Analytical Chemistry Report - Determination of Iron Iii - Gravimetric Analysis Worth
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ScribdTranslationsAnalytical Chemistry Report - Determination of Iron Iii - Gravimetric Analysis Worth
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ScribdTranslationsFEDERAL INSTITUTE OF EDUCATION, SCIENCE AND TECHNOLOGY
FROM CEARÁ
DEPARTMENT OF CHEMISTRY AND ENVIRONMENT - CAMPUS
FORTRESS
Course in Chemical Process Technology
JACKSON A. SENA RIBEIRO
VANDERSON ARAÚJO
FHILLIPE TORRES
VALMIR CARNEIRO NETO
DANIEL RUBENS
MILTON A. LEITE DE ANDRADE
DETERMINATION OF IRON III – GRAVIMETRIC ANALYSIS
FORTALEZA - CEARA
2018
FEDERAL INSTITUTE OF EDUCATION, SCIENCE AND TECHNOLOGY
DO CEARÁ – IFCE CAMPUS FORTALEZA
DISCIPLINE: BASIC ANALYTICAL CHEMISTRY
PROF.: DR. RITA MICKAELA B. DE ANDRADE
ALUNOS: JACKSON A. S. RIBEIRO, VANDERSON ARAÚJO,
FHILLIPE TORRES, VALMIR NETO, DANIEL RUBENS AND MILTON
ANDRADE
DETERMINATION OF IRON III - GRAVIMETRIC ANALYSIS
FORTALEZA - CEARA
2018
SUMMARY
1.INTRODUCTION........................................................................................4
2. OBJECTIVES OF THE EXPERIMENT..........................................................5
3.EXPERIMENTAL PART.......................................................................6
4. RESULTS AND DISCUSSIONS...........................................................8
5. CONCLUSION.........................................................................................11
6.REFERENCES......................................................................................12
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1. INTRODUCTION
A gravimetric analysis consists of a series of operations
essential for determining the quantity of a constituent of a
sample, both by direct weighing of the pure element and by a compound
derived, whose composition and stoichiometry are well defined and known.
This analytical procedure has extensive application in the determination of
components of the sample.
This technique is precise and accurate when using analytical balances.
modern and reliable, it is a very simple procedure to perform and more
easy to control potential sources of errors, equipment is used for
low cost for the execution of this type of analysis. The largest of its
disadvantages is the long amount of time needed for the
completion of the procedure.
The separation of the element can be carried out in three ways:
precipitation, volatilization, extraction or electrodeposition.
In gravimetry by chemical precipitation, the element to be determined is
isolated through the addition of a reagent capable of causing the formation of a
slightly soluble substance (precipitating reagent).
The precipitates are divided into: gradually crystalline precipitate,
finely crystalline precipitate, coagulated precipitate, and gelatinous precipitate
what type was formed in practice, this type of precipitate is formed from
of the flocculation of hydrophilic colloids. They are bulky and may present some
problems in filtration. Some examples of this type of precipitate are:
Iron(III) hydroxide3Bi(OH)3.
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2. OBJECTIVE OF THE EXPERIMENT
The objective of the experiment was the quantification of Fe (III) in a salt of
iron.
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3. MATERIALS AND METHODS
3.1. MATERIALS USED
Beaker (400 mL);
Spatula;
Metal clip (scissors);
Filter paper;
Glass rod;
Porcelain crucible;
Pipette (2 mL).
3.2. REGENTS AND SOLUTIONS USED
Iron salt;
Concentrated hydrochloric acid (HCl);
Distilled water;
Ammonium Nitrate (NH)4NO3);
Ammonium Hydroxide (NH4OH) 1:3;
Hydrogen Peroxide (H2O23%;
NH4NO3a 1% (with drops of NH)3OH).
3.3. EXPERIMENTAL PROCEDURE
1. 1.0g of iron salt was weighed and diluted in diluted hydrochloric acid.
In a 400 mL beaker, 300 mL of distilled water was diluted and added
2 mL of concentrated HCl and 1 mL to 2 mL of a peroxide solution
hydrogen (H2O23%.
The resulting solution was heated to about 300ºC and soon after having
heavy 3g of Ammonium Nitrate (NH4NO3), the resulting solution was added.
3. The system was brought close to boiling and slowly added,
under agitation, the precipitating agent ammonium hydroxide (NH4OH 1:3) up to a
high supersaturation, characterized by the odor of the vapor over the system.
