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Pre-reading

Applied • Introduction to matter and

measurement (matter, separating

Chemistry mixtures)

• Chemical Reactions and Reaction

Stoichiometry (Formula Weights,
Limiting Reactants)

Gravimetry • Reactions in Aqueous Solution

(Precipitation Reactions, Concentration
of Solutions, Solution Stoichiometry)

• Properties of Solutions.

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Understanding
Understanding
Gravimetry
Gravimetry
• Consider, as an analyst, you have been given a
task to determine the total suspended solids in
the water released by a sewage-treatment
facility.
• How about measuring the
moisture content of food?
• N.B. Suspended solids are just that: solid
matter that has yet to settle out of its solution
matrix.
• Lets say you are given an
• How would solve this problem? apple, how would
determine the moisture
• How about if the substance is in the solution, lets content?
say you have been asked to determine the
amount of salt in seawater.

• Can we use filtration?

• How would you go about it?

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Principle of Gravimetry Principle of Gravimetry

• The principle of gravimetric analysis is based on the estimation of the • Typical procedures used in gravimetric analysis include:
mass percent of an ion or substance in an impure compound of known
quantity by determining the mass of the same ion or substance in a pure
compound. • Making a solution with a known amount of the sample analyte.

• In this technique, the amount of an analyte in a sample is determined by • Separation of the desired ion/element/radical in pure forms by various
converting the analyte (ion or substance) to some product of known separation methods.
composition, and measuring the mass of that product formed.
• After the ion has been separated, weigh the amount of the pure
• In order to determine the mass, the product of interest that is formed insoluble compound formed.
needs to be completely isolated.
• Calculating the value of the individual component of interest, based on
• This isolation of ions is done with the help of precipitation or the weight of the compound observed.
vaporisation.

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Gravimetric Analysis Gravimetric Analysis

• Other types of gravimetric analysis methods
• In this chapter we will discuss two types of include.
gravimetric analysis techniques.

• Electrogravimetry: Used to quantify

• Precipitation Gravimetry: The analyte is
ions by electrodeposition. The metal are
determined by converting to a precipitate which
can be filtered out of the solution, and
electrodeposited on the electrode, the
measured. difference in the masses of the electrode
• Example: 2l-(aq) + Pb+2 (aq) → Pbl2(s) before and after electrodeposition is
used to quantify the analyte of interest.
• Volatilisation Gravimetry: the analyte is
separated from other constituents of a sample • Thermogravimetry: technique of
by converting it to a gas of known chemical thermal analysis in which changes in
composition. The mass of the gas then serves
as a measure of the analyte concentration. physical and chemical properties of
• Example: CaCO3 (s) → CaO (s) + CO2 (g) substances are measured as a function
of increasing temperature or as a
characteristic of time.

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Precipitation Gravimetry Precipitating Agent

• Precipitation gravimetry is an analytical technique that uses the formation and
mass of a precipitate to determine the mass of an analyte. • An example of a selective reagent is AgNO3.

• Reagent + Analyte → Solid Product • The only common ions that it precipitates from an acidic
(collect the precipitate and measure mass)
solution are Cl-, Br-, I-, and SCN-.
• In order to use precipitation Gravimetry, the analyte must selectively react with
a reagent called a precipitating agent, to form a precipitate. • Dimethylglyoxime, is a specific reagent that precipitates
only Ni2+ from alkaline solutions.

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Steps involved in Precipitation Gravimetry Steps involved in Precipitation Gravimetry

• Weigh the sample to be analysed • Dry the precipitate by heating to remove water

• Dissolve the sample in a suitable solvent, eg, water. • Cool the precipitate in a dessicator to prevent the precipitate absorbing
moisture from the air

• Add an excess of the precipitating reagent to precipitate the analyte from

the solution containing the analyte. • After the analyte has been separated and dried, the total amount
• In most of the methods the precipitate is the product of a simple metathesis reaction collected of the amount of the pure insoluble compound formed is
(that is, exchange reaction or double replacement reaction) among the analyte and the weighed.
precipitant; though, any reaction producing a precipitate can potentially serve up as a
gravimetric process.
• The amount of the individual component of interest from the original
substance is then determined based on the weight of the amount of the
• Filter the mixture to separate the precipitate from the solution
insoluble compound observed.

