EXPERIMENT 2: SEPARATION OF THE COMPONENTS OF A MIXTURE

In this lab, we will be taking a mixture of three substances and separating them based on some of their
physical properties. The mixture you will be working with is composed of ammonium chloride (NH 4Cl), sodium
chloride (NaCl) (table salt) and silicon dioxide (SiO2) (sand).

MATERIALS

Mixture to separate and analyze Balance

spatula Tongs
Bunsen Burner 2 Evaporating dish or crucible
Ring stand and ring 1 Watch glass
Clay triangle Glass stick or stir rod
25 mL graduated cylinder

PROCEDURES:

1. Tare a clean, dry evaporating dish and record the mass, i.e. evaporating dish #1.
2. Add about 2 grams of your mixture.
3. Record the new mass.
4. Determine the mass of the mixture alone.
5. Heat the mixture on high heat for at least 20 minutes. Use a glass stick to agitate the mixture. White
“smoke” will start to evolve when the sample becomes hot. This is the ammonium chloride subliming in
the evaporating dish. Do not touch the dish with your hands. Hot things look just like cold ones!
6. Let the evaporating dish cool and its contents cool.
7. Reweigh the dish and its contents. Record the mass. (Do not weigh a hot or warm dish, convection
currents can affect mass reading by balance.)
8. Determine the mass lost to sublimation (i.e.mass of ammonium chloride)
9. a) Add 25 ml of water to the remaining salt/sand mixture and b) stir for approximately five minutes.
10. Let the residue settle for approximately 3-5 min.
11. Tare a clean evaporating dish covered with a watch glass, i.e. evaporating dish #2.
12. Remove the watch glass and decant the extract from the salt/sand mixture into the evaporating dish #
2, making sure not to transfer any solid residue. It is better to leave a small amount of solution in the
sand than to get the sand in the evaporating dish # 2.
13. Add 10mL more of water to the residue in the evaporating dish # 1, stir and decant as described in
steps 9b), 10 and 12.
14. Repeat with another 10mL of water.
15. Place the evaporating dish # 2 on a clay triangle supported on a tripod above a Bunsen burner.
16. Gently evaporate the water from the salt water extract until most of the water is gone.
17. Near the end, cover the evaporating dish with the watch glass to prevent splattering.
18. When the salt is completely dry, no more water will condense on the watch glass. Carefully remove
from the Bunsen burner and allow tocool. Go to step 20. While you wait for cooling to occur.
19. Weigh the evaporating dish with the dried salt and watch glass. Record its mass and use it to calculate
the mass of the salt.
20. Place the evaporating dish # 1 with the sand on the clay triangle and heat for approximately ten
minutes over a low fire. Do not overheat or the dish may break.
21. Carefully remove from the Bunsen burner and allow to cool. Go to step 19 if the dish is cool.
22. Weigh the evaporating dish with the dried sand. Record its mass and use it to calculate the mass of
the sand.
23. Determine the percent composition for each chemical and the overall recovery of the mixture. Provide
the answer on the datasheet below. Show your answer to your lecturer before you leave the lab.

Percent composition = mass of component ×100%

Mass of initial mixture
 The procedures for the lab are summarized by the flow chart below:
Mixture of NaCl, SiO2
and NH4Cl Heated Sublimed NH4Cl

(obtain mass by
Remaining after heating difference)

Mixture of NaCl and

SiO2
Extract with water insoluble in water
(dissolved NaCl) (residue)

Solution of NaCl Wet SiO2

Heat to dryness heat to dryness

NaCl (s) SiO2(s)

Obtain mass Obtain mass

Analysis Questions: The answers to these questions should be included in (but not limit) your discussion in
the form of paragraphs. Remember that your discussion is like an essay (intro., topic statement, paragraphs
that exhibit coherency, etc.)

1. What physical properties were used to separate the different components of the mixture? In your
results/data section compare these properties for ammonium chloride, sand and salt in the form of a table.
In this table include physical state at room temperature as a property. Comment on it in your discussion.

2. Elaborate on the different separating techniques used in this lab, relating it to the actual experiment
conducted and the physical properties listed in #1 above. Hint: There are at least four different separating
techniques used in this experiment.

