neutralization reactions, detailing objectives such as understanding acidimetric titration and calculating the purity of acidic drugs. It includes methods for direct and residual titration, examples of drugs analyzed, and formulas for calculating the percentage of analytes. Additionally, it provides practice problems and references for further study in pharmaceutical analysis.

Uploaded by

Bryan Yu
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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TITRIMETRIC ANALYSIS -

NEUTRALIZATION REACTIONS
OBJECTIVES

 Understand acidimetric direct and residual


titration.
 Givedifferent drugs that are assayed by
acidimetric titration.
 Compute for the percentage amount/purity
of acidic drugs
NEUTRALIZATION REACTIONS

ACID SALT+
BASE
Water
COMPUTING FOR THE EQUIVALENT VOLUME OF
LIQUID SOLUTIONS IN PREPARING NORMAL AND
MOLAR SOLUTIONS

Prepare 1000 mL of 1N HCl and 1 N H2SO4. How


many mL of HCl and H2SO4 is needed? The
concentrations of available HCl and H2SO4 are
36% and 95% respectively and the sp. gravity of
HCl is 1.18 and H2SO4 is 1.83.

Weight of HCl = V x N x meq


Volume of HCl = weight/ sp.g x %conc
SOLUTIONS
SOLUTIONS
Acidimetric Analysis
ACIDIMETRIC TITRATION

 Analyte - Basic substance


Examples: NaOH, Na2CO3, NaHCO3
 Standard solution – Acid solutions
Examples: HCl, H2SO4
 Indicators – pH indicators
Example: Phenolpthalein
ACIDIMETRIC ANALYSIS

Direct titration = standard solution of


acid + base solution

Residual Titration = standard solution


of acid + base solution + excess
standard solution of acid + standard
solution of base
INDICATORS
Indicators pH range Acid (color Base (color
change) change)
Malachite green 0.0-2.0 Yellow Green
Bromophenol blue 3.0-4.6 Yellow Blue
Bromocresol 5.2-6.8 Yellow Purple
purple
Bromothymol blue 6.0-7.6 Yellow Blue
Phenol red 6.8-8.2 Yellow Red
Cresol red 7.2-8.8 Yellow Red
Thymol blue 8.0-9.2 Yellow Blue
Bromocresol green 4.0-6.4 Yellow Blue
Methtyl yellow 2.8-4.0 Red Yellow
Methyl orange 3.2-4.4 Pink Yellow
Methyl red 4.2-6.2 Red Yellow
Thymopthalein 9.3-10.5 Colorless Blue
Phenolpthalein 8.0-10 Colorless Red
GENRAL FORMULA FOR VOLUMETRIC ANLAYSIS

% amount of analyte = Volume x Normality x meq x 100


weight of analyte
EXAMPLE OF ACIDIMETRIC DIRECT
TITRATION METHOD

 50 ml sample of calcium hydroxide solution


required 19.50 mL of 0.1050N hydrochloric
acid solution to neutralize it. Calculate the
amount of calcium hydroxide in the solution?
What is the % amount of calcium hydroxide?
SOLUTION:
EXAMPLE OF ACIDIMETRIC DIRECT
TITRATION METHOD (PAGE 86)
Assay of Sodium Bicarbonate
Analyte = 3 g of NaHCO3
Titrant = 21mL of 1N H2SO4
Indicator = Methyl orange

Chemical Reaction:
2NaHCO3 + H2SO4 = Na2SO4 + 2H2O + 2CO2

Formula: % of NaHCO3 = ml x N x mEq x 100


wt of sample
ASSAY OF SODIUM SALICYLATE
TABLETS
Twenty sodium salicylate tablets labeled 325
mg were dissolved in 200mL. A 15 mL aliquot
of the filtrate was titrated with a bromophenol
blue end point in the usual way by 29.11 mL
of 0.1N hydrochloric acid. Calculate the
percentage labeled amount. Each ml of 0.1N
HCl is equivalent to 16.01mg of C7H5NaO3
ASSAY OF SODIUM SALICYLATE
TABLETS
Analyte = 20 sodium salicylate tablets in 200ml
Volume of titrant = 29.11mL
N of Titrant = 0.1N HCl
Indicator = Bromophenol blue
Titer = 16.01mg
SOLUTION:

Formulas:
Amt/tab = V x N x meq x Ave. wt
wt of sample

% Labelled amt = Amt/tab x 100


labelled amt
SOLUTION:
Other pharmaceutical products assayed by
Acidimetry -DTM
 Aminophylline
 Caffeine
 Diethylamine
 Ammonia spirit
 Ca(OH)2
 Sodium borate
 Potassium hydroxide
 Pyrazinamide
 Ammonium chloride
 Sodium salicylate
Acidimetric Analysis

Residual titration
Reasons for Residual Titration
 Reaction proceeds slowly
 The substance being assayed does
not give a distinct, sharp end point
with an indicator using direct titration.
Theory involved in Residual titration