• Wash the precipitate to remove any impurities

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Typical Setup for a gravimetric determination

The set up for the filtration process is shown

in the diagram.

After drying the precipitate, sometimes the

precipitate formed cannot be weighed with D Harris: Page 631
the necessary accuracy in place on the filter
paper; nor can the precipitate be completely
removed from the filter paper in order to
weigh it.

The precipitate can be carefully heated in a

crucible until the filter paper has burned
away; this leaves only the precipitate.

If you use crucible then after the precipitate

is allowed to cool (preferably in a desiccator
to keep it from absorbing moisture), it is
weighed (in the crucible).

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Precipitating Reagents
• The diagram above shows typical inorganic ions that are analyzed by
gravimetric methods.
D Harris: Page 630

• It is important to note the stoichiometric relationship between the

species analyzed and the form weighed.

• For example, in the analysis of PO4-3 , it is precipitated as

Mg(NH4)PO4.6 H2O but weighed as Mg2P2O7

It is also important to note that the form that the product to be weighed is not always
what was precipitated, because heating or drying may alter the product.

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Precipitation Gravimetry Precipitation Gravimetry

• Not every substance that form a precipitate can be determined using this • Not every substance that form a precipitate can be determined using this
method. method.

• Ideal Precipitate: • Ideal Precipitate:

• sufficiently low solubility that no significant loss of the analyte occurs during • sufficiently low solubility that no significant loss of the analyte occurs during
filtration and washing; filtration and washing;
• Easily filtered and washed free of contaminants; (i.e., large crystals) • Easily filtered and washed free of contaminants; (i.e., large crystals)
• Should be stable (unreactive with constituents of the atmosphere) • Should be stable (unreactive with constituents of the atmosphere)
• Should have a known and constant composition • Should have a known and constant composition

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Precipitation Gravimetry The Solubility Product

• Consider the dissolution of BaSO 4 in water to form the respective ions .
• BaSO4 (s) ⇌ Ba2+ (aq) + SO42- (aq) Ksp = 1.5 x 10-9
• To provide an accurate result, a precipitate’s solubility must be
minimal to avoid analyte loss.
• Ksp = [Ba 2+][SO 42-]

• This will ensure that the precipitate’s solubility will not limit the • The solubility of BaSO 4 = [Ba 2+] = [SO 42-] = S BaSO4
accuracy of a gravimetric analysis.
• The conditions that affect this equilibrium will affect the solubility of BaSO 4.

• To achieve this, we therefore need to understand and try to control the

conditions under which the precipitate forms.

Solubility vs.
Solubility vs. Com m on Ion Solubility vs.
pH
Effect Tem perature

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pH Dependence of Solubility
pH Dependence of Solubility
• pH is an important parameter that may affect a precipitate’s solubility.
• For example, a hydroxide precipitate, such as Fe(OH)3 , will be more
soluble at lower pH levels where the concentration of OH is small.

• Fe(OH)3 ⇌ Fe 3+(aq) + OH - (aq)

• Consider the effect of adding an acid e.g. HCl(aq) on the solubility of

Fe(OH)3(s).

• H 3O + (aq) + OH - (aq) ⇌ H 2O (l)

• How will this affect the above reaction?

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Equilibrium Considerations Equilibrium Considerations

• Consider the dissolution of AgCl in water to form the respective ions .

• AgCl (s) ⇌ Ag + (aq) + Cl- (aq) Ksp = 1.8 x 10 -10

• Ksp = [Ag +][Cl-]

• The solubility of AgCl(s) = [Ag +] = [Cl-] = S AgCl

The formation of AgCl(aq) from AgCl(s)
is called AgCl’s intrinsic solubility.

As the concentration Cl- increases, the solubility of AgCl starts increasing

In the precipitation of AgCl, this equation suggests that we can as the higher-order soluble complexes of AgCl2− and AgCl32- are the
minimize solubility losses by adding a large excess of Cl . predominate species in solution.

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Precipitation Gravimetry Particle Size of the Precipitate

• Precipitates consisting of large particles are generally desirable for
• Not every substance that form a precipitate can be determined using this gravimetric work because they are easy to filter and wash free of
method. impurities.

