Precipitation Gravimetry

1/29/2015
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ChemWiki: The Dynamic Chemistry E-textbook > Analytical Chemistry > Analytical Chemistry 2.0 > 8: Gravimetric Methods > 8B: Precipitation
Gravimetry
8B: Precipitation Gravimetry
In precipitation gravimetry an insoluble compound forms when we add a precipitating reagent, or precipitant, to a solution containing our analyte. In
most methods the precipitate is the product of a simple metathesis reaction between the analyte and the precipitant; however, any reaction generating
a precipitate can potentially serve as a gravimetric method.
Most precipitation gravimetric methods were developed in the nineteenth century, or earlier, often for the analysis of ores. Figure 1.1 in Chapter 1,
for example, illustrates a precipitation gravimetric method for the analysis of nickel in ores.
8B.1 Theory and Practice

All precipitation gravimetric analysis share two important attributes. First, the precipitate must be of low solubility, of high purity, and of known
composition if its mass is to accurately reflect the analytes mass. Second, the precipitate must be easy to separate from the reaction mixture.
Solubility Considerations
To provide accurate results, a precipitates solubility must be minimal. The accuracy of a total analysis technique typically is better than 0.1%,
which means that the precipitate must account for at least 99.9% of the analyte. Extending this requirement to 99.99% ensures that the precipitates
solubility does not limit the accuracy of a gravimetric analysis.
A total analysis technique is one in which the analytical signalmass in this caseis proportional to the absolute amount of analyte in the sample.
See Chapter 3 for a discussion of the difference between total analysis techniques and concentration techniques.
We can minimize solubility losses by carefully controlling the conditions under which the precipitate forms. This, in turn, requires that we account
for every equilibrium reaction affecting the precipitates solubility. For example, we can determine Ag+ gravimetrically by adding NaCl as a
precipitant, forming a precipitate of AgCl.
If this is the only reaction we consider, then we predict that the precipitates solubility, SAgCl, is given by the following equation.
Equation 8.2 suggests that we can minimize solubility losses by adding a large excess of Cl. In fact, as shown in Figure 8.1, adding a large excess of
Cl increases the precipitates solubility.
http://chemwiki.ucdavis.edu/Analytical_Chemistry/Analytical_Chemistry_2.0/08%3A_Gravimetric_Methods/8B%3A_Precipitation_Gravimetry
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Figure 8.1 Solubility of AgCl as a function of pCl. The dashed red line shows our prediction for SAgCl if we incorrectly assume that only reaction 8.1
and equation 8.2 affect silver chlorides solubility. The solid blue curve is calculated using equation 8.7, which accounts for reaction 8.1 and
reactions 8.38.5. Because the solubility of AgCl spans several orders of magnitude, SAgCl is displayed on the y-axis in logarithmic form.
To understand why the solubility of AgCl is more complicated than the relationship suggested by equation 8.2, we must recognize that Ag+ also
forms a series of soluble silver-chloro metalligand complexes.
The actual solubility of AgCl is the sum of the equilibrium concentrations for all soluble forms of Ag+, as shown by the following equation.
By substituting into equation 8.6 the equilibrium constant expressions for reaction 8.1 and reactions 8.38.5, we can define the solubility of AgCl as
Problem 1 in the end-of-chapter problems asks you to show that equation 8.7 is correct by completing the derivation.
Equation 8.7 explains the solubility curve for AgCl shown in Figure 8.1. As we add NaCl to a solution of Ag+, the solubility of AgCl initially
decreases because of reaction 8.1. Under these conditions, the final three terms in equation 8.7 are small and equation 8.1 is sufficient to describe
AgCls solubility. At higher concentrations of Cl, reaction 8.4 and reaction 8.5 increase the solubility of AgCl. Clearly the equilibrium concentration
of chloride is important if we want to determine the concentration of silver by precipitating AgCl. In particular, we must avoid a large excess of
chloride.
The predominate silver-chloro complexes for different values of pCl are shown by the ladder diagram along the x-axis in Figure 8.1 Note that the
increase in solubility begins when the higher-order soluble complexes, AgCl2 and AgCl32, become the predominate species.
Another important parameter that may affect a precipitates solubility is pH. For example, a hydroxide precipitates such as Fe(OH)3 is more soluble
at lower pH levels where the concentration of OH is small. Because fluoride is a weak base, the solubility of calcium fluoride, SCaF2, also is pHdependent. We can derive an equation for SCaF2 by considering the following equilibrium reactions
and the following equation for the solubility of CaF2.
Be sure that equation 8.10 makes sense to you. Reaction 8.8 tells us that the dissolution of CaF2 produces one mole of Ca2+ for every two moles of
F, which explains the term of 1/2 in equation 8.10. Because F is a weak base, we need to account for both of its chemical forms in solution, which
explains why we include HF.
Substituting the equilibrium constant expressions for reaction 8.8 and reaction 8.9 into equation 8.10 defines the solubility of CaF2 in terms of the
equilibrium concentration of H3O+.
Problem 4 in the end-of-chapter problems asks you to show that equation 8.11 is correct by completing the derivation.
Figure 8.2 shows how pH affects the solubility of CaF2. Depending on the solutions pH, the predominate form of fluoride is either HF or F. When
the pH is greater than 4.17, the predominate species is F and the solubility of CaF2 is independent of pH because only reaction 8.8 occurs to an
appreciable extent. At more acidic pH levels, the solubility of CaF2 increases because of the contribution of reaction 8.9.
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Figure 8.2 Solubility of CaF2 as a function of pH. The solid blue curve is a plot of equation 8.11. The predominate form of fluoride in solution is
shown by the ladder diagram along the x-axis, with the black rectangle showing the region where both HF and F are important species. Note that the
solubility of CaF2 is independent of pH for pH levels greater than 4.17, and that its solubility increases dramatically at lower pH levels where HF is
the predominate species. Because the solubility of CaF2 spans several orders of magnitude, its solubility is shown in logarithmic form.
When solubility is a concern, it may be possible to decrease solubility by using a non-aqueous solvent. A precipitates solubility is generally greater
in an aqueous solution because of waters ability to stabilize ions through solvation. The poorer solvating ability of non-aqueous solvents, even those
which are polar, leads to a smaller solubility product. For example, the Ksp of PbSO4 is 2 108 in H2O and 2.6 1012 in a 50:50 mixture of H2O
and ethanol.
Practice Exercise 8.1

