Gravimetric Analysis
based upon the basic computations for
measurement of mass percent analyte:
data taken from any = ( wt A / wt S ) x 100
analysis
= ( wt PW x GF/ wt S x 100
weight of the analyte or
product weighed
weight of sample
Gravimetric Factor
constant made up of
two conversion factors a MM sought (A)
and the stoichiometric = --- x -------------------
relationship between b MM weighed (PW)
the analyte and the
product weighed
Gravimetric Methods of Analysis
1. Precipitation Method
analyte is converted to a converted to a product
sparingly soluble of known composition
precipitate by suitable heat
treatment
precipitate is filtered,
washed free of product is then weighed
impurities
Mechanisms of Precipitate Formation
a. Nucleation b. Particle Growth
precipitate containing a a smaller number of
large number of small larger particles is
particles results produced
if nucleation if particle growth
predominates predominates
colloidal precipitate crystalline precipitate
Properties of Crystalline Precipitate
readily filtered and washed free of contaminants
of sufficiently low solubility
unreactive with constituents of the atmosphere
of known composition after it is dried or, if
necessary, ignited
Precipitating Reagent Elements
Agent Precipitated
OH1- Urea Al, Ga, Th,
a technique Bi, Fe, Sn
in which a H2S Thioacetamide Sb, Mo, Cu, Cd
precipitating DMG Biacetyl + Ni
hydroxylamine
agent is HOQ 8- Al, U, Mg, Zn
generated in Acetoxyquinoline
a solution of C2O42- Ethyl oxalate Mg, Zn, Ca
the analyte SO42- Dimethyl sulfate Ba, Ca, Sr, Pb
Source:
by a slow Analytical Chemistry – 7th Edition ; Table 5-3, page 92
chemical
reaction Precipitation from
Homogeneous Solution
Gravimetric Methods of Analysis
2. Volatilization Method
the analyte or its H2O and CO2 are the most
decomposition products common volatile products
are volatilized at a suitable sulfides and sulfites are
temperature also determined H2S or
volatile product is then SO2
collected and weighed or carbon and hydrogen in
alternatively the mass of organic compounds in
the product is determined which combustions
indirectly from the loss in products are collected
mass of the sample selectively on weighed
absorbents
Exercise 16
The mercury in a 0.7152-g sample was precipitated
with an excess of paraperiodic acid, H5IO6, according
to the following reactions:
5 Hg 2+ + 2 H5IO6 Hg5(IO6)2 (s) + 10 H 1+
The precipitate was filtered, washed free of
precipitating agent, dried and found to weigh 0.3408-
g. Calculate the percentage of Hg2Cl2 in the sample.
Molar Masses:
Hg5(IO6)2 = 1448.75 Hg2Cl2 = 472.09
Exercise 16
At elevated temperatures, NaHCO3 is converted
quantitatively to Na2CO3:
2 NaHCO3 (s) Na2CO3 (s) + CO2 (g) + H2O (g)
Ignition of a 0.3592-g sample containing NaHCO3
and non-volatile impurities yielded a residue
weighing 0.2362-g. Calculate the percent purity of
the sample.
Molar masses:
NaHCO3 = 84.01 CO2 = 44.01 H2O = 18.02
Exercise 16
A pure organic compound weighing 0.9256-g was
heated in a stream of oxygen. The effluent gas (CO2 &
H2O) was swept through a tube of MgClO4 desiccant
weighing 18.2718-g and a tube of Ascarite weighing
16.2710-g. After several minutes the tubes were sealed
and reweighed: the tube containing the MgClO4
weighed 18.3029-g and the tube containing the
Ascarite weighed 16.3383-g. Calculate the percent
hydrogen and percent carbon in the organic
compound.
Molar Masses:
CO2 = 44.01 H2O = 18.02 C = 12.01 H = 1.008
Exercise 16
An antacid tablet weighing 3.408-g was dissolved and
diluted to 100.0-mL in a volumetric flask. A 10.00-mL
aliquot was treated with sufficient 8-hydroxyquinoline to
precipitate all of the Al and Mg. After proper collection
and drying, the precipitate weighed 0.7099-g.
Al 3+ + Mg 2+ + 8-hydroxyquinoline
Al(C9H6NO)3 (s) + Mg(C9H6NO)3 (s)
Another 40.00-mL aliquot of the sample was treated with
enough ammonia to precipitate Al(OH)3. After ignition at
800oC, the residue weighed 0.1867-g.
Al(OH)3 (s) --800oC Al2O3 (s)
Calculate the percent Al and percent Mg in the antacid
sample.
Molar Masses:
Al(C9H6NO)3 = 459.4 Mg(C9H6NO)3 = 456.8
Al2O3 = 102.0 Al = 26.98 Mg = 24.31
