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CH 12 Gravimetric Methods of Analysis PDF
CH 12 Gravimetric Methods of Analysis PDF
Chapter 12
Gravimetric Methods of Analysis
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dimethylglyoxime
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(12-1)
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Figure 12-1 A
colloidal silver
chloride particle
suspended in a
solution of silver
nitrate.
Electric double
layer (電雙層)
Figure 12-2
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Dilute AgNO3(aq)
solution
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12A-5 Coprecipitation
Coprecipitation (共沉澱) is a process in which normally
soluble compounds are carried out of solution by a precipitate.
There are four types of coprecipitation: surface adsorption,
mixed-crystal formation, occlusion, and mechanical
entrapment.
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12A-5 Coprecipitation
Surface Adsorption
Coagulation of a colloid does not significantly decrease the
amount of adsorption.
The net effect of surface adsorption is therefore the
carrying down of an otherwise soluble compound as a
surface contaminant. (Ex. Coagulated silver chloride is
contaminated with primarily adsorbed Ag+ along with nitrate or
other anions).
12A-5 Coprecipitation
Surface Adsorption
Minimizing Adsorbed Impurities on Colloids.
The purity of many coagulated colloids is improved by
digestion (浸煮).
Regardless of the method of treatment, a coagulated colloid is
always contaminated to some degree, even after extensive
washing.
Reprecipitation.
A drastic but effective way to minimize the effects of adsorption
is reprecipitation (再沉澱), or double precipitation.
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12A-5 Coprecipitation
Mixed-Crystal Formation (混合晶體形成)
In mixed-crystal formation, one of the ions in the crystal lattice of a
solid is replaced by an ion of another element. (ex)
The extent of mixed-crystal contamination is governed by the law
of mass action and increases as the ratio of contaminant to analyte
concentration increases.
Occlusion (包留) and Mechanical Entrapment (力學誘陷)
When a crystal is growing rapidly during precipitate formation,
foreign ions in the counter-ion layer may become trapped, or
occluded, within the growing crystal.
Occlusion is a type of coprecipitation in which a compound is
trapped within a pocket formed during rapid crystal growth.
12A-5 Coprecipitation
Occlusion and Mechanical Entrapment
Mixed-crystal formation may occur in both colloidal and crystalline
precipitates, whereas occlusion and mechanical entrapment are
confined to crystalline precipitates.
Mechanical entrapment occurs when crystals lie close together
during growth.
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12A-5 Coprecipitation
Coprecipitation Errors
Coprecipitation can cause either negative or positive errors.
Al(OH)3
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Figure 12-6
Example 12-2
An iron ore was analyzed by dissolving a 1.1324-g sample in
concentrated HCl. The resulting solution was diluted with water, and
the iron(III) was precipitated as the hydrous oxide Fe2O3‧xH2O by
the addition of NH3. After filtration and washing, the residue was
ignited at a high temperature to give 0.5394 g of pure Fe2O3 (159.69
g/mol). Calculate (a) the % Fe (55.847 g/mol) and (b) the % Fe3O4
(231.54 g/mol) in the sample.
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Example 12-2
Example 12-2
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8-Hydroxyquinoline (HOQ)
Dimethylglyoxime (DMG)
Sodium Tetraphenylborate
Sodium tetraphenylborate, (C6H5) 4B-Na+, is an important example
of an organic precipitating reagent that forms salt-like precipitates.
(Ca2+, NH4+)
Sodium Tetraphenylborate
Molecular model
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