You can use a ladder diagram to predict the conditions for minimizing a precipitates solubility. Draw a
ladder diagram for oxalic acid, H2C2O4, and use it to establish a suitable range of pH values for
minimizing the solubility of CaC2O4. Relevant equilibrium constants may be found in the appendices.
Click here to review your answer to this exercise.
Avoiding Impurities
In addition to having a low solubility, the precipitate must be free from impurities. Because precipitation usually occurs in a solution that is rich in
dissolved solids, the initial precipitate is often impure. We must remove these impurities before determining the precipitates mass.
The greatest source of impurities is the result of chemical and physical interactions occurring at the precipitates surface. A precipitate is generally
crystallineeven if only on a microscopic scalewith a well-defined lattice of cations and anions. Those cations and anions at the precipitates
surface carry, respectively, a positive or a negative charge because they have incomplete coordination spheres. In a precipitate of AgCl, for example,
each silver ion in the precipitates interior is bound to six chloride ions. A silver ion at the surface, however, is bound to no more than five chloride
ions and carries a partial positive charge (Figure 8.3). The presence of these partial charges makes the precipitates surface an active site for the
chemical and physical interactions that produce impurities.
Figure 8.3 Ball-and-stick diagram showing the lattice structure of AgCl. Each silver ion in the lattices interior binds with six chloride ions, and each
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chloride ion in the interior binds with six silver ions. Those ions on the lattices surface or edges bind to fewer than six ions and carry a partial
charge. A silver ion on the surface, for example, carries a partial positive charge. These charges make the surface of a precipitate an active site for
chemical and physical interactions.
One common impurity is an inclusion. A potential interfering ion whose size and charge is similar to a lattice ion, may substitute into the lattice
structure, provided that the interferent precipitates with the same crystal structure (Figure 8.4a). The probability of forming an inclusion is greatest
when the concentration of the interfering ion is substantially greater than the lattice ions concentration. An inclusion does not decrease the amount of
analyte that precipitates, provided that the precipitant is present in sufficient excess. Thus, the precipitates mass is always larger than expected.
Figure 8.4 Three examples of impurities that may form during precipitation. The cubic frame represents the precipitate and the blue marks are
impurities: (a) inclusions, (b) occlusions, and (c) surface adsorbates. Inclusions are randomly distributed throughout the precipitate. Occlusions are
localized within the interior of the precipitate and surface adsorbates are localized on the precipitates exterior. For ease of viewing, in (c) adsorption
is shown on only one surface.
An inclusion is difficult to remove since it is chemically part of the precipitates lattice. The only way to remove an inclusion is through
reprecipitation. After isolating the precipitate from its supernatant solution, we dissolve it by heating in a small portion of a suitable solvent. We
then allow the solution to cool, reforming the precipitate. Because the interferents concentration is less than that in the original solution, the amount
of included material is smaller. We can repeat the process of reprecipitation until the inclusions mass is insignificant. The loss of analyte during
reprecipitation, however, can be a significant source of error.
Suppose that 10% of an interferent forms an inclusion during each precipitation. When we initially form the precipitate, 10% of the original
interferent is present as an inclusion. After the first reprecipitation, 10% of the included interferent remains, which is 1% of the original interferent.
A second reprecipitation decreases the interferent to 0.1% of the original amount.
Occlusions form when interfering ions become trapped within the growing precipitate. Unlike inclusions, which are randomly dispersed within the
precipitate, an occlusion is localized, either along flaws within the precipitates lattice structure or within aggregates of individual precipitate
particles (Figure 8.4b). An occlusion usually increases a precipitates mass; however, the mass is smaller if the occlusion includes the analyte in a
lower molecular weight form than that of the precipitate.
We can minimize occlusions by maintaining the precipitate in equilibrium with its supernatant solution for an extended time. This process is called a
digestion. During digestion, the dynamic nature of the solubilityprecipitation equilibrium, in which the precipitate dissolves and reforms, ensures
that the occlusion is reexposed to the supernatant solution. Because the rates of dissolution and reprecipitation are slow, there is less opportunity for
forming new occlusions.
After precipitation is complete the surface continues to attract ions from solution (Figure 8.4c). These surface adsorbates comprise a third type of
impurity. We can minimize surface adsorption by decreasing the precipitates available surface area. One benefit of digesting a precipitate is that it
increases the average particle size. Because the probability of a particle completely dissolving is inversely proportional to its size, during digestion
larger particles increase in size at the expense of smaller particles. One consequence of forming a smaller number of larger particles is an overall
decrease in the precipitates surface area. We also can remove surface adsorbates by washing the precipitate, although the potential loss of analyte
can not be ignored.
Inclusions, occlusions, and surface adsorbates are examples of coprecipitatesotherwise soluble species that form within the precipitate containing
the analyte. Another type of impurity is an interferent that forms an independent precipitate under the conditions of the analysis. For example, the
precipitation of nickel dimethylglyoxime requires a slightly basic pH. Under these conditions, any Fe3+ in the sample precipitates as Fe(OH)3. In
addition, because most precipitants are rarely selective toward a single analyte, there is always a risk that the precipitant will react with both the
analyte and an interferent.
In addition to forming a precipitate with Ni2+, dimethylglyoxime also forms precipitates with Pd2+ and Pt2+. These cations are potential interferents
in an analysis for nickel.
We can minimize the formation of additional precipitates by carefully controlling solution conditions. If an interferent forms a precipitate that is less
soluble than the analytes precipitate, we can precipitate the interferent and remove it by filtration, leaving the analyte behind in solution.
Alternatively, we can mask the analyte or the interferent to prevent its precipitation.
Both of the above-mentioned approaches are illustrated in Fresenius analytical method for determining Ni in ores containing Pb2+, Cu2+, and Fe3+
(see Figure 1.1 in Chapter 1). Dissolving the ore in the presence of H2SO4 selectively precipitates Pb2+ as PbSO4. Treating the supernatant with H2S
precipitates the Cu2+ as CuS. After removing the CuS by filtration, adding ammonia precipitates Fe3+ as Fe(OH)3. Nickel, which forms a soluble
amine complex, remains in solution.
Controlling Particle Size

Size matters when it comes to forming a precipitate. Larger particles are easier to filter, and, as noted earlier, a smaller surface area means there is
less opportunity for surface adsorbates to form. By carefully controlling the reaction conditions we can significantly increase a precipitates average
particle size.
Precipitation consists of two distinct events: nucleation, the initial formation of smaller stable particles of precipitate, and particle growth. Larger
particles form when the rate of particle growth exceeds the rate of nucleation. Understanding the conditions favoring particle growth is important
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when designing a gravimetric method of analysis.

