CHEMISTRY

Escuela Politécnica de
Ingeniería de Gijón
Universidad de Oviedo EXPERIMENT 2

BASIC LABORATORY OPERATIONS

OBJECTIVES: Become familiar with the material and simple operations more frequently
that are carried out in a chemistry laboratory.

MATERIAL REAGENTS
Name Formula
2 beakers of 100 mL potassium permanganate
1 beaker of 250 mL hydrated copper sulphate
1 pipette
1 graduated cylinder
1 burette
1 volumetric flask
1 watch glass
test tube clamps
1 wash bottle
test tube rack with 6 test tubes
1 dropper
1 ring stand with utility clamps
1 rubber stopper
1 thermometer

1
PART 1: PREPARARING a POTASSIUM PERMANGANATE SOLUTION

Preparing aqueous solutions of known concentration will be the most common activity during the
chemistry lab. Preparing solutions must always be carried out with attention avoiding all types of
reagents and/or solutions losses, in order to achieve needed degree of accuracy. Please, always
keep in mind that many chemicals could be harmful or toxic, and they must be handled with safety.

During this experiment a potassium permanganate solution 0.01 M will be prepared. Potassium
permanganate, KMnO4, is a strong oxidizing agent and has tendency to accept electrons easily in
redox processes.

Q1. Which is the oxidation state of Mn within the permanganate species? Detail your answer.

KMnO4 is an ionic compound formed by potassium cations (K+) and permanganate anions
(MnO4). Potassium permanganate is a strong electrolyte soluble in water.

Q2. Write the chemical equation corresponding to the dissociation of potassium

permanganate.

KMnO4(s) 

Before starting, let’s have a look to the potassium permanganate label:

Q3. What is the molecular weight of KMnO4?

Q4. What is its purity?

2
Q5. Indicate the meaning of the corresponding R statement. What precautions should be taken
for the storage and handling of this solid product?

To prepare the required KMnO4 solution, a volumetric flask, a beaker, a stir rod and distilled
water will be needed. The solid reagent (KMnO4) could be found in a bottle located next to the
electronic balances.

The volumetric flask has a known accurate volume.

Q6. What is the capacity of your volumetric flask?

What mass of KMnO4 do you need? To answer this question, a simple stoichiometric calculation
is required.

Example: What mass of NaCl(s) is needed to prepare 250.0 mL of a solution aqueous 0.1 M?

Q8. Within the previous conversion factors, indicate which magnitudes are subject to an
experimental determination (expressed with significant figures) and which are not
(expressed with NO significant figures).

Q9. Calculate the mass of KMnO4 need to prepare 100 mL of 0.01M solution.

Q10. How many significant figures does the result have? Why?

3
Preparing Chemical Solution: Experimental Procedure
1. Select a clean dry beaker. This is the glassware in which you will carry out the weighing.
2. Place the beaker on the balance plate, and zero (tare) the scale.
3. Using a spatula, slowly add the solid KMnO4 into the baker. After each addition, let the
reading of the balance stabilize before continuing to add solid until reaching the desired
weight.
4. Add approximately 40 mL of deionized water. Mix the contents of the glass with the stirring
rod until total dissolution.
5. Transfer the content from the beaker into the volumetric flask, which must be rinsed
previously with distilled water.
6. Collect the remaining solution portions in the beaker. Add a small volume of deionized water,
stir, and pour. Repeat if necessary.
7. Make up the volumetric flask with deionized water. Do not forget to use the dropper to
complete the making up. Homogenise its content.

When preparing a solution, NEVER dissolve the solid reagent in a greater volume of
solvent (water) than the corresponding volume of the volumetric flask.

Once the permanganate solution is prepared, you must transfer a portion to a reagent bottle. At
your lab working place, you will find a glass bottle with a stopper dropper. Check that it is clean and
dry (we want to preserve the conditions of the dissolution we transfer in). In order to identify the
solution you must label the bottle indicating the name, formula and concentration of the reagent
similar to the one shown in the figure below.

Name / Formula

Concentration / MW Date

Q11. What chemical species is responsible for the purple color of the solution?

All used glassware for this experiment must be washed with detergent (using a brush)
and rinsed with tap water before putting it away.

