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GRAVIMETRIC
ANALYSIS
GROUP 1 :MIC 3A1
GRAVIMETRIC
ANALYSIS
Gravimetric
2.
3.
4.
5.
PRECIPITATION
PRECIPITATION PROCESS:
Relative supersaturation
Q -S
S
3.
4.
DIGESTION
To make precipitate become larger and more pure
crystals.
Also known as Ostwald ripening (digestion).
Ostwald ripening improves the purity and
crystallinity of the precipitate.
In digestion, colloidal particles formed counter
layer(secondary layer) , primary absorptive layer
and colloidal(large number of small particle) AgCl.
There are 2 types of colloidal particles which is
hydrophilic and hydrophobic.
FILTRATION(IMPURITIES IN PRECIPITATE)
1.
o
2. SURFACE ADSORPTION
The surface of the precipitate will have a primary adsorbed
layer of the lattice ions in excess.
For example, after the barium sulfate is completely
precipitated, the lattice ion in excess will be barium, and this
will form the primary layer.
Digestion reduces the surface area and the amount of
adsorption.
Surface adsorption of impurities is the most common source of
error in gravimetry. It is reduced by proper precipitation
technique, digestion, and washing.
3. ISOMORPHOUS REPLACEMENT
Two compound are said to be isomorphous if they have same
type of formula and crystallize in similar geometric forms.
When the lattice dimensions are about the same, one ions can
replace another in the crystal, resulting in a mixed crystal.
For example, in the precipitation of Mg2+ as magnesium
ammonium phosphate, K+ has nearly the same ionic size as
NH4+ and can replace it to form magnesium potassium
phosphate.
It is very serios and little can be done about it,so precipitates in
which it occurs are seldom used analytically.
4. POSTPRECIPITATION.
When the precipitate is allowed to stand in contact with the
mother liquor(the solution from it was precipitate), a second
substance will slowly form a precipitate with the precipitating
regent.
For example, when calcium oxalate is precipitated in the
presence of magnesium ions, magnesium oxalate does not
immediately precipitate because it tends to form
supersaturated solutions.
It will come down if the solution is allowed to stand too long
before being filtered.
WASHING
DRYING OR IGNITING
This process is to removes the solvent and wash
electrolytes.
If the collected precipitate is in a form suitable for
weighing, it must be heated to remove the water
and the absorbed electrolyte from the wash liquid.
The preferable temperature use for drying is by
drying it at 110C to 120C for 1 or 2 hours.
Ignition at a higher temperature are required if a
precipitate must be converted to a more suitable
form for weighing.
CALCULATION
f wt analyte (g/mol)
a
GF
(mol analyte/mol precipitate)
f wt precipitate (g /mol) b
g analyte/g precipitate
EXAMPLE 1
CALCULATE THE GRAMS OF ANALYTE PER GRAM OF
PRECIPITATE FOR THE FOLLOWING CONVERSION:
Analyte
Precipitate
Ag3PO4
K2HPO4
Ag3PO4
Bi2s3
3BaSO4
Solution
at wt P (g/mol)
1
( mol P/mol Ag3PO4)
g wt Ag3PO4 (g/mol) 1
30.97 (g P/mol )
1
418.58( g Ag3PO4/mol) 1
0.07399g P/g Ag3PO4 GF
g P/g Ag3PO4
f wt K2HPO4 (g/mol) 1
(mol K2HPO4/mol Ag3PO4)
f wt Ag3PO4 (g/mol) 1
174.18(g K2HPO4(g/mol ) 1
418.58( g Ag3PO4/mol) 1
0.41612g K2HPO4/g Ag3PO4 GF
g K2HPO4/g Ag3PO4
f wt Bi 2S3 (g/mol) 1
g Bi 2S3/g BaSO 4
(mol Bi 2S3/mol BaSO 4)
f wt BaSO 4 (g/mol) 3
514.15 (g Bi 2S3/mol) 1
233.40 (g BaSO 4)
3
0.73429g Bi 2S3/g BaSO 4 GF
EXAMPLE 2
An ore is analyzed for the manganese content by converting the
manganese
to Mn3O4 and weighing it. If a 1.52g sample yeilds Mn3O4 weighing
0.126g,what would be the percent Mn2O3 in the sample? The percent
Mn?
Solution
3Mn2O3
(g Mn2O3 / g Mn3O4)
2Mn3O4
% Mn2O3
100%
1.52g sample
0.126 g 3(157.9)/2(228.8)
100% 8.58%
1.52 g
0.126 g Mn3O4
3Mn
( g Mn/ g Mn3O4)
Mn3O4
% Mn
100%
1.52 g sample
0.126 g 3(54.94)/228.8
100% 5.97%
1.52 g
0.126 g Mn3O4
EXAMPLE 3:
What weight of pyrite ore (impure FeS2 ) must be taken for analysis so
that
the BaSO 4 precipitate weight obtained will be equal to one-half that of
the
percent S in the sample?
Solution:
gA
100%
g sample
1
S
A(g BaSO 4)
(g S/g BaSO 4)
BaSO 4
A %S 2
100%
g sample
1 32.064
2
233.40 100%
1% S
g sample
g sample 6.869g
%A
THE END.