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BSc Sem III (Principal)

Analytical Chemistry:
Classical methods of
analysis (2 Credits)
UNIT 2
PRAKASH SAMNANI

Gravimetric Analysis – Unit II

Principles of gravimetric analysis, apparatus used for gravimetric analysis
(balance – care and use of analytical balance, crucible, desiccator, burner, oven),
preparation of solutions and reagents, precipitation conditions, impurities in
precipitates, digestion, filtration, washing, drying, incineration, ignition,
weighing of precipitate, gravimetric calculations.
Precipitation titrations – precipitation reactions, determining end points in
precipitation titrations. Volhard’s method, Mohr’s method and Fajan’s method,
Determination of Cl−

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Reference books
P B Samnani, R C Shah’s Quantitative Chemical
Analysis, Ria Publishing House, Anand, 2014.
D A Skoog, D M West, F J Holler, S R Crouch,
Fundamentals of Analytical Chemistry,
Brooks/Cole, 2014.
Garry D Christian, Analytical Chemistry, John
Willey & Sons. 6th Edition.2004.

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Importance
Major component of TYBSc chemistry practicals, also in MSc Chemistry
practicals
Industry QC and R&D laboratory (Pharma, fine chemicals), Testing laboratories
(esp Environmental)
Principles – basic chemistry
Pre-requisite – content from FYBSc (in Teams files – Recap_intro_analchem)
◦ Analytical chemistry, chemical analysis, method, technique, expression of concentration,
common ion effect, solubility product

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Chemical Analysis
Qualitative and Quantitative analysis
Methods of analysis
◦ Classical – inorganic qualitative analysis, organic spotting, titrimetry, gravimetry (also called
absolute methods of analysis – based on some fundamental physical property)
◦ Advantages – simple, based on stoichiometry of reaction, less expensive, do not require
expensive equipment, conventional laboratory ware and chemicals sufficient, a good balance
needed
◦ Disadvantages – time consuming, not very sensitive ( poor limit of detection – smallest
concentration to be detected / determined)
◦ Instrumental / modern – spectroscopy like uv-vis, IR, NMR, chromatography (also called
relative methods of analysis)
◦ Advantages – fast, very sensitive
◦ Disadvantages – expensive

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Principles of Gravimetric Analysis

Physical or physico-chemical methods of quantitative analysis which involves
the measure of certain physical property of the substance which is reliant
(dependent) on its concentration.
The most important methods of gravimetric analysis are the precipitation
methods.
They involve complete precipitation of the constituents to be determined
(analyte) as an insoluble chemical compound, having a definite chemical
composition or convertible to one of that.
Analytical method based on measurement of mass / weight. (analytical signal)

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Principles of Gravimetric Analysis

The analyte is separated from the sample solution as precipitate.
Thus, in determination of silver, it is precipitated as AgCl, washed, dried and
weighed as such, whereas iron is precipitated as hydrated oxide (with no defined
chemical composition) and weighed as Fe2O3 after ignition.
Other analytical methods based on measurement of mass are volatilisation
gravimetry and electrogravimetry.
You do not always get the sample in solution form. So, if you have to determine, by gravimetry,
amount of copper in brass (an alloy of copper and zinc), a solid material, you will weigh a known
amount of brass sample, dissolve it in suitable medium (in this case, acid) and convert it into
sample solution.

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Principles of Gravimetric Analysis (theory)

The solubility or rather insolubility of salts / compounds causes precipitation
from solution.
The compound that precipitates is considered sparingly soluble salt, and the
relevant equilibria calculations are applied.
In principle, the concepts of solubility product (Ksp) and common ion effect are
used in precipitation gravimetry to bring about selective precipitation of the
desired analyte ion. (taught to you in lower classes)
Solubility of a compound in a solvent depends on several factors. Similarly,
precipitation of an insoluble compound from solution depends on factors like
temperature, Ksp, pH, ionic concentration, rate of addition of reagent and so on.

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Conservation of Mass
An accurate gravimetric analysis requires that the analytical signal—whether it is a
mass or a change in mass—be proportional to the amount of analyte in our
sample. For all gravimetric methods this proportionality involves a conservation of
mass. If the method relies on one or more chemical reactions, then the
stoichiometry of the reactions must be known. Thus, for the analysis of PO33– , we
know that each mole of Hg2Cl2 corresponds to a mole of PO33– in our sample. If we
remove the analyte from its matrix, then the separation must be selective for the
analyte. Phosphite reduces mercuric ion to mercurous ion, which in presence of
chloride ion in solution precipitates as mercurous chloride.
2HgCl2(aq) + 2PO33−(aq) + 2H2O(l)  Hg2Cl2(s) + 2H3O+(aq) + 2Cl−(aq) + 2PO43−(aq)
Each mole of phosphite produces one mole of mercurous chloride, which is
weighed, indirectly giving amount of phosphite. Remember relation between mole and g
weight of a substance.
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Steps of Gravimetric Analysis

1. Preparation of sample solution
2. Separation of the desired analyte as precipitate
3. Filtration (using paper or perforated glass crucible) Gooch Crucible

4. Washing of the precipitate

5. Drying
6. Incineration (of paper)
7. Ignition of precipitate
8. Weighing and calculation

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Reagents used for precipitation

The reagent used to bring about precipitation of the desired analyte from
sample solution is called precipitating reagent / agent.
E.g., Oxalic acid (H2C2O4) or oxalate anion (C2O42−) (aqueous solution) for
precipitation of Ca2+ ion; calcium oxalate(CaC2O4) precipitates
An excess of oxalic acid is added to an aqueous solution of the sample. Ammonia
is then added, which neutralises the acid causes essentially all of the calcium in
the sample to precipitate as calcium oxalate.
2NH3 + H2C2O4 → 2NH4+ + C2O42−
Ca2+(aq) + C2O42− → CaC2O4(s)

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and then ……….

The precipitate is filtered using a special filter paper (e.g., Whatman), dried,
transferred to a pre-weighed crucible, the paper burnt (incinerated), and the
remaining precipitate ignited. This process converts the precipitates to calcium
oxide, as shown in the reaction below:
Δ
CaC2O4(s) CaO(s) + CO(g) + CO2(g)
After cooling, the crucible and precipitate are weighed and mass of calcium
oxide is determined by subtracting the known mass of the crucible. From this
amount of calcium is computed (as explained later).