3. Propose a different separating technique(s) from what was used in the lab to separate the sand/salt
mixture after the sublimation of ammonium chloride. List the steps you would conduct.

4. Add up the masses of your individual ingredients. Do they match the mass of your original mixture? Did
you get a 100% recovery? Discuss reasons why this might happen. Note- acceptable reasons for errors in
lab are not “human error” or “calculation error”. Be specific (refer to a step(s) in the lab and discuss what
might have happened).

5. How does this lab illustrate the law of conservation of mass?

RESULTS: Name____________________________________
Partners
name:____________________________

a) mass of evaporating dish #1 __________________ g

b) mass of evaporating dish #1 + mixture __________________ g
c) mass of mixture __________________ g
What chemicals are present in the mixture?

d) mass of evaporating dish #1 + mixture after heating __________________ g

e) mass of ammonium chloride (NH4Cl) __________________ g
What chemicals are left in the mixture now?

f) % of ammonium chloride in original sample __________________ %

Show working here for f):

g) mass of evaporating dish #2 + watchglass __________________ g

h) mass of evaporating dish #2 + watchglass+ NaCl __________________ g
i) mass of sodium chloride (NaCl) __________________ g
j) % of sodium chloride in original sample __________________ %
Show working here for j):

k) mass of evaporating dish #1 + SiO2 __________________ g

l) mass of silicon dioxide (SiO2) __________________ g
m) % of silicon dioxide in original sample __________________ %
Show working here for m):

n) sum of masses of NH4Cl, NaCl and SiO2 (e+i+l) __________________ g

o) % recovery [(n/c)x100%] __________________ %
Experiment 1: PRE-LAB

Define the following terms and give an example in each case.

Mixture- 2 or more substances in which each substance retains its own chemical identity. The composition can vary.
Example: Cup of sweetened coffee.
Substance- A pure substance (usually referred to simply as a substance) is matter that has distinct properties and a
composition that does not vary from sample to sample. Water and table salt (sodium chloride), the primary components of
seawater are examples of pure substances.
Compound- are substances composed of two or more elements; they contain two or more kinds of atoms. Water for
example is a compound composed of two elements: hydrogen and oxygen.
Element- are substances that cannot be decomposed into simpler substances. Example: Carbon
Solution- is a special type of homogeneous mixture composed of two or more substances. Example: Sugar dissolved in
water.
Extraction- is a separation process consisting in the separation of a substance from a matrix. It includes Liquid-liquid
extraction, and Solid phase extraction. Making tea is a good example of extraction. Water is placed in contact with tea
bags and the "tea" is extracted from the tea leaves into the water. This works because the "tea" is soluble in water but the
leaves are not.
Sublimation (besides NH4Cl) - it is a process in which a solid, when heated, vaporizes directly with out passing through
the liquid phase and these vapors can be condensed to for solid again. Example: Mothballs, like dry ice (solid CO2),
undergo a physical change called sublimation. In this change the solid goes directly into the gas state without first melting.
Taring- The weight of a container or wrapper that is deducted from the gross weight to obtain net weight. Example:
Physical change- is any change involving changes in the chemical identity of the substance. Example: change of state fro
solid to liquid to gas. Or Cutting a piece of paper into smaller pieces.
Chemical change- one in which reactants are changed in one or more different product. During this change there is a
chemical reaction that makes or breaks chemical bond. Example: adding Kool-Aid into water.
Physical property- Properties that do not change the chemical nature of matter. Example: color, smell, freezing point,
boiling point, melting point, infra-red spectrum, attraction (paramagnetic) or repulsion (diamagnetic) to magnets, opacity,
viscosity and density.

Label the processes of physical separation illustrated in the diagrams below based on the descriptions given on the
following page.
Decantation Filtration Chromatography

Centrifuging Distillation
Extraction is the process of selectively removing a compound of interest from a mixture using a solvent. For an
extraction to be successful the compound must be more soluble in the solvent than in the mixture. Additionally,
the solvent and mixture must be immiscible (not soluble in one another).