We define a solutes relative supersaturation, RSS, as
where Q is the solutes actual concentration and S is the solutes concentration at equilibrium.4 The numerator of equation 8.12, Q S, is a measure
of the solutes supersaturation. A solution with a large, positive value of RSS has a high rate of nucleation, producing a precipitate with many small
particles. When the RSS is small, precipitation is more likely to occur by particle growth than by nucleation.
A supersaturated solution is one that contains more dissolved solute than that predicted by equilibrium chemistry. The solution is inherently
unstable and precipitates solute to reach its equilibrium position. How quickly this process occurs depends, in part, on the value of RSS.
Examining equation 8.12 shows that we can minimize RSS by decreasing the solutes concentration, Q, or by increasing the precipitates solubility, S.
A precipitates solubility usually increases at higher temperatures, and adjusting pH may affect a precipitates solubility if it contains an acidic or a
basic ion. Temperature and pH, therefore, are useful ways to increase the value of S. Conducting the precipitation in a dilute solution of analyte, or
adding the precipitant slowly and with vigorous stirring are ways to decrease the value of Q.
There are practical limitations to minimizing RSS. Some precipitates, such as Fe(OH)3 and PbS, are so insoluble that S is very small and a large RSS
is unavoidable. Such solutes inevitably form small particles. In addition, conditions favoring a small RSS may lead to a relatively stable
supersaturated solution that requires a long time to fully precipitate. For example, almost a month is required to form a visible precipitate of BaSO4
under conditions in which the initial RSS is 5.5
A visible precipitate takes longer to form when RSS is small both because there is a slow rate of nucleation and because there is a steady decrease in
RSS as the precipitate forms. One solution to the latter problem is to generate the precipitant in situ as the product of a slow chemical reaction. This
maintains the RSS at an effectively constant level. Because the precipitate forms under conditions of low RSS, initial nucleation produces a small
number of particles. As additional precipitant forms, particle growth supersedes nucleation, resulting in larger precipitate particles. This process is
called homogeneous precipitation.6
Two general methods are used for homogeneous precipitation. If the precipitates solubility is pH-dependent, then we can mix the analyte and the
precipitant under conditions where precipitation does not occur, and then increase or decrease the pH by chemically generating OH or H3O+. For
example, the hydrolysis of urea is a source of OH.
Because the hydrolysis of urea is temperature-dependentit is negligible at room temperaturewe can use temperature to control the rate of
hydrolysis and the rate of precipitate formation. Precipitates of CaC2O4, for example, have been produced by this method. After dissolving the
sample containing Ca2+, the solution is made acidic with HCl before adding a solution of 5% w/v (NH4)2C2O4. Because the solution is acidic, a
precipitate of CaC2O4 does not form. The solution is heated to approximately 50oC and urea is added. After several minutes, a precipitate of CaC2O4
begins to form, with precipitation reaching completion in about 30 min.
In the second method of homogeneous precipitation, the precipitant is generated by a chemical reaction. For example, Pb2+ is precipitated
homogeneously as PbCrO4 by using bromate, BrO3, to oxidize Cr3+ to CrO42.
Figure 8.5 shows the result of preparing PbCrO4 by the direct addition of KCrO4 (Beaker A) and by homogenous precipitation (Beaker B). Both
beakers contain the same amount of PbCrO4. Because the direct addition of KCrO4 leads to rapid precipitation and the formation of smaller particles,
the precipitate remains less settled than the precipitate prepared homogeneously. Note, as well, the difference in the color of the two precipitates.
Figure 8.5 Two precipitates of PbCrO4. In Beaker A, combining 0.1 M Pb(NO3)2 and 0.1 M K2CrO4 forms the precipitate under conditions of high
RSS. The precipitate forms rapidly and consists of very small particles. In Beaker B, heating a solution of 0.1 M Pb(NO3)2, 0.1 M Cr(NO3)3, and 0.1
M KBrO3 slowly oxidizes Cr3+ to CrO42, precipitating PbCrO4 under conditions of low RSS. The precipitate forms slowly and consists of much
larger particles.
The effect of particle size on color is well-known to geologists, who use a streak test to help identify minerals. The color of a bulk mineral and its
color when powdered are often different. Rubbing a mineral across an unglazed porcelain plate leaves behind a small streak of the powdered
mineral. Bulk samples of hematite, Fe2O3, are black in color, but its streak is a familiar rust-red. Crocite, the mineral PbCrO4, is red-orange in
color; its streak is orange-yellow.
A homogeneous precipitation produces large particles of precipitate that are relatively free from impurities. These advantages, however, are offset by
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requiring more time to produce the precipitate and a tendency for the precipitate to deposit as a thin film on the containers walls. The latter problem
is particularly severe for hydroxide precipitates generated using urea.
An additional method for increasing particle size deserves mention. When a precipitates particles are electrically neutral they tend to coagulate into
larger particles that are easier to filter. Surface adsorption of excess lattice ions, however, provides the precipitates particles with a net positive or a
net negative surface charge. Electrostatic repulsion between the particles prevents them from coagulating into larger particles.
Lets use the precipitation of AgCl from a solution of AgNO3 using NaCl as a precipitant to illustrate this effect. Early in the precipitation, when
NaCl is the limiting reagent, excess Ag+ ions chemically adsorb to the AgCl particles, forming a positively charged primary adsorption layer (Figure
8.6a). The solution in contact with this layer contains more inert anions, NO3 in this case, than inert cations, Na+, giving a secondary adsorption
layer with a negative charge that balances the primary adsorption layers positive charge. The solution outside the secondary adsorption layer remains
electrically neutral. Coagulation cannot occur if the secondary adsorption layer is too thick because the individual particles of AgCl are unable to
approach each other closely enough.
Figure 8.6 Two methods for coagulating a precipitate of AgCl. (a) Coagulation does not happen due to the electrostatic repulsion between the two
positively charged particles. (b) Decreasing the charge within the primary adsorption layer, by adding additional NaCl, decreases the electrostatic
repulsion, allowing the particles to coagulate. (c) Adding additional inert ions decreases the thickness of the secondary adsorption layer. Because the
particles can approach each other more closely, they are able to coagulate.
We can induce coagulation in three ways: by decreasing the number of chemically adsorbed Ag+ ions, by increasing the concentration of inert ions,
or by heating the solution. As we add additional NaCl, precipitating more of the excess Ag+, the number of chemically adsorbed silver ions decreases
and coagulation occurs (Figure 8.6b). Adding too much NaCl, however, creates a primary adsorption layer of excess Cl with a loss of coagulation.
The coagulation and decoagulation of AgCl as we add NaCl to a solution of AgNO3 can serve as an endpoint for a titration. See Chapter 9 for
additional details.
A second way to induce coagulation is to add an inert electrolyte, which increases the concentration of ions in the secondary adsorption layer. With
more ions available, the thickness of the secondary absorption layer decreases. Particles of precipitate may now approach each other more closely,
allowing the precipitate to coagulate. The amount of electrolyte needed to cause spontaneous coagulation is called the critical coagulation
concentration.
Heating the solution and precipitate provides a third way to induce coagulation. As the temperature increases, the number of ions in the primary
adsorption layer decreases, lowering the precipitates surface charge. In addition, heating increases the particles kinetic energy, allowing them to
overcome the electrostatic repulsion that prevents coagulation at lower temperatures.
Filtering the Precipitate

