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CHEMESTRY

LABORATORY
PRACTICES
MATERIAL PER GROUP

 Rack with 10 test tubes


 Support with walnut
 Tripod
 Asbestos grid
 Lighter
 Test tube (100 mL)
 Funnel
 Small beaker
 Large beaker
 Erlenmeyer flask
 Watch glass
 Crystallizer
 Washing bottle
 Wood clamp
 Spatula with spoon
 Glass rod
 Large brush
 Small brush
 Esparto
 Baize
 Matches
 Gloves
 Dressing gown
 Bowl with soap
 Dropper
INDEX

Unit 1: Work in Laboratory..........................................................................3

Unit 2: Volume Measurement ....................................................................14

Unit 3: Measurement of masses and densities............................................ 25

Unit 4: Mixture separation techniques ........................................................ 31

Unit 5: Thermochemistry.............................................................................55

Unit 6: Kinetics............................................................................................60

Unit 7: Acid-base reactions ........................................................................ 66

Unit 8: Redox reactions .............................................................................. 81


UNIT 1:
Work in the laboratory
WORK IN THE LABORATORY

SAFETY STANDARDS IN THE LABORATORY

In the laboratory it is essential that a series of safety standards are complied with
to avoid possible accidents. Many times, because you don't know what you're doing or
careless or irresponsible behavior, you can endanger yourself and others. It is therefore
imperative that the following rules are complied with:

1. Each internship group will be responsible for its work area and its material.
2. Place utensils and reagents away from the edge of the table.
3. Before starting an internship, you must know and understand the processes you are
going to carry out.
4. Focus on what you're doing. Don’t get distracted.
5. Avoid unnecessary travel and never run through the laboratory.
6. You need to wear a lab coat as it prevents chemicals from reaching your clothes and
skin.
7. In the laboratory it is strictly forbidden to smoke, eat, drink ..., since there may be
toxic and flammable remains (both solid and liquid, as well as gaseous).
8. When you must pass a compound or a container to your partner, do not throw it,
give it in your hand.
9. Before using a compound, make sure it is the one you need. If in doubt, ask your
teacher.
10. The remains of the products used should never be returned to the original bottles, as
the entire product could be contaminated.
11. Never look through the mouth of test tubes or flasks when a reaction is taking place
in anticipation of possible splashes.
12. In general, all products should be mixed in small quantities and slowly.
13. When waste chemicals are poured into the drain basin, you must first find out if
they can damage the pipe and always turn on the tap and let water circulate for a
while.
14. Throw solid waste in the bin.
15. Never throw traces of alkali metals into the drain pile (even if they are small), as the
reaction is explosive.
16. Do not touch chemicals with your hand or mouth. Use the spatula when you have to
touch them. A laboratory product should never be tested, even if it is harmless, as
there may be an error or it may have been in contact with toxic substances.
17. To smell vapors, do not suck directly through your nose, but you must approach the
steam with a wave of the hand.
18. When preparing solutions of acids, water will never be poured over the acid, but
ACID WILL ALWAYS BE POURED OVER THE WATER.
19. If an acid or any other corrosive product falls on your skin, wash immediately with
plenty of water and notify the teacher.
20. Flammable products should not be near heat sources.
21. To heat a test tube, you should not heat only a specific area, because it would break.
It should be heated by moving the tube through the flame of the lighter, starting at
the top (to avoid splashing). Never direct the test tube to where there are people.
22. When working with glass, it must be allowed to cool before any manipulation.
23. When preparing a solution, it shall be placed in a clean flask with a label indicating,
in addition to the product and the concentration, the date of preparation and the
group of practices that prepared it.
24. At the end of the practice, leave the material and the worktable clean and dry. The
material is cleaned with detergent and a brush. After rinsing with tap water, one or
more rinses should be given with small amounts of distilled water.
25. The material you are using has an economic value, sometimes very high. Treat it
carefully and don't break it through carelessness or negligence.
DANGEROUS CHEMICALS

Many of the chemicals that we are going to use in the laboratory are dangerous, either
because they are toxic, or corrosive, or because they burn easily... etc. It is convenient that we
know which are dangerous, to treat them with the greatest care.
In Royal Decree 363 of 1985, published in the B.O.E. of June 5 of the same year we find the
regulation on classification, packaging and labeling of dangerous substances, with the indications of
dangerousness in each case. The symbols that represent the dangerousness of the products are the
following:

Identify those substances that are ignited by brief


contact with an ignition source and continue to burn
after being separated from said ignition source.

Identify those substances that at room temperature and in


contact with air burn spontaneously.

Identify those substances that can explode due to flame,


shock or friction.

Identify those substances that produce a strong exothermic


reaction (great heat release), especially in contact with
flammable substances.
Identify those substances that destroy living tissues
upon contact with them.

Identify those substances that, due to contact with the


skin or mucous membranes, can cause an inflammatory
reaction.

These two symbols identify those substances that by


inhalation, ingestion or skin penetration can pose health
risks and even death if they are not handled with adequate
safety measures.

Identify those substances and preparations which, by


ingestion, penetration of the skin or by inhalation, can
involve risks of limited severity.
LABORATORY EQUIPMENT

BURETTE TEST
It is used to measure volumes of TUBE
liquids. As it has a lower It is a graduated glass
stopcock, it is usually used for container that is used to
valuations. It is glass material. measure volumes of
liquids quite accurately.

PIPETTES
They are used to measure
volumes of liquids with greater
accuracy than specimens. It is ERLENMEYER FLASK
glass material and can be
graduated or fixed volume. It is a glass flask that only
measures volumes
approximately. It can be heated
and solutions can be stirred in it.

KITASATO FLASK
It is similar in shape to the previous one,
but with a lateral branch. It is usually
connected to a water tube to filter under
vacuum along with a Buchner funnel.

BUCHNER FUNNEL WATER TRUNK


It is a porcelain funnel, to which a It is a plastic or glass utensil that
filter paper is attached at the connects to the water tap and
bottom. It is used with a water together with the kitasate flask
trunk and the kitasate flask. and the Buchner funnel is used to
filter under vacuum.
SETTLING
TEST TUBES FUNNEL
They are glass containers of It is a glass utensil with a
different sizes that can be stopcock at the bottom, which
heated directly to the flame serves to separate immiscible
and serve to perform liquids and of different
qualitative reactions in the densities.
laboratory.

DISTILLATION FLASK
It is a round glass flask with a side branch that is
usually attached to the refrigerant tube. It is used in
distillations.

BEAKER
CRYSTALLIZER There are many types. They
It is a glass container that are made of glass. They can
is used so that the be heated (with grid) and can
solutions evaporate easily measure volumes
and can crystallize the approximately. Some are not
solute. graduates.

DESICCATOR
It is made of glass and is used so
that solid substances do not
absorb moisture. At the bottom it
carries a dehydrator. WATCH GLASS
It is shaped like a watch
face. It is mostly used to
weigh solids.
FLASKS GRADUATED FLASK
They are made of glass. It is a flask whose mission is to
They can be flat- measure volumes with great
bottomed or round. precision. Each volumetric flask
They are used to heat is inscribed with the volume
substances and to carry that the liquid inside will
out chemical reactions. measure when filled to the brim.

COOLING TUBES
They are made of glass and FUNNEL
serve to cool the steam that It is made of glass and
passes through the inner tube serves to fill
by passing running water containers and to filter
around it. They are used in (in this case with filter
distillations. paper).

SUPPORT

WASH- BOTTLE The support is


usually metallic.
It is made of plastic and With the nut and the
contains distilled water. It tweezers, it serves to
is provided with a tube for hold small objects. If,
ease of use. instead of a clamp, it
has a ring and grid, it
serves to heat with
the lighter.

TRIPOD
MORTAR It serves to heat
It is made of porcelain beakers, erlenmeyer’s
or glass. It serves to and other containers. It
crush solids. is used with the grid.
NUT
PINCERS
Serves to RING
Attach the They are attached S
tweezers to the support by
and rings to walnut. They are made of metal. They are
the attached to the support by walnut; and
supports. serve to heat flasks of spherical base.

GRID WITH ASBESTOS


PORCELAIN CAPSULE
It is made of wire with a circle of
asbestos. It is used with the tripod. It is used, among other things, to heat solids or
Asbestos protects glass utensils from evaporate liquids to dryness.
fire.

CRUCIBLE
It is made of porcelain or
SPATULA WITH
any other material that
SPOON
resists high
It is made of metal and temperatures. It is used,
serves to take small among other things, to
amounts of solid. melt solids.

BUNSEN LIGHTER
It is the lighter used in laboratories with internal gas
circuit. It has a faucet that regulates the amount of gas
(butane or propane) that comes out and a washer that
regulates the air intake. This washer allows to regulate the
type of flame that is used for heating. The ideal flame is
achieved when it is bluish and, thus, a temperature of up to
1600ºC is reached.
DROPPER
It is a glass tube, finished in peak
WOODEN TWEEZERS that allows us to measure the
number of drops that we throw
They are used to hold test tubes into a container.
and be able to heat them
directly to the flame.

RACK
It is used to hold test tubes. It can be made of
wood, plastic or metal. Some have holes of
different sizes to hold test tubes of different
diameters.