• Ideal Precipitate: • In addition, precipitates of this type are usually purer than are precipitates
• sufficiently low solubility that no significant loss of the analyte occurs during made up of fine particles
filtration and washing;
• Easily filtered and washed free of contaminants; (i.e., large crystals)
• Should be stable (unreactive with constituents of the atmosphere) • Small particles can clog the filters and also can pass through filters.
• Should have a known and constant composition

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Particle Size of the Precipitate Mechanism of precipitation formation

• Can we control the particle sizes of the precipitates formed?
• At one extreme are colloidal suspensions, tiny particles are invisible to
the naked eye (10 -7 to 10 -4 cm in diameter).
• Yes its possible, but that needs understanding that favor the formation of
each of the two particle types.
• Colloidal particles show no tendency to settle from solution and are difficult
to filter.
• Therefore, by controlling the reaction conditions we can significantly
increase a precipitate’s average particle size.
• At the other extreme are particles with dimensions on the order of tenths of
a millimeter or greater – Crystalline Suspensions.

• The particles of a crystalline suspension tend to settle spontaneously and

are easily filtered.

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Mechanism of precipitation formation Mechanism of precipitation formation

• The mechanism of precipitation is not well understood.
• The formation of a precipitate consists of two distinct events:
• nucleation, the initial formation of smaller, stable particles of the precipitate • But research has shown that the particle size of a precipitate is influenced by
when ions, atoms or molecules come together (~4-5). Process often starts on precipitate solubility, temperature, reactant concentrations, and the rate at
the surface of suspended contaminants such as dust particles. which reactants are mixed.

• and particle growth (growth of existing nuclei formed by the nucleation

process). • To account for the factors, we assume that the particle size is related to a
single property of the system called relative supersaturation.

• Further precipitation is governed by the competition between these two

processes.

where Q is the solute’s actual concentration and S is the solute’s concentration at

• Larger particles form when the rate of particle growth exceeds the rate of equilibrium.
nucleation.

• Understanding the conditions that favor particle growth is important when

we design a gravimetric method of analysis.

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Mechanism of precipitation formation Mechanism of precipitation formation

• The numerator of equation , Q – S, is a measure of the solute’s

supersaturation. • Based on the given information, it can be deduced that this equation
predicts that we can minimize the Relative Supersaturation:
• A solution with a large, positive value of RSS has a high rate of nucleation and • If we decrease the solute’s concentration, Q, or
produces a precipitate with many small particles. • if we increase the precipitate’s solubility, S.

• When the RSS is small, precipitation is more likely to occur by particle growth • A precipitate’s solubility usually increases at higher temperatures and
than by nucleation. adjusting pH may affect a precipitate’s solubility if it contains an acidic or a
basic ion.

• Temperature and pH, therefore, are useful ways to increase the value of S.
•
• Forming the precipitate in a dilute solution of analyte or adding the
precipitant slowly and with vigorous stirring are ways to decrease the value
of Q.

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Mechanism of precipitation formation

Homogeneous Precipitation
• There are practical limits to minimizing RSS.
• Homogeneous Precipitation: the slow generation of the precipitation
reagent by a chemical reaction in situ in low concentrations which
• Some precipitates, such as Fe(OH)3 and PbS, are so insoluble that S is produces purer and larger crystals of the precipitate.
very small and a large RSS is unavoidable.
• For example, if OH - is the precipitating reagent, it might be prepared
• Such solutes inevitably form small particles. homogeneously by the hydrolysis of urea:

(NH 2)2CO + H 2O ® CO 2 + 2 NH 4+ + 2 OH -
• One solution to the challenge is to generate the precipitant in situ as the
product of a slow chemical reaction.
• Another example is the homogeneous generation of the hydrogen sulfide
by the hydrolysis of thioacetamide.
• By using an example, explain how this can be achieved.
•
CH 3(CS)NH 2 + H 2O ® CH 3(CO)NH 2 + H 2S(g)

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Impurities in Precipitates
Coagulation/Agglomeration of Precipitates (Coprecipitation)
• Another approach to increasing the size of the precipitate particles into • Coprecipitation occurs when substances which are normally soluble
larger particles that are easier to filter is by coagulation/agglomeration of are carried out of solution by precipitate.
the colloidal particles.

