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
decomposition products
are volatilized at a suitable
temperature
 volatile product is then
collected and weighed or
alternatively the mass of
the product is determined
indirectly from the loss in
mass of the sample
 H2O and CO2 are the most
common volatile products
 sulfides and sulfites are
also determined  H2S or
SO2
 carbon and hydrogen in
organic compounds in
which combustions
products are collected
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