Module 3 3.

1 Volumetric precipitation
Reactions involving Combination of Ions

III. Reactions involving Combination of Ions

1. Volumetric precipitation 2. Complexation/ Chelometry reaction

Volhard Method
Mohr Method
Fajans Method
Gay Lussac’s method
Liebig Method
Volumetric Precipitation
 In volumetric precipitimetry a class of  Complexation methods of
reactions is dealt with that require the analysis will also be
formation of relatively insoluble substances considered in this module,
or precipitates to cause the reactions to go together with sodium
to sufficient completion to be quantitative tetraphenyl boron titrations
in nature.

Determination of the End Point

The end point of a reaction in analysis by precipitation methods may be determined in the following
ways:

1. Cessation of precipitation or the 2. Use of internal indicators

appearance of a turbidity 3. Instrumental methods, i.e. potentiometric or
amperometric
Indicators
The indicators used in the official volumetric precipitation assays are:
1. Ferric ammonium sulfate TS
This indicator is used both in direct and residual titrations employing standard ammonium thiocyanate
solution. The thiocyanate reacts with the silver or mercuric ions present to form a white precipitate of
3.2 Complexation Direct CaCO3, ZnO, Mg
silver or mercuric thiocyanate but, as soon as all the silver or mercury has been precipitated, the
o Vs: Ca EDTA (hexa dentate ligand)
thiocyanate ion reacts with ferric ammonium sulfate to form a red ferric thiocyanate; the first Residual Analysis of Bi and Al
appearance of the red color marks the end point of the reaction. o 1 std: CaCO3
compounds
2. Potassium chromate o Indicators:
It forms a red precipitate of silver chromate which is seen against the background of white silver hydroxynaphthol blue, dithizone, eriochrome black
chloride . Using the proper concentration of chromate ion will ensure its co-precipitation with silver
MASKING - metal detection in the presence of another metal
chloride at the point where the chloride-ion concentration is reduced to that value calculated as the
stoichiometric point. Masking agents Elements masked
3. Adsorption indicators
1. Triethanolamine Al, Fe, Mn
Examples: Eosin Y TS,
DCF (Dichlorofluorescein) 2. Thioglycol (aka: 2,3-dimercaptopropanol) Hg, Cu, Bi
TEE (Tetrabromophenolpthalein Ethyl ester) TS
3. Cyanide Zn, Ni, Cu, Co
Standard Solutions (ZiCoNiCu)
The standard solutions employed in the official assays by precipitation methods are: 4. Fluoride (Mg Almusal Ca ng Fluoride) Ca, Mg, Al
o N silver nitrate
o N ammonium thiocyanate
Computation