COLLEGE OF PHARMACY

Valenzuela. Quezon City. Antipolo. Pampanga. Cabanatuan. Laguna

Pharmaceutical
Analysis 1
DAY 13

Name of Instructor
College of Pharmacy
COURSE FACILITATOR
GRAVIMETRIC
METHOD
 Objectives
❖ Explain the principles involved in
Gravimetric Method of analysis
❖ Demonstrate the usage of proper
procedures and equipment handling
techniques
❖ Demonstrate ability to calculate the
percentage purity or potency of samples.
❖ Interpret the results obtained from the
analysis.
 Outline
1. GRAVIMETRIC ASSAY
- Gravimetric method by precipitation

2. SAMPLE PROBLEMS
 GRAVIMETRIC ASSAY
❖ Gravimetric analysis consists of isolating
from the sample the constituent to be
determined in its pure state and weighing it
accurately
❖ Isolation may be done by:
❖ precipitating the sought substance in an
insoluble form
❖ electrolysis
❖ converting the substance to a gas which is
absorbed in a suitable reagent.
 Precipitation
❑ Of low solubility

❑ Large in particle

❑ Easily filtered

❑ Pure and stable

 Precipitation
1. Solubility Product principle
❖ The ionic product exceeds the solubility product
constant, precipitation will occur
2. The common ion effect
❖ If there is an excess of one ion over the other, the
solubility of the precipitate will decrease

3. Law of mass action

❖ The rate of the reaction is directly proportional to
the product of the molecular concentrations of the
reacting substance
 Gravimetric method by
precipitation
❖ Dissolve sample
❖ Add ppt’ing reagent
❖ Filter
❖ Dry
❖ Weigh
 ASSAY OF SODIUM SULFATE
GRAVIMETRIC METHOD BY PRECIPITATION

500 mg
sample Add 12 mL Pour 20 mL
Stand
dissolved in conc HCl BaCl2
150 mL dw

The supernatant liquid is decanted and the precipitate is washed three

times with warm water. The residue is white. It is then cooled and
weighed
Identify weight of precipitate

Compute for the gravimetric

factor

MW sought
GF =
MW ppt

Compute for the weight of

pure substance

Wt ppt X GF x 100
%=
Wt sample
 The residue weighed And bears a DEFINITE
must have a DEFINITE RELATION with the
CHEMICAL constituent to be
COMPOSITION determined

FACTOR

Commonly known as
Chemical factor, Na2 SO4 142.52
Calculation factor, GF = =
BaSO4 233.43
Equivalent factor,
Gravimetric factor
 Practice Problem
1. A 0.3056-g sample of soluble
chloride was analyzed gravimetrically
for Cl and 0.7265 g of AgCl was
obtained. Calculate the Cl and NaCl
contents of the sample, expressing
each in %w/w.
 Practice Problem
SAMPLE
1. A 0.3056-g sample of soluble
chloride was analyzed gravimetrically
PRECIPITATE
for Cl and 0.7265 g of AgCl was
obtained. Calculate the Cl and NaCl
contents of the sample, expressing
each in %w/w.
 Identify weight of
precipitate
0.7265 g AgCl
Compute for the gravimetric factor
𝐌𝐖 𝒔𝒐𝒖𝒈𝒉𝒕
𝐆𝐅 =
𝐌𝐖 𝒑𝒑𝒕
35.5 58.5
GFCl = 143.5= 0.2474 GFNaCl = 143.5= 0.4077
Compute for the weight of pure substance
Wt ppt X GF x 100
%=
Wt sample
0.7265g X 0.2474 x 100 0.7265g X 0.4077 x 100
%Cl = %NaCl =
0.3056g 0.3056g
%Cl = 58.81% %NaCl = 96.92%
 Practice Problem

2. A 0.5463 g sample of the silver salt of

a monobasic organic acid yielded
0.4690 g of AgCl. Calculate the (a) Ag
content of the sample in %w/w
 Identify weight of
precipitate
0.4690 g AgCl
Compute for the gravimetric factor
𝐌𝐖 𝒔𝒐𝒖𝒈𝒉𝒕
𝐆𝐅 =
𝐌𝐖 𝒑𝒑𝒕
108
GFAg = 143.5= 0.7526
Compute for the weight of pure substance
Wt ppt X GF x 100
%=
Wt sample
0.4690g X 0.7526 x 100
%Ag =
0.5463g
%Ag = 64.61%
 Practice Problem

3. If 0.4600-g sample of sodium iodide

yielded 0.7200 g of AgI (a) what was the
weight of iodine in the sample (b) what
was the iodine content of the sample in
%w/w
 Identify weight of
precipitate
0.7200 g AgI
Compute for the gravimetric factor
𝐌𝐖 𝒔𝒐𝒖𝒈𝒉𝒕
𝐆𝐅 =
𝐌𝐖 𝒑𝒑𝒕
108
GFI2 = 235= 0.4596
Compute for the weight of pure substance
Wt ppt X GF x 100
%=
Wt sample
0.7200g X 0.4596 x 100
%I2 =
0.4600g
%I2 = 71.94%
 Practice Problems

1.A sample consisting only of pure KCl and pure KI weighs 0.4811
g, it is quantitatively converted into KCl and now weighs
0.2892 g. Calculate how much KI was present in the original
sample.

2. A sample consisting only of pure KCl and pure KI weighs 0.4811

g, it is quantitatively converted into KCl and now weighs
0.2892 g. Calculate how much KI was present in the original
sample

3. An unknown sample of a soluble sulfate weighing 1.80 g yielded

0.90 g of BaSO4. Compute for % S in the sample.

- MgSO4, K2SO4, Al2(SO4)3

 Practice Problems

4. An unknown sample of a soluble sulfate weighing 1.80 g yielded

0.90 g of BaSO4. Compute for % S in the sample.

- MgSO4, K2SO4, Al2(SO4)3

5. What weight of AgCl could be obtained from a sample of

mercury bichloride capable of yielding 0.3750 g of HgS?

Hg=201Al=27 Mg= 24
Related Links

Practice Problem: Gravimetric Analysis

❖ https://www.youtube.com/watch?v=YtX3SuHqK
Os

Redox Titration Lab

❖ https://www.youtube.com/watch?v=mjPyZI37TG
k
 References
TEXTBOOK: Knevel, A.M. and Digangi, F.E., Jenkin’s Quantitative Pharmaceutical
Chemistry.USA: Mc Graw Hill. 1977.

REFERENCES:
• Watson, David G. Pharmaceuticals analysis: a textbook for pharmacy students and
pharmaceutical chemists, 4th ed. Singapore: Elsevier. 2017.
• Remington’s Pharmaceutical Sciences, (2013) Philadelphia: Lippincott William
and Wilkin
• WHO Expert Committee on Specifications for Pharmaceutical Preparations .
Geneva: World Health
• British Pharmacopeia . 2017.
• The United States Pharmacopeia(USP 40) : NF 35: The National Formulary
.Rockville, Md.: United States Pharmacopeial Convention. 2017.
• Handbook of Modern Pharmaceutical Analysis (2011) Amsterdam; Boston:
Academic Press/Elsevier
• Harris, D.C., Quantitative Chemical Analysis, 9th ed. New York :
W.H. Freeman. 2015
 ANY
QUESTIONS?
You can find me at:
@fatima.edu.ph

facebook.com/
OLFUValenzuelaPharmacy/ (8)-661-3023 loc. 106