After precipitating and digesting the precipitate, we separate it from solution by filtering. The most common filtration method uses filter paper, which
is classified according to its speed, its size, and its ash content on ignition. Speed, or how quickly the supernatant passes through the filter paper, is a
function of the papers pore size. A larger pore allows the supernatant to pass more quickly through the filter paper, but does not retain small particles
of precipitate. Filter paper is rated as fast (retains particles larger than 2025 m), mediumfast (retains particles larger than 16 m), medium (retains
particles larger than 8 m), and slow (retains particles larger than 23 m). The proper choice of filtering speed is important. If the filtering speed is
too fast, we may fail to retain some of the precipitate, causing a negative determinate error. On the other hand, the precipitate may clog the pores if
we use a filter paper that is too slow.
A filter papers size is just its diameter. Filter paper comes in many sizes, including 4.25 cm, 7.0 cm, 11.0 cm, 12.5 cm, 15.0 cm, and 27.0 cm.
Choose a size that fits comfortably into your funnel. For a typical 65-mm long-stem funnel, 11.0 cm and 12.5 cm filter paper are good choices.
Because filter paper is hygroscopic, it is not easy to dry it to a constant weight. When accuracy is important, the filter paper is removed before
determining the precipitates mass. After transferring the precipitate and filter paper to a covered crucible, we heat the crucible to a temperature that
coverts the paper to CO2(g) and H2O(g), a process called ignition.
Igniting a poor quality filter paper leaves behind a residue of inorganic ash. For quantitative work, use a low-ash filter paper. This grade of filter
paper is pretreated with a mixture of HCl and HF to remove inorganic materials. Quantitative filter paper typically has an ash content of less than
0.010% w/w.
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Gravity filtering is accomplished by folding the filter paper into a cone and placing it in a long-stem funnel (Figure 8.7). A seal between the filter
cone and the funnel is formed by dampening the paper with water or supernatant, and pressing the paper to the wall of the funnel. When properly
prepared, the funnels stem fills with the supernatant, increasing the rate of filtration.
Figure 8.7 Preparing a filter paper cone. The filter paper circle in (a) is folded in half (b), and folded in half again (c). The folded filter paper is
parted (d) and a small corner is torn off (e). The filter paper is opened up into a cone and placed in the funnel (f ).
The precipitate is transferred to the filter in several steps. The first step is to decant the majority of the supernatant through the filter paper without
transferring the precipitate (Figure 8.8). This prevents the filter paper from clogging at the beginning of the filtration process. The precipitate is
rinsed while it remains in its beaker, with the rinsings decanted through the filter paper. Finally, the precipitate is transferred onto the filter paper
using a stream of rinse solution. Any precipitate clinging to the walls of the beaker is transferred using a rubber policeman (a flexible rubber spatula
attached to the end of a glass stirring rod).
Figure 8.8 Proper procedure for transferring the supernatant to the filter paper cone.
An alternative method for filtering a precipitate is a filtering crucible. The most common is a fritted-glass crucible containing a porous glass disk
filter. Fritted-glass crucibles are classified by their porosity: coarse (retaining particles larger than 4060 m), medium (retaining particles greater
than 1015 m), and fine (retaining particles greater than 45.5 m). Another type of filtering crucible is the Gooch crucible, which is a porcelain
crucible with a perforated bottom. A glass fiber mat is placed in the crucible to retain the precipitate. For both types of crucibles, the precipitate is
transferred in the same manner described earlier for filter paper. Instead of using gravity, the supernatant is drawn through the crucible with the
assistance of suction from a vacuum aspirator or pump (Figure 8.9).
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Figure 8.9 Procedure for filtering a precipitate through a filtering crucible. The trap prevents water from an aspirator from back-washing into the
suction flask.
Rinsing the Precipitate

Because the supernatant is rich with dissolved inert ions, we must remove any residual traces of supernatant to avoid a positive determinate error
without incurring solubility losses. In many cases this simply involves the use of cold solvents or rinse solutions containing organic solvents such as
ethanol. The pH of the rinse solution is critical if the precipitate contains an acidic or basic ion. When coagulation plays an important role in
determining particle size, adding a volatile inert electrolyte to the rinse solution prevents the precipitate from reverting into smaller particles that
might pass through the filter. This process of reverting to smaller particles is called peptization. The volatile electrolyte is removed when drying the
precipitate.
In general, we can minimize the loss of analyte by using several small portions of rinse solution instead of a single large volume. Testing the used
rinse solution for the presence of impurities is another way to guard against over rinsing the precipitate. For example, if Cl is a residual ion in the
supernatant, we can test for its presence using AgNO3. After collecting a small portion of the rinse solution, we add a few drops of AgNO3 and look
for the presence or absence of a precipitate of AgCl. If a precipitate forms, then we know that Cl is present and continue to rinse the precipitate.
Additional rinsing is not needed if the AgNO3 does not produce a precipitate.
Drying the Precipitate

