Gravimetric Determination of Chloride from Seawater and Brackish Water

Introduction
Gravimetric chloride determination is a technique for determining the chloride
concentration of a solution by precipitating it as silver chloride. Chloride, on the other hand, is
one essential ion found in natural water sources that affect the overall salinity and makeup of
aquatic ecosystems.
Natural waters, which include seawater and the water found in rivers and lakes, are
aqueous solutions because they contain soluble chloride salts that, when dissolved in water,
release chloride ionsC l −¿ ¿. AgCl is insoluble in water. This means that rather than dissolving to
produce ions in an aqueous solution, the ions remain bound to one another in a crystal lattice,
forming a solid. An insoluble solid (precipitate) of silver chloride can be created by mixing a
−¿ ¿
water sample containing C l (aq), a water-soluble silver salt, such as silver nitrate, AgN O3(aq)
(Stubbings, n.d.).

Objectives
 Determine the chloride content of both seawater and brackish water quantitatively using
gravimetric methods.
 To provide precise and reliable data for the measurement of salt content in varied water
samples.
 Examine the precipitate through analytical techniques.

Materials and Procedure

A. Materials
-Pipette -Aspirator - Nitric acid(HN O3)
-Volumetric flask -Wash bottle -Silver nitrate ( AgN O3 ¿
-Erlenmeyer flask -Beaker -Seawater
-Filter paper -Glass dropper -Brackish water
-Hot plate -Stirring rod -Distilled water
-Watch glass -Foil
-Digital balance -Desiccator
-Funnel -Graduated cylinder
-Analytical balance

B. Procedure
For the experiment proper, 100 mL of seawater and brackish water was filtered in a dry
conical flask using filter paper. About 50 mL of filtered seawater was then transferred
into a 100 mL volumetric flask with deionized water using a pipette making up to the
mark of a volumetric flask. The process was repeated for brackish water. To make trials
 in each solution, 20 mL of dilute seawater was transferred into a beaker and another 20
mL of dilute seawater was transferred into another beaker. The process was repeated for
brackish water.
After transferring the sample solution, 6 mL of 1 M nitric acid was added to the samples.
Now that the solutions were acidified, it was stirred, and using a glass dropper, 0.1 M
silver nitrate solution was added continuously until no more white precipitate formed.
When the solution showed no sign of white precipitate, it was heated on a hot plate with
gentle stirring until the solution nearly boiled, the precipitate coagulated, and the
supernatant liquid was clear.
After the solution was boiled, the beaker was then removed and covered with a watch
glass to allow the solution to cool, until the precipitate settled. After this, the solution was
then tested again by the addition of silver nitrate to see if it still formed more precipitate.
When the test was completed, the beaker was then covered wrapped in foil, and placed in
a dark cupboard for 24 hours.
The next day, the settled mixture was filtered using filter paper, but before it, the mass of
the filter paper was obtained. After the filtering was done, the filter paper containing the
precipitate was placed in a watch glass and placed in a dry oven for an hour at 90 ℃.
When the precipitate and filter paper were dry enough, it was then placed in a desiccator
to cool. After the precipitate was cooled, the filter paper with the precipitate was
weighed.

Chemicals SDS
1. Nitric acid
Properties (appearance, color, odor) Solid, white, odorless
Signal word Danger
Hazard statements  May intensify fire; oxidizer
 May be corrosive to metals.
 Causes severe skin burns and eye
damage.
 Toxic if inhaled.
 Corrosive to the respiratory tract.
Storage  Store locked up
 Store in a well-ventilated place.
Keep container tightly closed.
 Store in a dry place.
Disposal Dispose of contents/containers to an
approved waste disposal plant.
NFPA Health – 4
Flammability – 0
Instability – 0
Physical hazards - OX
 2. Silver nitrate
Properties (appearance, color, odor) Liquid, clear colorless, light yellow,
strong acid odor
Signal word Danger
Hazard statements  May intensify fire; oxidizer
 May be corrosive to metals.
 Causes severe skin burns and eye
damage.
 May cause respiratory irritation.
 May cause damage to organs
through prolonged or repeated
exposure
Storage  Store locked up
 Store in a well-ventilated place.
Keep container tightly closed.
Disposal Dispose of contents/containers to an
approved waste disposal plant.
NFPA Health – 3
Flammability – 0
Instability – 2
Physical hazards - OX

