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Gravimetric Calculations
The results of a gravimetric analysis are generally computed from two experimental measurements: the weight of sample and the weight of a known composition precipitate. The precipitate we weigh is usually in a different form than the analyte whose weight we wish to find. The principles of converting the weight of one substance to that of another depend on using the stoichiometric mole relationships.
We introduced the gravimetric factor(GF), which represents the weight of analyte per unit weight of precipitate. It is obtained from the ratio of the formula weight of the analyte to that of the precipitate, multiplied by the moles of analyte per mole of precipitate obtained from each mole of analyte, that is,
- GF= mw of analyte (g/mole) X R = g analyte
- mw of precipitate(g/mole g precipitate
Where R is the number of moles of analyte in one mole of precipitate
GF= mw of analyte (g/mole) X R (no. of moles of analyte in one mole of ppt.)
Moles of ppt
Example :
- Calculate the gravimetric factor for
- Phosphorous in Ag3PO4precipitate
- Molecular weight(mw) for Ag3PO4 = 419
- Molecular weight for P= 31
- R= Mole ration of P in Ag3PO4 = 1
- GF = mw of analyte (g/mole) X R = g analyte
- mw of precipitate(g/mole g precipitate
- = 31 X 1 = 0.074
- 419
Aluminium in Aluminium sulphite (Al2S3) precipitate
- Molecular weight(mw) for Al2S3= 150
- Molecular weight for Al= 27
- R= Mole ration of Al in Al2S3= 2
- GF = mw of analyte (g/mole) X R = g analyte
- mw of precipitate(g/mole g precipitate
- = 27 X 2 = 0.54
- 150
- In gravimetric analysis, we may also be interested in determining the percentage composition by weight of the analyte in the sample.
- % analyte =Weight of analyte (g) X 100
- Weight of sample (g)
Weight of the analyte (g) = weight of the precipitate (g) X GF
We can rewrite a general formula for calculating the percentage composition of the analyte as:
-
% analyte =weight of the ppt (g) X GF ( g analyte / g ppt ) X 100
-
Weight of sample (g)
Example :A 0.5962 g sample of iron ore is dissolved in perchloric acid (HClO4). All iron present is oxidized to Fe3+. The solution is filtered to remove solid matrix materials and made basic with addition of ammonium hydroxide. The iron precipitates as the Fe(OH)3 .xH2O gel. The precipitate is collected in a cistern crucible and ignited to produce Fe2O3. What is the wt. % of iron in the sample if the analysis produced 0.3210 g Fe2O3?
Solution : The overall reaction is :
2 Fe3+ + 3 OH– → Fe2O3 + 3/2 H2
From this we derive the gravimetric factor relating weight of final material to the weight of iron analyte :
- GF= mw of analyte (g/mole) X R
- mw of precipitate(g/mole
- Molecular weight(mw) for Fe2O3 = 159.69
- Molecular weight for Fe = 55.85
- R= Mole ration of Fe in Fe2O3= 2
- = 55.85 X 2 = 0.6696
- 159.69
- Weight of iron (Fe) = weight of the precipitate (g) X GF
- = 0.3210 X 0.6995
- = 0.2245
- % weight of Fe in the ore =0.2245 X 100
- 0.5962
- = 37.66
Gravimetric analysis, if methods are followed carefully, provides for exceedingly precise analysis. In fact, gravimetric analysis was used to determine the atomic masses of many elements to six figure accuracy.
Gravimetry provides very little room for instrumental error and does not require a series of standards for calculation of an unknown.
Also, methods often do not require expensive equipment. Gravimetric analysis, due to its high degree of accuracy, when performed correctly, can also be used to calibrate other instruments in place of reference standards.
However, the long time needed for the analysis makes it tedious and time consuming for this reason, the volumetric analysis starts to overshadow gravimetry that is why we did not discuss gravimetry in more details .
Gravimetric methods have been developed for most inorganic anions and cations, as well as for such neutral species as water, sulfurdioxide, carbon dioxide, and Iodine.
A variety of organic substances can also be easily determined gravimetrically. Examples include lactose in milk products, salkylates in drug preparations, phenolphthalein in laxatives, nicotine in pesticides, cholesterol in cereals, and benzaldehyde in almond extracts.