be volatile and the ions of the electrolyte should not be part of the product complex. +or example, use of ammonium nitrate (,-',.&) or ammonium hydroxide (,-'.-) in distilled water results in the volatile species/ ,-&, -,.&, and -#.. Digestion he precipitate often contains ions that where trapped when the precipitate was formed. his is mostly a problem for crystalline precipitates. If the trapped ions are not volatile, then their presence will corrupt the weighing step. 0oncentration of interfering species may be reduced by digestion. 1igestion is a process where the precipitate is re%dissolved and precipitated out of a cleaner environment (solution). he precipitate obtained in the separation step is placed into a volatile electrolyte solution and heated. 2arge particles are broken up to speed up digestion. his 3solution3 is often heated to increase the kinetic rates of dissolution and precipitation. Since the solid is in dynamic e$uilibrium with the solution, in time, all material will cycle from solid to solution and back. .bservation does not speed up the chemical kinetics, so we take a cola break during digestion. he solution is cooled after digesting for an hour or more. he precipitate is now refiltered. Preparation for Weighing After separation, the material must be prepared for weighing. his is accomplished by heating up the precipitate to drive off excess solvent and volatile electrolytes. 2ow temperature drying may be used for some lyophobic (solvent phobic) precipitates. -igh temperature drying, called ignition, is used for the lyophilic (solvent liking) precipitates. he thing to remember is that drying or ignition may change the chemical composition of the precipitate. Weighing he dried or ignited is solid cooled prior to weighing. his avoids convection currents from altering the mass measurement. he hot sample is placed into a desiccator during the cooling stage to reduce adsorption of water from the air. Since weighing is performed in a vessel, e.g, a weighing bottle or a crucible, the dry weight of the vessel must be determined before hand. he solid weight is determined by difference. More Rules for a Successful Gravimetric Analysis A few additional rules of thumb for a successful $uantitative precipitation are! he precipitate must be large enough to settle out of solution he precipitate must be large enough to be filtered
he precipitation process must be complete he precipitate must be pure he precipitate must be stable when dry, or produce a stable product upon ignition
Example of a Gravimetric Analysis A 4.567# g sample of iron ore is dissolved in perchloric acid (-0l.'). All iron present is oxidi*ed to +e&8. he solution is filtered to remove solid matrix materials and made basic with addition of ammonium hydroxide. he iron precipitates as the +e(.-)& .x-#. gel. he precipitate is collected in a cistern crucible and ignited to produce +e#.&. (hat is the wt. 9 of iron in the sample if the analysis produced 4.&#"4 g +e#.&: irst! examine the chemistry he overall reaction is +rom this we derive the gravimetric factor relating weight of final material to the weight of iron analyte
Secon"! calculate the mass of iron he mass of iron in the ignited precipitate is
#ast! calculate $eight % he weight 9 of iron in the ore is obtained from the mass of iron and the sample weight,
;ack to 0hemistry &744 -ome his page was created by <rofessor Stephen ;ialkowski, =tah State =niversity. 2ast =pdated uesday, August 4&, #44'