Experiment # 3 Identification of a Compound by Mass Relationships

I. Objectives
a. Use the relationship between masses of the reactants and products to identify an
unknown compound (NaHCO3, Na2CO3, KHCO3, K2CO3).
mass of chloride−original mass
i. Q=
originalmass
b. Identify whether a compound is a carbonate or hydrogen carbonate.
i. Carbonate – no chemical reaction when it is heated
ii. Hydrogen Carbonate – chemical reaction occurs when it is heated;
decrease in the mass of compound
II. Materials and Chemicals Needed
a. Materials
i. Crucible
ii. Distilled water
iii. Clay triangle
iv. Bunsen burner
v. Analytical balance
b. Chemicals
i. Unknown compound
ii. 6 M HCl
III. Experimental Procedure
a. Clean crucible and its cover with distilled water.
b. Heat it gently for 2 minutes then strongly for another 2 minutes.
c. Allow the crucible and its cover to cool down then weigh on an analytical
balance.
d. Place about 0.5 g of unknown compound in the crucible, then weigh again.
e. To heat the sample, utilize a clay triangle supported by an iron stand. Bunsen
burner will be the source of heat.
f. Heat gently for a few minutes, then gradually increase the flame intensity to the
point where the bottom of the crucible is red hot. Heat for 10 more minutes.
g. Allow it to cool for 10 minutes, then weigh again. At this point, the residue is in
carbonate form.
h. Return the crucible in the assembled apparatus previously. Add about 25 drops of
6M HCl, one drop at a time. Effervescence will occur after each drop, let this
subside before adding the next drop. Once finished the solid should be completely
dissolved.
i. Heat the crucible gently and intermittently, for about 10 minutes to slowly
evaporate the water and excess HCl.
j. When sample is dry, gradually increase the flame intensity, until the bottom of the
crucible is red hot. Then heat at full flame for 10 minutes.
k. Allow the crucible to cool then weigh again.
Experiment # 6 Molar Mass of a Volatile Liquid
I. Objectives
a. Determine the molar masses of gasses and vapors using the following equations:
i. Ideal Gas Law: PV =nRT
PV
ii. n=
RT
m
iii. MM=
n
b. Determine the mass of a given sample under known temperature and pressure
II. Materials and Chemicals Needed
a. Materials
i. Special round-bottomed flask
ii. Stopper and cap
iii. Evaporating dish/beaker
iv. Analytical balance
v. Cork ring
vi. Hot plate
vii. Thermometer
viii. Barometer
ix. Distilled water
b. Chemicals
i. Unknown liquid
III. Experimental Procedure
a. Weigh an empty and dry round-bottomed flask with a loosely inserted cork-
stopper on an analytical balance.
b. Pour 5 ml of unknown liquid in the flask.
c. Add 300 mL of water to a 600 mL beaker. Assemble the apparatus as shown
below.
d. Heat the water to the boiling point. At this point liquid inside the flask must have
vaporized already. If so, lower the heat but continue to gently heat for 5 to 8
minutes.
e. Measure the temperature of the boiling water. Turn off the hotplate and wait for
the water to stop boiling. Remove the cap immediately and replace with the cork-
stopper used previously.
f. Immerse the flask in a beaker of cool water for 2 minutes. Carefully remove the
cork-stopper for a second or two then replace immediately. This will allow the
vapor inside the flask to condense and make the pressure drop.
g. Dry the outside of the flask and obtain its weight. Also measure the atmospheric
pressure and record it.
h. Obtain the volume of the flask. It may be given by the instructor or it can be
obtained by weighing the flask stoppered and full of water on a top-loading
balance.
i. Repeat the procedure.
