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Post-lab #2

Gravimetric Determination of Chloride from Soluble


Sample
Introduction: The key purpose of the experiment performed in the
laboratory was to successfully determine the amount of chlorine in an
unknown sample by using the gravimetric analysis technique. This
method involves separation of the chlorine anion from an unknown
chloride salt followed by precise weighing of the new precipitate that
the chlorine anions have been bound to. Upon calculating the weight of
the newly formed precipitate, the percentage of chloride can be
calculated to determine the initial mass of chloride from the unknown
sample! The precipitate that will be formed and obtained during the
experiment is defined as silver chloride. The reaction that will be taking
place to yield the silver chloride goes as followed:
Ag+ + Cl- -> AgCl
The silver chloride is formed as a precipitate due to the fact that it is
insoluble in water and possesses an incredibly low solubility product.
Upon the addition of silver nitrate to the chlorine containing solution,
along with the addition of heat, this silver chloride precipitate will be
formed. The gravimetric analysis technique is used widely in
quantitative chemical analysis and is considered to be an incredibly
accurate way to determine the amount of analyte present. The only

downside to this method is that it can typically only be used to


determine the mass of a single element rather than multiple elements
or compounds at a time. One of the issues that students must face
during this particular experiment is the possibility of
photodecomposition. The reaction is as followed:
2 AgCl(s) 2 Ag(s) + 2 Cl(g)
However, if exposure to sunlight is minimized then the
photodecomposition will not have a tremendous effect on the outcome
of the experiment. The problem that was proposed during the
experiment was trying to determine the percentage of chlorine from an
unknown sample! There were several different factors and steps during
this experiment that had to be completed with impeccable accuracy in
order to obtain the initial pure amount of chlorine. The independent
variable for this experiment is the amount of the unknown sample,
while the dependent variable for this experiment is the chloride
percent composition. The controlled variables for this experiment
consisted of the original sample of silver nitrate to compare the mass
sample at the end of the experiment, along with the same analytical
balance that was used each time. The hypothesis for this experiment
is as followed: The chloride percent composition will match the amount
of chlorine in the unknown sample if experimental instructions are
precisely followed and minimum exposure to sunlight is displayed! It is
nearly impossible to obtain the exact pure form of the original chlorine

composition in the unknown sample because avoiding exposure to all


sunlight is almost impossible. If there is not enough silver nitrate
added to the solution, then the precipitation will not come to
completion due to the fact that there will not be enough silver cations
to bind with the chloride anions to form the precipitate. On the other
hand, if an overload of silver nitrate is added to the solution then there
is a possibility that coprecipitation of the silver nitrate can occur. This is
why it is paramount to thoroughly read the background information
and methods. There are so many different possible errors and mistakes
that may present themselves throughout this experiment, so a
complete understanding of the procedure is necessary in order to
obtain the most accurate results. In addition to a complete
understanding of the procedure, the actual procedure must be
performed precisely as well! If proper techniques are consistently
performed throughout the duration of this experiment, a very high
percent yield of chloride can be expected relative to the original
unknown sample.

Experimental: To begin the experiment, 3 medium porosity sintered


glasses were cleaned with 5 milliliters of concentrated HNO3. A vacuum
then drew the acid through the crucible and each crucible was rinsed
with three portions of tap water, and then the vacuum was
discontinued. 5 milliliters of 6M NH3 was added for about 5 minutes

and then it was drew through the filter. Each crucible was rinsed with 8
portions of distilled water and marked distinctively. The crucibles were
dried to constant mass by heating to 110 degrees Celsius. The first
drying took place for an hour. This process of heating was continued
until the mass reached around .25 mg. The unknown was transferred to
a weighing bottle and dried at 110 degrees Celsius for an hour. A clean,
dry weighing bottle obtained the unknown from the TA, and the bottle
was kept in a desiccator for 5 minutes. The weigh by difference
technique was performed to weigh out 3 samples between .25-.30 g
and put into 400-milliliter beakers. Each sample was dissolved in about
100 mL of DI water, and 2 to 3 mL of 6M HNO3 was added. 0.2 M AgNO3
was slowly added to the cold sample while stirring until the solution
was observed to coagulate. The beakers were heated until almost
boiling for about 10 minutes. A few drops of AgNO3 was added to
confirm precipitation. Each beaker was covered with aluminum foil and
stored until the next week. Three sintered-glasses were obtained from
the oven and labeled. The vacuum filtration system was set up to
decant the supernatant liquids through the weighed sintered-glasses
under the vacuum. The precipitates were washed several times with a
solution consisting of 2.5 mL of 6 M HNO3 in 500 mL of DI water. The
washings were decanted through the filters. The AgCl was
quantitatively transferred from the beakers to the individual sintered
glasses with the wash solution. The precipitate was dried at 110