4
Use of Bunsen burner
The Bunsen burner is used frequently in the laboratory as a source of heat. It produces an open
flame which can be very hot. Bunsen burners provide safe, efficient heat when used properly.

To light the burner, follow the steps below:

1. Clear the area over and around the burner of flammable materials
2. Check that the air supply dial is completely closed.
3. Open the gas flow regulator dial.
4. Light the burner. You should observe a small flame in the mouth of the burner.
5. Increase the gas flow by opening the regulator dial. You should observe a flocculant reddish
flame of low calorific value.
6. Adjust the gas and air flow to produce a flame of the desired size. This flame will have a blue
colour, and a high calorific value, and two distinct blue zones, the inner of which is a bright
blue cone could be distinguished. The hottest part of the flame is just above the tip of the
inner bright blue cone. Set up any material to be heated so it contacts this hot zone. No
combustion occurs within the bright blue cone.

reddish low calorific power flame blue l calorific power flame

To extinguish the flame, turn off the air and gas flows.

Q12. How do you explain, in chemical and energetic terms, the change between the reddish/blue
flames depending on the air flow inlet?

5
How to heat a test tube

 Hold the test tube at an angle.

 Point the test tube away from yourself and all
other people.
 Heat the test tube gently from the top of the
substance being heated, and always wear
safety glasses.
 Hold it above the tip of the maximum
temperature area of the flame.
 Heat gradually and slowly to avoid "bumping".
 Remove the test tube from the flame
periodically, to avoid overheating.

NEVER touch hot glassware

PART 3: DETERMINATION of the AMOUNT of WATER PRESENT in

COPPER SULFATE HYDRATE

In this experiment, a known mass of hydrated copper(II) sulphate is heated to remove the water of
crystallization. The mass of water is found by weighing before and after heating. This information is
used to find n in the formula CuSO4·nH2O, using mole calculations.

If you dehydrate, by heating, a known amount of hydrated salt and later you find out the weight of
the resulting anhydrous salt, it is clear that by simple difference you will know the mass of water
that was in the hydrated salt:

mass of hydration water = mass of hydrated salt – mass of anhydrous salt

From the corresponding molecular weights, the mass of water and anhydrous salt could be
converted in moles, and thus obtain the degree of hydration as the entire number closest to the
relationship:

n ~ (mole of hydration water / mole of anhydrous salt)  hydration degree

6
To perform this experiment, you will need a test tube, another two large test tubes, a beaker, a
watch glass and a test tube clamps. Hydrated copper sulphate could be found in a bottle
located next to the electronic balances.

Procedure

a) Weight the EMPTY test tube (cold). Record the value.

b) Introduce a small amount of hydrated copper (II) sulphate with the help of a spatula.
c) Weight the test tube containing the hydrated copper sulphate (cold). Record the value.
d) Heat the test tube and content, gently at first, over a medium Bunsen flame, so that the water
of crystallisation is driven off steadily.
e) The blue colour of the hydrated compound should gradually fade to the greyish-white of
anhydrous copper(II) sulphate.
f) Avoid over-heating, which may cause further decomposition, and stop heating immediately if
the colour starts to blacken. If over-heated, toxic or corrosive fumes may be evolved.
g) Allow the test tube and content to cool.
h) Re-weigh the test tube and content once cold. Record the value.

Calculation:

weigh of empty test tube

weigh of test tube containing the hydrated salt

weigh of test tube containing the anhydrous salt

mass of hydrated CuSO4·nH2O

mass of anhydrous CuSO4

mass of driven off H2O

Q13. Describe the observed changes during the dehydration process.

Q14. Write the chemical equation corresponding to the dehydration copper sulphate process.

7
Q15. By means of conversion factor, determine the degree of hydration.

Water is driven off from hydrated copper sulfate when it is heated, so the forward reaction is
endothermic - energy must be transferred from the surroundings for it to happen.
What can be said about the backward reaction?

1. Hold the bottom part of the small test tube containing the anhydrous salt.
2. Add a few drops of water with the help of a dropper.

Q16. What have you observed? The hydration of anhydrous copper sulphate is an
endothermic or an exothermic process?