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Characteristics of precipitating reagents

The precipitating agent should react specifically or selectively with the analyte
ion. Further it should result into precipitates with certain characteristics.
Characteristics of the precipitates
o Easily filterable, washed free of impurities / contaminants (coarse particles)
o Of low solubility so that there is no significant loss of ppt during washing and
filtration
o Unreactive with the constituents of atmosphere
o Of known chemical composition after drying or ignition

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Particle size and filterability of precipitates

Precipitates consisting of large particles are generally desirable for gravimetric work
because these particles are easy to filter and wash free of impurities. In addition.
precipitates of this type are usually purer than are precipitates made up of fine particles.
Factors That Determine the Particle Size of Precipitates
The particle size of solids formed by precipitation varies enormously. At one extreme are
colloidal suspensions, whose tiny particles are invisible to the naked eye (10 −7 to 10−4 cm
in diameter). Colloidal particles show no tendency to settle from solution and are not
easily filtered. At the other extreme are particles with dimensions on the order of tenths
of a millimeter or greater. The temporary dispersion of such particles in the liquid phase is
called a crystalline suspension. The particles of a crystalline suspension tend to settle
spontaneously and are easily filtered.

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Particle size and filterability of precipitates

Particle size of a precipitate is influenced by such experimental variables as precipitate
solubility, temperature, reactant concentrations, and rate at which reactants are mixed.
The net effect of these variables can be qualitatively accounted for, by assuming that the
particle size is related to a single property of the system called the relative supersaturation
(RSS) or the Von-Weimar ratio,
Relative supersaturation = (Q – S) / S
where Q is the concentration of the solute (ppt) at any instant and S is its equilibrium
solubility. The particle size of a precipitate varies inversely with the average relative
supersaturation during the time when the reagent is being introduced. Thus, when (Q -
S)/S is large, the precipitate tends to be colloidal; when (Q - S)/S is small, a crystalline solid
is more likely.

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The main difference between saturated and supersaturated solution is

that, at a given temperature, a saturated solution has a maximum
amount of solutes in the solution whereas a supersaturated solution has
more than the maximum amount of solutes in the solution. Then, the
amount of solute present in the supersaturated solution will be higher

Precipitation of analyte ion as compound occurs when the product of

concentration of the ions (that make up the precipitate, ionic product,
IP) exceeds the Ksp for the compound.
Thus, in an aqueous solution containing NaCl (Na+ and Cl− ions), when
AgNO3 solution is added, the product of ionic concentration of Ag+ and
Cl− exceeds Ksp for AgCl, and hence AgCl precipitates.

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Experimental parameters that control particle size

Parameters that influence particle size of the precipitate particles are the ones
that minimize supersaturation so that crystalline, bigger particles are
◦ Increased temperature, which increases solubility of precipitates
◦ pH of the solution, in cases where solubility of ppt depends on pH, e.g., Calcium oxalate
◦ Carrying out precipitation of analyte from dilute solutions, to reduce Q
◦ Slow addition of the precipitating reagent, with good stirring
the last two parameters also reduce concentration Q of the precipitate at any
given instant
In many cases, the precipitate formed are colloidal particles / gel, especially in
cases when S negligible compared to Q, bringing the relative super saturation
very high most of the time; e.g., hydrous oxides of Fe(III), Al(III) and Cr(III),
sulphides of heavy metals like Ni(II).

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Colloidal precipitates
Individual colloidal particles are so small that they are not retained by ordinary
filters. Moreover, Brownian motion prevents their settling out of solution under
the influence of gravity. Fortunately, however, we can coagulate, or agglomerate,
the individual particles of most colloids to give a filterable, amorphous mass that
will settle out of solution and can then be filtered and washed.
Colloidal suspensions are stable because all of the particles of the colloid are
either positively or negatively charged. This charge results from cations or
anions that are bound to the surface of the particles. The process by which ions
are retained on the surface of a solid is known as adsorption. Thus, freshly
precipitated particles of silver chloride are colloidal in nature and will be
positively charged if there is excess of Ag+ ions in solution, and negatively
charged if there is excess of anion like NO3− or Cl− in solution.(later, we will use
this information during Fajan’s method of titration)

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Examples of colloidal precipitates

Aluminium hydroxide

Precipitation of ferric hydroxide

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A colloidal silver chloride particle suspended in a solution of silver nitrate

Image from Skoog, West

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Colloidal precipitates
Coagulation of a colloidal suspension can often be brought about by a short
period of heating, particularly if accompanied by stirring. Heating decreases the
number of adsorbed ions. The particles may also gain enough kinetic energy at
the higher temperature to overcome the barrier to close approach posed by the
layer of adsorbed ions (double layer).
An even more effective way to coagulate a colloid is to increase the electrolyte
concentration of the solution. If we add a suitable ionic compound to a colloidal
suspension, the concentration of counter-ions increases in the vicinity of each
particle. As a result, the volume of solution that contains sufficient counter-ions
to balance the charge of the primary adsorption layer decreases. The net effect
of adding an electrolyte is thus a shrinkage of the counter-ion layer. The
particles can then approach one another more closely and agglomerate.

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Figure. 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 (like nitrate ions in this case) decreases
the thickness of the secondary adsorption layer.
Because the particles can approach each other
more closely, they are able to coagulate.

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Peptization of Colloids
Peptization is the process by which a coagulated colloid reverts to its original
dispersed state. When a coagulated colloid is washed, some of the electrolyte
responsible for its coagulation is leached from the internal liquid in contact with
the solid particles. Removal of this electrolyte has the effect of increasing the
volume of the counter-ion layer. The repulsive forces responsible for the original
colloidal state are then re-established, and particles detach themselves from the
coagulated mass. The washings become cloudy as the freshly dispersed particles
pass through the filter. Washing of the ppt is needed to minimize contamination,
however, there is a risk of losses resulting from peptization if pure water is used
for washing. The problem is commonly solved by washing the precipitate with a
solution containing an electrolyte that volatilizes when the precipitate is dried or
ignited.
E.g., silver chloride ppt washed with aqueous nitric acid; hydrated iron(III) oxide
ppt washed with aqueous ammonium nitrate solution. (wash liquid)

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Practical Treatment of Colloidal Precipitates

