OUR LADY OF FATIMA UNIVERSITY

COLLEGE OF PHARMACY
Pharmaceutical Analysis I

EXERCISE NO. 9
Assay of NaCl Injection
[Precipitation Method]
Post Laboratory Discussion
OBJECTIVES
1.To conduct analysis
using direct titration
with silver nitrate
solution
2.To determine percent
purity of the sample
Introduction
•In Precipitation titrations, the
analyte reacts with the titrant to
form an insoluble substance. At the
slight excess of the titrant, the
indicator reacts with it to signal the
end point. Also known as
Argentometry, silver nitrate is used
as the standard solution.
NaCl
•Table salt, halite, salt, common
salt
•MW – 58.5 g/mol
•USP purity requirement – 99.0
to 100.5%
Used as Primary standard, the
analyte
AgNO3
•Lunar caustic, indelible ink, Lapiz
infernularis
•MW = 169.87g/mole
•Contains nlt 99.8% and 100.5% of
AgNO3
•Preserve in a tight, light resistant
container
•Used as volumetric solution, titrant
Preparation and Standardization of 0.1 N
Silver Nitrate
 Objective: Normality
Standardization by Volumetric method

N = grams NaCl
-----------------------
meq NaCl x ml AgNO3
NOTES:
•Titration is carried out in the dark
•Sodium chloride used is dried prior to use
•Eosin Y is used as indicator. As an anion, it forms
complex with excess silver cation.
•Methanol is added for the fluorescence to be
pronounced
•Acetic acid is used to acidify the solution preventing
the ionization of the indicator
Preparation and Standardization of 0.1 N
Silver Nitrate
TITRANT ANALYTE INDICATOR ENDPOINT
AgNO3 NaCl Eosin Y TS Formation of wht
AgCl ↓
In pink suspension

AgNO3 + NaCl -------- > AgCl + NaNO3

Assay of Sodium Chloride Injection
• TITRANT: 0.1N Silver Nitrate
• ANALYTE: 90mg of Sodium Chloride
• INDICATOR: EOSIN Y
• ENDPOINT: Pink suspension
NH4SCN
•AKA Ammonium
sulfocyanate
•Hygroscopic, crystalline
solid
•MW = 76.122g/mole
•Reacts with several
metals
•Used as volumetric
solution, titrant
 Precipitation Titration Methods
Method Manifestation Volumetric Soln Indicator/s Primary Example (Assay)
Standard
•
VOLHARD/ Formation of VS1: AgNO3 FAS AgNO3- Aminophylline,
RESIDUAL insoluble VS2: NH4SCN Secondary NaCl
PRECIPITATION
complex standard for
NH4SCN
MOHR Formation of a AgNO3 K2CrO4 NaCl SLS
2nd ppt
GAY LUSAAC/ Cessation of ppt AgNO3 NaCl NaCl
METHOD OF EVEN
TURBIDITY
LEIBIG Appearance of Sodium Bromophenol KHC8H4O4 Organic N
Teraphenylboron
turbidity Compounds
C24H20BNa
FAJANS/ Change in color AgNO3 Adsorption NaCl Phenylephrine
KHODACOV’S of ppt indicator HCl
METHOD Tubocurarine
Ex. DCF,
HCl
Eosin Y, TEE
 Answers – Assay of Sodium chloride
Injection

•AgNO3 is hydrolyzed by light forming Ag2O and HNO3

•Ammonium thiocyanate is paired with silver nitrate
during residual titration requiring ferric alum as
indicator.
• Nitric acid is used with ferric alum to prevent
hydrolysis
Reference:
•Precipitation Titrations. (2020). Retrieved June
16, 2021, from
https://www.oreilly.com/library/view/pharmace
utical-
analysis/9789332515659/xhtml/chapter016.xh tml
•Knevel, A.M; DiGangi, F.E; (1977) Jenkins’ Quantitative
Pharmaceutical Chemistry Seventh Edition.
Merriam Webster Bookstore
Any questions??