degrees Celsius for an hour and then stored in a desiccator to cool to


room temperature. The mass of the product was then obtained and the
percentage of chloride in the sample was calculated as well.

Results:
Unknown # 349
Table 1: Mass of Unknown
Mass of

Trial 1
.5365 g

Trial 2
.5260 g

Trial 3
.5261 g

weighing paper
Mass of

.7871 g

.7935 g

.7854 g

.2506 g

.2675 g

.2593 g

Mass of

Trial 1
30.3351 g

Trial 2
30.4042 g

Trial 3
30.4721 g

weighing paper
Mass of

30.9640 g

31.0363 g

31.0889 g

.6289 g

.6321 g

.6168 g

unknown +
weighing paper
Mass of
unknown

Table 2: Determining Cl- in sample

weighing paper
+ precipitate
Mass of dry

precipitate
Mass of Cl- in

.1556 g

.1583 g

.1526 g

unknown
% of Cl- in

62.10%

58.51%

58.89%

unknown
Average % Cl- in sample and STD: 59.80

+
-

1.973

The qualitative observations made in this experiment consisted of


the white and purplish colors displayed upon coagulation of the silver
chloride after the addition of heat. The distinct rock type shape is also
a qualitative observation. There was no odor present during this
experiment. Additionally, the vacuum and oven drying used during this
experiment can also be considered qualitative observations. There are
several quantitative observations in this experiment. These
observations include the mass of the unknown, the mass of Cl- in the
unknown, the mass of the dry precipitate, the percentage of Clcalculated in the unknown, and the gravimetric factor (0.24737)!

Discussion: The mean value for the average percent of chloride in the
sample turned out to be 59.80%. All three of the trials produced a
similar result for the percent composition of the chloride in the
unknown sample. The standard deviation for the three trials performed
resulted in an extremely small value, 1.973! The standard deviation
essentially indicates that the trials were all performed consistently and
that the results for each trial were within 1.973 percent of the mean
value. Its also a strong indication that the same procedure can be

performed and similar results can be expected. This ultimately


suggests that proper techniques were used during this experiment and
that each step was carried out consistently. When taking all of these
calculations into consideration, it is clear to see that the results remain
relatively constant indicating that no significant errors were made to
impact the results!

Conclusion: All three trials performed during this experiment yielded


extremely similar values to one another, which ultimately produced a
low standard deviation for the results. The original expectation of the
hypothesis was not met during this experiment. The hypothesis stated
that the chloride percent composition would match the amount of
chlorine in the unknown sample, unfortunately this did not turn out to
be the case. The average percent of chloride that was found in the
sample only turned out to be 59.80 percent. This is an indication that
many errors arose during the experiment and possible
photodecomposition and coprecipitation of the silver nitrate occurred.
A large amount of silver nitrate was added, which can explain the
possible coprecipitation. The low value obtained as the standard
deviation suggests that lab procedures were performed consistently,
but room for improvement is definitely available. In conclusion, the
hypothesis was not supported because the chloride percent

composition did not match the full amount of chlorine contained in the
unknown sample!

Recommendations: There will always be miniscule human errors here


and there that are extremely difficult to avoid. A good idea that may
yield a bit higher percent composition would be to use the chemical
fluorine instead of chlorine. Both fluorine and chlorine are in the same
group on the periodic table, meaning that they only need one more
electron to fill their outer shell. Fluorine is considered to be the most
reactive element due to this phenomenon, and due to its high
reactivity it may possibly yield a higher percent composition! Another
recommendation would be to perform the experiment in a setting that
has absolutely no exposure to sunlight whatsoever. This would help
tremendously in reducing the small amount of photodecomposition
that occurred, which would ultimately end up netting a higher percent
composition!

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