3. Distilled water
Properties (appearance, color, odor) Clear, liquid, colorless, odorless
Signal word Not applicable
Hazard statements None
Storage  Store in cool, dry conditions in
well-sealed containers.
Disposal Consult federal state/ provincial and local
regulations regarding the proper disposal
of waste material that may incorporate
some amount of this product.
NFPA No data available

Result and Discussion

1. In this laboratory experiment, we used seawater and brackish water as test samples. The
samples were treated with silver nitrate to form white precipitates of silver chloride.
When aqueous solutions of silver nitrate and sodium chloride are mixed, the following
reaction occurs:
AgN O3(aq) + NaC l(aq) → AgC l (s ) + NaN O3(aq )
2. To determine how much 0.1 M AgN O3 was needed to add to precipitate out all the
Chlorine content:
50 mL AgN O 3 (
1.00 L
1000 mL L )(
0.1 mol
AgN O3
169.87 g
1 mol )(
AgN O 3 =0.8494 g AgN O 3 )
Therefore, we dissolved 0.8494 g of AgN O3 in sufficient H2o and diluted it to 50 mL
mark.
Before treating the brackish water and seawater with silver nitrate, it was observed that
nitric acid was added to both the brackish water and seawater solution. This is because, in
gravimetric analysis, nitric acid is utilized to maintain a high electrolyte concentration
and prevent peptization during the washing process. It is also employed to acidify the
precipitation solution, preventing competing precipitation processes utilizing A g+1.
Because washing with water may dissolve the precipitates, washing with nitric acid
assures that they are kept and makes sure that the precipitate doesn’t break back up into
colloids. When the precipitate is dried, the acid decomposes to produce volatile
compounds.
During the laboratory experiment, we avoided not to expose the mixture to light, because
when it is exposed to light, it photo-decomposes to give elemental silver and chlorine gas.
The elemental silver (violet color seen in precipitate) combines with another chloride ion
to form silver chloride; however, due to the chloride that escaped as gas, the product is
lost, and that gives a low yield.
3. After that, the silver chloride is filtered and weighed. The silver chloride mass can be
used to compute the chloride mass and concentration in the original solution.
Table 1. Determination of Chloride from Brackish water

Trial 1 Trial 2
Mass of filter paper (a) 1.0356 g 1.0469 g
Mass of filter paper + precipitate (b) 1.4698 g 1.3370 g
(AgCl) Mass of precipitate (b-a) 0.4342 g 0.2901 g
Mass of Cl 0.1074 g 0.0718 g
% 1.074 0.7175

Given the data, we can determine the chloride content of brackish water by this:
a. moles of AgCl precipitated:
1 mol −3
Trial 1: 0.4342 g AgCl x AgCl=3.0296 x 10 mol AgClTrial 2:
143.32 g
1 mol −3
0.2901 g AgCl x AgCl=2.0241 x 10 mol AgCl
143.32 g
b. moles of C l −¿ ¿ present in the 20 mL of diluted brackish water:
 Trial 1: mole ratio of AgCl and C l −¿ ¿ is 1:1, therefore there is 3.0296 x 10−3 mol of C l −¿ ¿
in 3.0296 x 10−3 mol of AgCl.

Trial 2: mole ratio of AgCl and C l −¿ ¿ is 1:1, therefore there is 2.0241 x 10−3 mol of C l −¿ ¿
in 2.0241 x 10−3mol of AgCl.
−¿ ¿
c. concentration (M) of C l in the diluted brackish water sample:
Trial 1:
−¿
l
M =mol C −¿ ¿
−¿ −3 l −¿¿
volume C l =3.0296 x 10 mol C =0.1515 M C l ¿¿ Trial
1L
20 mL x
1000 mL
−¿
l
M =mol C −¿ ¿
−¿ −3 l −¿ ¿
2: volume C l =2.0241 x 10 mol C =0.1012 M C l ¿¿ d.
1L
20 mL x
1000 mL
concentration (M) of C l −¿ ¿ in original, undiluted seawater
M2 V 2
Trial 1: M 1 V 1= M 2 V 2 ⇉ M 1 = ;
V1

