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A Gravimetric analysis is based upon the measurement of the weight of a substance that has a KNOWN composition AND IS chemically related to the analyte.
Gravimetric Analysis
It is an ABSOLUTE method.
Relatively inexpensive
Gravimetric Analysis
Electrogravimetry.
Thermogravimetry.
Gravimetric Analysis
In precipitation methods, the species to be determined is precipitated by a reagent that yields a sparingly soluble product that has a known composition or can be converted to such a substance.
Gravimetric Analysis
Precipitation methods.
Analyte
(or chemically related species) isolated as a sparingly soluble precipitate of known composition. (or chemically related species) isolated as a sparingly soluble precipitate that can be converted by heat to species of known composition.
Analyte
Gravimetric Analysis
Determination of silver.
A
solution of Ag+ is treated with an excess of NaCl or KCl solution, the precipitate is filtered off, washed well with water to remove soluble salts, dried at 130 - 150C and weighed as AgCl.
Gravimetric Analysis
Frequently the constituent being estimated is weighed in a form other than that it was precipitated in.
Mg2+: precipitated as Mg(NH4)PO4.6H20 but is weighed as magnesium pyrophosphate Mg2P2O7 after ignition.
Gravimetric Analysis
Conditions:
1. Must be a stoichiometric reaction. 2. A stable product; no oxidation, dehydration or gelatinous precipitates. 3. Must avoid side reactions which result in coprecipitates.
Gravimetric Analysis
Accuracy
Solubility
Gravimetric Analysis
Solubility Products
Even
the most insoluble products have at least a certain solubility. It is therefore more correct to call these compounds sparingly soluble substances, eg: AgCl
Gravimetric Analysis
AgCl(s)
Ag+(aq) + Cl-(aq)
Gravimetric Analysis
Gravimetric Analysis
KTSP = [Ag+][Cl-]
Gravimetric Analysis
Solubility.
Common
ion effect Ionic strength Fractional precipitation Complex ions Temperature Solvent
Gravimetric Analysis
Particle size.
Colloidal
suspension (10-6 - 10-4 mm diameter) to crystalline precipitate. on nucleation and particle growth.
Depends
Gravimetric Analysis
Coprecipitates.
Removal
Gravimetric Analysis
Gravimetric Analysis
Inorganic:
H2S,
Organic
2,4-DNP
Gravimetric Analysis
8-Hydroxyquinoline
O Mg2+ + 2 N OH O N Mg N + 2H+
Selectivity
through pH control
Gravimetric Analysis
8-Hydroxyquinoline Examples
Metal pH Initial Ppt. pH Complete Ppt 4.7 9.8 5.2 9.4 5.5 13.2 9.2 12.7 4.9 11.6 >3.3 4.1 11.2 8.4 12.3 >8.7 Metal pH Initial Ppt. pH Complete Ppt 5.9 9.5 3.6 7.3 4.6 10.0 4.4 8.8 4.8 8.6 5.0 5.7 4.9 9.3 2.7 6.1 >4.4
Gravimetric Analysis
Dimethylglyoxine
CH3 C C CH3 O N N O H H + 2H+ Ni O N N O
Ni2+ + 2 CH3 HO
CH3 OH
N N
CH3
CH3
Summary
Principles
Solution
reaction between analytes and reagents to give sparingly soluble products. Drying or ignition of precipitates. Weighing
Apparatus
Flasks,
beakers, pipettes, crucibles and filter papers. Oven or furnace and a dessicator. Analytical quality balance.
Summary
Applications
Extensive
numbers of inorganic ions are determined with excellent precision and accuracy. Routine assays of metallurgical samples. Relative precision 0.1 to 1%. Good accuracy
Summary
Disadvantages
Careful
and time consuming. Scrupulously clean glassware. Very accurate weighing. Coprecipitation.