Colloids are best precipitated from hot, stirred solutions containing sufficient
electrolyte to ensure coagulation. The filterability of a coagulated colloid
frequently improves if it is allowed to stand for an hour or more in contact with
the hot solution from which it was formed (mother liquor). During this process,
which is known as digestion, weakly bound water appears to be lost from the
precipitate: the result is a denser mass that is easier to filter.
These precipitates are better washed by the method of decantation, and require
special filter paper for filtration, washing of the precipitate also requires special
care, like the ppt should not be allowed to dry in some cases due to possible
caking. E.g., precipitates of hydrous oxides of Fe(III) and Al(III)

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Crystalline Precipitates
Crystalline precipitates are generally more easily filtered and purified than are
coagulated colloids. In addition, the size of individual crystalline particles, and
thus their filterability, can be controlled to some extent.
Methods of Improving Particle Size and Filterability
The particle size of crystalline solids can often be improved significantly by
minimizing Q or maximizing S, or both. Minimization of Q is generally
accomplished by using dilute (sample) solutions and adding the precipitating
reagent slowly and with good mixing. Often S is increased by precipitating from
hot solution or by adjusting the pH of the precipitation medium.

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Crystalline Precipitates
Digestion of crystalline precipitates (without stirring) for some time after
formation frequently yields a purer, more filterable product (precipitates). The
improvement in filterability results from the dissolution and recrystallization
that occur continuously and at an enhanced rate at elevated temperatures.
Recrystallization apparently results in bridging between adjacent particles, a
process that yields larger and more easily filtered crystalline aggregates. This
view is supported by the observation that little improvement in filtering
characteristic, occurs if the mixture is stirred during digestion.

Purity of Precipitates
Various phenomena affect purity of precipitates. They are co-precipitation, post
precipitation…

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1. Coprecipitation
Coprecipitation is a phenomenon in which otherwise soluble compounds are removed
from solution during precipitate formation (i.e., get precipitated along with precipitates
of analyte, they would not have precipitated in absence of analyte). It is important to
understand that contamination of a precipitate by a second substance whose solubility
product has been exceeded does not constitute coprecipitation.
There are four types of coprecipitation: surface adsorption, mixed-crystal formation,
occlusion, and mechanical entrapment.
Surface adsorption and mixed-crystal formation are equilibrium processes, whereas
occlusion and mechanical entrapment arise from the kinetics of crystal growth.
a. Surface Adsorption
Adsorption is a common source of coprecipitation and is likely to cause significant
contamination of precipitates with large specific surface areas-that is, coagulated
colloids. Although adsorption does occur in crystalline solids, its effects on purity are
usually undetectable because of the relatively small specific surface area of these
solids.
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Coagulation of a colloid does not significantly decrease the amount of adsorption

because the coagulated solid still contains large internal surface areas that
remain exposed to the solvent. The coprecipitated contaminant on the
coagulated colloid consists of the lattice ion originally adsorbed on the surface
before coagulation plus the counter-ion of opposite charge held in the film of
solution immediately adjacent to the particle (e.g., AgCl particle can have Ag+ ion
adsorbed on its surface, making it positively charged and counter anion for
electrical neutrality). The net effect of surface adsorption is therefore the
carrying down of an otherwise soluble compound as a surface contaminant.
For example, the coagulated silver chloride formed in the gravimetric
determination of chloride ion is contaminated with primarily adsorbed silver ions
with nitrate or other anions in the counter-ion layer. As a consequence, silver
nitrate, a normally soluble compound, is coprecipitated with the silver chloride.

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Minimizing Adsorbed Impurities on Colloids

The purity of many coagulated colloids is improved by digestion. During this
process, water is expelled from the solid to give a denser mass, that has a smaller
specific surface area for adsorption. Washing a coagulated colloid with a solution
containing a volatile electrolyte (like ammonium nitrate) may also be helpful
because any nonvolatile electrolyte added earlier to cause coagulation is
displaced by the volatile species. Washing generally does not remove much of
the primarily adsorbed ions because the attraction between these ions and the
surface of the solid is too strong. Exchange occurs, however, between existing
counter-ions and ions in the wash liquid. For example, in the determination of
silver by precipitation with chloride ion, the primarily adsorbed species is
chloride. Washing with an acidic solution converts the counter-ion layer largely
to hydrogen ions so that both chloride and hydrogen ions are retained by the
solid. Volatile HCI is then given off when the precipitate is dried.

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Regardless of the method of treatment, a coagulated precipitate is always

contaminated to some degree, even after extensive washing. The error
introduced into the analysis from this source can be as low as I to 2 ppt, as in the
coprecipitation of silver nitrate on silver chloride. In contrast, coprecipitation of
heavy-metal hydroxides on the hydrous oxides of trivalent iron or aluminium can
result in errors as large as several percent, which is generally intolerable.
Reprecipitation A drastic but effective way to minimize the effects of adsorption
is reprecipitation. In this process. the filtered solid is re-dissolved and
reprecipitated. The first precipitate ordinarily carries down only a fraction of the
contaminant present in the original solvent. Thus, the solution containing the re-
dissolved precipitate has a significantly lower contaminant concentration than
the original, and even less adsorption occurs during the second precipitation.
Reprecipitation adds substantially to the time required for an analysis but is often
necessary for such precipitates as the hydrous oxides of iron(llI) and aluminium,
which have extraordinary tendencies to adsorb the hydroxides of heavy-metal
cations such as zinc, cadmium, and manganese.
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b. Mixed-Crystal Formation
In mixed-crystal formation, one of the ions in the crystal lattice of a solid is replaced by
an ion of another element. For this exchange to occur, it is necessary that the two ions
have the same charge and that their sizes differ by no more than about 5%. Furthermore,
the two salts must belong to the same Crystal class. For example, barium sulfate formed
by adding barium chloride to a solution containing sulfate, lead, and acetate ions is found
to be severely contaminated by lead sulfate even though acetate ions normally prevent
precipitation of lead sulfate by complexing the lead. Here, lead ions replace some of the
barium ions in the barium sulfate crystals. Other examples of coprecipitation by mixed-
crystal formation include MgKPO4 in MgNH4PO4, SrSO4 in BaSO4, and MnS in CdS.
Mixed-crystal formation is a particularly troublesome type of coprecipitation because
little can be done about it when certain combinations of ions are present in a sample
matrix. This problem is encountered with both colloidal suspensions and crystalline
precipitates. When mixed-crystal formation occurs, the interfering ion may have to be
separated before the final precipitation step. Alternatively. a different precipitating
reagent that does not give mixed crystals with the ions in question may be used. E.g.
BaCrO4 instead of BaSO4.
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c. Occlusion and Mechanical Entrapment