BRUSH
Utensil used to clean the
glass material. The
smallest diameter is used
for
test tubes. GLASS RODS
They are used to remove
solutions.
ISSUES

1. Objective of the topic.


2. What should you do to avoid splashing in the eyes?
3. You already know that it is convenient to wear a coat in the laboratory, but why
is it convenient that you do not wear clothes of synthetic material?
4. How would you dilute a concentrated solution of sulfuric acid?
5. Describes how a test tube should be heated.
6. It describes how to check the smell of substances in the laboratory.
7. Indicates what the following symbols represent:
(a) b( c)

8. Indicate the material you know to measure volumes of liquids.


9. Name some material used to heat test tubes.
10. What is a rack for?
11. Name the following material:
a) b) c) d)
UNIT 2:
Volume measurement
VOLUME MEASUREMENT

INTRODUCTION

Many times, when performing a practice, we will need to measure an amount of


a liquid. In this case it is much simpler to measure a volume than a mass. Special
containers are used to measure volumes of liquids. These containers are usually high
and narrow, since the error made when measuring a volume, in these cases, is less than
if it were wider containers, for that reason the beakers and the erlenmeyer flasks are
only used to measure the volume in an approximate way: they are not used to measure
volumes in which it is required accuracy.
They are usually glass containers and can measure a fixed volume (gauge) or
they can measure different volumes when they have a scale. Both in one case and in
the other, the liquid must reach the line that marks the appropriate level of
liquid: the flush line.
To make up to the mark, we must take into account that the surface of the liquids
is not perfectly horizontal but rather has a curvature called meniscus. On large surfaces
the meniscus is not noticeable, but in the containers, we use to accurately measure
volumes it is important to take it into account. Usually the meniscus is concave although
in some cases it can be convex:

To measure the volume in the concave meniscus, it is necessary to make a mark


so that the lower part of the meniscus is at the height of the flush line. In cases of
convex meniscus, the flush line should be at the height of the top of the meniscus. To
make up to the mark well, the eyes must be placed at the same height as the flush line,
to avoid the error called parallax.
Volumetric material must always be used clean. Otherwise, they contaminate
the liquid they measure. To clean the material, soap and water are used, rubbing with a
brush. It is also convenient to rinse it with the liquid you want to measure (especially in
pipettes).
The volume marked by these containers has been measured at 20ºC, therefore,
for different temperatures an error is made. It must be taken into account that the
volumetric material cannot be heated, since when dilated it would not measure the
volume well, and when it cools it does not recover, exactly the initial volume.
To measure the volume of liquids, the following containers are normally used:
test tube, pipette, burette, graduated flask.
INTERNSHIP

PRACTICE 1: THE TEST TUBE

INTRODUCTION
In this practice we will learn how to use the test tube, how to level it and when it
is convenient to use it. There are test tubes of various sizes and have a scale to measure
different volumes. The scale values are normally dependent on the capacity of the test
tube. This capacity usually ranges from 10cm 3 to 1000cm 3. It is an instrument of low
precision, the lower the greater its capacity.

When using the test tube, the liquid must be poured carefully so as not to exceed
the flush line. The last drops can be added with an eyedropper. When emptying the
cylinder we will pour the liquid gently so that it does not splash.

MATERIAL
Test tube, dropper, beaker.

PROCEDURE
1. Take the test tube and look at the scale, paying attention to the value of each division.
2. Fill it with water up to the following volumes: 20 cm3; 30 cm3; 50 cm3; 100 cm3.
Be careful when making up with the parallax error.
3. Empty the test tube into the beaker each time.

ISSUES
1. Objective of the practice.
2. Material used.
3. Describes the procedure followed
4. What is parallax error? How can it be avoided?
5. Why can't you heat a test tube?
6. If we need to measure a volume of water of 100 cc, indicate, reasoning, which
of these containers is more suitable: Test tube, 1000 cc beaker, 100cc test tube
100cc.
PRACTICE 2: THE PIPETTE

INTRODUCTION
The pipette is used to measure small volumes. The volume is poured from the
pipette into another container. In this practice we will learn how to use the pipette, how
to make it up to date and when it is convenient to use it.

There are two types of pipettes:

 Volumetric pipettes: It has a deposit in its central part and a flushing line in its
upper part. The most frequent capacities are from 5 to 50 cm3.
 Graduated pipettes: They have the same section along their entire length.
They are of a somewhat less precision than the volumetric pipettes. They can
measure different volumes of liquids.
To handle the pipettes, they are introduced through the lower part in the liquid to
be measured and absorbed with the mouth, with great caution, through the upper part.
Then it is covered with the index finger and is flush uncovering with careful. Next, it is
emptied into the container where we are going to use the liquid by raising the index
finger.

In the event that a small amount of liquid remains in the pipette, it should not be
blown so that it falls for two reasons:

 When blowing we introduce CO2 inside the pipette, and it can react with the liquid
of the same.
 The pipette gauging already takes into account the liquid that does not fall when
uncovering the finger.

MATERIAL
Pipette, beaker, rack with test tubes.

PROCEDURE
1. Take the graduated pipette and observe the scale.
2. Put water in the beaker and fill and empty the pipette several times , trying to
make up to the mark well.
3. Prepare a rack with 10 test tubes. Fill with water and make the pipette up to scratch.
4. Pour 1 cm3 into each of the test tubes.
5. Take a graduated pipette and make some measurement.
ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. Why to measure a volume of 5 cm3 it is better to use a 10-cc pipette than a test
tube of the same volume?
5. Indicates the differences between graduated pipettes and graduated pipettes.
6. Why not blow through the pipette so that the last drops of liquid fall?
PRACTICE 3: THE BURETTE

INTRODUCTION
This container is used to measure varying volumes of liquids poured from the
burette into a beaker or an erlenmeyer flask. In this practice we will learn how to use the
burette, make it up to date and when it is convenient to use it. The most frequent
capacity of burettes ranges from 25 to 100 cm3.

It is also a cylindrical glass container, but its scale has a much more precise
graduation than that of the test tube. At the bottom it has a stopcock.

To use the burette is placed, vertically, attached to a support by a clamp and a


walnut, as shown in the figure:

It is filled at the top, taking into account that before flushing you must
open the stopcock so that the dropper at the bottom is filled. If this
were not done, when opening the stopcock, the volume of the burette
would begin to decrease but still would not fall dissolution in the
beaker, but the dropper would be filled, with which we would be
making a mistake.

By having the 0 at the top, when we close the stopcock, we


know the liquid we have used at that moment.

Many times, when pouring a liquid from the burette to another container, it is
necessary to shake the latter. This is achieved by handling the stopcock with the left
hand and shaking the container with the right.

After using a burette you have to clean well, especially if we have used alkaline
solutions, as they attack the ground glass.
MATERIAL
Burette, support, clamp, walnut, beaker, rack with 10 test tubes, erlenmeyer
flask.

PROCEDURE
1. Mount the burette on the stand.
2. Fill it until it exceeds 0.
3. Place a beaker under the burette and open the stopcock until the dropper at the
bottom of the burette is filled.
4. If the volume of the liquid has fallen below zero, fill it again and make the
volume up to zero.
5. Place the rack with the test tubes under the burette and pour 1 cm 3 of water
into each of them.
6. Practice using the burette by moving the erlenmeyer from underneath at once.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. Describe how a burette is flushed.
5. Why does the burette have the 0 at the top?
6. Can there be a parallax error in the handling of the burette?
PRACTICE 4: SOLIDS VOLUMES

INTRODUCTION
Solids could be classified into regular solids: those that have known geometric
shapes, such as the sphere, the cube, the prism, and irregular solids, which are those that
do not have a definite shape.

To calculate the volume of the former, it would be enough to measure their side,
an edge, the diameter and substitute these values in the corresponding mathematical
formula. But to calculate the volume of seconds, we have no mathematical formula to
do so. We will measure its volume by water displacement. In this practice we will learn
to measure the volume of the latter.

MATERIAL
Irregular solids, test tube.

PROCEDURE
1. It measures an amount of water inside a cylinder. Write down its value: V0.
2. Introduce in the same test tube one of the solids whose volume we want to
measure. Write down its value: Vr.
3. Calculate the volume of the solid by subtracting both volumes: V s = V r – V0.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. Calculate the volume of irregular solids.
5. Would this method be used to calculate the volume of regular solids? Would it
be better or worse than using the mathematical formula?
PRACTICE 5: LIQUID VOLUMES

INTRODUCTION
In the following practice we will apply the knowledge acquired in previous
experiences. This experience will consist of the measurement of volumes while being a
fun experience.

We will start from a known volume of tap water and make a little "magic trick."
It will consist of changing the water in the glass and it will seem to be transformed in
wine. By transferring the contents to a third glass, it will appear to be transformed into
beer. In the First conversion what happens is that potassium permanganate, which is
Intense violet color, dissolves in water. In the second conversion, water oxygenated
reduces permanganate ion MnO4 – (deep violet) to manganese dioxide, a yellowish solid
that remains in suspension; It is also formed oxygen What is the responsible of the
Bubbles. How already Know the oxygen is indispensable in the combustion, y by that
reason Yes Approach one small flame an atmosphere rich in this gas, it will burn more
vividly. The chemical reaction What does it have? Place is:

KMnO4 + H 2 O 2 MnO2 + KOH + H2O + O 2

MATERIAL
Two beakers, test tube 100 cc, pipette, filter paper. Products: Potassium
permanganate, hydrogen peroxide.

