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Purpose
You will be given a solid powder, which has been dried to constant mass. The sample is water soluble.
The purpose of this experiment is to determine the concentration of sulfate in your solid sample using
gravimetric analysis.
Background
Gravimetric Analysis
The goal of most quantitative chemical analysis measurements is to estimate the relative abundance of
an analyte in a chemical sample. For solid and liquid samples, a very common expression of analyte
content is based on the mass fraction. This fraction is commonly expressed as a percentage (w/w %),
as parts per million (ppm) or as parts per billion (ppb), depending on the concentration level of the
analyte. Classical chemical analysis methods are excellent for the determination of analyte
concentrations in the range of 1100 w/w %. In order to estimate the analyte mass fraction of any solid
sample, we typically need two measurements, one to estimate the sample mass and one to estimate the
analyte mass.
In gravimetric analysis, measurements of mass are used to determine the analyte concentration in a
sample. In the most common form of gravimetric analysis, the analyte is separated from the rest of the
sample in the form of a solid precipitate. In this experiment, the analysis of sulfate is performed using
barium chloride as a reagent to precipitate sulfate from the dissolved sample. The mass of sulfate in the
sample can be calculated by simple stoichiometry from the mass of the weighing form of the sulfate
precipitate.
In order to ensure maximum filterability and minimum contamination, the sulfate is precipitated under
conditions that maximize the particle size. These conditions include: (a) avoiding excessively high
concentrations of precipitating reagent; (b) slow addition of reagent to a hot solution, with vigorous
stirring; (c) avoiding a great excess of reagent. The digestion of the precipitant after the reaction
minimizes errors due to coprecipitation.
For accurate measurements, we must be sure that the composition of the weighing form is known
exactly. You must be very careful in your mass measurements throughout this experiment for
example, do not handle your weighing bottle with your bare hands, to avoid leaving fingerprints that
would increase the mass of the bottle. Of course, the recovery of the sulfate precipitate must be
quantitative, and the final weighing form must be pure.
water after the precipitate has settled. Empty the filtrate from the beaker below the funnel unless the
filtrate is cloudy. If the filtrate is cloudy, refilter the filtrate through another piece of ashless filter
paper.
Using a stirring rod and wash bottle, transfer the filtrate to the filter paper. Police the walls of the
beaker to remove the last traces of the precipitate. Wash the precipitate in the filter three times with 3-5
mL portions of warm distilled water each time.
Fold the filter paper and place in the previously weighed porcelain crucible (see Harris fig 29-2). Place
the crucible in a triangle and heat very gently to dry the paper. Next char the paper with gentle heat.
The heat should be regulated so that the paper does not burst into flame. A clean crucible cover should
be located nearby, ready for use if necessary. If the paper does burst into flame, the burner must be
quickly removed and the cover used to snuff out the flame.
After the paper has burned away, you will want to burn away deposited carbon particles by applying
increased heat to the crucible. Do not point your flame directly into the crucible you will probably
blow your precipitate across the room. You should always position your flame so that the precipitate
has access to atmospheric oxygen; otherwise you might reduce your precipitate from BaSO4 to BaS.
When the carbon is gone from the crucible, place the crucible upright in the triangle and ignite for at
least fifteen minutes at the highest temperature of the burner. You should note that the hottest portion
of the flame is just above the top of the inner blue cone. After ignition, allow the crucible to cool until
the red glow disappears and then place it in the desiccator until it cools to room temperature. Weigh
each crucible to the nearest 0.1 mg. Finally, bring each crucible to constant weight, as directed
previously.
Name:
sample A
sample B
sample C
before:
after:
crucible mass
(heated to constant mass)