Separation Techniques:

Separating Components of a Mixture

Purpose

The purpose of this experiment is to separate a mixture of NaCl, NH4 Cl, and SiO2 into the three components
by sublimating the NH4 Cl will be sublimed, extracting the NaCl will be extracted into water, and drying the
remaining SiO2 .

Learning Objectives
Describe the separation techniques of decantation, filtration, extraction, and sublimation.

Define homogeneous and heterogeneous mixtures.

Separate a mixture of NaCl, NH4 Cl, and SiO2 into the three components.

Calculate a percent composition for each component and a percent recovery of the total.

Laboratory Skills
Perform a decantation.

Perform a gravity filtration.

Perform an extraction.

Perform a sublimation.

Follow a flowchart for a procedure.

Calculate percent recovery.

Equipment Chemicals
Balance 50 or 100 mL silicon dioxide unknown mixture of
Crucible tongs graduated cylinder ammonium chloride sodium chloride
Clay triangle or wire Watch glass (NH4 Cl) (NaCl)
gauze Ring stand
Bunsen burner and Glass stirring rod
hose

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Introduction

Mixtures

Most of the matter people encounter in everyday life consists of mixtures of different substances. Mixtures are
combinations of two or more substances in which each substance retains its own chemical identity and there-
fore its own properties. Whereas pure substances have fixed compositions, the composition of mixtures can vary.
For example, a glass of sweetened tea may contain little or a lot of sweetener. The substances making up a mix-
ture are called components. Mixtures such as cement, wood, rocks, and soil do not have the same composition,
properties, and appearance throughout the mixture. Such mixtures are called heterogeneous. Mixtures that are
uniform in composition, properties, and appearance throughout are called homogeneous. Homogeneous mix-
tures are also called solutions. Such mixtures include sugar-water solution, and air. Mixtures are characterized
by two fundamental properties:

• Each of the substances in the mixture retains its chemical identity.

• Mixtures are separable into these components by physical means.

If one of the substances in a mixture is in excess, it is an impure substance containing impurities (that is, the
minor components).

Separating the Components of a Mixture

The preparation of compounds usually involves their separation or isolation from reactants or other impurities.
Thus, the separation of mixtures into their components and the purification of impure substances are common
problems, not just in chemistry but in everyday problems. For example, drinking water usually begins as a mixture
of silt, sand, dissolved salts, and water. Because water is by far the largest component in this mixture, it is usually
called impure water. How is it purified? The separation of the components of mixtures is based upon the fact
that each component has different physical properties.

The components of mixtures are substances, either compounds or elements, and each substance possesses a
unique set of properties. The properties of every sample of a substance are identical under the same conditions
of temperature and pressure. This means that once you have determined that a sample of sodium chloride (table
salt), NaCl, is water soluble and a sample of silicon dioxide (sand), SiO2 , is not, you realize that all samples of
sodium chloride are water-soluble, and all samples of silicon dioxide are not.

Likewise, every crystal of a pure substance melts at a specific temperature and a given pressure, and every pure
substance boils at a specific temperature and a given pressure.

Although numerous physical properties can be used to identify a particular substance, this experiment involves
only the separation of the components and not their identification. The methods used for the separation depend

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 Separating Components of a Mixture

upon differences in physical properties, and include the following:

• Decantation. This is the process of separating a liquid from a solid (sediment) by gently pouring the
liquid from the solid so as not to disturb the solid.(Figure MX.1)
• Filtration. This is the process of separating a solid from a liquid by means of a porous substance-
a filter-which allows the liquid but not the solid to pass through (see Figure MX.1.) Common filter
materials are paper, layers of charcoal, and sand. Silt and sand can be removed from drinking water by
this process.

Figure MX.1: Difference between decantation and filtration

• Extraction. This is the separation of a substance from a mixture by preferentially dissolving that sub-
stance in a suitable solvent. By this process, a soluble compound is usually separated from an insoluble
compound.
• Sublimation. This is the process in which a solid is converted directly to the gaseous state and back
to the solid state without the appearance of the liquid state. Not all substances possess the ability to be
sublimed. Iodine, naphthalene, and ammonium chloride (NH4 Cl) are common substances that easily
sublime.

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 Separating Components of a Mixture

Calculating Percent Composition and Percent Recovery

At the end of the laboratory, the mass of each component from the mixture is used to calculate the percent
composition of that component, as shown in Example MX.1.

Example MX.1: Calculating Percent Composition

What is the percentage of SiO2 in a 2.56 g sample mixture if 1.25 g of SiO2 has been recovered?
The percentage of each substance in such a mixture can be calculated using Equation MX.1:

mass of component
% component = × 100% (Equation MX.1)
mass of sample in grams

Therefore, the percentage of SiO2 in this particular sample mixture is as follows:

1.25 𝑔
% SiO2 = × 100% = 48.8%
2.56 𝑔

The combined masses of all components is used to calculate the percent recovery, according to Equation MX.2.

𝑔 NaCl + 𝑔 NH4 Cl + 𝑔 SiO2

percent recovery = × 100 (Equation MX.2)
g mixture

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 Separating Components of a Mixture

Procedure

Safety Precautions
Always wear safety glasses.

Use caution when heating substances.