PROCEDURE
1. Make a small stick about 10 cm long with rolled filter paper. Leave it prepared.
2. Weigh 0.5 g of solid potassium permanganate and deposit them in the first
beaker.
3. Measure 20 cc of hydrogen peroxide with the pipette and pour them into the
second beaker.
4. Measure 60 cc of water with the test tube and transfer them to the first beaker:
where the potassium permanganate is. Watch what happens.
5. Transfer the contents of the first glass to the second. Observe and write down what happens.
6. Light the cane and bring it close to the beaker very close to the bubbles. You
must hurry and perform the operation before the reaction ends, and therefore
before the bubbles run out. Observe and write down what happens.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. Indicates that it occurred during the first transformation. Is it a physical or
chemical process?
5. Write down the chemical reaction that took place during the second
transformation. Adjust it.
6. What happened when the lit cane was brought closer to dissolution? Why is
that?
UNIT 3:
Measurement of masses and densities
MEASUREMENT OF MASSES AND DENSITIES

THEORETICAL INTRODUCTION

Mass measurement

In the laboratory it is very common to weigh a quantity of substance. We use a


scale to weigh. There are different types of balances:
 Two-plate scale.
 Single-plate scale.
 Analytical balance.
 Electronic scale.

Currently it is common to find electronic scales in laboratories, obviously, much


more comfortable to use. Let's see how to use them.
The weighing in this type of scales is very fast and very practical since it is read
directly on a digital scale. The biggest drawback is its price, the higher the more
accurate it is.
To weigh it is convenient to follow the following general rules:
1. Never weigh hot objects.
2. Use watch glasses or weigh substances (large containers) for weighing. Never
place substances directly in the saucer.
3. If you have to add substance, use a spatula, and do it with great care.
4. If you are going to weigh liquids using a beaker, and you have to add some more
liquid, it is convenient that you remove it from the scale to avoid splashing.
5. When you finish weighing, always leave the scale clean.

To weigh a substance using a watch glass, if it is solid; or a beaker if it is liquid,


we will follow these steps:
1. Connect the switch.
2. When the illuminated scale appears, check that it is set to 0.0.
3. Place the recipient on the saucer and press the "tare" key.
4. Check that the balance has been set back to 0.0.
5. Add the substance until you reach the desired value.
6. Remember to disconnect it and clean it in case you have dropped something.

Density measurement
The density of a body is a specific property of each pure substance, which means
that it is a property independent of the amount of substance we have. At the end of the
introduction there is a table of densities of solids and liquids that can serve as a
reference. Density is usually measured indirectly from

of the mass and volume according to their m


 .
definition: V
The units in which this magnitude is expressed are Kg/m 3 in the International
System; but gr/cm3, gr/L, etc. are also used.
To measure the density of both a solid and a liquid, all we have to do is known
its mass: weigh it on the balance, and calculate its volume: if it is a liquid directly:
measuring it; and if it is a solid or indirectly: as we saw in previous practices.

SOLIDS DENSITIES
SUBSTANCE DENSITY SUBSTANCE DENSITY
Aluminum 2.7 Brass 8.5
Bronze 8.78 Nickel 8.9
Copper 8.93 Gold 19.3
Quartz 2.66 Silver 10.5
Tin 7.29 Platinum 21.5
Ice 0.92 Lead 11.37
Iron 7.5 Zinc 7.12

LIQUID DENSITIES
SUBSTANCE DENSITY SUBSTANCE DENSITY
Water 1 Chloroform 1.49
Acetone 0.79 Dimethyl ether 0.71
Olive oil 0.91 Glycerin 1.26
Ethyl alcohol 0.79 Mercury 13.59
Alcohol 0.79 Tetrachloride 1.59
Dichlorometha 1.3 Xylene 0.86
ne
Toluene 0.86 Acetaldehyde 0.78
INTERNSHIP

PRACTICE 1: DENSITIES OF IRREGULAR SOLIDS

INTRODUCTION
In this practice we will learn to calculate the density of irregular solids, for
which it will be necessary to remember what we have learned about the calculation of
volumes and measurement of masses.

MATERIAL
Test tube, irregular solids (the same as in the practice of measuring volumes),
balance.

PROCEDURE
1. Weighs the irregular solid.
2. Take the first irregular solid and calculate its volume by displacement.
3. Calculate its density.
4. Take another irregular solid and repeat the process.
5. It collects the values obtained in a table in which the number and name of the
solid, its volume, its mass and, finally , its density appear.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. Draw the table with all the values.
PRACTICE 2: DENSITIES OF SOLIDS OF THE SAME NATURE

INTRODUCTION
In this practice we will continue to calculate densities of solids but with the
particularity of being the same in each case. We will use tables and graphs as
complements to laboratory activities.

MATERIAL
Test tube, scale, and nails.

PROCEDURE
1. Weigh two iron nails and write down the
2. ir value on the table below.
3. Put 50 mL of water in a cylinder and calculate the volume of the two nails per
displacement, and write it down on the table.
4. Repeat the process for 5, 7, 11 and 15 iron nails. Complete the table.

2 5 7 11 15
Number of nails
Volume (cm3)
Mass (gr)

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. On graph paper, it graphically represents mass versus volume. From the graph
calculate the density of iron as the slope of the line, and then compare the value
obtained with that of the table of values you had in the theoretical introduction.
PRACTICE 3: LIQUID DENSITIES

INTRODUCTION
In this practice we will calculate the density of various liquids: water, oil and
alcohol. We will also learn to make the necessary calculations to obtain a solution of
water and alcohol of a certain density.

MATERIAL
Test tube, beaker, water, alcohol and oil.

PROCEDURE
1. Measure 10 mL of water and pour them over an empty beaker and weighed on
the scale.
2. Weigh it and calculate the density of the water.
3. Repeat the process with 30 mL of water and recalculate its density. In the event
that the difference is very noticeable, make another new calculation with another
volume.
4. Do the same with alcohol and oil.
5. Make the necessary calculations to know the volume of water and alcohol
needed to obtain 70 mL of a mixture of both whose density is 0.95 gr / cc.
6. Prepare this mixture in the cylinder and check its density.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. Indicate the calculations made to know the volume of water and alcohol needed
to prepare the mixture.
5. Oil and water are two immiscible liquids. Why does oil float on water?
UNIT 4:
Mixture separation techniques
MIXTURE SEPARATION TECHNIQUES

THEORETICAL INTRODUCTION

In this block of practices we will study the different techniques that can be used
in a laboratory to separate mixtures, both homogeneous and heterogeneous. As a
starting point it will be interesting to remember what a mixture is, and how
homogeneous mixtures differ from heterogeneous ones:

Mixture is a substance formed by the union of two or more substances that do not
react with each other. They can be separated by physical methods (they are the ones we
are going to use) and their composition and properties are variable. Mixtures are
classified into homogeneous and heterogeneous:
 Homogeneous mixture is one in which the components that form it are not
distinguished and its properties are the same at any point. Homogeneous
mixtures are also called solutions.
 Heterogeneous mixture is one in which it is possible to observe the
different compounds that form it, and therefore, its properties vary from one
point to another of the mixture.

The different types of mixtures require the use of various physical methods to
separate their components, among which are: filtration, decantation, crystallization,
distillation, solvent extraction and adsorption.

1.-FILTRATION
Filtration allows the separation between a solid and a liquid that is in suspension,
that is, forming a heterogeneous mixture. For this, a permeable body is used, usually
filter paper, whose pores let the liquid pass through and retain the only left. Filtration
can be by gravity or reduced pressure.
1.1.-Gravity filtration
In this technique the filtered liquid falls under its own weight and the solid is
retained in a filter paper that is placed in a funnel. The filter can be conical or folded.

Conical filter
This filter is used when it is intended to study the solid residue that remains in
the filter after filtration. To build it, the following steps are followed:

Cut a square of filter paper whose


side is approximately one and a half
diameter of the funnel. Then it is
folded several times as shown in the
figure and given a conical shape by
cutting by the dotted line.

To filter with the conical filter, it must be inserted into the funnel taking into
account the following rules:
 The filter paper must be one finger below the level of the funnel.
 You have to wet the filter with distilled water and press with your fingers so that
there is no air bubble and it is perfectly coupled. This is very important to make
a quick filtration: if the paper is well adjusted to the funnel, when filtering, the
lower tube of the funnel will be filled with liquid that when descending will suck
the one that is above.

