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Types of gravimetric methods

1. Precipitation methods – A gravimetric methods in which the signal is the mass of the precipitate. 2. Volatilization gravimetric – A gravimetric method in which the loss of a volatile species gives rise to the signal.

Precipitation methods
The eight steps of precipitation methods 1. Preparation of solutions 2. Precipitation 3. Digestion 4. Filtering 5. Washing 6. Drying 7. Weighing 8. Calculation 1. Theory and methods Solubility considerations Require the solubility to be minimal. Usually the total accuracy should be +/- 0.1% Solubility losses can be minimized by controlling the composition of solution Reacts with analyte to form insoluble material. Precipitate has known composition or can be converted to known composition

Avoiding Impurities Inclusion – potential interfering ions whose ion and charge are similar to a lattice ion may substitute into the lattice structure by chemical adsorption. It may cause the precipitate masses to be larger than the expected but does not change the percentage of the analyte. Occlusion – when physical adsorbed interfering ions become trapped within the growing precipitate. ( mass larger) 2 cases of occlusions – when rapid precipitation traps a pocket of solution.(mass lesser) Inclusions can be only minimized by the re-precipitation and occlusions can be reduced by the digestions.

Filter paper is also rated as fast. Done for crystalline ppts (e. or a localized region of solution. It produces numerous small particles.RSS can be expressed as Relative supersaturation = Q : degree supersaturation ( [ ] Of mixed reagents before ppt) S : solubility of ppts at equilibrium Relative supersaturation can also be known as a measure of the extent to which a solution. contains more dissolved solute than that expected at equilibrium. increase the temperatures. adjusting the pH . use the low ash filter paper. precipitation is likely to occur by particle growth than by nucleation. medium and fast. When RSS is small. During digestion.- Digestion is the process of maintaining the ppts in equilibrium with its supernatant solution for an extended time. it might have clogged. Solution containing ppts are heated before filtering Heating the ppts within the mother liquor (or solution from which it precipitated) for a certain period of time. Precipitate that are usually insoluble and a big RSS is unavoidable. - Filtering the precipitate Filtration is done by filter paper/ filtering crucible. Ash is being left. Filter paper is hygroscopic and not easily dried to constant weight.g: BaSO4) diameter >10-4cm. How to minimize the RSS? By decreasing the solute’s concentration or increasing the precipitate’s solubility. If RSS is small. If the filtration is too fast. . it may need a very long time to form a precipitate. Igniting the filter paper is a must. The most common filtering crucible is cellulose based filter paper. If the filtration is too slow. A solution with high RSS can have a solutions which highly supersaturated. Controlling Particle Size A solute relative supersaturation. Practically. Such solutions are unstable and show high rates of nucleation. If was quantitative analytical procedure. small particles tend to dissolve and reprecipitate on larger ones. there might have a ppts loss. The additional ppts can be minimized by controlling solution conditions.

Filtering crucible is also another way to filter the precipitate. Any supernatant solution is being left into the funnel. .- When the filter paper is made into a cone. Supernatant solution is the solution that remains after the precipitate forms. Rinsing the ppts The residual traces of supernatant must be removed in order avoid the sources of determinate error. the water is dampened to seal the cone and the funnel.