AC Gaje

Chem 23 (Lab)/Chem 28.1 v.1.0

20 August 2014
Experiment 2
Gravimetric Determination of SO3 in a Soluble Sulfate
Introduction
There is a gravimetric method for almost every element in the periodic table. The sulfur in
different sulfur-containing species can be determined by oxidizing the sulfur to sulfate and then
precipitating barium sulfate. The precipitate is then collected ith a filter paper! the paper is
charred off and the precipitate is ignited to constant eight. The sulfur is then reported as SO3
content.
Prerequisite reading
"efore the start of the experiment! ma#e sure that you have read $hapter % section & 'pp. 33-3()
and $hapter *% '3*+-333) of S#oog et al. %,,+ 'or the e-uivalent chapters in later editions) .
Apparatus and Equipment
*. $rucible '3 pcs.)
%. .atchglass '3 pcs.)
3. "ea#er '3 pcs.! /,, m0 or larger)
+. Tirrill burner
/. &ilter paper!.hatman 1o. +%
2. 3ron stand
4. Desiccator
5. Tongs
(. Test tubes6vials
Solutions and Chemicals
*. 7rovided. ,.* 8 9g1O3! conc. :1O3! conc. :%SO+! conc. :$l
%. To prepare. ,.%/ 8 "a$l%. Dissolve about /.% g "a$l% 'need not be dried) in *,, ml
distilled ater.
Procedure
1. Preparing the Crucibles
a. $lean and label three crucibles.
b. 7lace them over Tirill burners and heat to redness at maximum temperature of the burner
for */ min.
c. 7lace the hot crucibles on a cleaned area of the bench! and allo to cool for % min.
d. 7lace the crucibles in a desiccator! allo to cool for 3, min! and eigh accurately each
crucible.
e. ;epeat steps % to + until successive eighings agree ithin ,.3 mg. "eteen heating and
eighing the crucibles should be handles ith a pair of tongs.
2. Preparation of sample
a. Dry the sample in an oven at *,,
o
$ to *%,
o
$ for at least % h.
b. 9llo to cool in a desiccator for at least ,./ h.
c. .eigh out accurately three samples of ,./ to ,.5 g each.
d. Transfer -uantitatively to +,,-ml bea#ers.
e. Dissolve in %,, to %/, ml of distilled ater and add * ml of concentrated :$l to each.
3. Precipitation
a. 9ssume that the sample is pure 1a%SO+ and calculate the volume of "a$l% solution
re-uired to precipitate the sulfate in each sample! including a *, < excess.
b. 8easure this volume of solution into a clean bea#er using a graduated cylinder.
c. :eat both sample solution and "a$l% solution nearly to boiling.
d. 7our the hot "a$l% solution -uic#ly but carefully into the hot sample and stir vigorously.
e. 9llo the precipitate to settle and test the supernatant li-uid for completeness of
precipitation by adding a fe more drops of barium chloride solution.
f. 0eave the stirring rods in bea#ers and cover ith atch glass and digest on a steam bath
until the supernatant li-uid is clear. This ill re-uire 3, to 2, min or longer.
g. 9dd more distilled ater if the volume drops to %,, ml.
. !iltration and "ashing the precipitate
a. 7repare three .hatman 1o. +% filter papers or e-uivalent for filtration 'see S#oog et al.
%,,+ 'or later editions) for the details on preparing filter paper).
b. &ilter the solution hile hot. Decant first the clear supernatant through the filter paper
and discard the clear filtrate and then transfer the bul# of the precipitate 'see S#oog et al.
%,,+ 'or later editions) for the suggested procedures for filtration and transfer of
precipitate).
c. =sing a ash bottle! remove any precipitate from the alls of the bea#er into the funnel
ith hot ater! and then rinse the precipitate into the filter paper.
d. "e careful not to fill the filter paper to more than > of the capacity as the barium sulfate
has the ability to ?creep@ above the edge of the paper.
e. 3f the filtrate is cloudy! it must be refiltered! in hich case! the second passage generally
clears it up.
f. $ontinue to rinse the precipitate in the filter paper ith hot ater until a drop of silver
nitrate solution added to a test portion of the ashings collected in a test tube shos that
chloride is absent.
Ignition and "eighing of the precipitate
1. 9fter ashing is complete! transfer the paper and precipitate carefully to the previously
prepared crucible 'see S#oog et al. %,,+ 'or later editions) for the suggested procedure).
2. Axamine the funnel for traces of precipitatesB if any precipitate is found! ipe it off ith a
small piece of moist ashless paper and add to the proper crucible.
3. Dry the precipitate sloly in an oven for at least 3, min! and heat it sloly using a Tirrill
burner until the paper char carefully and burn off completely. 9 red gloing of the carbon
as it burns is normal but there should be no flame.
4. 3gnite the precipitate for about */ min at the highest temperature of the Tirrill burner. The
particle should be hite ith no blac# particles.
5. 3f any blac# particle is present after heating! reduction ith carbon might have occurred.
3n this case! cool the precipitate and moistened it ith a little sulfuric acid. $arefully raise
the temperature! finishing the ignition once again at the highest temperature of the burner.
2
6. $ool the crucible and its contents first on a clean area in the bench for % min and then in a
desiccator for at least 3, min. .eigh the crucible and its contents.
7. ;epeat +! / and 2 until constant eighed is attained.
$alculate and report the percent SO3 in your un#non for each portion analyzed. ;eport also
the mean and relative standard deviation.
#ata and $esults
A. Constant %eighing of Crucibles
Crucible &o. 1 2 3
.eighing *
.eighing %
.eighing 3
.eighing +
Constant %eight' g
(. Sample Si)e
Crucible &o. 1 2 3
Sample %eight' g
C. Constant %eighing of Crucible and Precipitate
Crucible &o. 1 2 3
.eighing *
.eighing %
.eighing 3
.eighing +
$onstant .eight of crucible
C precipitate! g
$onstant .eight of empty
crucible! g
1et .eight of 7recipitate! g
#. $eported *alues
Crucible &o. 1 2 3
8ass of SO3
< SO3 in the sample
9verage < SO3
;elative standard deviation
'in ppt)
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