Exam 2 Flashcards
advantages of gravimetric
- not many measurements
- mass is easy to measure
- fairly accurate
- inexpensive
disadvantages of gravimetric
- prone to error
- meticulous
- time consuming
- not suited to many trials
3 types of gravimetric
precipitation
combustion analysis
thermogravimetric analysis
TGA curve
percent original mass as a function of temperature (gravimetric)
methods of precipitating non-water-soluble analytes for gravimetric
- in concentrated acids
- wet ashing
- dry ashing
- fusion
aqua regia
HCl + HNO3
wet ashing
heat + acid
metals converted to metallic cations
dry ashing
heating to extremely high temps in air
metals converted to oxides soluble in acid
fusion
used for rocks and minerals
mix with Na2CO3 and heat to high temp
Na2SiO3 is formed, soluble in water
_________ agent is added in excess in gravimetric precipitation
precipitating
characteristics of good precipitates for gravimetric
- stable at high temp
- not colloidal - settle out
- filterable - large particles
- purity
- very insoluble
- known composition
explain primary adsorbed layer
outer layer of precipitate particle
usually made of ion in excess in solution (precipitating agent)
gives a surface charge, and opposite charged spectators are attracted
explain counter-ion layer
layer of spectator ions attracted to primary adsorbed layer of precipitate
______ held counter-ion layer produces a colloidal suspension
loosely
explain saturation during precipitation
requires supersaturation, but not too much, because supersaturation favors nucleation but not crystal growth
2 steps of precipitate formation
- nucleation - formation of small nuclei of prec.
- crystal growth - combination of nuclei upon collision
how to achieve correct supersaturation in precipitate formation
- high temp
- don’t use overexcess of prec agent
- stir with addition of prec agent
- use large volumes of faily dilute solutions
- homogenous precipitation
explain homogenous precipitation
precipitating agent is formed by a slow reaction in situ, and released slowly
explain digestion (Ostwald ripening)
product is allowed to sit in mother liquor for long period at high temp
increases purity and crystal size