• There are four types of coprecipitation:

• Coagulation can be induced in three ways:
• surface adsorption,
• by heating,
• mixed-crystal formation,
• by stirring, and
• occlusion,
• by adding an electrolyte to the medium.
• mechanical entrapment.

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Impurities in Precipitates Impurities in Precipitates

(Coprecipitation) (Coprecipitation)
• There are four types of coprecipitation:
• There are four types of coprecipitation:
• surface adsorption,
• surface adsorption,
• mixed-crystal formation,
• mixed-crystal formation,
• occlusion,
• occlusion,
• mechanical entrapment.
• mechanical entrapment.
• Surface adsorption always results in positive errors in gravimetric
procedures.
• This happens when one of the in the crystal lattice of a solid is replaced
by an ion of another element (happens when the two ions have the same
• The net effect of surface adsorption is therefore the carrying down of an charge and that their sizes differ by no more than about 5%).
otherwise soluble compound as a surface contaminant, and is a major
contaminant for colloidal suspensions.
• The interfering ion may have to be separated before the final precipitation
step.
• Adsorbed Impurities on colloids can be minimized by
• coagulated colloids is improved by digestion
• Washing a coagulated colloid containing a volatile electrolyte
• Reprecipitation
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Impurities in Precipitates Impurities in Precipitates

(Coprecipitation) (Coprecipitation)
• There are four types of coprecipitation:
• surface adsorption, • There are four types of coprecipitation:
• surface adsorption,
• mixed-crystal formation,
• mixed-crystal formation,
• occlusion,
• occlusion,
• mechanical entrapment.
• mechanical entrapment.
• occurs when a portion of the solution is trapped in tiny pockets created
• type of coprecipitation in which some constituents of the precipitation
as several crystals close to each other grow together, forming larger
medium become trapped within the crystal structure during rapid crystal
growth resulting in positive or negative errors. crystals.

• The trapped materials can be water, analyte ions, precipitating agent ions,
or other constituents in the medium.

• Slow addition of precipitating agent and stirring may avoid occlusion but if
it does occur, dissolution of precipitate and reprecipitation may have to be
done.

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Volatilisation Gravimetry
Digestion • In this method for gravimetric analysis, a sample is thermally or
chemically decomposed, and the resulting change in its mass is
measured.
• Digestion is a process in which a precipitate is heated in the solution
from which it was formed (the mother liquor) and allowed to stand in
contact with the solution. • In other cases, a volatile decomposition product formed is trapped,
and weighed.

• Because the release of a volatile species is an essential part of these

methods, they are classified collectively as volatilization gravimetric
methods of analysis.

• If thermal decomposition is performed on the sample, the change in

the sample mass will be monitored as a function of temperature, this is
a process called thermogravimetry.

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Volatilisation Gravimetry Calculations in Gravimetric

Analysis

• As an example, in order to • How is the mass of the analyte in the original sample
determine the number of moles calculated?
of water of crystallisation present
in a hydrated salt, the sample
would be heated to remove the
water and the difference in mass
can then be used to determine
the amount of water present and
thus the number of moles of
water needed for one mole of the
anhydrous salt.

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Gravimetric Calculations
Gravimetric Calculations
• A 0.825 g sample of an ionic compound containing chloride ions and • A 0.825 g sample of an ionic compound containing chloride ions and an unknown
metal is dissolved in water and treated with excess silver nitrate. If 1.725 g of AgCl
an unknown metal is dissolved in water and treated with excess silver precipitate forms, what is the percent by mass of Cl in the original sample?
nitrate. If 1.725 g of AgCl precipitate forms, what is the percent by
mass of Cl in the original sample?
• Steps in solution:
• Find the % of Cl in AgCl
• Multiply the % of Cl by the mass of the precipitate to obtain the Cl in the sample
• Divide the mass of Cl in sample by total mass of sample (multiply by 100%)

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Gravimetric Calculations Gravimetric Calculations

• Example 1: First Approach
• Example 1: Second Approach
• What is the %KCl in a solid if 5.1367 g of solid gives rise to 0.8246 g AgCl?
• What is the %KCl in a solid if 5.1367 g of solid gives rise to 0.8246 g AgCl?
• Cl- + Ag+ è AgCl(s)
• Cl- + Ag+ è AgCl(s)

• KCl(s) è K +(aq) + Cl- (aq)

• KCl(s) è K +(aq) + Cl- (aq)
• Cl- + Ag + è AgCl(s)
• Cl- + Ag + è AgCl(s)

• n KCl = n Cl- = n AgCl = 0.8246 g AgCl/143.32 g.mol-1 = 5.754 x 10 -3 mols.