Fold filter
It is used when you want to filter more quickly and what you want to study is
filtering. To build it, a square of filter paper is also cut whose side has a diameter and a
half of the funnel and the steps for the construction of a conical filter are followed ,
but then successive folds are made .
To filter with a filter or folds, the following rules must be taken into account :
 The filter must be one finger above the edge of the funnel.
 This filter should not get wet.
Gravity filtration technique
To filter , the device in the figure is mounted, taking into account the following
precautions:
 The mixture must be poured into the funnel with
the help of a glass rod, through which the
liquid will slide to the wall of the funnel. The rod
should not touch the funnel as it could pierce the
paper.
 The bottom tube of the funnel should be left
touching the wall of the beaker, so that splashes
do not occur.
 It is convenient to let the mixture rest, since this
will achieve a faster filtration: first the liquid part
will pass and then the solid.
 If there is a little solid left in the flask where we
had the mixture it can be collected with a little
distilled water.
 If the filtering is cloudy, it is necessary to filter
again several times until a transparent filter is
obtained.
 If the solid is very fine, it is advisable to use two
filter papers to avoid the previous problem.

1.2.-Reduced pressure filtration


This technique consists of making a quick filtration thanks to a device called a
water pump. To filter at reduced pressure we need a Buchner funnel, a kitasate flask, a
water pump and rubbers to connect the kitasate to the water pump. This pump is a
device that lowers the pressure inside the kitasate; in this way it absorbs the liquid and
the filtration is faster.
To perform the filtration, a piece of circular filter paper (smooth filter) that has
the same diameter as the Buchner funnel is prepared and placed inside it. The assembly
is that of the figure. In this technique the rules to follow are:
 The filter must not protrude from the base of the
funnel and no holes must remain unplugged. In the
first case you have to cut the paper a little and in
the second you have to make a new filter.
 The filter must be wet well with distilled water so
that it is well adhered to.
 When the filtration is finished, the rubber must be
disconnected from the kitasate before closing the
water tap, otherwise water could enter the kitasate.
2.-DECANTATION
This technique consists of separating two immiscible liquids or a solid and a
liquid that cannot be mixed with each other.
The procedure consists of separating both phases (the two liquid phases or the
liquid phase and the solid phase) taking advantage of the difference in density of both.
This process depends on the type of mixture:
 To separate the two liquid phases of an emulsion, a separating funnel is used.
 To separate the liquid phase from the solid phase that remains at the bottom of
the beaker, the beaker is tilted and the liquid is poured .
 To separate the solid phase, in the event that it floats on the liquid, it can be
collected with a spatula.

3.-CRYSTALLIZATION
It consists of separating a solid dissolved in a liquid. For crystallization to occur,
it is necessary that a concentration greater than the solubility of the solute in that
solvent is reached in the solution ; That is, we have a solution that is called super
saturated. This can be achieved in two ways:
 Cooling a saturated solution, as solubility decreases with decreasing
temperature.
 Removing part of the solvent, either by evaporation (slower) or by boiling
(faster).

The speed of cooling will define the size of the resulting crystals. Rapid cooling
will produce small crystals, while slow cooling will produce large crystals. One way
to obtain large crystals is to introduce into the supersaturated solution a crystal of this
substance that will act as a germ; so that crystallization will take place around the initial
crystal that will grow.
4.-DISTILLATION
Distillation is a technique of separating the various components that make up a
homogeneous mixture by boiling. If one component is liquid and the other solid, the
liquid shall be boiled and the solid shall remain in the flask. When the components of
the mixture are liquids, we take advantage of the different boiling points that these
liquids present.
It consists of heating the mixture to boiling and subsequent condensation of
the steam that has formed.
There are up to four different types of distillation:
1. Simple distillation (the most common in the laboratory).
2. Fractional distillation (used to obtain all petroleum derivatives: gas, gasoline,
kerosene, tar, ...)
3. Vacuum distillation .
4. Steam distillation.

We are going to study, only, simple distillation: it allows to separate a solid


from a liquid or two liquids of very different boiling points (80ºC or more). The
distillation temperature shall be intermediate between that of the two pure components
of the mixture. This distillation will give better results the greater the difference in the
boiling temperatures of each component.
The basic scheme of a simple distillation consists of a round flask that is
attached to a support and rests on a grid. Underneath is the lighter. Inside this flask, the
solution to be distilled is found together with a few small piece of porcelain (or porous
brick) that makes the liquid boil with small bubbles (we achieve with this a more
uniform boiling and avoid splashes). In the mouth of the flask there is a thermometer
with which we control the temperature of the steam. Then a cooling tube is placed that
is fixed in another support. This device allows that while the steam circulates through
the inner tube, the outer part is filled with running water, causing a decrease in
temperature and, therefore, the condensation of the steam. This is collected in a beaker.
All the above can be observed in the following
scheme:

When carrying out a distillation we must take into account the following rules:
 The tweezers with which the flask is supported must have a plastic coating,
otherwise the glass may break by direct contact with the metal.
 The water in the cooling tube must enter through the lowest part and exit
through the upper part : in this way we get the tube to be always full of water.
 The distillation flask must not be filled more than two thirds of its capacity.
 The mercury reservoir of the thermometer must be at the height of the steam
outlet, as indicated in the diagram, so that it marks the temperature of the vapor.
 The distillation should be slow but without interruptions, watching that the
temperature is constant.
 For the boiling to be homogeneous, it is necessary to introduce some pieces of
porcelain into the flask as we had already mentioned.
5.-SOLVENT EXTRACTION
This technique is different depending on whether we want to separate two mixed
solids or two substances dissolved in a liquid.
In the first case we will add to the solid mixture a solvent that is only capable
of dissolving one of the substances that compose it, leaving the other in the bottom of
the glass. When the substance to be extracted has already been dissolved, the substance
that has not been dissolved by decantation or filtration is separated. If you want to
recover the one that has been dissolved, it can be done by crystallization or by
distillation.
In the second case we will take advantage of the different solubility of the two
substances in two immiscible solvents. This technique is normally used for the
extraction of substances dissolved in water: if the aqueous solution containing the
component to be separated is treated with a liquid immiscible in water, this component
will become part of the immiscible liquid (extractor liquid). This method makes it
possible to separate the desired component and leave the secondary products in the
aqueous solution .
To perform a good extraction we will need:
 An extractor liquid with great separating power, that is, that dissolves the
substance we want to separate better than the initial solvent (which will
normally be water).
 A good contact between the extractor liquid and the solution containing the
substance to be extracted.
This last requirement is achieved by mixing the two liquids, the extractor and the
solution, in a settling funnel, closing the main opening with a plug and then shaking for
a few minutes. After this time, with the settling funnel in an inverted position, we will
open the stopcock so that the possible gases released in the agitation can escape and
thus avoid an overpressure inside the funnel.
When we have finished shaking, we will leave the funnel on the support, already
without the plug, to get the two phases to separate, and finally, we will remove the
densest phase from the bottom by opening the key and the least dense from the top.
Finally, to achieve greater performance, we must perform this procedure
several times in a row.
6.-ADSORPTION
On the surface of a solid the forces between atoms, molecules and ions are not
compensated. In this way, if a solid comes into contact with a liquid or gas, unions can
be created between the solid and the fluid, so that the atoms, molecules or ions of
the latter are trapped between the particles of the solid. We call this phenomenon
adsorption.
The amount of substance adsorbed will be a function of the contact surface of
the solid, so that a larger contact surface we will have a greater adsorption. An example
of this is activated carbon: substance that is very finely divided into very small
particles, which gives it a large contact surface.
Activated carbon is widely used in the laboratory to remove impurities that give
color to solutions. It is also used to remove the odor from these same solutions.
The procedure consists of intimately mixing the activated carbon with the
solution, so that the particles of the liquid come into contact with those of the solid.
Let stand for a few moments and filter into a funnel. In this way the dissolution is
transparent. If the filtered solution is gray, it is because some activated carbon has been
roasted to the solution. This often happens given the very small size of activated
carbon particles. In this case, when filtering, it is convenient to use two filter papers
instead of one.
ISSUES

1. Objective of the topic.


2. It lists the physical methods for separating mixtures that have been studied in
this topic.
3. The pleated filter, in what situations is it used?
4. Indicates the laboratory material used in reduced pressure filtration.
5. In a crystallization, what does the speed of cooling of the saturated solution
influence ?
6. Why are small pieces of porcelain used in a distillation inside the flask?
7. What is the function of the cooling tube in a distillation?
8. Explain the complete process you would use to separate a mixture of sand and
salt.
FILTRATION PRACTICES

INTRODUCTION
The objective of these practices is to learn how to use one of the filtration
techniques described in the introduction to the topic: gravity separation. We will learn
how to prepare the filters and apply them to the funnel.
On the other hand we will use some precipitation reactions, so that when
mixing different solutions we obtain some precipitated solids, which we will then
separate by filtration. The reactions that take place in each case are as follows:
CaCl2 (ac) + Na 2 CO 3 (ac)  CaCO 3 (s) + 2 NaCl
(ac) 3 NaOH (ac) + FeCl 3 (ac)  Fe(OH)3 (s) + 3
NaCl (ac) Pb(NO 3)2 (ac) + 2 KI (ac)  PbI 2 (s ) +
2 KNO 3 (ac)

PRACTICE 1: FORMATION OF A PRECIPITATE OF CaCO3

MATERIAL

Funnel, filter paper, two beakers, support, walnut, support ring , stirring rod.
Products: Calcium chloride and sodium carbonate.

