Gravimetric Analysis

WEJ1
Group 4
Lobo, Liana
Lopez, Marylaine

Gravimetry
A quantitative analytical method that
is based on the measurement of mass of
a pure compound to which the analyte is
chemically related.

Classifications of Gravi
Electrogravimetric Method
Volatilization Method
Particulate Gravimetry
PRECIPITATION METHOD

Precipitation Method

The analyte is CONVERTED to an insoluble

substance (precipitate) which is ISOLATED and
WEIGHED.

Mechanisms of Precipitation
Nucleation
Formation of the smallest aggregate
of molecules capable of growing into a
large precipitate particle
induction period - time
between mixing and the visual
appearance of a precipitate.

Mechanisms of Precipitation
Crystal Growth
Once a nucleation aggregate has
formed, it begins to grow as ions or
molecules from the solution deposit on
the surface in a regular, geometric
pattern.

Mechanisms of Precipitation
Aggregate Growth
Natural cohesive forces exist between
small particles -> aggregates of
crystals
Small particles can properties that
counteract the forces of aggregation
-> colloidal suspension

Mechanisms of Precipitation
Purity
coprecipitation - occurs when
there are unwanted ions/molecules in
the precipitate
adsorption (attraction to surface)
inclusion (substitution in lattice)
occlusion (physical trapping)

Mechanisms of Precipitation
Purity
postprecipitation - formation
of a second insoluble substance on an
existing precipitate
result of a difference in the rates of
precipitation of the analyte and
contaminant

Methodology

Preparation of Solution
Precipitation
Digestion
Filtration
Washing

Drying & Igniting

Weighing
Calculation of Results

Precipitation
Favoring Growth over Nucleation

Q - concentration of the solute at

any given instant
S - equilibrium solubility

Precipitation

Coagulating colloids
sometimes the supersaturation ratio
cannot be maintained small enough
encourage colloidal particles to
coagulate into larger particles by
REDUCING SIZE (and influence) of
electrical double layer

Precipitation

For larger particles:

increase solubility
dilute solution (to minimize Q)
slow addition of the precipitating
agent (to minimize Q)
increase temperature

Digestion

Minimizing impurities and

coprecipitation
presence of impurities usually
because precipitation process was too
fast.
digestion - heating of
precipitates to get larger and purer
particles by giving the the crystals a
chance to dissolve and reprecipitate

Filtration & Washing

Done using:
paper
sintered glass
sintered porcelain
volatile inert electrolyte
may be added to the wash to
avoid peptization

Drying & Igniting

the precipitate is heated until it

reaches a constant weight
during the heating process:
moisture and volatile electrolytes are
removed
in some cases, the chemical form of
the precipitate is changed

Weighing

after heating, the precipitate must be

COOLED to room temperature
(even slightly warm objects placed in
the analytical balance will set up air
currents that cause very erratic and
incorrect weights to be recorded)

Weighing

to avoid picking up of moisture while

cooling, the precipitate is placed in a
moisture-free contained called a
DESSICATOR

Calculation of Results

Result of gravimetric determination is

usually reported as a percentage of
analyte.
% analyte =

wt of analyte
wt of sample

x 100

Calculation of Results

The precipitate is seldom the analyte

itself
Gravimetric factor - relationship
between the precipitate and the
analyte. used to convert known
weight of precipitate to corresponding
weight of analyte

Determination of Sulfur in Soluble

Sulfate

Dry sample in an oven at

100-120C

Weigh out one portion of 1.6253g,

dissolve in acid and dilute to
100mL

Allow precipitate to settle and test

for completeness of precipitation
(by adding a few drops of BaCl2)

Get three 10mL aliquots of the

solution and combine each with
excess BaCl2 solution

Allow precipitate to digest for

30mins. Collect precipitate using
a funnel (Whatman No. 42)

Clean, rinse & heat to constant

weight three crucibles and lids.

Transfer paper and precipitate to

prepared crucible. Dry precipitate
burn paper off completely.

Filter and repeatedly rinse until a

test portion of the washings
collected shows that Cl is absent.

Ignite precipitate for 20mins at

highest temperature of Tirrill
burner.

Cool and weigh the crucible and

its contents. Reignite and repeat
until constant weight is attained.

CRUCIBLE

Trial 1

Trial 2

Trial 3

Trial 4

Constant
Weight, g

33.5272g 33.5275g 33.5276g 33.5276g 33.5276g

34.9322g 34.9320g 34.9319g 34.9319g 34.9319g

34.8226g 34.8231g 34.8232g 34.8232g 34.8232g

Crucible No.

Weighing 1

33.9225g

35.3280g

35.2191g

Weighing 2

33.9220g

35.3271g

35.2180g

Weighing 3

33.9218g

35.3269g

35.2177g

Weighing 4

33.9218g

35.3269g

35.2177g

Const. Wt. of
crucible + precpt.

33.9218g

35.3269g

35.2177g

Const. Wt. of
empty crucible

33.5276g

34.9319g

34.8232g

Net Wt. of
precipitate

0.3942g

0.3950g

0.3945g

gravimetric factor

= 1.3523 g SO3

= 83.20% SO3

Crucible No.

Mass of SO3

1.3523g

1.3550g

1.3533g

%SO3

83.20%

83.37%

83.26%

Average %SO3

83.28%

Gravi Advantages
If methods are followed carefully, gravi
provides precise analysis (was used to
determine atomic masses of many
elements to six figure accuracy)
Provides very little room for
instrumental error
Methods often do not require expensive
equipment

Gravi Disadvantages
Usually only provides analysis of a
single element or a limited group of
elements
A slight misstep in a procedure can
often mean disaster for the analysis
Takes a LOT OF TIME

Applications
Used in determination of organic
substances
lactose in milk products
salicylates in drug preparation
nicotine in pesticides
cholesterol in cereals

Thank you for listening :)