When a crystal is growing rapidly during precipitate formation, foreign ions in the
counter-ion layer may become trapped, or occluded, within the growing crystal.
Because supersaturation and thus growth rate decrease as precipitation
progresses, the amount of occluded material is greatest in that part of a crystal
that forms first.
Mechanical entrapment occurs when crystals lie close together during growth.
Several crystals grow together and in so doing trap a portion of the solution in a
tiny pocket.
Both occlusion and mechanical entrapment are at a minimum when the rate of
precipitate formation is low, that is, under conditions of low supersaturation. In
addition, digestion is often remarkably helpful in reducing these types of
coprecipitation. Undoubtedly, the rapid solution and reprecipitation that go on at
the elevated temperature of digestion open up the pockets and allow the
impurities to escape into the solution.

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Coprecipitation Errors
Coprecipitated impurities may cause either negative or positive errors in an
analysis. If the contaminant is not a compound of the ion being determined, a
positive error will always result. Thus, a positive error is observed whenever
colloidal silver chloride adsorbs silver nitrate during a chloride analysis. In
contrast, when the contaminant does contain the ion being determined, either
positive or negative errors may be observed.
For example. in the determination of barium by precipitation as barium sulfate,
occlusion of other barium salts occurs. If the occluded contaminant is barium
nitrate, a positive error is observed because this compound has a larger molar
mass than the barium sulfate that would have formed had no coprecipitation
occurred. If barium chloride is the contaminant, the error is negative because its
molar mass is less than that of the sulfate salt.
BaSO4 – 233.4; Ba(NO3)2 – 261.3; BaCl2 – 208.2

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2. Postprecipitation
When the precipitates are left along with its mother liquor, the soluble salts
present in the mother liquor may get deposited on the precipitates. The
phenomenon is called postprecipitation.
If Calcium oxalate (CaC2O4) precipitates are left in contact with mother liquor
containing Mg2+, MgC2O4 (magnesium oxalate) is postprecipitated. CaC2O4
adsorbs its own oxalate ion; as the concentration of oxalate ions on the surface
of Ca-oxalate precipitate is increased, the solubility product of MgC2O4 is
exceeded and hence it gets precipitated to a certain extent on CaC2O4
precipitates.
Thus, the ageing or cooking of the precipitates is not always advantageous as it
favours post-precipitation.

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Precipitation from Homogeneous Solution

Precipitation from homogeneous solution is a technique in which a precipitating
agent is generated in a solution of the analyte by a slow chemical reaction. Local
reagent excesses do not occur because the precipitating agent appears gradually
and homogeneously throughout the solution and reacts immediately with the
analyte. As a result, the relative supersaturation is kept low during the entire
precipitation. In general, homogeneously formed precipitates, both colloidal and
crystalline, are better suited for analysis than a solid formed by direct addition of
a precipitating reagent.
Urea is often used for the homogeneous generation of hydroxide ion. The
reaction can be expressed by the equation:
(H2N)2CO + 3H2O → CO2 + 2NH4+ + 2OH−
This hydrolysis proceeds slowly at temperatures just below 100°C, and 1 to 2
hours is needed to complete a typical precipitation.

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Urea is particularly valuable for the precipitation of hydrous oxides or basic salts.
For example, hydrous oxides of iron(lIl) and aluminium, formed by direct addition
of base, are bulky and gelatinous masses that are heavily contaminated and
difficult to filter. In contrast, when these same products are produced by
homogeneous generation of hydroxide ion, they are dense and easily filtered and
have considerably higher purity. This is also called Homogeneous precipitation.
Pb2+ is precipitated homogeneously as PbCrO4 by using bromate, BrO3–, to oxidize
Cr3+ to CrO42−
6BrO3−(aq) + 10Cr3+(aq) + 22H2O(l)  3Br2(aq) + 10CrO42−(aq) + 44H+(aq)
Homogeneous precipitation of crystalline precipitates also results in marked
increases in crystal size as well as improvement in purity. There are several other
reagents used for homogenous precipitation of various ions in gravimetry.

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Two precipitates of PbCrO4. In Beaker

A B
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. (RSS
Relative Super Saturation)

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Drying and Ignition of Precipitates

After filtration, a gravimetric precipitate is heated until its mass becomes
constant. Heating removes the solvent and any volatile species carried down
with the precipitate. Some precipitates are also ignited to decompose the solid
and form a compound of known composition. This new compound is often called
the weighing form.
The temperature required to produce a suitable weighing form varies from
precipitate to precipitate. Figure 12-6 shows mass loss as a function of
temperature for several common analytical precipitates. These data were
obtained with an automatic thermobalance, an instrument that records the mass
of a substance continuously as its temperature is increased at a constant rate
(Figure 12-7). Heating three of the precipitates - silver chloride, barium sulfate,
and aluminium oxide – simply causes removal of water and perhaps volatile
electrolytes.

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Note the vastly different temperatures required to produce an

anhydrous precipitate of constant mass. Moisture is
completely removed from silver chloride at temperatures
higher than 100 °C, but dehydration of aluminium oxide is not
complete until a temperature greater than 1000°C is achieved.
Aluminium oxide formed homogeneously with urea can be
completely dehydrated at about 650°C.