PROCEDURE
1. Measure 100 mL of water and place them in a beaker (beaker 1).
2. Weigh 10 g of calcium chloride and dissolve them in the 100 mL of water.
3. Measure another 100 mL of water and place them in the other beaker (beaker 2).
4. Weigh 5 g of sodium carbonate and dissolve them in the water of the glass 2.
5. Pour the contents of one of the glasses into the other.
6. Observe the appearance of a precipitate and separate it by filtration.
7. Let the solid dry, several days and weigh it.
ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. Write the reaction that has taken place, indicating the states of aggregation of
each of the substances that have participated in it.
5. How is the precipitate of calcium carbonate that has been formed?
6. Write the reaction that has taken place and write the weight of the precipitate.
7. It calculates, by stoichiometry, the theoretical amount that should be obtained of
calcium carbonate.
8. Why do you think the actual amount is less than the theoretical amount?
9. Calculate the performance of the reaction.
PRACTICE 2: FORMATION OF A PRECIPITATE OF Fe(OH)3

MATERIAL
Funnel, filter paper, two beakers, support, walnut, support ring , stirring rod.
Products: iron trichloride solution, sodium hydroxide solution.

PROCEDURE
1. Measure 25 mL of sodium hydroxide solution and place them in a beaker.
2. Measure 25 mL of the iron trichloride solution and place them in the other vessel.
3. Write down the concentrations of both solutions.
4. Mix the two solutions and shake with the stirring rod .
5. Observe the precipitate that has formed and filter it.
6. Let the solid dry for a few days and weigh it.

ISSUES
1. Objective of the practice.
2. Material used.
3. It describes, briefly, the procedure followed.
4. How is the iron hydroxide precipitate that has been formed?
5. Write the reaction that has taken place, indicating the states of aggregation of
each of the substances that have participated in it.
6. Knowing the concentrations of ferric chloride and sodium hydroxide
solutions, he calculates the theoretical amount of iron hydroxide that could be
obtained .
PRACTICE 3: FORMATION OF A PRECIPITATE OF PbI2

MATERIAL
Funnel, filter paper, two test tubes, lighter, tweezers.
Products: solution of lead (II) nitrate, solution of potassium iodide.

PROCEDURE
1. Place 3 cc of the lead (II) nitrate solution in a test tube.
2. Place the same amount of potassium iodide solution in another test tube.
3. Mix both solutions and observe the formation of the precipitate.
4. Write down the concentrations of both solutions.
5. Heat the solution. (Remember the precautions you should take when heating a
solution in a test tube.)
6. Let the solution cool.
7. Observe the formation of the phenomenon called "golden rain" when the
solution is cold.

ISSUES
1. Objective of the practice.
2. Material used.
3. It describes, briefly, the procedure followed.
4. How is the precipitate of lead (II) iodide that has been formed?
5. Write the reaction that has taken place, indicating the states of aggregation of
each of the substances that have participated in it.
6. What is observed when heating the solution?
7. How is the precipitate that is formed when the solution cools ?
8. It calculates, knowing the concentrations of both solutions, the mass of
precipitate of lead (II) iodide that could be obtained.
CRYSTALLIZATION PRACTICES

INTRODUCTION
In the following practices we will obtain crystals. Crystals are groupings of
ions or atoms, which repeat regularly in space. The structure adopted by each crystal
depends on the type of ions or atoms involved. For example, the structure of common
salt (sodium chloride) is cubic, that of copper sulfate pentahydrate is rhombic.
In nature crystallized minerals abound (silicates, calcite, precious stones such as
diamond, ...). Obtaining these crystals in the laboratory is very difficult since it requires
very high pressures and a lot of time. However, there are some chemical compounds
that crystallize easily. This characteristic can be used to obtain crystals of different
shapes and colors in the laboratory, or to purify substances that are not pure (such as
commercial copper sulfate).
It is also possible that the same substance can provide crystals of different
shapes, depending on the circumstances in which it is in solution, for example, if it is
in an acid medium or in a basic medium.

PRACTICE 1: CRYSTALLIZATION OF CuSO4 · 5H2O

MATERIAL
Beaker, stirring rod, support , walnut, ring, glass funnel, filter paper, lighter,
grid, crystallizer , balance.
Products: Distilled, water, commercial copper(II) sulfate .

PROCEDURE
1. Measure 50 mL of distilled water and place them in a beaker .
2. Weigh 25 g of commercial copper sulfate and add them to the glass.
3. Heat it, stirring it with the rod.
4. When all the copper sulfate has dissolved, continue heating until it starts to
boil.
5. Continue heating, at a gentle boil, until the volume of the solution is reduced to
approximately 50 mL
6. Turn off the lighter and remove the glass with the solution using a glove or a
filter paper pennant.
7. Filter the solution before it cools.
8. Place the solution in the crystallizer.
9. Observe the formation of crystals after a few days.
10. Store one or two crystals.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. Describe the crystals obtained.
5. Why do you have to filter the solution?
6. Why do you have to filter while hot?
PRACTICE 2 : CRYSTALLIZATION OF CuSO4 · 5H2O ON WIRE

MATERIAL
Beaker, stirring rod, support, ring, walnut, glass funnel, filter paper, lighter,
grid, test tube, wire, balance.
Products: Distilled water, commercial copper(II) sulfate .

PROCEDURE
1. Measure 100 mL of distilled water and place it in a beaker.
2. Weigh 50 g of commercial copper sulfate and add them to the glass.
3. Heat it, stirring it with the rod.
4. Meanwhile, with a wire, make a simple design that represents some object, for
example a fir.
5. When all the copper sulfate has dissolved, continue heating until it starts to boil.
6. Continue heating, at a gentle boil, until the volume of the solution is reduced to
approximately 100 mL
7. Turn off the lighter and remove the glass with the solution using a glove or a
filter paper pennant.
8. Hang the wire from a fishing line, without touching any of the walls of the glass.
9. Let the solution rest for about two days and shake it a little.
10. Observe the formation of crystals around the wire after a few days.
11. Take out the wire with the crystals and observe it.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. Compare the crystals obtained in this practice with those obtained in previous
practice.
PRACTICE 3: PURIFICATION OF COMMON SALT

MATERIAL

Beaker, stirring rod, support, ring, walnut, glass funnel, filter paper, lighter,
grid, crystallizer, test tube.
Products: Distilled water, sodium chloride.

PROCEDURE

1. It weighs 50 gr of coarse salt.


2. Measure 100 mL of distilled water and put them in the beaker .
3. Add coarse salt and shake with the rod until it dissolves further.
4. Heat the solution and continue adding salt.
5. When it comes to a boil and you check that no more salt dissolves, turn off the
lighter and filter hot. Use the glove or a filter paper pennant so you don't get
burned.
6. Transfer the solution to the crystallizer and observe the formation of crystals as
they cool.
7. Weigh the amount of coarse salt you have left.

ISSUES

1. Objective of the practice.


2. Material used.
3. Briefly describe the process followed.
4. Why do we heat the solution?
5. Describe the crystals obtained.
6. Compare the appearance of the new lenses with the ones you used at the
beginning of the practice.
7. Calculate the solubility of salt in hot water in mol/L.
PRACTICE 4: GROWTH OF A CRYSTAL OF CuSO4 · 5H2O

INTRODUCTION

Many times it is interesting to obtain large crystals to be able to better study their
shape and properties. We have already seen how to obtain crystals from supersaturated
solutions. In this practice we will use crystals obtained in a previous practice to get
larger ones . For this we will use:

1. A saturated solution of the same substance.


2. A previously obtained crystal that will act as a germ.
Crystallization will take place around the initial crystal, which will grow. We
have observed that the crystals obtained have different geometric shapes. When two
solids crystallize in the same system, we could use as a germ a crystal of one of the
solids and we would get the other to crystallize around the first.

MATERIAL

Beaker, stirring rod, support, walnut, glass funnel, filter paper, lighter, grid,
crystallizer, test tube, balance, thermometer.
Products: Distilled water, hydrated copper (II) sulphate, a crystal of those
obtained in previous practices of the same salt.

PROCEDURE

1. Measure 50 mL of distilled water and place them in a beaker .


2. It weighs 25 gr of copper sulfate.
3. Heat it by stirring with the glass rod.
4. When all the copper sulphate has dissolved, continue heating until it reaches a
temperature of approximately 60ºC.
5. Turn off the lighter and remove the beaker with the glove.
6. Let it cool. If any crystal precipitates, pour the rest of the solution into another
beaker.
7. Insert the copper sulfate crystal tied with a wire.
8. Cover the beaker with filter paper.
9. Observe the growth of the crystal after a few days.
ISSUES

1. Objective of the practice.


2. Material used.
3. Briefly describe the process followed.
4. What does it mean that the initial crystal acts as a germ?
5. Describe the crystals obtained and compare them with the first ones you
obtained in the first practice.
6. Why do you think it is necessary to cover the beaker?
PRACTICE 5: PREPARATION OF A SUPERSATURATED SOLUTION OF
SODIUM ACETATE (CH3–COONa · 3H2O)

INTRODUCTION

We have already seen how to obtain crystals from a supersaturated solution. In


this practice and in the next we will prepare supersaturated solutions that can remain
some time without precipitating the crystals. This does not happen with all solutions,
only with some, for example sodium acetate trihydrate and ammonium chloride.