After separating the precipitate from its supernatant solution, the precipitate is dried to remove residual traces of rinse solution and any volatile
impurities. The temperature and method of drying depend on the method of filtration and the precipitates desired chemical form. Placing the
precipitate in a laboratory oven and heating to a temperature of 110oC is sufficient when removing water and other easily volatilized impurities.
Higher temperatures require a muffle furnace, a Bunsen burner, or a Meker burner, and are necessary if we need to thermally decompose the
precipitate before weighing.
Because filter paper absorbs moisture, we must remove it before weighing the precipitate. This is accomplished by folding the filter paper over the
precipitate and transferring both the filter paper and the precipitate to a porcelain or platinum crucible. Gentle heating first dries and then chars the
filter paper. Once the paper begins to char, we slowly increase the temperature until all traces of the filter paper are gone and any remaining carbon is
oxidized to CO2.
Fritted-glass crucibles can not withstand high temperatures and must be dried in an oven at temperatures below 200oC. The glass fiber mats used in
Gooch crucibles can be heated to a maximum temperature of approximately 500oC.
Composition of the Final Precipitate

For a quantitative application, the final precipitate must have a well-defined composition. Precipitates containing volatile ions or substantial amounts
of hydrated water, are usually dried at a temperature that completely removes these volatile species. For example, one standard gravimetric method
for the determination of magnesium involves its precipitation as MgNH4PO46H2O. Unfortunately, this precipitate is difficult to dry at lower
temperatures without losing an inconsistent amount of hydrated water and ammonia. Instead, the precipitate is dried at temperatures above 1000oC
where it decomposes to magnesium pyrophosphate, Mg2P2O7.
An additional problem is encountered if the isolated solid is nonstoichiometric. For example, precipitating Mn2+ as Mn(OH)2 and heating frequently
produces a nonstoichiometric manganese oxide, MnOx, where x varies between one and two. In this case the nonstoichiometric product is the result
of forming of a mixture of oxides with different oxidation state of manganese. Other nonstoichiometric compounds form as a result of lattice defects
in the crystal structure.7
The best way to appreciate the theoretical and practical details discussed in this section is to carefully examine a typical precipitation gravimetric
method. Although each method is unique, the determination of Mg2+ in water and wastewater by precipitating MgNH4PO4 6H2O and isolating
Mg2P2O7 provides an instructive example of a typical procedure. The description here is based on Method 3500-Mg D in Standard Methods for the
Examination of Water and Wastewater, 19th Ed., American Public Health Association: Washington, D. C., 1995. With the publication of the 20th
Edition in 1998, this method is no longer listed as an approved method.
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Representative Method 8.1

Determination of Mg2+ in Water and Wastewater
Description of Method
Magnesium is precipitated as MgNH4PO4 6H2O using (NH4)2HPO4 as the precipitant. The precipitates solubility in neutral solutions is relatively
high (0.0065 g/100 mL in pure water at 10oC), but it is much less soluble in the presence of dilute ammonia (0.0003 g/100 mL in 0.6 M NH3).
Because the precipitant is not selective, a preliminary separation of Mg2+ from potential interferents is necessary. Calcium, which is the most
significant interferent, is removed by precipitating it as CaC2O4. The presence of excess ammonium salts from the precipitant, or the addition of too
much ammonia leads to the formation of Mg(NH4)4(PO4)2, which forms Mg(PO3)2 after drying. The precipitate is isolated by filtering, using a
rinse solution of dilute ammonia. After filtering, the precipitate is converted to Mg2P2O7 and weighed.
Procedure
Transfer a sample containing no more than 60 mg of Mg2+ into a 600-mL beaker. Add 23 drops of methyl red indicator, and, if necessary, adjust
the volume to 150 mL. Acidify the solution with 6 M HCl and add 10 mL of 30% w/v (NH4)2HPO4. After cooling and with constant stirring, add
concentrated NH3 dropwise until the methyl red indicator turns yellow (pH > 6.3). After stirring for 5 min, add 5 mL of concentrated NH3 and
continue stirring for an additional 10 min. Allow the resulting solution and precipitate to stand overnight. Isolate the precipitate by filtering through
filter paper, rinsing with 5% v/v NH3. Dissolve the precipitate in 50 mL of 10% v/v HCl, and precipitate a second time following the same
procedure. After filtering, carefully remove the filter paper by charring. Heat the precipitate at 500oC until the residue is white, and then bring the
precipitate to constant weight at 1100oC.
Questions
1. Why does the procedure call for a sample containing no more than 60 mg of Mg2+?
A 60-mg portion of Mg2+ generates approximately 600 mg of MgNH4PO4 6H2O. This is a substantial amount of precipitate. A larger quantity of
precipitate may be difficult to filter and difficult to adequately rinse free of impurities.
2. Why is the solution acidified with HCl before adding the precipitant?
The HCl ensures that MgNH4PO4 6H2O does not immediately precipitate when adding the precipitant. Because PO43 is a weak base, the
precipitate is soluble in a strongly acidic solution. If the precipitant is added under neutral or basic conditions (high RSS) the resulting precipitate
consists of smaller, less pure particles. Increasing the pH by adding base allows the precipitate to form under more favorable (low RSS) conditions.
3. Why is the acidbase indicator methyl red added to the solution?
The indicators color change, which occurs at a pH of approximately 6.3, indicates when there is sufficient NH3 to neutralize the HCl added at the
beginning of the procedure. The amount of NH3 is crucial to this procedure. If we add insufficient NH3, then the solution is too acidic, which
increases the precipitates solubility and leads to a negative determinate error. If we add too much NH3, the precipitate may contain traces of
Mg(NH4)4(PO4)2, which, on drying, forms Mg(PO3)2 instead of Mg2P2O7. This increases the mass of the ignited precipitate, giving a positive
determinate error. After adding enough NH3 to neutralize the HCl, we add the additional 5 mL of NH3 to quantitatively precipitate MgNH4PO4
6H2O.
4. Explain why forming Mg(PO3)2 instead of Mg2P2O7 increases the precipitates mass.
Each mole of Mg2P2O7 contains two moles of phosphorous and each mole of Mg(PO3)2 contains only one mole of phosphorous A conservation of
mass, therefore, requires that two moles of Mg(PO3)2 form in place of each mole of Mg2P2O7. One mole of Mg2P2O7 weighs 222.6 g. Two moles
of Mg(PO3)2 weigh 364.5 g. Any replacement of Mg2P2O7 with Mg(PO3)2 must increase the precipitates mass.
5. What additional steps, beyond those discussed in questions 2 and 3, help improve the precipitates purity?
Two additional steps in the procedure help in forming a precipitate that is free of impurities: digestion and reprecipitation.
6. Why is the precipitate rinsed with a solution of 5% v/v NH3?
This is done for the same reason that precipitation is carried out in an ammonical solution; using dilute ammonia minimizes solubility losses when
rinsing the precipitate.
8B.2 Quantitative Applications

