gravi metric
(weighing measure)
7 Steps in Gravimetric
Analysis
Precipitation:
Dissolve
sample
Add
precipitating
reagent
Filter
Dry
Weigh
dissolved
components
sample
precipitating agent
Calculating Amount
of Precipitation Reagent
GravimetricOverview
Measure
tools for gravimetric analysis
filter crucibles, an oven, balance
Calculate
stoichiometry
Report
values
% composition, ppt, ppm, ppb
uncertainty
average
standard deviation, confidence interval
Precipitate Formation
crystallization
nucleation:
particles join to produce aggregates
crystal growth
aggregate grows and 'fall out' of solution
Precipitate Formation
Precipitate Formation
Controlling Precipitation
Increase S
Increase temperature
Decrease Q
Dilute solution
Well mixed (stirring)
Controlling Precipitation
High Electrolyte
Concentration
to Aid Precipitation
Excess charge on colloid creates
ionic atmosphere around particle
High Electrolyte
Concentration
to Aid Precipitation
Presence another electrolyte will cause
counterions (2nd layer) to be forced into
closer contact with primary layer
promoting coagulation
Washing with water dilute and remove
foreign ions and the counterions occupy
large volume, with more solvent molecule
bteween particle and 1st layer colloidal
state
D.C. Harris, Quantitative Chemical
High Electrolyte
Concentration
to Aid Precipitation
Gravimetric Interferences
Coprecipitated impurities
Surface adsorption
Contaminants bound to the surface
Dry the sample
Mixed crystals
Replacements in the crystal lattice
Reprecipitation
Occlusions/mechanical entrapment
Impurity pockets
Slow digestion/masking agents
Why AgCl?
Reaction
is highly selective - no
interferents
AgCl
22 mg/L at 1000C
Composition by
Gravimetric Analysis
Ni2+ (aq) + H2DMG Ni(DMG)2 + 2 H+
A 0.8234 g ore sample produced
0.1397 g of bis(dimethylglyoximate)
nickel (II) (FW = 288.91 g/mol). Find
the nickel content.
Explain how to create a large,
filterable precipitate.
Problem
ANS: Mg2+
Answer
174.25
x 96.06
Problem
Answer
2 * 200.59 * x 2 * 200.59 2 x
1.50
472.09
560.99