After obtaining the supersaturated solution, we will let cool, and then, it should
precipitate the excess dissolved substance. However, this does not happen, but the
dissolution remains in an unstable equilibrium. At the moment we want the crystals to
precipitate, it is enough that we add some particles of solid or dust. This solid acts as a
germ so that it begins to precipitate the solute and continues until the concentration of
the solute is that of the saturated solution.

MATERIAL

Erlenmeyer flask, support, ring, walnut, glass funnel, lighter, grid, specimen
and balance.

Products: Sodium acetate trihydrate and distilled water.

PROCEDURE

1. Clean the Erlenmeyer very well, using dilute hydrochloric acid.


2. Place it on the scale and weigh 21 g of sodium acetate trihydrate.
3. Add 12 mL of distilled water.
4. Heat until all the precipitate has dissolved.
5. Let the solution cool at rest, several days, and if any crystal forms, heat again
until it dissolves again.
6. Let cool and check that no crystal has precipitated. This solution is
supersaturated.
7. Add a sodium acetate crystal . Watch what happens.
ISSUES

1. Objective of the practice.


2. Material used.
3. Briefly describe the process followed.
4. What is the difference between a saturated solution and a
supersaturated solution?
5. How would you define an unstable equilibrium?
6. Why do you think it is necessary to clean the Erlenmeyer flask well, even with
hydrochloric acid?
7. Describe what happens when you add the sodium acetate crystal to the
supersaturated, cold solution.
8. What do the crystallization process observed in this practice have in common
and how do they differ from the previous one (growth of a CuSO4 crystal)?
PRACTICE 6: PREPARATION OF A SUPERSATURATED SOLUTION OF
AMMONIUM CHLORIDE (NH4Cl)

MATERIAL

Test tube, lighter and test tube. Products:


Distilled water, ammonium chloride.

PROCEDURE

1. Clean the test tube using dilute hydrochloric acid.


2. Add about 6 mL of distilled water.
3. Add ammonium chloride and shake until it can no longer dissolve.
4. Heat the solution and continue adding ammonium chloride and stirring.
5. Let the solution cool at rest and check that no crystals precipitate.
6. Add some chalk powder. Watch what happens.

ISSUES

1. Objective of the practice.


2. Material used.
3. Briefly describe the process followed.
4. Why do you think it is not necessary for the germ to be of the same nature
as the dissolved substance?
5. What would happen if we added chalk to a saturated solution instead of a
supersaturated one?
PRACTICE 7: FORMATION OF A STALAGMITE

MATERIAL

Support , ring, grid, walnut, lighter, beaker, stirring rod , crystallizer.


Products: Distilled water, sodium acetate.

PROCEDURE

1. It measures approximately 20 mL of distilled water.


2. Place them in the beaker and add sodium acetate, shaking with the rod until
no more dissolves.
3. Heat the solution by adding sodium acetate, little by little, (approximately 31
gr) stirring with the rod until no more solute is dissolved.
4. Turn off the lighter and let the solution cool. If you have followed the
procedure carefully you will have obtained a supersaturated solution and it will
not precipitate anything when cooling.
5. Place some sodium acetate crystallites in the crystallizer.
6. Carefully pour the supersaturated solution over these crystals and observe the
formation of a kind of stalagmite.

ISSUES

1. Objective of the practice.


2. Material used.
3. Briefly describe the process followed.
4. What is it and how is a supersaturated solution obtained?
UNIT 5:
Thermochemical
THERMOCHEMISTRY PRACTICES

INTRODUCTION
One of the characteristics of chemical reactions is that in them there is always
some exchange of energy between the substances involved and the environment in
which they are found. This exchange of energy is usually in the form of heat. According
to the direction of heat exchange, we distinguish between endothermic reactions and
exothermic reactions:
Endothermic reactions are those in which energy is absorbed ; while
exothermic reactions are those in which energy is released.
The heat exchanged during a chemical reaction is called a reaction rate.
Most chemical reactions take place in open containers (i.e. at constant
pressure: atmospheric). Under these conditions, the heat of reaction is called the
enthalpy of reaction and is represented ΔH. Enthalpy is usually measured in KJ and
refers to the number of moles contained in the adjusted reaction.
In endothermic reactions the enthalpy is positive, while in exothermic
reactions the enthalpy is negative.
In the following practices we will work with endothermic reactions and with
exothermic reactions, and in the last we will calculate, approximately, the enthalpy of a
reaction.
PRACTICE 1: MEASUREMENT OF HEAT RELEASE IN AN EXOTHERMIC
REACTION

MATERIAL
Beakers, scales, thermometer.

Products: zinc, copper sulphate solution .

PROCEDURE
1. Put 20 mL of the copper sulphate solution in a beaker and measure the initial
temperature of the solution.
2. Weigh 0.5 g of zinc and add them to the solution. Shake and note the highest
temperature reached during dissolution. Observe the appearance of the
solution when the zinc reacts .
3. Repeat the same operation with other quantities of zinc: 1; 1.5; 2 and 2.5
gr, cleaning the beaker each time.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. Describes what the solution looks like when the different amounts of zinc are
added.
5. This is an exothermic reaction. On what basis do we know it?
6. Write down the reaction that has taken place.
7. Construct a graph representing the temperature increase as a function of the
amount of zinc added.
PRACTICE 2: MEASUREMENT OF HEAT RELEASE IN AN
ENDOTHERMIC PROCESS

MATERIAL
Two test tubes, balance, thermometer.
Products: ammonium nitrate, sodium
hydroxide.

PROCEDURE
1. Weigh one gram of ammonium nitrate and place it in a test tube.
2. In the other test tube we add water up to 3 or 4 cm high and measure its
temperature.
3. Introduce the thermometer into the test tube containing ammonium nitrate
and add the water.
4. We note the temperature every 30 seconds until it stops changing and the
measurement is stable.
5. We add a "lentil" of sodium hydroxide to the test tube and measure the
temperature again.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. When you add the water over the ammonium nitrate, does there be a reaction?
5. Indicates what temperature variation has taken place. Why do we know that it is
an endothermic process?
6. By adding sodium hydroxide if a chemical reaction takes place; we can tell why
a gas with a characteristic odor is released, what gas is this?
7. This last reaction is: endothermic or exothermic?
PRACTICE 3: CALCULATING THE HEAT OF A NEUTRALIZATION
REACTION

MATERIAL
Two beakers, test tube, thermometer.
Products: hydrochloric acid solution, sodium hydroxide solution.

PROCEDURE
1. Measure a volume of 50 cc of the hydrochloric acid solution and pour them
into one of the beakers.
2. Measure a volume of 50 cc of the sodium hydroxide solution and pour them
into the other beaker.
3. Measure the temperature of both solutions, which should be the same (room
temperature), and write it down. We'll call it T1.
4. Pour a solution into the other beaker .
5. Gently shake the mixture and measure the temperature until a maximum value
is reached that we will note. We'll call it T2.
6. We will repeat the entire process a second time.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. Write down the reaction that has taken place.
5. Calculate the heat given off with the formula: Q = m·c e·( T 2–T1). For which we
will assume that the mass is approximately 100 gr of water, and the specific heat
is that of water: 1 cal / gr·ºC. We will repeat the calculation with the values of
the second experience. Calculate the average between both values. (If the
difference between the two was very large, you would have to repeat the
experience again).
6. Calculate the moles of HCl and NaOH that have reacted; and with the calculated
heat and those moles, calculate the enthalpy for the reaction in KJ/mol.
(1cal=4.18J).
7. Compare it to the actual value: 57 KJ/mol. What could be the reason for the difference?
UNIT 6:
Kinetics
KINETICS PRACTICES

INTRODUCTION
In the following practices we will study the factors on which the speed of a
reaction depends. The most important are the concentration of the reactants, the degree
of division of the solid reactants, the temperature of the reaction and the catalysts.
A variation of any of these factors will cause an increase in the speed of the reaction.

PRACTICE 1: CONCENTRATION OF REAGENTS

MATERIAL
Three test tubes, beakers, balance.
Products: Zinc powder, very dilute hydrochloric acid solution , dilute
hydrochloric acid solution and concentrated hydrochloric acid solution.

PROCEDURE
1. We weigh one gram of zinc for each test tube and add it to each test tube .
(We will weigh it) on paper).
2. In a test tube we add, more or less, up to the middle of the tube , very dilute
hydrochloric acid and observe what happens.
3. In the second test tube we do the same with dilute hydrochloric acid.
4. In the third test tube we do the same with concentrated hydrochloric acid.
5. Write down the characteristics of the concentrated HCl.