It heated up for a few minutes (due to the irregular heating of the plate and in
next, we waited for the precipitate to settle.
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4. The solution was filtered, brought to the beaker, and the precipitate with a
hot solution of NH4NO3a 1%, containing some drops of NH4OH for
ensure that the solution is alkaline.
5. The filter paper with the precipitate was placed in a porcelain crucible.
and the hydroxide was calcined in a muffled furnace at a temperature above 800°C for 30
minutes, after this time, the crucible is removed from the mold and cooled in
desicador for 1 hour, and then weighed.
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4. RESULTS AND DISCUSSIONS
Table 1 shows the mass of the crucible along with the measured mass.
of the precipitate.
Mass do Mass of the set Mass of the ppt in Mass of Faith
foundry in in grams grams
grams
48.8876 g 49.1518 g 0.2642 g 0.01849g
The oxidation of iron is a natural process and occurs slowly through the
exposure of this element to air according to the reaction:
4Fe2++ O2+ 4H+ ⇄ 4Fe3++ 2H2O
A rapid oxidation can be carried out by hydrochloric acid and nitrate.
of ammonia according to the reaction:
Fe2++ 2NH4NO3+ 8HCl⇄ Fe3++ 2NOCl(g)+ 6Cl- + 4H2O
So that the iron would be more susceptible to reaction with the reagents
added to the solution was heated after their addition, as for the
most solid substances, the heat required to separate the
solute molecules é greater than o heat released by
dissolution of the solute. According to Le Chatelier's principle, the
solubility of such substances increases with temperature.
Ammonium hydroxide (NH) was added.4OH 1:3) the solution. Ammonia
Ammoniaé a colorless gas, quite toxic, that dissolves well in
water. Once in an aqueous medium, ammonia forms ammonium hydroxide
(NH4OH):
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NH3+H2The⇄ NH4++OH-
Solutions and ammonia in contact with Fe+3 ions produce a
gelatinous precipitate (colloids), reddish-brown, of Iron Hydroxide
III, Fe(OH)3, insoluble:
Fe(H2O)63++ 3NH3+H2O⇄ Fe(H2O)3(OH)3↓ + 3NH4+
The colloidal state of matter is defined by a specific magnitude.
of particles, as a consequence of which certain characteristic properties
become apparent. Colloidal properties are usually evidenced
in substances whose particles range between 0.2 x 10-6m e 5.10-9The Role
common filter retains particles up to a diameter of 10-20.10-6in such a way that
colloidal solutions, like true solutions, pass
through a filter paper. The new heating and consequently the
the increase in temperature caused the colloids to transform into
crystalline structures. These are more favorable for analysis purposes.
gravimetric, as they are denser and settle quickly, facilitating the
filtration and washing process.
To get rid of the present contaminations, during the filtration, it was
washed using ammonium nitrate (NH)4NO3) containing
some drops of NH4OH to ensure that the medium remains alkaline, a
since ammonium nitrate dissolves contaminants, but not Fe2(OH)3.
The crucible containing the precipitate was taken to calcination, cooled down.
subsequently and then weighed obtaining a mass of 0.2642 of
Iron Oxide.
A simple rule of three was used to determine the mass of Iron III.
in the sample.
Molar Mass of Fe2O3. = 160 g/mol
Molar mass of Fe = 56X2 = 112 g/mol
160g112g
↔
mol mol
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0.2642g ↔ X g X=0.01849g of Fe
To determine the percentage of Fe present in the sample, a was done
simple calculation.
1 g ↔ 1 0 0 % Y =18.5% of Fe
0.01849g↔Y
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5. CONCLUSION
Gravimetric analysis is easy to perform and yields quite satisfactory results.
reliable, but requires a relatively long time for its
term. The physical characteristics of a precipitate can depend on both the
its nature as well as the conditions under which the precipitate was
formed and evolved.
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6. REFERENCES
Daniel, C. Harris. Quantitative chemical analysis, 6th Ed, Rio de Janeiro,
LTC, 2005.
OHLWEILER. O. A. Quantitative Analytical Chemistry, 3rd edition, Rio de
January, LTC, 1981.
VOGEL. Quantitative Chemical Analysis, 5th edition, Guanabara Publisher
Koogan, Rio de Janeiro, 1992.
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