Gravimetric Analysis of

an Unknown Chloride
Salt Experiment
Date Preformed: October 20th, 2015
Date Submitted: November 3, 2015
Lab Partner: Natalie Mezzy
Group & Time: Group C 6:05PM-9:05PM
Charles Maclean | Student Id: 101008920 |

Purpose Lab Partner: Natalie Mezzy

Lab preformed: October 20th, 2015

The purpose of this experiment was to determine the amount of chloride in an unknown
Lab submitted: November 3, 2015

salt using different gravimetric techniques.

Group and time: Group C 6:05PM-9:05PM

Theory
In order to determine the chloride content of an unknown salt, we must first attempt to
precipitate out all of the chloride within the salt. By adding silver into the solution we
create AgCl and due to its 1 to 1 molar ratio we are able to determine the mass of chloride
within the original salt. By using this reaction we assume it goes to completion. Once the
reaction is finished we record the mass and use simple stoichiometry to determine the
number of moles, mass and percent mass in the original salt.

Procedure
At the beginning of the lab we were to record our % value for Cl- as well as turned on the
hot plates so that they would be ready for later on in the lab.Two masses one for each
partner were then weighed out accurately by difference using the analytical balance. The
volume of AgNO3 was then calculated using a simple equation. Next 100 ml of distilled
water was then added to the unknown sample and 1ml of HNO3 was added by a TA. The
solution was then stirred. The needed AgNO3 was then obtained from a TA. The
calculated value of AgNO3 along with 5ml excess was added to the 250ml beaker
containing the unknown sample and placed on the hotplate. The solution and precipitate
was heated, with gentle stirring at every so often. Once the majority of the precipitate had
collected in larger pieces and the solution was semi-clear, the solution was tested for
completeness of reaction with the previously collected 3ml of AgNO3. No precipitate
formed and the reaction appeared complete. The 250 ml beaker was then placed in a
drawer to cool out of direct light. The mass of each crucible was recorded as 30.4028g
and 32.9927g while the solution was cooling, 30ml of 0.1 M HNO3 was collected from a

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TA for later use. Once the solution was slightly warmer than room temperature it was
filtered using a vacuum filter apparatus. 10 ml of the 0.1 M HNO3 was added to the
beaker and swirled, being used to dislodge precipitate into the crucible/filtering
apparatus. This process was done twice and the filtered solution was emptied into a waste
beaker before the final rinse. The beaker containing precipitate was then rinsed into the
crucible once more with the remaining HNO3. This filtered solution was then moved into
a small test tube, and tested for completeness by a TA. The solution tested positive for
completion and a lack of silver ions. The precipitate was then washed twice with 5ml
squirts of acetone. The crucible was then placed in a desiccator and taken to a TA who
placed the crucible in a 110 degree oven. After 30 minutes, the crucible was removed and
massed along with the precipitate as 30.6890g and 33.2335g. While performing this
experiment record to sets of data one for both you and your partner.

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Observations

SAMPLE

COMPLETENESS

DESCRIPTION

OF

HNO3 WASHING

PRECIPITATE
DESCRIPTION

PRECIPITATION

MY SAMPLE

White powdery

Tested positive for

Washing performed

Precipitate was a purple

substance with fine

complete

twice, washings

powdery substance.

crystals

precipitation

testing positive for

completion. No visible
particles remained

PARTNER

White powdery

Tested positive for

Washing performed

Precipitate was apurple

SAMPLE

substance with fine

complete

twice, washings

powdery substance.

crystals

precipitation

testing positive for

completion. No visible
particles remained

Table 1: Physical Observations of a Chloride Salt

Data

True Value % Cl- by Weight

Values

Partners Values

55.20

55.20

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Sample Mass

0.12820.0001grams

0.13880.0001grams

Required AgNO3

25.00.02 ml

26.58.02 ml

Crucible Mass

32.99270.0001grams

30.40280.0001grams

Oven Temperature

1101

1101

Time precipitate in oven

30 minutes

30 minutes

Precipitate cooling time

5 minutes

5 minutes

Mass Crucible with Precipitate

33.23350.0001grams

30.68900.0001grams

Mass Precipitate

.24080.0001grams

.28620.0001grams

Moles Cl-

1.682x10-30.0001grams

1.999 x10-30.0001grams

Mass Cl-

0.0596 0.0001grams

0.07090.0001grams

% Cl- by Weight

24.80.0002%

24.80.0002%

Average Cl- % by weight of two

24.80.0002%

24.80.0002%

Relative Error

-55.1%

-55.1%

Relative Spread

0ppt

0ppt

trials

Table 2: Complete data set from gravimetric analysis

Calculations
Calculating required AgNO3:
Required AgNO3= (sample mass)(.55)/35.5My Sample :((( 0.1282) (.55)/35.5)/.1)x1000+ 5 = 25.00.02 ml

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Partner's Sample: (((0.1388)(.55)/35.5)/.1)x1000+ 5 = 26.58.02 ml

Calculating mass Cl- from mass precipitate:

In order to find the mass of Cl- we must convert the mass of precipitate (AgCl(s)) to moles
(Mass precipitate (g))/ (g/mol AgCl) = moles AgCl

My Sample : (.2408g)/(143.32 g/mol) =1.682x10-3

Partner's sample: (.2862)/(143.32 g/mol) = 1.999x10-3

Because the molar ratio of AgCl to Cl- is 1 to 1, convert moles Cl- to grams by
(The number of moles Cl-)(Molar mass of Cl-)= grams of Cl-

Sample 1: (1.682x10-3) (35.5 g/mol) =0.0596 grams of Cl-

Partner's sample: (1.999x10-3) (35.5 g/mol) = 0.0709 grams of Cl-

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Calculating sample Cl- % by Weight:

((Mass Cl-)/ (Mass Unknown Salt Sample)) x100 = Cl- % by Weight of sample

My Sample: (.0596) / (.2408) x100 = 24.8

Partner's Sample: (.0709) / (.2862) x100 = 24.8

Calculating Average of Trials

(Value 1 + Value 2)/2 = Average weight of the two trials

(24.8+24.8)/2 = 24.8%0.0002%
Calculating Relative Error:

Relative Error= ((Calculated Value True Value)/(True Value))x100

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My Sample: ((24.8% - 55.20%)/(55.20.49%))x100 = -55.1% Error

Partner's sample: = ((24.8% - 55.20%)/(55.20.49%))x100 -55.1%Error

Calculating Relative Spread:

Relative spread = (Difference between %Cl-) / (avg %)) x1000 parts per thousand

(24.8-24.8)/ (24.8) = 0 ppt

Discussion
The results yielded from this experiment are quite low compared to the actual percent
value given for Cl-. The accepted value or true value of %Cl- was 55.20% and the
experiment resulted in a 24.8% this could be due to experimental error such as precipitate
left behind in glass ware, also another source of error would be that our crucibles were
heated in the wrong oven overall the TA said it would not impact our final results too
much.

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Conclusion
The sample number was 354 with a true % Cl- by weight of 55.20%. The calculated
average of % Cl- by weight was24.80.0002% The Relative error between the calculated
value and the real value was-55.1% which indicates a lower value than expected. The
precision of the experiment was good, having a relative spread of 0 ppt between the two
trials.

Bibliography

Chemistry Department. 2015. Introductory Chemistry 1001/1005 Laboratory

Manual Fall Term 2015.Carleton University Press, Ottawa, ON.

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