Titrant
Analyte Is another
Is dissolved in standard
accurately solution, that End Point
measured will neutralize Reaction is
standard solution the excess of Completed
+ excess of this the 1st
standard soln. standard
solution used
FORMULA:

% = (Va x Na) – (Vb x Nb) (Meq) x 100


sample weight
SUBSTANCES ASSAYED BY RESIDUAL
ACIDIMETRY (USP)
 Alumina and magnesia tablets
 Calamine

 Dimenhydrinate syrup

 Lidocaine

 Milk of magnesia

 Magnesium hydroxide

 Magnesium trisilicate

 Ringers injection

 Zinc oxide
Examples of Products analyzed
using Acidimetry by residual
titration
ASSAY OF ZINC OXIDE

Materials Required: 1.5 g ZnO, 1N H2SO4, 1N


NaOH, methyl orange

Procedure: Dissolve 1.5g of Zinc oxide in 50mL


1N sulfuric acid, add methyl orange and titrate
the excess sulfuric acid with 1N NaOH.
Each mL of 1N sulfuric acid is equivalent to
40.69mg of ZnO. Compute for the % amount of
ZnO.
ASSAY OF ZINC OXIDE

Analyte = 1.5 g ZnO


Titrants = 50 ml of 1N H2SO4
= 15mL of 1N NaOH
Indicator = Methyl orange
Titer =40.69mg of ZnO
Chemical Reaction:
ZnO + H2SO4 = ZnSO4 + H2O
H2SO4 + 2NaOH = Na2SO4 +2H2O
Formula:
% = [(Va x Na) – (Vb x Nb) ](Meq) x100
sample weight
ASSAY OF MILK OF MAGNESIA

Analyte = 5.2430 g Milk of Magnesia


Titrants = 25 ml of 0.9915N H2SO4 and 9.85mL of 1.1402N
NaOH
Indicator = Methyl orange
USP req. = not less than 7 and not more than 8.5% of Mg(OH)2

Chemical Reaction:
Mg(OH)2 + H2SO4 = MgSO4 + 2H2O
H2SO4 + 2NaOH = Na2SO4 +2H2O
Formula:
% = (Va x Na) – (Vb x Nb) (Meq) x100
1. sample weight
SOLUTION:
PRACTICE PROBLEMS (PAGE 75 OF JENKINS)

 If 25mL of a HCl acid solution were required in


titration of a 0.65g sample of sodium
carbonate, what weight of the following pure
reagents would be required to neutralize 25 mL
of HCl solution?
a. NaHCO3
b. KOH
c. Ba(OH)2
d. CaO
PRACTICE PROBLEMS (PAGE 75 OF JENKINS)

 If 25 mL of NaOH solution required 40mL of


sulfuric acid solution in a titration, and 25 mL
of the sulfuric acid solution were required in
the titration of 0.3060g of pure sodium
carbonate, what was the normality of the
sodium hydroxide solution?
PRACTICE PROBLEM #1 (P 91 OF JENKINS)
If 1.25g sample of ZnO, 95% were treated with 50mL of
1.123N sulfuric acid in the usual way, what volume of
0.9765N sodium hydroxide would be required in the back
titration.
PRACTICE PROBLEM # 2 (P 95 OF JENKINS)

Calculate the Mg(OH)2 content of milk of,


magnesia, 12.32 g of which was dissolved in
50mL of 1.0340N sulfuric acid, producing a
mixture that required 24.60 mL of 1.1255N
sodium hydroxide.
PRACTICE PROBLEM # 3 (P 96)

If 0.4340g sample of methenamine were treated


in the usual way with 25mL of 0.65N sulfuric acid
and 9.45 mL of 0.45N sodium hydroxide was
required in the back titration, what was the % of
C6H12N4 in the sample? Each mL of 1N sulfuric
acid is equivalent to 35.05mg of C6H12N4.
REFERENCES

 Jenkins Quantitative Pharmaceutical Chemistry


 REFERENCE DG GARRATT., “THE QUALITATIVE ANALYSIS OF DRUG”,
3rd EDITION . J.MENDHAM, R.C. DENNY, JD BARNES, MJK THOMAS.,
“VOLGEL’S TEXT BOOK OF QUANTITATIVE CHEMICAL ANALYSIS”, 6th
EDITION. G.DEVALA RAO., “A TEXT BOOK OF PHARMACEUTICAL
ANALYSIS VOL-I”. A.A.NAPOLEON., “A TEXT BOOK OF PHYSICAL
CHEMISTRY AND PHARMACEUTICAL ANALYSIS”. DR.S.RAVI SANKAR.,
“A TEXT BOOK OF PHARMACEUTICAL ANALYSIS”. DAVID G. WATSON.,
“A TEXT BOOK FOR PHARMACY STUDENTS AND PHARMACEUTICAL
CHEMISTRY”, 2nd EDITION. ASHUTOSH KAR., “PHARMACEUTICAL
DRUG ANALYSIS”, REVISED SECOND EDITION. INDIAN
PHARMACOPIEA - 1996

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