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Module 4-Alkalimetry Methods of Analysis

The document provides an overview of alkalimetric analysis, focusing on titration methods involving acids and bases, particularly using NaOH as a titrant. It outlines the objectives, theory, and formulas for calculating the percentage of various substances, including acetic acid and aspirin, using different alkalimetric methods. Additionally, it includes sample assays and practice problems to illustrate the application of these methods.

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Bryan Yu
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52 views22 pages

Module 4-Alkalimetry Methods of Analysis

The document provides an overview of alkalimetric analysis, focusing on titration methods involving acids and bases, particularly using NaOH as a titrant. It outlines the objectives, theory, and formulas for calculating the percentage of various substances, including acetic acid and aspirin, using different alkalimetric methods. Additionally, it includes sample assays and practice problems to illustrate the application of these methods.

Uploaded by

Bryan Yu
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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ALKALIMETRIC ANALYSIS

OBJECTIVES

 To understand alkalimetric titration


 To compute problems involving alkalimetric
assay
THEORY OF ALKALIMETRIC ANALYSIS

 Analyte = acid
 Titrant = base (usually 0.1N or 1N NaOH)

- The acid sample should be dissolved


approximately to equal amount of the titrant
- Titrant consume is normally around 30-40 ml
DTM ALKALIMETRIC METHOD

 Requires only one standard solution, one


standard base
Acid analyte + Standard solution base = salt + water

Formula:
V x N x meq
% = ______________________x 100
wt of sample
SUBSTANCES ASSAYED BY DTM ALKALIMETRIC METHOD
(JENKINS - 109-110)

 Acetic acid
 Benzaldehyde
 Benzoic acid
 Bisulfan
 Citric acid
 Furosemide
 Hydrochloric acid
 Methenamine
 Salicylic acid
 Tartaric acid
SAMPLE ASSAY

 Assay of HCl
Wt of sample = 3g
Volume of NaOH = 30ml
Normality of NaOH = 1N
% of HCl =?
SAMPLE ASSAY

 Assay of Tartaric acid


 Wt of C4H6O6 = 2g

 Volume of NaOH = 32ml

 Normality = 1N

 Indicator- Phenolphthalein

 Each mL of 1N NaOH is equivalent to 75.04mg


of C4H6O6
 What is the percentage amount of C4H6O6.?
RESIDUAL ALKALIMETRIC METHOD

 used for those compounds that react too slowly


with the titrant because of poor solubility, thus
heating process is usually employed.
 Also, precipitation method is employed to
change substances to react with standard
base. The esters, acid anhydrides, acid
chlorides and aldehydes use this method of
titration.
 Blank titration is done = no sample present
SUBSTANCES ASSAYED BY RTM ALKALIMETRIC METHOD (PAGE
112)

 Acetylcholine chloride
 Aluminum acetate

 Aspirin

 Benzyl benzoate

 Lactic acid

 Ethyl acetate
FORMULAS:
For Capsules/Tablets
(Vblank –Vsample) x N x meq
Content/tab = ______________________________ x Ave. Wt
wt of sample

% labeled amount = content/tab ______ x 100


labeled amount

For single sample


(Vblank –Vsample) x N x meq
% content = ______________________________ x 100
wt of sample
ASSAY OF ASPIRIN
Assay Procedure
1. Weigh 0.5g of aspirin powder and add 20mL neutralized alcohol to dissolved the
powder.
2. Mix thoroughly in an Erlenmeyer flask.
3. Add 3 drops of phenolphthalein TS as the indicator.
4. Titrate immediately with 0.1N sodium hydroxide until light pink color is achieved.
5. Then add to the titrated solution the 0.1N sodium hydroxide the same volume
used in the titration with additional 15ml more.
6. Heat the solution in a water bath for 15 minutes with frequent agitation.
7. Cool the solution quickly and immediately titrate it with 0.1N sulfuric acid.
8. Repeat the operation without the aspirin (20 ml of neutralized alcohol only), this
will serve as your blank determination. Use the same reagents and volume (the
same volume of 0.1N NaOH used in the sample) in the same manner. Titrate it
with the same manner with 0.1N sulfuric acid.
9. Compute for the % amount of aspirin

 Each ml of 0.1N sodium hydroxide is equivalent to 18.01mg of aspirin(C9H8O4)
ASSAY OF ASPIRIN

Weight of ASA – 0.5g


Volume of 0.1N NaOH – 6+6+15= 27 mL
Vol of 0.1N H2SO4 used in the sample = 19mL
Vol of 0.1N H2SO4 used in the blank = 49mL
SOLUTION

% = (Vblank –V smaple) N x meq x100


wt of sample or analyte
SAMPLE PROBLEM (PG 113, # 1)

 The contents of 20 aspirin capsules was


dissolved in 100mL alcohol. If 10 mL aliquot
was found to contain 0.4880g of aspirin, what
was the % of the labeled amount (5gr)of aspirin
in the capsule.
SOLUTION
PRACTICE PROBLEMS (P. 104)

A 4.0520g sample of hydrochloric acid, required


44.15mL OF 0.9035N sodium hydroxide in a
titration. Calculate the % HCl content.
PRACTICE PROBLEM

 If 25 mL of hydrochloric acid solution required


26.25 mL of 0.0952N sodium hydroxide in a
titration, what volume of the solution of HCl
would produce 0.2867g of AgCl?
PRACTICE PROBLEM

A HCl solution has an AgCl titer of 0.1266g, what


is its Na2CO3 titer?
PRACTICE PROBLEM

 Assay of Methylparaben
Wt of sample 2.1 g

Volume of 1N NaOH for sample 40 mL


and blank

Volume of 1.1N sulfuric acid 41mL


used in the blank

Volume of 1.1N sulfuric acid 31 mL


used in the sample titration

Each mL of 1N NaOH is equivalent to 152.2 mg of methylparaben.


REFERENCES

 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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