Figure 12-7 Schematic of

thermobalance: A:beam; B:
sample cup and holder, C:
counterweight, D: lamp and
photodiodes; E: coil; F:
magnet: G:control amplifier:
H: tare calculator; I:
amplifier; and J: recorder.
Figure 12-6 Effect of temperature
on precipitate mass
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The thermal curve for calcium oxalate is considerably more

complex than the others shown in Figure 12-6. Below about
135°C, unbound water is eliminated to give the monohydrate
CaC2O4.H2O. This compound is then converted to the
anhydrous oxalate CaC2O4 at 225°C. The abrupt change in mass
at about 450°C signals the decomposition of calcium oxalate to
calcium carbonate and carbon monoxide. The final step in the
curve depicts the conversion of the carbonate to calcium oxide
and carbon dioxide. As can be seen, the compound finally
weighed in a gravimetric calcium determination based on
oxalate precipitation is highly dependent on the ignition
temperature. Therefore, in some cases, calcium is precipitated
as calcium oxalate, filtered, washed, and re-dissolved in acid
and then oxalic acid formed determined titrimetrically to
compute concentration of calcium.
Figure 12-6 Effect of temperature
on precipitate mass
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Operations involved in gravimetric analysis-

techniques of gravimetric analyses
1. Precipitation: The reagent used to bring about precipitation of the desired
analyte is called Precipitant. The precipitant, as far as possible, should be
specific; i.e., should neither form sparingly soluble compounds with other
constituents present nor the precipitate formed be vulnerable to interference of
associated constituents.
The general conditions of precipitation are summarised as under:
Solubility of the precipitate, time and subsequent operations permitting,
precipitation should be carried out in dilute solution to minimise co-
precipitation.

Reference: R C Shah 41
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(ii) Precipitant (in the form of solution) should be added by the side of the precipitation
beaker with the help of pipette or the glass tube, slowly i.e. dropwise with continuous
stirring of the solution. This avoids local concentration of the reagent which generally
leads to contamination of precipitate due to co-precipitation. While stirring care should
be exercised not to scratch sides or bottom of the beaker. Special care should be taken
not to allow the solution to splash, while adding the precipitant or stirring the solution.
(iii) Precipitation is generally effected from the hot dilute solutions as the higher
temperature assists coagulation and discourages the formation of colloidal particles
leading to easily filterable coarse grained large crystals. Moreover, the contamination of
precipitates due to co-precipitation is also lessened. The solution need not be heated to
boiling point but should be kept below the boiling point as, otherwise sudden liberation
of steam due to release of superheating on addition of precipitant solution may results
in the loss of solution leading subsequently, to erroneous results.

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(iv) In quantitative or complete precipitation a sufficient excess of the precipitant is to be

added but unnecessary large excess of it is, however, to be avoided as that may result in
increase in the solubility or contamination of precipitate. After precipitate has settled, a
few drops of precipitant should be added to see the completion of precipitation. If fresh
precipitates are formed, more of the precipitant should be added for complete
precipitation. Ni(DMG)2
(v) The order in which different reagents are added during precipitation should be strictly
followed as that has, sometimes, tremendous influence on the result of the analysis. In
several cases, use is made of the common ion effect to prevent precipitation of interferents
and bring about selective precipitation of the desired metal ion.
(vi) Generally, precipitate should not be filtered immediately after the precipitation but,
should be allowed to stand or better digested (or cooked) at higher temperature because of
following reasons:
(a) Solubility equilibrium may not be reached at once especially with substances having
tendency to form supersaturated solutions.
(b) Digestion has the corrective effect on the practical size of the precipitate as well as
purifying effect.
Digestion has little or no effect on amorphous or gelatinous precipitate.
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2. Filtration and washing of the Precipitate:

The operation involves separation of the precipitate (by filtration) from mother liquor and
washing of the precipitate to remove soluble impurities which contaminate the
precipitate.

Filtration of precipitate is generally carried out using Gooch Crucible or special

quantitative filter papers. One brand available is Whatman® quantitative filter papers.
Whatman quantitative (sometimes termed ‘ashless’ because of negligible weight (0.007 –
0.01%w/w) of ash produced when the filter paper is completely burnt) filter paper is
found satisfactory in practice .The average weight of ash per circle (12.7 mm diameter) of
quantitative filter paper is generally given by the manufacturer on the box containing it
alongwith average pore size (or on its website) or, if desired, can be found by igniting
several circles of filter paper in crucible. Weight of the ash of filter paper should be
deducted from the weight of ignited residue to get the weight of precipitate alone .The
size of filter paper (generally available in circles of diameter 9cm, 11cm, or 12.7cm) to be
chosen is governed by bulk of the precipitate to be collected and not by the volume of
mother liquor to be filtered.

Whatman is registered trademark of GE Healthcare Lifesciences www.gelifesciences.com 44

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The entire precipitate at the end of the operation should, preferably, occupy
one-third capacity filter and never more than one half. Different grades of
filter paper are available for different types of precipitate, largely based on
the particle size that can be retained by the paper.
Funnel selected for the operation should be of proper size. The top of filter
paper, when perfectly set in the funnel should be about 5-15 mm within or
below the rim of the funnel. It should have an apical angle of about 60° and
long stem with internal diameter of 3-5 mm, to increase the rate of filtration.
Much time is lost if funnels are poorly made or filter paper is imperfectly set. Incorrect way
Consequently, the washing of precipitate becomes a lengthy operation
leading to changes in the composition of precipitate, for e.g. the oxidation of
copper sulphide to soluble copper sulphate.

1 fluted filter paper

Appendix (R C Shah) gives possible usage of different grades of the filter paper. 45
45

The filter paper is now moistened with a jet of water from the wash bottle (see fig) and the
upper third is gently pressed against the funnel with clean forefinger. When water is now
poured into the filter, the stem of funnel should fill up. If it does not do so, the end of the stem
is closed with finger and stem allowed of fill until water rises into apex and above. The air
entrapped between funnel and paper is released by pulling the paper gently side at one point.
The paper is then carefully refitted to the funnel all round and
the finger removed; the stem should remain filled with the liquid.
It is essential to have an unbroken column of liquid in the stem
because the weight of column produces gentle suction that
hastens filtration. To carry out filtration, funnel with properly set
filter paper is supported on a funnel stand (which may be
wooden one or metal ring) and a clean beaker is kept under it in
such a way that the stem of the funnel touches the inside of the
beaker to prevent splashing.

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(this is absolutely necessary, if other constituents are to be estimated from the filtrate) and is
well above the bottom of the beaker, so that, the stem may not dip into the filtrate. The beaker
containing liquid to be filtered is brought close to and slightly above the funnel.