NOTE : YOU HAVE TO BE VERY CAREFUL WHEN WORKING WITH


ACIDS AND IN PARTICULAR WITH CONCENTRATED ACIDS.
ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. What have you observed in both test tubes when pouring the hydrochloric acid?
Write down the reaction that has taken place.
5. What difference have you observed in both tubes?
6. It explains, according to the theory, what this difference is due to.
7. Calculate the molarity of the concentrated HCl solution .
8. Calculate the volume of the concentrated solution that we should measure from
the concentrated solution to prepare 200 cc of the 0.2M solution of HCl.
9. Calculate the amount of water that we should add to the previous amount to
prepare the 200 cc.
10. Explain the steps you would follow in the laboratory to prepare the 200 cc of
solution.
PRACTICE 2: REACTION TEMPERATURE

MATERIAL
Two test tubes, balance, lighter, clamp, beaker. Products: Zinc
powder, dilute hydrochloric acid solution .

PROCEDURE
1. We weigh one gram of zinc for each test tube and add it to each test tube . (We
will weigh it) on paper).
2. In a test tube we add, more or less, up to half of the tube, dilute hydrochloric
acid and observe what happens.
3. In the other test tube, we do the same, but after adding the acid, heat
slightly. We watch what happens.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. What have you observed in both tubes when pouring the hydrochloric acid?
Write down the reaction that has taken place.
5. What difference have you observed between both tubes?
6. Explain, according to the theory, what this difference is due to.
PRACTICE 3: DEGREE OF DIVISION OF SOLID REAGENTS

MATERIAL
Two test tubes, beaker, balance.
Products: Zinc powder, zinc shot, dilute hydrochloric acid solution.

PROCEDURE
1. We weigh one gram of zinc powdered and put it in a test tube.
2. We weigh approximately one gram of zinc shot and introduce it into the other
test tube.
3. Add to both test tubes , more or less halfway up the tube, dilute hydrochloric
acid and observe what happens.
4. Heat the tube with the zinc shot.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. What have you observed in both tubes when pouring the hydrochloric acid ?
Write down the reaction that has taken place.
5. What difference have you observed between both tubes?
6. Explain, according to the theory, what this difference is due to.
7. What happened when the tube was heated?
PRACTICE 4: CATALYSTS

MATERIAL
Two test tubes, beaker, pipette. Products:
Hydrogen peroxide, manganese dioxide.

PROCEDURE
1. We measure with the pipette 5 mL of hydrogen peroxide for each test tube and
pour it into each tube.
2. We look at what happens in both test tubes .
3. Add a small amount of manganese dioxide (0.2 gr) in one of the two test tubes
and observe what happens.
4. Heat the other test tube and add 0.2 g of manganese dioxide.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. In both test tubes the reaction of decomposition of hydrogen peroxide into
oxygen and water is taking place. Write down and adjust that reaction.
5. Before heating, what difference have you observed in both tubes?
6. What is the function of manganese dioxide? Could we recover it once the
reaction is over?
8. Explain, according to the theory, what this difference is due to.
9. What happens when you do the same thing at a higher temperature?
UNIT 7:
Acid-base reactions
PRACTICES WITH ACID-BASE REACTIONS

INTRODUCTION
According to the Brönsted-Lowry theory, acids are substances that can transfer
protons, H+, to other substances capable of accepting them, the bases. Acids and bases
can be strong: if they dissociate completely when dissolved in water; or weak: if when
dissolved in water they partially dissociate, reaching a chemical equilibrium that is
marked by an equilibrium constant, ionization constant: acidity constant, Ka, if it is an
acid; and basicity constant Kb, if it is a base.
When an acid or a base is totally or partially dissociated in water, its conjugate
pair is obtained.
If we call an acid HA in general, the reaction that takes place when dissolved in
water is:
HA (ac) + H 2O (l)  A– (ac) + H3O+ (ac)
where A– is the conjugate base of HA acid; and both are an acid-base conjugate pair.
In the same way, if we call a base B in general, the reaction that takes place
when dissolved in water is:
B (ac) + H2O (l)  BH+ (ac) + OH– (ac)
where BH+ is the conjugate acid of base B; and both are an acid-base conjugate pair .
It is important to keep in mind that what marks the acidity of a solution is the
concentration of the H3O + ion
. To have a measurement of this concentration, pH is
usually used, whose definition is: pH = – log  H3O+. So the higher the  H3O+ the
lower the pH.
Taking into account the pH, a solution is neutral when it is 7; It is acidic when it
is less than 7 ; and basic when it is greater than 7.
Finally, we must remember the definition of pOH: pOH = – log  OH –; and
that for any solution the following equality is fulfilled pH + pOH = 14.
PRACTICE 0: PREPARATION OF SOLUTIONS

INTRODUCTION
The use of aqueous dissolutions is common in chemical laboratory work .
Therefore, the techniques of its preparation must be well known. In this practice,
different dissolutions of a given concentration will be prepared from the pure (solid)
product, or from some more concentrated dissolution of it.
For this it is important to remember the definitions of the two most used ways of
measuring the concentration of a solution: molarity and percentage by weight or
richness of a solution:
moles solute
 Molarity: M 
V ds (L)
solute mass
 Percentage by weight: ·100
% dissolution mass
The percentage by weight is accompanied, as data, by the density of the

dissolution  dissolution mass . Usually in gr/cc.



dissolution volume
:
In this practice we will prepare three dissolutions: one of sodium chloride,
another of sodium hydroxide and finally, one of hydrochloric acid.

A) DISSOLUTION 0,5 M NACL

MATERIAL
Balance, watch glass, spatula, test tube, 200 cc graduated flask, rod.
Products: sodium chloride.

PROCEDURE
1. Make the necessary calculations to know the amount of sodium chloride that
we must weigh to prepare 200 cc of a 0.5M solution of NaCl.
2. Weigh the calculated amount of NaCl on the scale.
3. Place this quantity in the graduated flask and add water to the flush line.
4. Shake the flask to homogenize the dissolution.
B) DISSOLVED N 0.2M NAOH

MATERIAL
Test piece, 500 cc volumetric flask, rod, funnel.
Products: 2M dissolution of NaOH.

PROCEDURE
1. Make the necessary calculations to know the volume we need of the 2M
NaOH dissolution to prepare 500 cc of 0.2M solution.
2. Measure this quantity in the cylinder and transfer it to the graduated flask.
3. Rinse the cylinder several times with distilled water in order to remove the
remains of NaOH 2M and pour them into the volumetric flask.
4. Add water in the flask to the flush.
5. Shake the flask to homogenize the dissolution.

C) 2M DISSOLUTION OF HCl

MATERIAL
Test piece, 500 cc volumetric flask, rod, funnel.
Products: 35% HCl dissolution.

PROCEDURE
1. Make the necessary calculations to know the volume we need of the 35% HCl
dissolution to prepare 500 cc of 0.5M solution.
2. Measure this quantity in the cylinder and transfer it to the graduated flask ,
taking care that some water has been added to the flask. (Remember that an acid
Concentrate should always be poured on water and not directly on acid).
3. Rinse the cylinder several times with distilled water in order to remove the HCl
residues and pour them into the volumetric flask.
4. Add water in the flask to the flush.
5. Shake the flask to homogenize the solution.
ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. For each of the three dissolutions, write down the calculations you've had to
do.
5. In the dissolution of NaCl, why we have not directly measured 200 cc of water.
6. Could it be prepared from the 2M solution of NaOH, a 3M dissolution?
7. Why should you pour a concentrated acid on the water and it is dangerous to
do it the other way around?
PRACTICE 1: ACID-BASE INDICATORS

INTRODUCTION
An acid-base indicator is a substance of weak acidic or basic character that has
the property of presenting different colors depending on the pH of the dissolution in
which it is dissolved.
The behavior of the indicators is easy to understand. Suppose an indicator
consisting of a weak monoprotic acid of general formula HIn.In aqueous solution it
will be slightly ionized, producing its conjugated base In–:
HIn + H 2O  In– + H3O+
As is characteristic in the indicators, the acid form HIn has a different color than
the basic form in–.
If a few drops of the indicator are added in a solution of an acid, the acid form of
the indicator predominates: the solution being colored by the color of the acid form. In
the same way, if they are added to a solution of a base, the basic form will predominate
coloring the solution of the color of the basic form.
It is important to keep in mind that each indicator has a characteristic turning
interval, that is, a more or less reduced environment of pH units, within which the color
change is made.
At pH below the lower limit of the turning interval the color of the acid form
predominates; and above the upper limit of the turning interval the color of the basic
form predominates. Within the interval there will be a mixture of the two colors.
The following table shows the indicators that we are going to use in practice,
together with their turning interval and the color they present when the pH is lower than
this interval and when it is higher:
Turning range (units
Indicator Color at lower pH Color at higher pH
de pH)

Congo Red Blue 3–5,2 Red

Phenol red Yellow 6,8–8,2 Red

Phenolphthal Colourless 8,3–10 Red


ein
Using these indicators we can only know if the dissolution has a pH higher or
lower than the values that mark the turning interval. In order to know exactly the
pH of a dissolution there are devices called pH-meters.
In any case, to know it in an approximate way, the universal indicator paper is
used : paper impregnated with a mixture of indicators that takes different colors
according to the pH of the dissolution.

MATERIAL
Rack with 8 test tubes, pipette, strips of universal indicator paper.
Products: 0.01M solution of HCl, 0.01M dissolution of NaOH, commercial
vinegar, commercial ammonia, dissolution of the three indicators: Congo red, phenol
red and phenolphthalein.