Although no longer a commonly used technique, precipitation gravimetry still provides a reliable means for assessing the accuracy of other methods
of analysis, or for verifying the composition of standard reference materials. In this section we review the general application of precipitation
gravimetry to the analysis of inorganic and organic compounds.
Inorganic Analysis
Table 8.1 provides a summary of some precipitation gravimetric methods for inorganic cations and anions. Several methods for the homogeneous
generation of precipitants are shown in Table 8.2. The majority of inorganic precipitants show poor selectivity for the analyte. Many organic
precipitants, however, are selective for one or two inorganic ions. Table 8.3 lists several common organic precipitants.
Precipitation gravimetry continues to be listed as a standard method for the determination of SO42 in water and wastewater analysis.8 Precipitation
is carried out using BaCl2 in an acidic solution (adjusted with HCl to a pH of 4.55.0) to prevent the possible precipitation of BaCO3 or Ba3(PO4)2,
and near the solutions boiling point. The precipitate is digested at 8090oC for at least two hours. Ashless filter paper pulp is added to the precipitate
to aid in filtration. After filtering, the precipitate is ignited to constant weight at 800oC. Alternatively, the precipitate is filtered through a fine
porosity fritted glass crucible (without adding filter paper pulp), and dried to constant weight at 105oC. This procedure is subject to a variety of
errors, including occlusions of Ba(NO3)2, BaCl2, and alkali sulfates.
Table 8.1 Selected Precipitation Gravimetric Methods for Inorganic Cations and Anions (Arranged by
Precipitant)
Analyte
Precipitant
Precipitate Formed
Precipitate Weighed
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Ba2+
(NH4)2CrO4
BaCrO4
BaCrO4
Pb2+
K2CrO4
PbCrO4
PbCrO4
Ag+
HCl
AgCl
AgCl
Hg22+
HCl
Hg2Cl2
Hg2Cl2
Al3+
NH3
Al(OH)3
Al2O3
Be2+
NH3
Be(OH)2
BeO
Fe3+
NH3
Fe(OH)3
Fe2O3
Ca2+
(NH4)2C2O4
CaC2O4
CaCO3 or CaO
Sb3+
H 2S
Sb2S3
Sb2S3
As3+
H 2S
As2S3
As2S3
Hg2+
H 2S
HgS
HgS
Ba2+
H2SO4
BaSO4
BaSO4
Pb2+
H2SO4
PbSO4
PbSO4
Sr2+
H2SO4
SrSO4
SrSO4
Be3+
(NH4)2HPO4
NH4BePO4
Be2P2O7
Mg2+
(NH4)2HPO4
NH4MgPO4
Mg2P2O7
Zn2+
(NH4)2HPO4
NH4ZnPO4
Zn2P2O7
Sr2+
KH2PO4
SrHPO4
Sr2P2O7
CN
AgNO3
AgCN
AgCN
AgNO3
AgI
AgI
Br
AgNO3
AgBr
AgBr
Cl
AgNO3
AgCl
AgCl
ClO3
FeSO4/ AgNO3
AgCl
AgCl
SCN
SO2/ CuSO4
CuSCN
CuSCN
SO42
BaCl2
BaSO4
BaSO4
Table 8.2 Reactions for the Homogeneous Preparation of Selected Inorganic Precipitants
Precipitant
OH
SO42
Reaction
2NH4+(aq) + CO2(g) + 2OH(aq)
(NH2)2CO(aq) + 3H2O(l)
NH2HSO3(aq) + 2H2O(l)
NH4+(aq) + H3O+(aq) + SO42(aq)
S2
CH3CSNH2(aq) + H2O(l)
IO3
HOCH2CH2OH(aq) + IO4(aq)
PO43
(CH3O)3PO(aq) + 3H2O(l)
C2O42
(C2H5)2C2O4(aq) + 2H2O(l)
CO32
Cl3CCOOH(aq) + 2OH(aq)
CH3CONH2(aq) + H2S (aq)

2HCHO(aq) + H2O(l) + IO3(aq)
3CH3OH(aq) + H3PO4(aq)
2C2H5OH(aq) + H2C2O4(aq)
CHCl3(aq) + CO32(aq) + H2O(l)
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Table 8.3 Selected Precipitation Gravimetric Methods for Inorganic Ions Using an Organic Precipitant
Precipitate
Formed
Precipitate
Weighed
dimethylglyoxime
Ni(C4H7O2N2)2
Ni(C4H7O2N2)2
Fe3+
cupferron
Fe(C6H5N2O2)3
Fe2O3
Cu2+
cupron
CuC14H11O2N
CuC14H11O2N
Co2+
1-nitrso-2-napthol
Co(C10H6O2N)3
Co or CoSO4
K+
sodium
tetraphenylborate
K[B(C6H5)4
K[B(C6H5)4
NO3
nitron
C20H16N4HNO3
C20H16N4HNO3
Analyte
Precipitant
Ni2+
Structure
Na[B(C6H5)4]
Organic Analysis
Several organic functional groups or heteroatoms can be determined using precipitation gravimetric methods. Table 8.4 provides a summary of
several representative examples. Note that the procedure for the determination of alkoxy functional groups is an indirect analysis.
Table 8.4 Selected Precipitation Gravimetric Methods for the Analysis of Organic Functional Groups and
Heteroatoms
Analyte
Organic
halides
RX
X = Cl, Br, I
Organic
halides
RX
X = Cl, Br, I
Treatment
Precipitant Precipitate
Oxidation with HNO3 in the presence of Ag+
AgNO3
AgX
Combustion in O2 (with a Pt catalyst) in the presence of Ag+
AgNO3
AgX
Organic sulfur Oxidation with HNO3 in the presence of Ba2+
BaCl2
BaSO4
Combustion in O (with Pt catalyst) with SO2 and SO3