The stirring rod , taking care not to allow any liquid to

fall outside the filter, is held vertically so that its lower
end is very close to (but not touching) and directed
towards the side (and not the apex) of filter having
three thicknesses of paper (see fig). The lip of the
beaker is then pressed against the rod and into the
filter without splashing (transference with the help of
glass rod prevents the liquid drops flowing out by the
side of the beaker; quantitative transfer of liquid
without the use of glass rod is inadmissible). The level
of liquid in the funnel should not rise above the point
2-3 mm down the top of the filter paper.

image courtesy: http://chemwiki.ucdavis.edu 47

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After all the precipitates are transferred to the filter paper, at once the washing
of the precipitate is started.
After say 8-10 washings, the filtrate is tested for the completeness of washing.
E.g. complete removal of chloride from the precipitate, reflected in the filtrate, is
tested by adding silver nitrate solution to the test solution (filtrate). If the
washing is over, as indicated by the negative test of soluble impurities in the final
filtrate, washing is discontinued and the filter is allowed to drain completely
before being subjected to subsequent operation of drying the precipitate.
The wash liquid used in the above operation is chosen by taking several factors
into consideration; such as solubility of precipitate in wash liquid, which should
be least, its effect on the determination of other constituents from the filtrate
and its effect on the physical state of precipitate.

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B
3. Drying, Ignition and weighing of precipitate:
Drying of the precipitate- This is effected by heating of the funnel with the
precipitate at a temperature of about 100°C in an oven. Funnel with precipitate
is covered by a paper folded down its rim and placed in the oven. The funnel is
removed from the oven when the precipitate and filter paper appear
completely dry. In cases where wet ignition is permissible, drying operation is
not generally necessary, e.g., precipitates of hydrous iron(III) oxide.
Ignition of the precipitate: the operation is carried out in crucible (A). Porcelain
crucibles find frequent use in instructional courses because of their low cost
and they can also be heated to a temperature of about 1000°C; silica crucibles
because of their greater resistance to thermal shock are preferable though
they are more expensive. In industry, for several gravimetric determinations,
crucibles made up of nickel or platinum are used.
A

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B
Incineration of filter paper apart from the precipitate:
If the carbon of paper or the gases of its combustion affect chemical
composition of the precipitate, it should be incinerated after separating
from the precipitate. For this, the dried ppt is carefully transferred to the
pre-weighed crucible, and then filter paper, while being held using a
platinum wire over the crucible, is burnt such that any particle from the
burning paper falls into the crucible. Finally, the charred paper is kept in
crucible and the crucible is placed on low flame.
After the paper has completely burnt out, the ppt is ignited on high
flame for specific time, till the definite composition of the ppt is A
achieved. Then the crucible is placed in to the desiccator and allowed to
cool, followed by its weighing. A muffle furnace, if available, is used in C
place of burner for ignition of the precipitates.
A – clay pipe triangle, used to hold crucible for heating on burner; alternately, metal wire
triangle is also used, as shown in B and C.

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Desiccator and desiccant

A desiccant is a hygroscopic substance that is used to induce or sustain a
state of dryness (desiccation) in its vicinity C

A Desiccator is an airtight or sealable enclosure, generally made up of glass,

which can be used to store substances or crucible in near dry (moisture free)
conditions. It contains, at bottom, a material called desiccant which
performs this job. Above this material, a ceramic plate acts as platform on
which crucible or substance to be stored can be placed. Commonly used
desiccants are: anhydrous calcium chloride, silica gel etc. These have strong
affinity for moisture present in air, hence in closed space, the moisture gets A
nearly completely absorbed / adsorbed by the desiccant and the air inside
the enclosure is almost free from moisture.
Image A: Glass desiccator with desiccator plate; B: desiccator plate; C:
indicating silica gel

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Calculations:
The results of a gravimetric analysis are generally computed from two
experimental measurements: the mass (volume) of sample and the mass of a
product (ppt) of known composition. The examples that follow illustrate how
such computations are carried out.
Example 12.1
The calcium in a 200.0-mL sample of a natural water was determined by
precipitating the cation as CaC2O4. The precipitate was filtered, washed, and
ignited in a crucible with an empty mass of 26.6002 g. The mass of the crucible
plus CaO (56.0n g/moI) was 26.7134 g. Calculate the concentration of Ca (40.078
g/mol) in water in units of grams per 100 mL of the water.
The mass of CaO is 26.7134 g - 26.6002 g = 0.1132 g
The number of moles Ca in the sample is equal to the number of moles CaO or

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Example 12.2:
An iron ore was analyzed by dissolving a 1.1324-g sample in concentrated HCl.
The resulting solution was diluted with water, and the iron(lII) was precipitated as
the hydrous oxide Fe2O3.xH2O by the addition of NH3. After filtration and
washing, the residue was ignited at a high temperature to give 0.5394 g of pure
Fe2O3 (159.69 g/mol). Calculate (a) the % Fe (55.847 g/mol) and (b) the % Fe3O4
(231.54 g/mol) in the sample.
For both parts of this problem, we need to calculate the number of moles of
Fe2O3, Thus,

(a) The number of moles of Fe is twice the number of moles of Fe2O3, and

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(b) As shown by the following balanced equation, 3 mol of Fe2O3 are chemically
equivalent to 2 mol of Fe3O4, That is,

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Applications of Gravimetric methods

Gravimetric methods have been developed for most inorganic anions and cations, as
well as for such neutral species as water, sulfur dioxide, carbon dioxide, and iodine. A
variety of organic substances can also be easily determined gravimetrically. Examples
include lactose in milk products, salicylates in drug preparations, phenolphthalein in
laxatives. nicotine in pesticides, cholesterol in cereals, and benzaldehyde in almond
extracts. Indeed, gravimetric methods are among the most widely applicable of all
analytical procedures.
Inorganic Precipitating Agents: Table 12-2 lists common inorganic precipitating agents.
These reagents typically form sIightly soluble salts or hydrous oxides with the analyte.
As you can see from the many entries for each reagent, few inorganic reagents are
selective.
Reducing Agents: Table 12-3 lists several reagents that convert an analyte to its
elemental form for weighing.

