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Department of Chemical Engineering

College of Engineering

Bicol University

Legazpi City

Gravimetric determination
of a soluble sulfate
Laboratory Plan No. 1

Engr. Junel B Borbo

Professor

Group No.2 members:

Aidan Kyle Sanglay

Kenneth Sta. Ana

Adrian Navarra

Heddy Suzane Chiong

Donabel Hina
I. Objective

To understand the gravimetric method of analysis and to gather sufficient

amounts of precipitates from an impure substance while applying the proper use of

laboratory equipments as well.

II. Materials and Rea gents

Materials Specifications Pieces


Crucible and holder 2
Clay triangle 2
Bunsen burner 2
Dessicator 1
Crucible tongs 2
Watch glass 70 mm 3
Beaker 500 ml 5
Beaker 100 ml 1
Measuring pipette 10 ml 2
Burette 50 ml 2
Burette clamp 2
Iron stand 2
Stirring rod glass 2
Thermometer 1
Volumetric flask 100 ml,glass 1
Volumetric flask 50 ml,glass 1
Iron ring 2
Wire gauze 2
Filter paper 2
Funnel 90 mm,glass 2
Filtration stand 1

Reagent Mass/volume
HCl 1 ml
Sulfuric acid 0.3 ml
Barium Chloride 5.205 g
III. Procedures

The amount of sulfate in the compound will be determined by precipitating it as barium


sulfate and weighing the precipitate.

1. Clean and rinse two 500 ml beaker. The experiment is to be done two times for two
amounts of analyte . Accurately weigh out on a previously weighed watch glass an impure
sample of ferrous sulfate. Note the weight and dry the sample for at least 15 minutes.
Weigh about 0.5 and 0.6 g of the sample and transfer each sample to one of the beakers.
2. Transfer each sample to one of the beakers. Rinse the watch glass with a small amount of
deionized water, collecting the rinsings in the beaker containing the sample. Add 200 ml of
deionized water to each beaker. Then add 0.5 ml of concentrated HCl to each.Stir until the
sample is dissolved.
3. Prepare the titration setup. Pour the 0.25 M BaCl2 into the burette while doing the setup
and heat both solutions almost but not quite to boiling (in between 50-80⁰ C). Hold at this
temperature while adjusting the burners. Cool the solutions first and add a few drops of the
titrant to the solution slowly so as not to rapidly increase the level of supersaturation .Add
some more until the amount of titrant reaches 13.16 ml to the 0.5g-analyte and 15.79 ml to
the 0.6g-analyte (the volume needed to form a precipitate of BaSO4 in the solution). Stir the
solution again and add some more titrant until it reaches 14.47 ml and 17.37 ml
respectively(10% more of the calculated volume of titrant). Let the precipitate settle in the
solution.
4. Repeat the above testing until precipitation is complete. Leave the stirring rod in the beaker
and covered with a watch glass. The precipitate formed is very finely divided, so the
solutions must be digested. The solutions can be effectively digested by heating them for 30
minutes. If the water level becomes too low, add some more water.
5. Mount the funnel support on a stand.Wash and rinse two funnels.Obtain two discs of
whatman filter paper from the laboratory instructor. A few minutes before the end of the
digestion period, fold the papers and place the papers in the funnels. Moisten with
deionized water until the paper fits the funnel. Place a beaker under each funnel to receive
the filtrate.
6. Filter the solution while hot slowly. Use a stirring rod while transferring. Rinse with hot
distilled water the stirring rod and beaker six times and add the rinse water to the
funnel.Wash the precipitate with hot distilled water until no turbidity in the filtrate appears.
The precipitate must be washed free of any BaCl2 it might contain.
7. While precipitating the BaSO4 ,some of the members must bring the crucibles to constant
mass with the use of heating, cooling and weighing again and again until a consistent weight
appears. The crucibles must be set aside in the dessicator while the experiment is ongoing.
After the digestion period, the filter paper must be placed in a sealed manner inside the
crucible and must be covered tightly. Heat the crucible vigorously on top of the burner for
10 minutes until moisture is driven off and the paper begins to char. Once the paper has
been completely charred, the crucible should be heated with the most intense flame the
burner can produce. Continue to heat until all of the carbon has been oxidized.
8. Allow the analyte to cool. Moisten it with 0.07M sulfuric acid and heat it again for 15
minutes to remove the acid. Place the crucible inside the dessicator and let it cool down.
Heat it again and do the same procedure of heating and drying repeatedly until the weights
are consistent.
IV. Calculations
a. ml of BaCl2 (BaCl2 and FeSO4 has 1:1 ratio)
0.2𝑚𝑜𝑙 1000 𝑚𝑚𝑜𝑙 𝑚𝑙
0.5g FeSO4( 152𝑔
) ( 1𝑚𝑜𝑙 ) (0.25 𝑚𝑚𝑜𝑙) = 13.5789𝑚𝑙 + 10% more = 14.47 ml
0.2𝑚𝑜𝑙 1000 𝑚𝑚𝑜𝑙 𝑚𝑙
0.6g FeSO4( )( )( ) = 15.789𝑚𝑙 +10% more =14.37 ml
152𝑔 1𝑚𝑜𝑙 0.25 𝑚𝑚𝑜𝑙
b. Volume of stock solution of H2SO4
(12M)(V1)=(50ml)(0.07M)
V1= 0.3 ml diluted to 50 ml

V. Assignments

Aidan Kyle Sanglay- prepare the H2SO4 concentration. Perform the titration of the impure
sulfate.Steam bath the solution.

Heddy Suzane Chiong- prepare the BaCl2 concentration. Filter and Wash the precipitate
formed.

Kenneth Sta. Ana- Perform the titration of the impure sulfate #2. Steam bath the solution.

Adrian Navarra- Prepare the crucibles and sample to be used and bring it to constant mass.
Ignite the 2nd analyte.

Donabel Hina –Filter and wash the precipitate formed.Ignite the first analyte and bring it to
constant mass.