Organic sulfur collected in dilute2 H O
2 2
BaCl2
BaSO4
AgNO3
AgI
Alkoxy groups
OR or
COOR
Reaction with HI to produce RI
R = CH3 or
C2H5
Quantitative Calculations
The stoichiometry of a precipitation reaction provides a mathematical relationship between the analyte and the precipitate. Because a precipitation
gravimetric method may involve several chemical reactions before the precipitation reaction, knowing the stoichiometry of the precipitation reaction
may not be sufficient. Even if you do not have a complete set of balanced chemical reactions, you can deduce the mathematical relationship between
the analyte and the precipitate using a conservation of mass. The following example demonstrates the application of this approach to the direct
analysis of a single analyte.
Example 8.1
To determine the amount of magnetite, Fe3O4, in an impure ore, a 1.5419-g sample is dissolved in concentrated HCl, giving a mixture of Fe2+ and
Fe3+. After adding HNO3 to oxidize Fe2+ to Fe3+ and diluting with water, Fe3+ is precipitated as Fe(OH)3 by adding NH3. Filtering, rinsing, and
igniting the precipitate provides 0.8525 g of pure Fe2O3. Calculate the %w/w Fe3O4 in the sample.
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Solution
A conservation of mass requires that all the iron from the ore is found in the Fe2O3. We know there are 2 moles of Fe per mole of Fe2O3 (FW =
159.69 g/mol) and 3 moles of Fe per mole of Fe3O4 (FW = 231.54 g/mol); thus
The % w/w s Fe3O4 in the sample, therefore, is

A 0.7336-g sample of an alloy containing copper and zinc is dissolved in 8 M HCl and diluted to 100 mL
in a volumetric flask. In one analysis, the zinc in a 25.00-mL portion of the solution is precipitated as
ZnNH4PO4, and subsequently isolated as Zn2P2O7, yielding 0.1163 g. The copper in a separate 25.00-mL
portion of the solution is treated to precipitate CuSCN, yielding 0.2931 g. Calculate the %w/w Zn and the
%w/w Cu in the sample.
In Practice Exercise 8.2 the sample contains two analytes. Because we can selectively precipitate each analyte, finding their respective concentrations
is a straightforward stoichiometric calculation. But what if we cannot precipitate the two analytes separately? To find the concentrations of both
analytes, we still need to generate two precipitates, at least one of which must contain both analytes. Although this complicates the calculations, we
can still use a conservation of mass to solve the problem.
Example 8.2
A 0.611-g sample of an alloy containing Al and Mg is dissolved and treated to prevent interferences by the alloys other constituents. Aluminum
and magnesium are precipitated using 8-hydroxyquinoline, providing a mixed precipitate of Al(C9H6NO)3 and Mg(C9H6NO)2 that weighs 7.815 g.
Igniting the precipitate converts it to a mixture of Al2O3 and MgO that weighs 1.002 g. Calculate the %w/w Al and %w/w Mg in the alloy.
Solution
The masses of the solids provide us with the following two equations.
With two equations and four unknowns, we need two additional equations to solve the problem. A conservation of mass requires that all the
aluminum in Al(C9H6NO)3 is found in Al2O3; thus
Using the same approach, a conservation of mass for magnesium gives
Substituting the equations for g MgO and g Al2O3 into the equation for the combined weights of MgO and Al2O3 leaves us with two equations and
two unknowns.
Multiplying the first equation by 0.11096 and subtracting the second equation gives
Now we can finish the problem using the approach from Example 8.1. A conservation of mass requires that all the aluminum and magnesium in the
sample of Dow metal is found in the precipitates of Al(C9H6NO)3 and the Mg(C9H6NO)2. For aluminum, we find that
and for magnesium we have
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A sample of a silicate rock weighing 0.8143 g is brought into solution and treated to yield a 0.2692-g
mixture of NaCl and KCl. The mixture of chloride salts is subsequently dissolved in a mixture of ethanol
and water, and treated with HClO4, precipitating 0.5713 g of KClO4. What is the %w/w Na2O in the
silicate rock?
The previous problems are examples of direct methods of analysis because the precipitate contains the analyte. In an indirect analysis the precipitate
forms as a result of a reaction with the analyte, but the analyte is not part of the precipitate. As shown by the following example, despite the
additional complexity, we can use conservation principles to organize our calculations.
Example 8.3
An impure sample of Na3PO3 weighing 0.1392 g is dissolved in 25 mL of water. A solution containing 50 mL of 3% w/v HgCl2, 20 mL of 10%
w/v sodium acetate, and 5 mL of glacial acetic acid is then prepared. Adding the solution of Na3PO3 to the solution containing HgCl2, oxidizes
PO33 to PO43, precipitating Hg2Cl2. After digesting, filtering, and rinsing the precipitate, 0.4320 g of Hg2Cl2 is obtained. Report the purity of the
original sample as % w/w Na3PO3.
Solution
This is an example of an indirect analysis because the precipitate, Hg2Cl2, does not contain the analyte, Na3PO3. Although the stoichiometry of the
reaction between Na3PO3 and HgCl2 is given earlier in the chapter, lets see how we can solve the problem using conservation principles.
The reaction between Na3PO3 and HgCl2 is a redox reaction in which phosphorous increases its oxidation state from +3 in Na3PO3 to +5 in
Na3PO4, and in which mercury decreases its oxidation state from +2 in HgCl2 to +1 in Hg2Cl2. A redox reaction must obey a conservation of
electronsall the electrons released by the reducing agent, Na3PO3, must be accepted by the oxidizing agent, HgCl2. Knowing this, we write the
following stoichiometric conversion factors:
Although you can write the balanced reactions for any analysis, applying conservation principles can save you a significant amount of time!
Now we are ready to solve the problem. First, we use a conservation of mass for mercury to convert the precipitates mass to the moles of HgCl2.
Next, we use the conservation of electrons to find the mass of Na3PO3.
As you become comfortable with using conservation principles, you will see opportunities for further simplifying problems. For example, a
conservation of electrons requires that the electrons released by Na3PO3 end up in the product, Hg2Cl2, yielding the following stoichiometric
conversion factor:
This conversion factor provides a direct link between the mass of Hg2Cl2 and the mass of Na3PO3.
Finally, we calculate the %w/w Na3PO3 in the sample.

