CHEM 87L ANALYTICAL CHEMISTRY LABORATORY

Name of Group Members: Section: EA1

Kathrina Krisha Pedarse
Vince Nixau Padel Date Performed: July 6,
2021

Expt. 4 Gravimetric Analysis of Iron Ore

Objectives: Preparation: /10

Data: /50
1.) To determine the mass percent of the Iron Sample Calculations: /10
samples using precipitation gravimetry. Analysis: /20
Conclusion: /10
TOTAL: /100

List of Apparatus:

Porcelain Crucibles

Oven Furnace/ Bunsen Burner

Desiccator

800mL Beaker

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List of Chemicals:

Name / Symbol of Hazards and Risks First Aid / Disposal

Chemical
Ammonia Can result to blindness, lung Dispose in the sink and flush
damage or death. with plenty water.
HCl Corrosive to the eyes, skin and Dilute with water then dispose
mucous membranes. in the sink while flushing it with
water.
Water None None
Bromine Water Skin irritation and possible Add sodium thiosulphate
burns solution in small portions and
dispose inn the sink after
solution becomes colourless.
Ferric Hydroxide Skin Irritation and eye irritation In case of skin contact wash
with soap and water. If irritation
occurs, consult physician.
HNO3 Extremely corrosive Small amounts can be washed
down in sinks as long as rinsed
with a large amount of water.
AgNO3 Can cause trouble in Breathing Dissolve or mix the material
and death with a combustible solvent and
burn in a chemical incinerator
equipped with an afterburner
and scrubber.
Fe2O3 Can cause metal fume fever Handle in an enclosed,
and eye discoloration. controlled process.

Data and Observations:

Mass Readings
Crucible Number 59 72
Mass reading 1 (empty), g 34.1115 39.0821
Mass reading 2 (empty), g 34.1114 39.0822
Average mass reading (empty), g 34.1115 39.0822
Mass reading 1 (w/ residue), g 34.2243 39.1994
Mass reading 2 (w/ residue), g 34.2242 39.1995
Average mass reading (w/ residue), g 34.2243 39.1995

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Observations table
Conditions/Reagents
Observation
Added
10 mL 6M HCl and 50 mL
The solution is transparent on
water added to the sample
both trials
ore
Mixture is heated at 80 Sample is dissolved but no color
degrees Celsius change
The mixture is turned to yellow-
Bromine-Water is added
orange on both trials
The mixture is still yellow orange
Diluting the mixture
but its color is paler

The mixture is turning brown

Adding the 6M ammonia
while adding the ammonia

There is a dark red precipitate at

Staying the mixture still
the bottom

Dissolving the precipitate The mixture turns to light yellow-

with hot 6M HCl orange

Diluting the mixture The mixture is with pale color

After boiling the mixture is

Heating the mixture
yellow

The mixture is turning brown

Adding the 6M ammonia
while adding the ammonia

Results Table
Trial 1 2
Mass of ore sample, g 0.5030 0.5013
Crucible no. 59 72
Average mass of crucible, empty, g 34.1115 39.0822
Average mass of crucible, w/ residue,
g 34.2243 39.1995
Mass of residue, g 0.1128 0.1173
% Fe by mass of sample ore 15.67% 16.37%
Average Fe by mass of sample ore 16.03%
Standard Deviation 0.48
RSD 3.01%

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Sample calculations:
Mass residue 34.2243 − 34.1115 = 0.1128 𝑔

𝑔
55.85 𝐹𝑒 (2)
0.1128 𝑔 𝑟𝑒𝑠𝑖𝑑𝑢𝑒 ( 𝑚𝑜𝑙 )
𝑔
159.69
%𝐹𝑒 𝑏𝑦 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑜𝑟𝑒: 𝑚𝑜𝑙 × 100 = 𝟏𝟓. 𝟔𝟕%
0.5030 𝑔 𝑠𝑎𝑚𝑝𝑙𝑒 𝑜𝑟𝑒

Analysis:

Gravimetric analysis measures the mass of material formed in the reaction of the analyte with the
reagent. The results also shows that there was a residue accumulated throughout the experiment.
This residue is determined as Fe2O3. This experiment aims to determine the %Fe of the Iron
samples using precipitation gravimetry. Results show that after two trials, trial 1 has a %Fe of
15.67% and trial 2 has 16.37%. Observations show that color indicates change all throughout the
experiment. Results show that the average %Fe by mass of sample ore is 16.02%.

Conclusion:

Precipitation gravimetry uses a precipitation reaction to separate one or more parts of a solution
by incorporating it into a solid. An insoluble compound forms when we add a precipitating reagent
to a solution that contains the analyte. To provide an accurate result, a precipitate’s solubility must
be minimal. Other studies conclude that the accuracy of a total analysis technique is 0.01% which
means that precipitate must account for at least 99.9% of the analyte. Solubility losses can be
minimized by controlling the conditions under which the precipitate forms. We therefore conclude
that pH affects solubility after going through the experiment. At more acidic pH levels, the solubility
of a substance increases because of the contribution of reaction. We also conclude that
precipitate has low solubility and that it should be freed from impurities such as inclusion,
occlusion and surface adsorbates to avoid a determinate error before we determine the
precipitate’s mass.

References:

Precipitation Gravimetry. (2021, July 1). Retrieved from

https://chem.libretexts.org/@go/page/163.

E.J. Bogan. Inorganic Gravimetric and Volumetric Analysis. Anal. Chem. 1958, 30(4), 805-822.

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Porcelain Crucibles
• Heat in an oven furnace or to a
full heat Bunsen Burner.
• Cool to some extent in air and
then completely in a desiccator
• Weigh
• Repeat process until constant
weight is obtained (0.0005g or
0.5mg)

800mL Beakers

Procedure 1:
Procedure 2
• Prepare 250mL 6M ammonia. Weigh to nearest
0.1mg and duplicate samples of about 0.5g • Allow filter paper to drain thoroughly, fold over the
each. edges, transfer to a previously weighed crucible.
Preferably with the mouth of the paper cone
• Add 10mL of 6M HCl and 50mL of water. Warm
toward the bottom of the crucible.
until salt is dissolved.
• Heat crucible in the furnace to constant weight
• Heat to about 80°C
that is usually less than 0.5mg.
• Add saturated bromine water as indicated by a
• Calculate the weight of Fe2 O3 . Calculate the
yellow orange color solution and persistent
percentage of Iron or iron compounds in the
bromine odor.
sample.
• Dilute to about 300mL. Heat nearly to boiling
point. Add 6M ammonia very slowly nd stir
constantly.
• Allow reddish precipitate of ferric hydroxide to
coagulate and settle.
• Don’t delay. Decant the hot liquid solution
through an ordinary coarse filter paper into
another beaker.
• Wash precipitate by decanting in little portions at
a time a total of 50mL hot water.
• Dissolve precipitate from filter paper with hot 6M
HCl. Use little as possible and collect solution in
the beaker.
• Examine paper and make sure all ferric
hydroxide has been removed.
• Dilute to 200mL. Heat near to boiling point.
Precipitate Fe with ammonia and allow the
precipitate to settle.
• Filter with ashless filter paper with no delay.
• Collect filtrate with the original beaker containing
the first filtrate.
• Wash twice by decantation with hot water.
• Wipe beaker with a small piece of dry ashless
filter paper to remove last traces of precipitate
and add the filter paper to the precipitate in the
funnel.
• Wash the precipitate on the paper thoroughly
with hot water until 3mL of the washings acidified
with HNO3 show not moe than a faint turbidity
when tested with AgNO3 .

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