Experiment 2: Separation of a Mixture

Prelab:
A general outline of the experimental procedure must be completed in your laboratory notebook
before your lab period. Additionally, a 10-point prelab quiz on Canvas is due 15 minutes before
the start of your laboratory period.

Safety Notes:
This lab involves open flames. Hair MUST be pulled back tight and secured so there is no
chance of catching hair on fire. If you have to be reminded repeatedly to secure your hair, or are
observed being careless with respect to the Bunsen burner, you will be dismissed from the lab.
This includes, but is not limited to, leaving a lit Bunsen burner unattended or reaching over a lit
Bunsen burner. If you are dismissed, you will not be allowed to make up the lab. Do not adjust
hair/touch face with gloves on.

Introduction:
When two or more non-reactive chemicals exist together, this is called a mixture. Mixtures may
be homogeneous (the same throughout, like the air we breathe) or heterogeneous (different
throughout, such as chicken noodle soup). If the chemicals do not react with one another, i.e.
and no bonds are formed or broken, the components of the mixture will maintain their unique
physical properties. As a result, differences between the physical properties of the compounds
can be used to separate them from one another. The most common separation strategies are
those associated with solubility, sublimation, and melting/boiling points.

Solubility is the ability of a compound (solute) to fully integrate into a larger amount of other
compound (solvent). As the age-old saying goes, “like dissolves like,” so polar species are
soluble in polar solvents (i.e. sugar into water), and nonpolar species tend to be soluble in
nonpolar solvents (i.e. oil in hexane).

Sublimation is the process by which a substance changes from a solid directly into a gas. Not
every compound can undergo sublimation at atmospheric pressures, and high temperature is
typically required. Because of these reasons, sublimation is most commonly used for inorganic
complexes or salts.

Melting point is the temperature at which a compound will convert from a solid to a liquid at
normal atmospheric pressure.

Boiling point is the temperature at which a compounds vapor pressure is equal to the total
pressure. **This is not the point where the whole sample will convert to a gas at once!

For this experiment, you will be given a mixture of sand (SiO2), table salt (NaCl) and
ammonium chloride (NH4Cl). The important properties for their separation are in Table 1. Once
each component is separated and isolated, the percent composition by mass of each compound
will be calculated.

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 Experiment 2: Separation of a Mixture

Table 1: Physical Properties of Mixture Components

sand (SiO2) salt (NaCl) NH4Cl
water soluble? no yes yes
melting point (°C) 1723 801 N/A
boiling point (°C) N/A N/A 340

Procedure: (In general, the separation process is illustrated in Figure 1 below.)

I. Acquire an unknown sample of the mixture.
II. Use your small beaker and the mass by difference method to calculate the mass of the sample.
Note: There should not be any paper labels on the beaker.

NH4Cl SiO2 (s)

H2O

1. transfer to
beaker + H2O filter
2. heat
NaCl (s)
SiO2 (s)
NH4Cl NaCl (aq.) NaCl (aq.)
NaCl
SiO2

Figure 1: Separation Protocol

III. Sublime ammonium chloride from salt.

1. Make sure your set up is well into the hood; no gas should escape the hood, as the NH4Cl
gas is dangerous.
2. Heat the sample using a Bunsen burner. You should observe white fumes (NH4Cl) as
the sample is heated.
3. As the sample is heated, a white film (re-solidified ammonium chloride) will appear on
the side of the beaker. You may lift the Bunsen burner from its base and carefully move
it around the outside of your beaker to remove the white film. A TA will help to
reposition the beaker if you cannot remove all of the ammonium chloride with a Bunsen
burner.
4. Continue heating until no additional white fumes appear and gas evolution has stopped.
5. Wait for the beaker to cool to room temperature.
6. Obtain the mass of the remaining solid (mass by difference) and record this in your Data
Table.
7. Repeat steps 2-5. Record the final mass after second heating in your Data Table. This is
done to ensure the removal of all of the NH4Cl.

IV. Filtration to separate the sand and salt

1. Mark a watch glass with your initials so that they can be seen with a filter paper on it.
2. Obtain a piece of filter paper and take its mass. Fold the filter paper in half once, then in
half again. You should see an X when you open the filter paper.

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 Experiment 2: Separation of a Mixture

3. Place the filter paper in a funnel. Be careful not to tear it. Wet the filter paper with a
small amount of DI water.
4. Pour ~15 mL of DI water into the 100 mL beaker containing your sample. Place your
magnetic stir bar in the beaker, and then place the beaker on a stir plate for ~5 minutes to
dissolve salt (Note: sand will not dissolve).
5. Pour the solution onto the filter paper in the glass funnel. Use your spatula to ensure all
solids are transferred.
6. Quantitative transfer of solution: You may rinse the beaker with minimal DI water (no
more than 5 mL). Pour that water over the sand to wash it.
7. After all liquid has passed through the filter paper, carefully unfold it onto watch glass
(concave side up) labeled with your name.
8. The TAs will put watch glasses into the oven in batches for ~30 minutes to remove the
water. Proceed to step V while your sample is in the oven. DO NOT open the oven.
9. After your sample has been in the oven for 30 min, allow the watch glass to cool to room
temperature.
10. Take the mass of the filter paper and sand.

V. Evaporate water from salt

1. Place evaporating dish containing salt water over Bunsen burner. Apply enough heat to
evaporate most of the water without causing splattering or popping.
2. If splattering/popping occurs, or when almost all of the water is gone, the evaporating
dish can be placed over a 250 mL beaker containing 150 mL of water.

Data: (Data must be in a table to receive credit.)

For Part I:
• Mass of weighing bottle (g)
• Mass of weighing bottle + initial sample (g)
• Mass of initial sample (g)
For Part III, Step 5:
Include all of the following data for first AND second heating:
• Mass of weighing bottle (g)
• Mass of weighing bottle + sample after heating (g)
• Mass of sample after heating (g)
For Part IV:
• Mass of filter paper (g)
• Mass of filter paper + sand after heating (g)
• Mass of sand (g)
For Part V:
• Mass of evaporating dish (g)
• Mass of evaporating dish + salt (g)
• Mass of salt (g)

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 Experiment 2: Separation of a Mixture

Calculations: (Do not round between steps as this will compound rounding error.)
Calculate mass of each component, then calculate its % composition using the equation:

𝑚𝑎𝑠𝑠-./0.123
% 𝑐𝑜𝑚𝑝𝑜𝑠𝑖𝑡𝑖𝑜𝑛 = × 100
Σ 𝑚𝑎𝑠𝑠5678 + 𝑚𝑎𝑠𝑠:;<= + 𝑚𝑎𝑠𝑠:>? <=

Calculate total % recovery using the following equation:

Σ 𝑚𝑎𝑠𝑠5678 + 𝑚𝑎𝑠𝑠:;<= + 𝑚𝑎𝑠𝑠:>? <=
𝑡𝑜𝑡𝑎𝑙 % 𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑦 = × 100
𝑚𝑎𝑠𝑠626H6;= H.H;= I;/0=J

Use the same format to show calculations as indicated last week, remembering to adhere to
significant figure rules.

Results: (Results must be in table to receive credit.)

Results table should include the following:
• Mass and % composition of NH4Cl
• Mass and % composition of sand
• Mass and % composition of salt
• Total mass recovered
• Total % recovery

Conclusion/Conclusion Questions: (Conclusion questions are found on the Digital Lab Report template.)