• % composition of Cl in AgCl = m Cl/m AgCl x 100% = 35.453/143.32g X 100% =
24.73%.
• Mass of KCl in solid = 5.754 x 10 -3 mols x 74.5513 g.mol-1 = 0.4289 g. • Mass of Cl in 0.8246 g of AgCl = 0.2473 x 0.8246g = 0.2040 g.

• 0.4289g / 5.1367 X 100% = 8.36%. • % composition of Cl in KCl = m Cl/m KCl x 100% = 35.453/74.5513g X 100% =
47.56%.

• Mass of KCl in solid = mcl/%composition X 100% = 0.4289 g.

• 0.4289g / 5.1367 X 100% = 8.36%.

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Gravimetric Calculations
• Example 2: A sample of impure pyrite, FeS 2, weighs 0.5080 g. After the sample has
been decomposed and dissolved, a precipitate of 1.561 g of BaSO 4 is obtained.
Calculate the percentage of S in the sample.
• 2Fe(OH)3 è Fe 2O 3 + ..
• We can use same approaches in previous example: 2 : 1
• n BaSO4 = 1.561 g/ 233.38 g.mol-1 = 6.689 x 10 -3 mols.
• nFe 2O 3 = 0.8525 g/ 159.69 g.mol-1 = 0.005338 moles
• Mole ratio:
• FeS 2 è Fe + 2BaSO 4
1 2 • Moles of Fe(OH)3 = 2 x nFe 2O 3 = 0.01068 moles

• n FeS2 = 1/2 x n BaSO4 = 0.003345 moles.

• Mass of FeS 2 = nM = 0.003345 x 119.98 = 0.4012 g. • 3Fe(OH)3 : Fe 3O 4 = 1/3 x n Fe(OH)3 = 1/3 x 0.01068 moles = 0.003559 moles.
3 : 1
• % composition of S in FeS 2 = 53.45% (0.2144 g S in the sample). 42.21%

• Mass of Fe 3O 4 in sample = 0.003559 moles x 231.533 g.mol-1 = 0.8239 g.

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Gravimetric Factors

• 2Fe(OH)3 è Fe2O3 + ..
2 : 1
• nFe2O3 = 0.8525 g/ 159.69 g.mol-1 = 0.005338 moles

• Moles of Fe(OH)3 = 2 x nFe2O3 = 0.01068 moles

• 3Fe(OH)3 : Fe3O4 = 1/3 x n Fe(OH)3 = 1/3 x 0.01068 moles = 0.003559 moles.

3 : 1

• Mass of Fe3O4 in sample = 0.003559 moles x 231.533 g.mol-1 = 0.8239 g.

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Gravimetric Factors

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• GF = 2 (MM Fe3O4) / (3 MM Fe2O3)

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Example
461.917
115.11
Example
• Tutorial: Question Number 2

3. Nitrobenzene, C 6H 5NO 2, is quantitatively reduced to aniline, C 6H 5NH 2, with metallic

• The nitrogen in a 0.5000 g sample of organic material is converted to tin:
NH 4HSO 4 by digestion with concentrated H 2SO 4. If the ammonium
ions are precipitated as (NH 4)3PtCl6 and the precipitate is ignited to Pt
that weighs 0.1756 g, what is the percentage of N in the sample?
•3Sn(s) + 2C 6H 5NO 2 + 12H + → 2 C 6H 5NH 2 + 4H 2O + 3Sn 4+

Molar Mass = 3(Mass N) + 12 (Mass H) + Mass Pt + 6(Mass Cl) =

• A 0.5078 g sample of impure nitrobenzene was treated with 1.044 g of tin. When
the reaction was complete, the residual tin was found to weigh 0.338 g. Calculate

the percentage nitrobenzene in the sample.