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Table 12.2 Some Inorganic Precipitating Agents

Table 12.3 Some Reducing Agents Employed in
Precipitating Agent Element Precipitated*
Gravimetric Methods
Be (BeO), Al (AI2O3), Sc (Sc2O3), Cr (Cr2O3)Ϯ, Fe
NH3 (aq) (Fe2O3), Ga (Ga2O3), Zr (ZrO2), In (ln2O3), Sn (SnO2), Reducing Agent Analyte
U (U3O8)
SO2 Se, Au
Cu (CuO)Ϯ, Zn (ZnO. or ZnSO4), Ge (GeO2), As
SO2 + H2NOH Te
H2S (As2O3, or As2O5), Mo (MoO3), Sn (SnO2)Ϯ Sb
(Sb2O3), or Sb2O5 ), Bi (Bi2S3) H2NOH Se
(NH4)2S Hg ( HgS ), Co (Co3O4) H2C2O4 Au
Mg (Mg2P2O7), Al (AlPO4 ), Mn (Mn2P2O7), Zn H2 Re, Ir
(NH4)2HPO4
(Zn2P2O7), Zr (Zr2P2O7), Cd (Cd2P2O7), Bi (BiPO4) HCOOH Pt
H2SO4 Li, Mn, Sr, Cd, Pb, Ba (all as sulfates) NaNO2 Au
H2PtCI6 K (K2PtCl6, or Pt), Rb ( Rb2PtCl6) , Cs ( Cs2PtCI6) SnCl2 Hg
H2C2O4 Ca (CaO), Sr (SrO), Th (ThO2) Co, Ni, Cu, Zn, Ag, In,
Electrolytic reduction
(NH4)2MoO4 Cd (CdMoO4)Ϯ, Pb ( PbMoO4) Sn, Sb, Cd, Re, Bi
Ag (AgCl), Hg (Hg2Cl2), Na (as NaCl from butyl
HCI
alcohol), Si (SiO2)
AgNO 3 CI (AgCl), Br ( AgBr) , I ( AgI )

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Organic Precipitating Agents: Numerous organic reagents have been developed for the
gravimetric determination of inorganic species. Some of these reagents are significantly more
selective in their reactions than are most of the inorganic reagents listed in Table 12-2. We
encounter two types of organic reagents. One forms slightly soluble non-ionic products called
coordination compounds; the other forms products in which the bonding between the inorganic
species and the reagent is largely ionic. Organic reagents that yield sparingly soluble
coordination compounds typically contain at least two functional groups (bidentate ligands).
Each of these groups is capable of bonding with a cation by donating a pair of electrons. The
functional groups are located in the molecule such that a five- or six-membered ring results
from the reaction. Reagents that form compounds of this type are called chelating agents, and
their products are called chelates.
Metal chelates are relatively nonpolar and as a consequence, have solubilities that are low in
water but high in organic liquids. Usually, these compounds possess low densities and are often
intensely colored. Because they are not wetted by water, coordination compounds are easily
freed of moisture at low temperatures. Two widely used chelating reagents are described in the
paragraphs that follow.

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8-Hydroxyquinoline (oxine): Approximately two dozen cations form sparingly soluble chelates
with 8-hydroxy-quinoline. The structure of magnesium 8-hydroxyquinolate is typical of these
OH
chelates. (shown in A). This is a bis- complex of Mg and oxine – two ligands in complex. N
The solubilities of metal 8-hydroxyquinolates vary widely from cation to cation and are pH
dependent because 8-hydroxyquinoline is always deprotonated during chelation reaction.
Therefore, we can achieve a considerable degree of selectivity in the use of 8-hydroxyquinoline
by controlling pH.
Dimethylglyoxime: Dimethylglyoxime (DMG) is an organic precipitating agent of unparalleled
specificity. Only nickel(Il) is precipitated from a weakly alkaline solution. The reaction is shown in
B. This precipitate is so bulky that only small amounts of nickel can be handled conveniently. It
also has an exasperating tendency to creep up the sides of the container as it is filtered and
washed. The solid is conveniently dried at 110°C and has the composition indicated by its
formula, Ni(DMG)2. this is a bis- complex of Ni and DMG.
A B

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Even the Ni(DMG)2 (pink colour) and may metal oxinates can be easily A
extracted into solvents like chloroform or n-hexane (solvent
extraction) and spectrophotometric determination can be performed
to find out concentration. This forms the basis for several such
determinations.

Sodium Tetraphenylborate (A): Sodium tetraphenylborate, (C6H5)4B−Na+, is an important

example of an organic precipitating reagent that forms salt-like precipitates. In cold mineral acid
solutions, it is a near-specific precipitating agent for potassium and ammonium ions. The
precipitates have stoichiometric composition and contain one mole of potassium or ammoniurn
ion for each mole of tetraphenylborate ion: these ionic compounds are easily filtered and can be
brought to constant mass at 105°C to 120°C. Only mercury(II), rubidium, and cesiurn interfere
and must be removed by prior treatment. (Q. how do Hg(II), Rb(II) and Cs(II) interfere?)
Organic Functional Group Analysis: Several reagents react selectively with certain organic
functional groups and thus can be used for the determination of most compounds containing
these group. A list of gravimetric functional group reagents is given in Table 12-4. Many of the
reactions shown can also be used for volumetric and spectrophotometric determinations.

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Apparatus used in Gravimetry

balance – care and use of analytical balance, crucible, desiccator, burner, oven
Burner: The Bunsen burner is named after Robert Wilhelm Bunsen, though it was not invented
by him! Bunsen, a German chemist, improved the burner's design to aid his endeavors in
spectroscopy.
Most of the laboratories use natural gas as fuel and air as oxidant for Bunsen burner. Near the
bottom, the burner has holes for introduction of air; these holes can be closed completely or
partially by rotating screw over them. By closing the holes at the base of the burner, all of the
oxygen used for burning comes from the space near the top of the barrel. The temperature is
lower. A quiet flame is formed. Combustion is not complete; elemental carbon, called lamp
black, is produced. This is also called soot. The particles of carbon are heated in the flame to give
a yellow color. Much more visible light is given off from this flame than a blue flame. The yellow
flame is called a luminous flame or reducing flame due to presence of free carbon and carbon
monoxide. When the holes at base are completely open, there is complete combustion of the
gas, giving blue or non-luminous flame, also called oxidizing flame.

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The non-luminous flame consists of three parts:

an inner, blue cone, consisting largely of un-burnt gas;
a luminous tip of the inner cone (this is only visible
when the air holes are slightly closed); and
an outer mantle in which complete combustion of the
gas occurs.
The lowest temperature is at the base of the flame –
this is used for testing volatile substances to
determine whether they impart any colour to the
flame. The hottest part of the flame is the fusion zone
that lies at about one third of the height of the flame
and approximately equidistant from the outside and
inside of the outer mantle – this is used for testing the
fusibility of the substances or ignition of ppt.