The mixture you will separate contains three components: NaCl, NH4 Cl, and SiO2 . The separation will be accom-
plished by heating the mixture to sublime the NH4 Cl, extracting the NaCl with water, and drying the remaining
SiO2 , as illustrated in Figure MX.2

Figure MX.2: Flow diagram for the separation of the components of a mixture

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 Separating Components of a Mixture

1. Clean and dry two evaporating dishes. Label them 1 and 2.

2. Record the mass of evaporating dish #1 to the nearest 0.001 g on the report sheet.

3. Obtain from your instructor a sample of the unknown mixture. Write the unknown number on your
report sheet. If you obtain your unknown from a bottle, shake the bottle to make the sample mixture as
uniform as possible. Add between 0.8 to 1.0 g of the sample to the evaporating dish, recording the exact
sample mass to the nearest 0.001 g.

Figure MX.3: Correct assembly of the evaporating dish on the ring

stand

4. In the fume hood, assemble the setup shown in Figure MX.3, consisting of a clay triangle (or wire gauze), ring
and ring-stand. Place the evaporating dish containing the mixture on the clay triangle (or wire gauze). Heat
the evaporating dish gently with a Bunsen burner until white fumes no longer form (about 15 min). Heat
carefully to avoid spattering. Occasionally, gently shake the evaporating dish, using crucible tongs during
the sublimation process to ensure sublimation is complete.

Do not use a watch glass as a lid in the sublimation step!

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 Separating Components of a Mixture

5. Allow the evaporating dish to cool until it reaches room temperature; then weigh the evaporating dish with
the contained solid. The loss in mass represents the amount of NH4 Cl in your mixture. Calculate and record
the mass lost. Never weigh hot or warm objects.

6. Record the mass of evaporating dish #2 and separately, the mass of a watch glass to use as a lid.

7. Measure 25 mL of DI water in a graduated cylinder.

8. Remove the salt from the sand by adding small portions (2-3 mL) of DI water (from the graduated cylinder)
to the sand-salt mixture in evaporating dish #1. With a stirring rod gently, stir the mixture. Decant the liquid
carefully into the evaporating dish #2, which you have weighed, being careful not to transfer any of the solid
into evaporating dish #2.

9. Add more DI water to the solid in evaporating dish #1, stir, and decant this liquid into evaporating dish
#2 as before. Repeat the process a total of three times, using no more than 25 mL of DI water. This process
dissolves (extracts) the NaCl from the sand. You now have two evaporating dishes - one containing wet sand,
#1, and the other containing a solution of sodium chloride, #2.

10. Carefully place evaporating dish #2, which contains the sodium chloride solution, on the clay triangle on the
ring stand. Begin heating the solution gently to evaporate the water. Take care to avoid boiling or spattering,
especially when liquid is present.

NOTE When drying both the NaCl and SiO2 , use a pre-weighed watch glass on top of the
evaporating dish. Heat slowly and do not flame the edges of the watch glass that extend
beyond the edge of the evaporating dish.

11. Near the end of the process, cover the evaporating dish with the watch glass that was weighed with evaporat-
ing dish #2 and reduce the heat to prevent spattering. When you have dried the sodium chloride completely,
no more water will condense on the watch glass and it too will be dry.

If you have another Bunsen burner available, you may proceed to dry the SiO2 in evapo-
rating dish #1 as explained in step 13 while the water is evaporating.

12. Let the evaporating dish and watch glass cool to room temperature on a wire gauze and weigh them. The

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 Separating Components of a Mixture

difference between this mass and the mass of the empty evaporating dish and watch glass is the mass of the
NaCl. Calculate this mass.

13. Place evaporating dish #1, containing the wet sand, on a clay triangle on a ring stand and cover the evaporat-
ing dish with a clean, dry watch glass. Heat slowly at first until the lumps break up and the sand appears dry.
Then heat evaporating dish #1 to dull redness, maintaining this heat for 10 min. Take care not to overheat
the dish; otherwise, it will crack. When the sand is dry, remove the heat and let evaporating dish #1 cool to
room temperature. Weigh evaporating dish #1 with the dry sand after it has cooled to room temperature. Be
sure to not include the watch glass when weighing. The difference between this mass and the mass of the
empty dish is the mass of the sand. Calculate this mass. Dispose of the sand in the marked container.

14. Calculate the percentage of each substance in the mixture using an approach similar to that shown in Ex-
ample MX.1.

If the experiment is carried out correctly and carefully, the combined total of your three components should
be approximately 99%. If it is less than 99%, you have been sloppy. If it is more than 100%, you have not
sufficiently dried the sand and salt.

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 Name:
Report Sheet:
Section: Date: Separating Components of a Mixture

Unknown number

Determination of the Mass Percent of NH4 Cl Recovered from the Mixture

Mass of evaporating dish #1
Mass of evaporating dish and original sample
Mass of original sample
Mass of evaporating dish after subliming NH4 Cl
Mass of NH4 Cl
Percent by mass of NH4 Cl
Show calculation of percent NH4 Cl∶

Determination of the Mass Percent of NaCl Recovered from the Mixture

Mass of evaporating dish #2
Mass of watch glass
Mass of evaporating dish #2, watch glass, and NaCl
Mass of NaCl recovered
Percent by mass of NaCl
Show calculation of percent NaCl∶

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To access our full list of experiments visit [Link] Lab Version MX Release 3.28. MX.1
 Separating Components of a Mixture Report Sheet

Determination of Mass Percent of SiO2 Recovered from the Mixture

Mass of evaporating dish #1
Mass of evaporating dish #1 with dry sand
Mass of SiO2 recovered
Percent of SiO2
Show calculation of percent SiO2 ∶

Calculating Percent Recovery

Mass of original sample
Total Experimental mass determined of (NH4 Cl + NaCl + SiO2 )
Differences between these masses
g experimental mass determined
Percent recovery of sample = × 100%
g of original sample

Show calculation of percent recovery∶

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