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Example Example
3.If the Fe in the solution has been precipitated as Fe(OH)3 and ignited to Fe 2O 3,
what weight of ignited precipitate would have been obtained?
1.A 2.00g sample of limestone was dissolved in hydrochloric acid and all the calcium
present in the sample was converted to Ca 2+(aq).
• Excess ammonium oxalate solution, (NH 4)2C 2O 4(aq), was added to the solution to
4.What mass of AgI can be produced from a 0.512 g sample that assays 20.1% AlI3?
precipitate the calcium ions as calcium oxalate, CaC 2O 4(s).
• The precipitate was filtered, dried and weighed to a constant mass of 2.43g.
• Determine the percentage by mass of calcium in the limestone sample. 5.How many grams of CO 2 are evolved from a 1.500 g sample that is 38.0%
Pb(CO 3)2 and 42% K 2CO 3 by mass?

6.A 0.8720 g sample of a mixture consisting only of magnesium bromide and

potassium chloride yields 1.505 g of silver bromide. What are the percentages of
the two salts in the sample?

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Applications of Gravimetry Applications of Gravimetry

• Uses of gravimetric analysis in quality control • Inorganic Analysis
• Measurement of the “essential” elements in plant foods (phosphorus, for example, is • Determining the inorganic ash content of an organic material, such as a
converted into the insoluble salt, magnesium ammonium phosphate) polymer
• Estimation of pollutants in the air, such as sulphur dioxide (by conversion to insoluble • determination of dissolved solids in natural waters and wastewaters
barium sulphate) • ` Moisture content determination
• Determination of silica in waters, wastewaters, and rocks.
• Estimation of sulphur dioxide (used to prevent microbial spoilage) in soft drinks, such as
orange juice.
• Estimation of chloride ions in water supplies (by conversion to insoluble silver chloride).

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Applications of Gravimetry
Total, Suspended and Dissolved Solids
• A simple application of gravimetry in environmental analysis is the determination of total,
suspended and dissolved solids in water.
• Organic Analysis
• Total Dissolved Solids (TDS) describes to the solid particles that can pass through a 2-
• elemental analysis of organic materials for the mass of carbon and hydrogen in the sample. micron filter.
• Determination of alkaline metals and earths in organic materials.
• The solids in a liquid that cannot pass through this filter, i.e. the larger particles, are
• Determination of biomass in waters and wastewaters. described as suspended solids.
• Particles that are even larger are known as settleable solids.
• Total solids (TS) is the sum of both the total suspended solids (TSS) and total dissolved
solids (TDS) in the process of water: TS = TSS + TDS.
• TSS and TDS measure the amount of particulate matter (tiny pieces of things) floating in
water.
• In lakes and rivers this can include particles from algae, other organic matter, silt and
clay, and other inorganic substances (such as minerals, salts and metals).

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Total, Suspended and Dissolved Solids

Total, Suspended and Dissolved Solids
• Total suspended solids (TSS) values are often related to the turbidity (cloudiness) of water. • Total dissolved solids (TDS) include dissolved minerals and salts in the water.
• If TSS is high and the water is murky then light from the sun will not travel well through the
water, making it difficult for plants and algae to grow. • As a result, TDS is often closely related to conductivity, salinity, alkalinity, and hardness
• This, in turn, can reduce productivity (the amount of plant and animal life that a river or lake measures.
can support) and oxygen generation.
• Lots of soil and silt in the water can also clog fish gills and, if it settles to the bottom, bury fish • Most freshwater fish and bugs cannot tolerate high TDS because they are not adapted to
eggs. saline (salty) water, like marine fish are.

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Extra Practice Problems

• A mixture containing only FeCl3 (FW = 162.2) and AlCl3 (FW = 133.34) weighs 5.95 g.
The chlorides are converted to hydroxides and ignited to Fe2O 3 (FW = 159.7) and
Al2O 3 (FW = 101.96). The oxide mixture weighs 2.62 g. Calculate the percentage Fe
(at wt = 55.85) and Al (at wt = 26.98) in the sample.

• Solution:
• % Fe = (1.07/5.95) x 100 = 18.0%
• % Al = (0.58/5.95) x 100 = 9.8%

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