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Chem 01 Exp #1 Separation and Analysis of a Ternary Mixture

Pre-laboratory Assignment
Before coming into the laboratory, put the following information into your laboratory notebook.
a. Title of Experiment
b. Purpose of Experiment
c. Procedure (reference)
Also, draw Table 2 in your laboratory notebook (this will be completed during the experiment).
Introduction
Mixtures are defined as material consisting of two or more substances mixed together with each
component retaining its original properties and separable by physical means. In a homogeneous
mixture, the composition is uniform throughout the sample. In a heterogeneous mixture, the
composition is not uniform throughout the sample. If one component in the mixture has greater
prevalence than the others, this would be called an impure substance with the other called the
impurities.
There are many laboratory techniques that exploited the differences in physical and chemical
properties of the components of the mixture and allow for the separation of the individual components
(as shown in Fig 1).
Fig 1 Separation Techniques: Decanting and Filtering

Decanting Filtering
2


Decantation: The process of separating a liquid substance from a settled solid substance by carefully
pouring the liquid from the solid without disrupting the solid.


Dissolution: The molecular dispersion of a solid in a liquid substance; for example, the process of
dissolving sugar in water.


Evaporation: The process of converting a liquid into a vapor leaving only the dry solid portion.


Filtration: The process of separating a heterogeneous mixture in which the mixture is poured into a
funnel equipped with filtering paper. The solid is retained in the filter paper while the
liquid is collected in a separate container.


Sublimation: The direct transformation of a solid into a gaseous state without passing through the
liquid state.


In this lab, a mixture of solid sodium chloride (NaCl), ammonium chloride (NH
4
Cl), and silicon
dioxide (SiO
2
, sand) will be separated into individual components. The differences in their physical
and chemical properties will be used in the separation process (see Table 1). The techniques of
sublimation, extraction, and decantation will be used to separate the components of the mixture (see
Fig 2).


Table 1 Chemical and Physical Properties
Substance Soluble in H
2
O (25
o
C) Sublimes (1 Atm)
SiO
2
(sand) No No
NaCl 0.34 g/mL No
NH
4
Cl 0.28 g/mL Yes




3
Fig 2 Separation of a Ternary Mixture

Mixture: SiO
2
(s), NaCl (s), NH
4
Cl (s)
SiO
2
(s), NaCl (s)
heat with Bunsen burner flame (> 500
o
C) in hood
solid
NH
4
Cl (g)
vapor
SiO
2
(s)
insoluble in water
NaCl (aq)
soluble in water
sublimation
extraction add water and decant
gently evaporate water using hotplate
evaporating dish #1
evaporating dish #1 evaporating dish #2
vaporized
NaCl (s)
evaporating dish #2



Procedure
In the hood, heat a clean evaporating dish using a Bunsen burner (and the clay triangle and
iron ring apparatus, as shown in Fig 3), removing any contaminates from the outside of the dish. Let
the dish cool and carefully weigh the dish to the nearest 0.001 g. Measure 2-3 g of the unknown
mixture into the evaporating dish. Record (see Table 2) the weight of the dish and mixture to the
nearest 0.001 g.


4
In the hood, place the evaporating dish containing the mixture on the clay triangle (see Fig 3).
Carefully, heat the evaporating dish with the burner and continue until no more white vapor is
produced (approximately 15 min). Stir occasionally with a glass stirrer to be sure all of the NH
4
Cl has
vaporized. Once the sublimation is complete allow the dish to cool on a cooling pad on the lab bench
top. With the dish at room temperature, weigh the evaporating dish containing the remaining mixture.
Record (see Table 2) the weight to the nearest 0.001 g.

Fig 3 Sublimation Apparatus



Add 5.0 mL of deionized water to the mixture in the evaporating dish and stir gently for 5 min. Obtain
another evaporating dish. Clean, heat, cool, and weigh the dish as done previously. Also, weigh a
clean, dry watch glass and set aside for later use. On the bench top, use a hotplate to heat water in a
beaker. If using a 9 cm evaporating dish, use a 400-mL beaker about half full of water. If using a 10
cm evaporating dish, use a 600-mL beaker about half full of water. Check to be sure that the
evaporating dish fits securely at the top of the beaker before continuing (as shown in Fig 4).

Fig 4 Evaporation of Water



5
Decant the solution from the first evaporating dish into the second dish. Again, add 5.0 mL of
deionized water to the mixture in the first evaporating dish, stir gently for 5 min, and again decant into
the second dish. Repeat with an additional 5 mL of water.

With the extraction steps complete, place the evaporating dish containing the aqueous sodium chloride
solution on top of the beaker of boiling water (as shown in Fig 4). Gently, evaporate all of the water
from the dish. Take care to avoid spattering and use the pre-weighed water glass if needed to catch any
spatter. Occasionally stir with a glass stirrer. Once the sample is dry, allow the dish to cool on a
cooling pad on the lab bench top. With the dish at room temperature, weigh the evaporating dish
containing the sodium chloride. Record (see Table 2) the weight to the nearest 0.001 g. If the watch
glass was used, obtain the weight of the spattered covered watch glass and record in Table 2.

Place the evaporating dish containing the sand directly on the hotplate and gentle evaporate any
remaining water. Occasionally stir with a glass stirrer. Once the sample is dry, allow the dish to cool
on a cooling pad on the lab bench top. With the dish at room temperature, weigh the evaporating dish
containing the sand. Record (see Table 2) the weight to the nearest 0.001 g.

Questions
1. What distinguishes a mixture from an impure substance?
2. Define the process of sublimation.
3. How do decantation and filtration differ? Which should be faster?
4. Why does one never weigh a hot object?
5. How does this experiment illustrate the principle of conservation of matter?
6. A mixture was found to contain 3.10 g of SiO
2
, 0.38 g of cellulose, and 6.72 g of calcium
carbonate. What is the percentage of CaCO
3
in this mixture?
6

Table 2 Separation and Analysis of a Ternary Mixture Data Table
Weight of evaporating dish and original sample g
Weight of evaporating dish g
Weight of original sample g
Weight of evaporating dish after subliming NH
4
Cl g
Weight of NH
4
Cl g

Percent of NH
4
Cl (show calculations)
g
g
100% = % NH
4
Cl

%
Weight of evaporating dish, watch glass, and NaCl g
Weight of evaporating dish and watch glass g
Weight of NaCl g

Percent of NaCl (show calculations)
g
g
100% = % NaCl

%
Weight of evaporating dish and SiO
2
g
Weight of evaporating dish g
Weight of SiO
2
g

Percent of SiO
2
(show calculations)
g
g
100% = % SiO
2

%
Weight of original sample g
Weight of determined sample (NH
4
Cl + NaCl + SiO
2
) g
Differences in these weights g

Percent recovery of matter (show calculations)
g
g
100%
= % recovery of matter
matter recovered
original sample


%


Before leaving the laboratory, submit the copy pages from your laboratory notebook to your
teaching assistant.