PROCEDURE
1. Carefully clean the eight test tubes.
2. Pour in four of them 2 mL of the HCl dissolution and in the other four 2 mL
of the NaOH dissolution.
3. Investigate the color of each indicator by dropping a few drops on a tube
containing HCl and as many on another tube containing NaOH. Shake,
observe and note the color of the indicator in each case. Measure the pH in
the fourth test tube approximately with the indicator paper.
4. Carefully clean the eight test tubes.
5. It proceeds in the same way with the solutions of vinegar and ammonia.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. With the results obtained, complete the following table:
Congo red Phenol Color Approximate pH
Dissolutions color red phenolphthale indicator paper
color in
HCl solution

NaOH solution

Vinegar

Ammonia

5. If, when a few drops of phenolphthalein are added to an aqueous solution, it


remains colourless, what can be deduced about the acidic, basic or neutral
character of that solution?
6. It explains the mechanism by which an indicator consisting of a weak base B,
presents two different colors depending on the pH of the medium.
PRACTICE 2: HYDROLYSIS OF SALTS

INTRODUCTION
Many salts, when dissolved in water, cause the resulting solution to be acidic or
basic. The reason is that the ions that are produced in their dissociation, when the salt
is dissolved in water, are acids or Brönsted-Lowry bases, and are capable of
transferring H+ ions to water or receiving them from it. When either or both ions react
with water, the salt is said to undergo hydrolysis.
If we consider BA salt, when dissolved in water it dissociates into its
ions: BA  A– (ac ) + B+ (ac)
The A– ion is always the conjugate base of an acid. If the acid is strong, the A –
ion will not react as a base. However, if the acid is weak, the A– ion will react as a
base, producing OH– ions in the solution.
The B+ ion is always the conjugated acid of a base. If the base is strong, the B +
ion will not react as acid. However, if the base is weak, the B+ ion will react as acid,
producing H3O+ ions in solution.
Depending on whether or not the A– and B+ ions react, the solutions will be
acidic, basic or neutral:
– If neither ion reacts, the solution will be neutral.
– If only the A– ion reacts, the dissolution will be basic.
– If only the B+ ion reacts, the solution will be acidic.
– If the two ions react, it will depend on which of the two has a higher ionization
constant, Kb the A– ion and Ka the B+ ion, to know what the pH will be like. If Kb
(A–) > Ka (B+) the solution will be basic, and if it is the other way around acidic.
Only if the two constants were equal would the solution be neutral.

In this practice we will highlight all of the above with some quite common salts.
For which we will measure the pH of the solutions of these salts using universal
indicator paper, in order to know if these solutions are acidic, basic or neutral.
MATERIAL
Spatula, six test tubes, pieces of universal indicator paper.
Products: sodium carbonate, sodium chloride, ammonium chloride, sodium
bicarbonate, sodium acetate, sodium nitrate.

PROCEDURE
1. Carefully clean the six test tubes.
2. Add a small amount of each salt to each test tube. Label the test tubes to know
the salt in each.
3. Add a few milliliters of distilled water to each tube and stir it, so that the salt
dissolves perfectly.
4. Drop a piece of indicator paper into each tube and write down the color it takes
in order to know the acidic, basic or neutral character of the solution.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. It indicates for each salt the color that the indicator paper has taken, and,
therefore, the acidic, basic or neutral character of the solution of said salt. It
explains, by means of the necessary reactions, this fact.
PRACTICE 3: ASSESSMENT OF A DISSOLUTION OF HCl

INTRODUCTION
An acid-base titration is the determination of the concentration of an acid in
solution from the known concentration of a base, or vice versa, based on the
neutralization reaction of the acid with the base.
It should be remembered that the neutralization reaction, from the
stoichiometric point of view, can be formulated as follows: acid + base  salt + water.
However, from the acid-base point of view, the neutralization reaction is the
reaction between the ion H 3 O+ that comes from the dissociation of the acid, with the
ion OH– that comes from the dissociation of the base, to form water: H 3 O+ + OH–  2
H 2 O.
Titration is performed by gradually mixing the acid and base until the
equivalence point is reached, i.e. the moment when the neutralization reaction has
been complete. At this point the moles of H 3 O +
ions from the acid are the same as
those of OH– ions from the base.
The endpoint of the valuation is reached when a change in the color of the
indicator used in the valuation is observed.
In this practice we will perform the assessment of a strong acid: hydrochloric
acid; while in the next one we will do it with commercial vinegar, a solution of a
weak acid: acetic acid.

MATERIAL
Pipette, burette, Erlenmeyer flask, support, beaker, test tube. Products:
HCl solution, 0.2 M NaOH solution, phenolphthalein.

PROCEDURE
1. Take with a pipette 25 mL of the HCl problem solution and pour them into the
Erlenmeyer flask. Dilute by adding distilled water to a volume of
approximately 100 mL
2. Add about 10 drops of the phenolphthalein solution to the solution.
3. Place in the support the burette clean and previously rinsed with a small amount
of the 0.2 M solution of NaOH.
4. Fill the burette with the solution of NaOH exceeding the flush. Make up to the
mark now, carefully dropping the excess NaOH into the glass.
5. Slowly drop the NaOH solution from the burette onto the HCl, while lightly
moving the flask to mix the reagents well.
6. Observe the color change that can be seen on the surface of the HCl when a
drop of NaOH solution falls on it. When shaking, the coloration will
disappear.
7. When you notice that the end point of the titration is near, since the color change
is increasingly persistent, drop the sodium hydroxide, drop by drop, until the
definitive variation of the color of the indicator occurs . At that time, close the
burette key and note the volume of NaOH solution used.
8. Repeat again all the volumetry and take as final value the average value of the
volume of NaOH.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. It formulates the reaction that has taken place, from the stoichiometric point of
view, between HCl and NaOH.
5. Calculates the concentration of the initial HCl solution.
6. Does the fact of initially adding water to the HCl solution influence the result
of the titration?
7. Reason how the pH will be: acidic, basic or neutral, at the point of equivalence
of the valuation.
PRACTICE 4: VALUATION OF A COMMERCIAL VINEGAR

MATERIAL
Pipette, burette, Erlenmeyer flask, support, beaker, test tube. Products:
Vinegar, 0.2 M solution of NaOH, phenolphthalein.

PROCEDURE
1. Take with a pipette 10 mL of vinegar (acetic acid solution) and pour them into
the Erlenmeyer flask. Dilute by adding distilled water to a volume of
approximately 100 mL.
2. Add about 10 drops of the phenolphthalein solution to the solution.
3. Place in the support the burette clean and previously rinsed with a small amount
of the 0.2 M solution of NaOH.
4. Fill the burette with the solution of NaOH exceeding the flush. Make up to the
mark now, carefully dropping the excess NaOH into the glass.
5. Slowly drop the NaOH solution from the burette onto the vinegar, while lightly
stirring the flask to mix the reagents well.
6. Notice the color change on the surface of the vinegar when a drop of NaOH
solution falls on it. When shaking, the coloration will disappear.
7. When you notice that the end point of the titration is near, since the color change
is increasingly persistent, drop the sodium hydroxide, drop by drop, until the
definitive variation of the color of the indicator occurs. At that moment close the
burette faucet and note the volume of NaOH solution used.
8. Repeat again all the volumetry and take as final value the average value of the
volume of NaOH.
9. Using the pipette, a beaker and the electronic scale; measure 10 mL of
commercial vinegar, weigh them and calculate their density.
ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. Formulate the reaction that has taken place, from the stoichiometric point of
view, between acetic acid, AcH, and NaOH.
5. Calculate the molarity of commercial vinegar.
6. Knowing the molarity and density of commercial vinegar, calculate the
percentage by weight of such a solution.
7. Why do you think it is convenient to rinse the burette with the NaOH
solution?
8. Why when filling the burette it is convenient to exceed the flush?
9. Reason how the pH will be: acidic, basic or neutral, at the point of equivalence
of the valuation.
UNIT 8:
Redox reactions
PRACTICE 1: REACTIVITY OF DIFFERENT METALS WITH
HYDROCHLORIC ACID

MATERIAL
Test tubes .
Products: Mg, Sn, Fe, Al, Zn ,Cu and 3M solution of HCl.

PROCEDURE
1. Put a small amount of each metal in test tubes.
2. Add to each test tube some of the hydrochloric acid solution.
3. Observe what happens.

ISSUES
1. Objective of the practice.
2. Material used.
3. Briefly describe the process followed.
4. In practice you have used 3M solution of hydrochloric acid, which has been
prepared from a concentrated solution of hydrochloric acid . Calculate the
volume of the concentrated solution (37% and 1.19 gr/cc) needed to
prepare 200 cc of the 3 M solution.
5. It indicates which metals react with hydrochloric acid and which do not.
What is the gas that is released in these reactions?
6. For those who react complete the redox reactions that take place.
7. He reasons whether chlorine could be obtained from the reaction of a metal
with hydrochloric acid.
8. It explains why Cu does not react with hydrochloric acid and why Mg does
from reduction potentials.

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