V 1=50 mL (0.05 L)M 2=0.1515 M V 2=100 mL(0.1 L)

M 2 V 2 ( 0.1515 M ) (0.1 L)
M 1= = =0.303 M 1
V1 0.05 L
M2 V 2
Trial 2: M 1 V 1= M 2 V 2 ⇉ M 1 = ;
V1
V 1=50 mL (0.05 L)M 2=0.1012 M V 2 =100 mL(0.1 L)
M 2 V 2 ( 0.1012 M ) (0.1 L)
M 1= = =0.2024 M 1
V1 0.05 L
w
e. % ( ) of C l −¿ ¿
v
1L 0.3030 mol 35.45 g −¿¿
Trial 1: 100 mL x x Cl x Cl=1.0741 g C l
1000 mL 1L 1 mol
−¿
l

( )
w −¿=1.0471 g C ¿¿
% of C l 100mL
; 100 mL of solution contains 1.0741 g C l −¿ ¿Trial 2:
v
1L 0.2024 mol 35.45 g −¿¿
100 mL x x Cl x Cl=0.7175 g C l
1000 mL 1L 1mol
−¿
l
w
( )
−¿=0.7175 g C ¿¿
% of C l 100mL
; 100 mL of solution contains 0.7175 g C l −¿ ¿
v

f. concentration of C l −¿ ¿ in g/L
 1L 0.3030 mol 35.45 g
100 mL x x Cl x Cl
1000 mL 1L 1 mol
Trial 1: =10.741 gC l−¿¿ Trial 2:
1L
100 mL x
1000 mL
1L 0.2024 mol 35.45 g
100 mL x x Cl x Cl
1000 mL 1L 1 mol
=71.75 g C l −¿¿
1L
100 mL x
1000 mL
Table 2. Determination of Chloride from Seawater

Trial 1 Trial 2
Mass of filter paper (a)
Mass of filter paper with precipitate (b)
(AgCl) mass of precipitate (b-a)
Mass of Cl
%
From the obtained results above, the average percentage of the chloride ions for brackish water is
0.8958 g per 100 mL solution, while seawater is 0.8104 g per 100 mL solution. We can see that
the % w/v of chloride ions in brackish water is greater than seawater. Generally, the
concentration of chloride in seawater is 19.4 g/L while the concentration of brackish water is
between 0.5 – 5 g/L. We can observe that the concentration of chloride ions in g/L in different
trials of seawater is relatively low, while in brackish water is a bit high This could mean that the
precipitation reaction is not complete then not all chloride ions that are present in the samples are
converted into AgCl. Additionally, according to the procedure, we should have done trials of
drying and weighing the precipitate until a constant mass is achieved to determine the chloride
ions present in the sample accurately. As a result, the amount of chloride ions in seawater
measured is relatively low.
Conclusion
This lab used seawater and brackish water as test samples. The samples were treated with silver
nitrate to obtain white precipitates of silver chloride; the silver chloride initially formed as a
colloidal solution; after subsequent heating, the nucleation process was dominated by particle
growth, and the precipitates separated as coagulated mass.
Determination of chloride content in each sample is successfully obtained. However, upon
comparing the general concentration of the sample to the obtained resulting concentration, the
results misaligned with the general concentration. Which let us conclude that the precipitation
was incomplete. This type of error will serve as a lesson for the next laboratory activities to
avoid less precise results.
References
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https://chem.libretexts.org/Bookshelves/Introductory_Chemistry/Introductory_Chemistry

_(CK-12)/11%3A_Chemical_Reactions/11.09%3A_Double_Replacement_Reactions

 Stubbings, J. (n.d.). Chloride in seawater Gravimetric Analysis Chemistry tutorial.

https://www.ausetute.com.au/seawaterCl.html#google_vignette

 ThermoFisher Scientific. (2009, March 12). msds. https://www.fishersci.com/msds?

productName=A467250%26productDescription=NITRIC.
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