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Do not let any solution / liquid / solid

fall on the burner, burner tube; this
may cause damage to tubing / metal
parts of the burner, cause corrosion
and blockage.
Crucible – described earlier
Desiccator – described earlier
Hot air oven – used for drying of ppt in
funnel after washing is over, ensure
that no liquid is dripping from funnel
while placing it in oven A

Meker burner (A) produces multiple open gas

flames, used for heating, sterilization, and
combustion. It is used for ignition of
precipitates at higher temperatures of 1100 –
Meker burner top part 1200 °C, whereas bunsen burner can achieve
temperatures of 800 – 1000 °C.
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Hot air / microwave oven

Microwave oven takes shorter

times for drying ppt provided ppt
is stable

For drying ppt in hot air oven, set to a temp of 105 – 110 °C for drying of ppt in funnel / gooch crucible

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Calibration and care of equipment for Weight Measurements:

A balance is an instrument used in laboratories to measure the mass or weight of a body. A balance
functions by measuring the force of gravity that the earth exerts on an object, i.e., its weight. Since the
mass of an object is directly proportional to its weight, a balance can also be used to measure mass.
There are various balances with varied degrees of sensitivity as follows:
•Physical balance.
•Analytical balance (Two Pan Chemical balance)
•Triple beam balance.
•Torsion type balance.
•Single pan electronic balance (Top loading).
Amongst above all types of balances, generally 'analytical balance' is used for quantitative analysis.

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The Analytical Balance or the Two Pan Balance: Also called The Equal-Arm Balance or
the Beam balance. In this simplest type of balance there is an application of a lever. A
uniform bar, the beam, is suspended at its exact centre on a knife-edge set at right
angles to it. The point of support is called the fulcrum. Two pans of equal weight are
suspended from the beam, one at each end, at points equidistant from the fulcrum.
Since the centre of gravity of a uniform bar is at its midpoint, the beam supporting the
pans will be in equilibrium, i.e., will balance on the knife-edge. A long pointer attached
at right angles to the beam at the fulcrum indicates zero on a scale when the beam is at
rest parallel to a level surface. It shows also the extent of swing of the beam on one
side or the other, acting somewhat as a pendulum, when the beam is coming to rest.
The object to be weighed is placed on one pan, and standard weights are added to the
other until the balance of the beam is established again. The unknown weight can then
be determined by adding up the standard weights in the pan. This balance can weigh up
to fourth decimal place with the help of rider. The standard weights need calibration on
regular intervals.

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Digital balance: this is also called electronic balance and is single pan top loading
balance. After setting zero on empty pan, on placing an object to be weighed on
it, the weight is directly seen on digital output display. This type of balance
requires regular calibration using certified standard weights.

The Single-Pan Mechanical Analytical Balance Components: Although they differ

considerably in appearance and performance characteristics, all mechanical
balances, equal-arm as well as single-pan, have several common components.
Figure 2-4 is a diagram of a typical single-pan mechanical balance. Fundamental
to this instrument is a lightweight beam that is supported on a planar surface by a
prism-shaped knife edge (A) attached to the left end of the beam is a pan for
holding the object to be weighed and a full set of masses held in place by
hangers. These masses can be lifted from the beam one at a time by a mechanical
arrangement that is controlled by a set of knobs on the exterior of the balance
case. The right end of the beam holds a counterweight of such size as to just
balance the pan and masses on the left end of the beam. Single pan balance
description for information

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A second knife edge (B) is located near the left end of the beam
and support as a second planar surface, which is located in the
inner side of a stirrup that couples the pan to the beam. The two
knife edges and their planar surfaces are fabricated from
extraordinarily hard material (agate or synthetic sapphire) and
form two bearings that permit motion of the beam and pan with
a minimum of friction. The performance of a mechanical balance
is critically dependent on the perfection of these two bearings.
Single-pan balances are also equipped with a beam arrest and a
pan arrest. The beam arrest is a mechanical device that raises
the beam so that the central knife edge no longer touches its
bearing surface and simultaneously frees the stirrup from
contact with the outer knife edge. The purpose of both arrest
mechanisms is to prevent damage to the bearings while objects
are being placed on or removed from the pan. When engaged,
Figure 2-4 Single-pan mechanical
the pan arrest supports most of the mass of the pan and its
analytical balance.
contents and thus prevents oscillation. Both arrests are
controlled by a lever mounted on the outside of the balance case
and should be engaged whenever the balance is not in use.

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Handling and care of balances:

Good weighing practices require you to:
•Keep your balance clean. Cleanliness reduces error.
•Place balance on firm surface, free from vibrations
•Level the balance
•Protect from drafts of air
•Do not set up in direct sunlight
•Never place a wet container on the scales.
•Never place or allow chemicals directly on the pan.
•Use papers boats or pans for weighing solids.
•When you have finished weighing, clean the balance with a brush or a piece of chamois leather to
remove possible spillage or other dirt.
•Never change balances in the middle of an experiment.

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Handling and care of standard weights

•Remove dust with (camel hair) brush
•Never touch weights
•Fingerprints are acidic and greasy
•Polish the weights with cotton or chamois (free from fibre)
•Use Alcohol to remove absorption layer or grease
•Store the Standards weight box in clean and dry place.
•While using fractional weights (i.e., weights less than 1 g) care must be taken not to place them at
dirty place. These weights should be handled using clean forceps meant for the purpose.

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Handling samples to be weighed:

If the objects weighed (sample/container) are too warm, the value displayed will be too low; if too cold,
then the value will be too high. Object being weighed must be at room temperature.
Object being placed on the pan must be placed at centre. In case of weights, heaviest weight must be at
the centre of the pan and lighter ones around it.
Calibration of weights: Weights used for weighing substances or crucible on a two pan balance may not
be of the exact weight designated hence knowing their true weight is important. Also, weights used for
weighing are subject to wear and corrosion during use and environmental factors; hence their weight
may differ from designated value. For example, after use, a 1.000 g weight may actually weigh 0.995 g,
introducing an error of 0.005 g during each use! It is necessary therefore to verify its designated weight
by comparison with a standard weight periodically. Standard weights are available from several agencies,
for example, National Physical Laboratory (NPL). Such weights come with a certificate of precision
associated with their use and hence are called certified weights. These can be used to calibrate a single
pan balance or to calibrate weights using a two pan chemical balance.

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