Experiment # 4 Properties of Hydrates
I. Objectives
a. Identify hydrates in a group of compounds
i. Hydrates – if heated, droplets of water condense on the cool upper walls of
the container; tends to dissolve in water
ii. Carbohydrate – if heated, it will give off water and tend to char; when
dissolved in water, solution will be caramel colored
b. Observe the reversibility of the hydration reaction
c. Test substances for efflorescence or deliquescence
i. Efflorescence - spontaneous loss of water by a hydrated salt, which occurs
when the aqueous vapor pressure of the hydrate is greater than the partial
pressure of the water vapor in the air
ii. Deliquescence - a substance absorbs moisture from the atmosphere until it
dissolves in the absorbed water and forms a solution
d. Determine amount of water lost by a sample of unknown hydrate when heated
e. Given the formula or molar mass of the anhydrous sample, determine the formula
of the hydrate
A. Identification of Hydrates
a. Materials and Chemicals Needed
i. Materials
1. Test tubes
2. Bunsen burner
3. Distilled water
ii. Chemicals
1. Nickel chloride
2. Potassium chloride
3. Sodium tetraborate
4. Sucrose
5. Calcium carbonate
6. Barium chloride
b. Experimental Procedure
i. Place 0.5g of NiCl2, KCl, B4Na2O7, C12H22O11, CaCO3, and BaCl2 in
different test tubes.
ii. Heat each test tube gently with a Bunsen burner. Observe the behavior of
each compound.
iii. Let the test tube cool then dissolve each residue in a few cubic centimeters
of water.
iv. Identify whether each compound is a hydrate or a carbonate based on the
characteristics listed in objective # 1.
B. Reversibility of Hydration
a. Materials and Chemicals Needed
i. Materials
1. Evaporating dish
 2. Distilled water
3. Bunsen burner
ii. Chemicals
1. Cobalt (II) chloride hexahydrate
2. CoCl2 ⸱ 6H2O
b. Experimental Procedure
i. Gently heat 0.3 g of Cobalt (II) chloride hexahydrate and CoCl2 ⸱ 6H2O in
an evaporating dish until complete color change occurs.
ii. Dissolve the residue in few cubic centimeters of water.
iii. Heat the solution and boil it to dryness.
iv. Put the evaporating dish on the lab bench and note any color changes.
C. Deliquescence and Efflorescence
a. Materials and Chemicals Needed
i. Materials
1. Watch glasses
2. Analytical balance
ii. Chemicals
1. Na2CO3 ⸱ 10 H2O
2. CaCl2
3. KAl(SO4)2 ⸱ 12 H2O
4. CuSO4
5. Prepared dish of CoCl2 in part B
b. Experimental Procedure
i. Place few crystals of Na2CO3 ⸱ 10 H2O, CaCl2, KAl(SO4)2 ⸱ 12 H2O,
CuSO4 in separate watch glasses and place next to the prepared dish of
CoCl2 in part B.
ii. Record the weight of each watch glass.
iii. Weigh them again after an hour to detect any change in mass.
iv. Observe any changes in color, crystal structure, or degree of wetness that
may occur.
D. Percent Water in a Hydrate
a. Materials and Chemicals Needed
i. Materials
1. Porcelain crucible with cover
2. Distilled water
3. Clay triangle
4. Bunsen burner
5. Analytical balance
6. Crucible tongs
7.
ii. Chemicals
1. 6M HNO3
2. Unknown hydrate
b. Experimental Procedure
i. Clean a crucible and its cover with 6M HNO3. Then, rinse with distilled
water.
ii. Heat the crucible with its cover slightly ajar using a Bunsen burner for 2
minutes.
iii. Allow to cool then weigh on an analytical balance. Use clean crucible
tongs to handle the crucible.
iv. Obtain an unknown hydrate and place about a gram of it in the crucible.
v. Weigh the crucible with the unknown hydrate and its cover in an
analytical balance.
vi. Put the crucible containing the unknown hydrate on the clay triangle and
put the cover slightly ajar to allow water vapor to escape.
vii. Heat gently at first then strongly, keeping the bottom of the crucible in red
heat for 10 minutes.
viii. Completely cover the crucible and let it cool.
ix. Weight the cooled crucible along with the cover and unknown hydrate.
x. Note any changes on the solid residue.
xi. Add water to the crucible up to two thirds full and stir.
xii. Warm gently if it the residue does not dissolve readily. Observe if the
residue is soluble in the water.