One approach for determining phosphate, PO43, is to precipitate it as ammonium phosphomolybdate,
(NH4)3PO412MoO3. After isolating the precipitate by filtration, it is dissolved in acid and the molybdate
precipitated and weighed as PbMoO3. Suppose we know that our samples contain at least 12.5% Na3PO4
and we need to recover a minimum of 0.600 g of PbMoO3? What is the minimum amount of sample
needed for each analysis?
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8B.2 Qualitative Applications

A precipitation reaction is a useful method for identifying inorganic and organic analytes. Because a qualitative analysis does not require quantitative
measurements, the analytical signal is simply the observation that a precipitate has formed. Although qualitative applications of precipitation
gravimetry have been largely replaced by spectroscopic methods of analysis, they continue to find application in spot testing for the presence of
specific analytes.9
Any of the precipitants listed in Table 8.1, Table 8.3, and Table 8.4 can be used for a qualitative analysis.
8B.3 Evaluating Precipitation Gravimetry

Scale of Operation
The scale of operation for precipitation gravimetry is limited by the sensitivity of the balance and the availability of sample. To achieve an accuracy
of 0.1% using an analytical balance with a sensitivity of 0.1 mg, we must isolate at least 100 mg of precipitate. As a consequence, precipitation
gravimetry is usually limited to major or minor analytes, in macro or meso samples (see Figure 3.5 in Chapter 3). The analysis of trace level analytes
or micro samples usually requires a microanalytical balance.
Accuracy
For a macro sample containing a major analyte, a relative error of 0.10.2% is routinely achieved. The principle limitations are solubility losses,
impurities in the precipitate, and the loss of precipitate during handling. When it is difficult to obtain a precipitate that is free from impurities, it may
be possible to determine an empirical relationship between the precipitates mass and the mass of the analyte by an appropriate calibration.
Problem 8.27 provides an example of how to determine an analytes concentration by establishing an empirical relationship between the analyte
and the precipitate.
Precision
The relative precision of precipitation gravimetry depends on the samples size and the precipitates mass. For a smaller amount of sample or
precipitate, a relative precision of 12 ppt is routinely obtained. When working with larger amounts of sample or precipitate, the relative precision
can be extended to several ppm. Few quantitative techniques can achieve this level of precision.
Sensitivity
For any precipitation gravimetric method we can write the following general equation relating the signal (grams of precipitate) to the absolute
amount of analyte in the sample
Equation 8.13 assumes that we have used a suitable blank to correct the signal for any contributions of the reagent to the precipitates mass.
where k, the methods sensitivity, is determined by the stoichiometry between the precipitate and the analyte. Consider, for example, the
determination of Fe as Fe2O3. Using a conservation of mass for iron, the precipitates mass is
and the value of k is
As we can see from equation 8.14, there are two ways to improve a methods sensitivity. The most obvious way to improve sensitivity is to increase
the ratio of the precipitates molar mass to that of the analyte. In other words, it helps to form a precipitate with the largest possible formula weight.
A less obvious way to improve a methods sensitivity is indicated by the term of 1/2 in equation 8.14, which accounts for the stoichiometry between
the analyte and precipitate. We can also improve sensitivity by forming a precipitate that contains fewer units of the analyte.

Suppose you wish to determine the amount of iron in a sample. Which of the following compoundsFeO,
Fe2O3, or Fe3O4provides the greatest sensitivity?
Selectivity
Due to the chemical nature of the precipitation process, precipitants are usually not selective for a single analyte. For example, silver is not a selective
precipitant for chloride because it also forms precipitates with bromide and iodide. Interferents are often a serious problem and must be considered if
accurate results are to be obtained.
Time, Cost, and Equipment

Precipitation gravimetry is time intensive and rarely practical if you have a large number of samples to analyze. However, because much of the time
invested in precipitation gravimetry does not require an analysts immediate supervision, it may be a practical alternative when working with only a
few samples. Equipment needs are fewbeakers, filtering devices, ovens or burners, and balancesinexpensive, routinely available in most
laboratories, and easy to maintain.
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8C Volatilization Gravimetry
Contributors
David Harvey (DePauw University)
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Periodic Table of the Elements

Units & Conversions

8B: Precipitation Gravimetry

8B.1 Theory and Practice

8B: Precipitation Gravimetry - Chemwiki

and the following equation for the solubility of CaF2.

8B: Precipitation Gravimetry - Chemwiki

Practice Exercise 8.1

8B: Precipitation Gravimetry - Chemwiki

Controlling Particle Size

8B: Precipitation Gravimetry - Chemwiki

when designing a gravimetric method of analysis.

8B: Precipitation Gravimetry - Chemwiki

Filtering the Precipitate

8B: Precipitation Gravimetry - Chemwiki

8B: Precipitation Gravimetry - Chemwiki

Rinsing the Precipitate

Drying the Precipitate

Composition of the Final Precipitate

8B: Precipitation Gravimetry - Chemwiki

Representative Method 8.1

8B.2 Quantitative Applications

8B: Precipitation Gravimetry - Chemwiki

NH4+(aq) + H3O+(aq) + SO42(aq)

CH3CONH2(aq) + H2S (aq)

8B: Precipitation Gravimetry - Chemwiki

Oxidation with HNO3 in the presence of Ag+

Combustion in O2 (with a Pt catalyst) in the presence of Ag+

Organic sulfur Oxidation with HNO3 in the presence of Ba2+

Combustion in O (with Pt catalyst) with SO2 and SO3

8B: Precipitation Gravimetry - Chemwiki

The % w/w s Fe3O4 in the sample, therefore, is

Practice Exercise 8.2

Using the same approach, a conservation of mass for magnesium gives

and for magnesium we have

8B: Precipitation Gravimetry - Chemwiki

Practice Exercise 8.3

Next, we use the conservation of electrons to find the mass of Na3PO3.

Practice Exercise 8.4

8B: Precipitation Gravimetry - Chemwiki

8B.2 Qualitative Applications

8B.3 Evaluating Precipitation Gravimetry

and the value of k is

Practice Exercise 8.5

Time, Cost, and Equipment

8B: Precipitation Gravimetry - Chemwiki

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